WO2008043303A1 - System and method for sample testing - Google Patents

System and method for sample testing Download PDF

Info

Publication number
WO2008043303A1
WO2008043303A1 PCT/CN2007/070824 CN2007070824W WO2008043303A1 WO 2008043303 A1 WO2008043303 A1 WO 2008043303A1 CN 2007070824 W CN2007070824 W CN 2007070824W WO 2008043303 A1 WO2008043303 A1 WO 2008043303A1
Authority
WO
WIPO (PCT)
Prior art keywords
samples
substrate
reactor
testing
probe
Prior art date
Application number
PCT/CN2007/070824
Other languages
French (fr)
Inventor
Wenge Wang
Wenhui Wang
Guilin Wang
Xixiang Xu
Schwiedernoch Renate
Xianzhong Zhao
Sibiao Xu
Guangping Xie
Original Assignee
Accelergy Shanghai R & D Center Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Accelergy Shanghai R & D Center Co., Ltd. filed Critical Accelergy Shanghai R & D Center Co., Ltd.
Publication of WO2008043303A1 publication Critical patent/WO2008043303A1/en

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00279Features relating to reactor vessels
    • B01J2219/00306Reactor vessels in a multiple arrangement
    • B01J2219/00324Reactor vessels in a multiple arrangement the reactor vessels or wells being arranged in plates moving in parallel to each other
    • B01J2219/00328Movement by linear translation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00495Means for heating or cooling the reaction vessels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00497Features relating to the solid phase supports
    • B01J2219/00527Sheets
    • B01J2219/00531Sheets essentially square
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583Features relative to the processes being carried out
    • B01J2219/00603Making arrays on substantially continuous surfaces
    • B01J2219/00659Two-dimensional arrays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068Means for controlling the apparatus of the process
    • B01J2219/00682Manual means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068Means for controlling the apparatus of the process
    • B01J2219/00684Semi-automatic means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718Type of compounds synthesised
    • B01J2219/00745Inorganic compounds
    • B01J2219/00747Catalysts
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/00029Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor provided with flat sample substrates, e.g. slides
    • G01N2035/00099Characterised by type of test elements
    • G01N2035/00158Elements containing microarrays, i.e. "biochip"
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis

Definitions

  • the invention relates to a system and a method for testing samples, especially catalyst samples.
  • micro-reaction technology solves this difficult problem by conducting chemical reactions in micro-reactors each requiring only a small volume of reactants.
  • the micro-reaction technology can reduce research costs, improve work efficiency, and make better use of materials and resources because of its associated high heat transfer, high mass transfer, high security, and rapid response time.
  • the micro-reaction technology can lead to high throughput micro-reaction systems.
  • sample preparation is a complex process that may comprise steps of screening, grinding, resolving and/or heating.
  • sample contamination may occur, such as by steam or oxygen from the air, so that the samples may be oxygenated or otherwise reacted with to possess undesired variations.
  • a testing system for testing a plurality of samples on a substrate comprises an enclosed cavity having a first region and a second region.
  • a pretreatment unit is provided to pretreat the samples while the substrate is in the first region.
  • a test unit is provided to receive the substrate after the samples are pretreated and to test the samples while the substrate is in the second region.
  • the test unit includes a test mechanism for determining characteristics of the samples while the substrate is in the second region.
  • a sample testing system comprises a pretreatment unit including a substrate holder to hold a substrate carrying a plurality of samples and a pretreating mechanism to pretreat the samples.
  • a test unit is coupled to the pretreatment unit and to receive the substrate from the pretreatment unit.
  • the test unit includes a test mechanism to determine characteristics of the samples while the substrate is situated in the test unit.
  • Embodiment of the present invention further provides a sample testing method for testing samples on a substrate.
  • the method comprises pretreating the samples in a pretreatment unit; moving the substrate from the pretreatment unit to a testing unit through a channel coupling the pretreatment unit to the testing unit such that the samples are not exposed to the atmosphere after being pretreated in the pretreatment unit and before being tested in the testing unit; and testing samples in the testing unit, wherein testing sample includes determining characteristics of the samples while the substrate is in the testing unit.
  • Embodiment of the present invention further provides a reactor for testing samples, comprises a top portion, a bottom portion for holding a substrate carrying a plurality of samples, and a middle portion disposed between the top portion and the bottom portion.
  • the top, middle and bottom portions together define a reaction cavity.
  • a probe is disposed in the reaction cavity and mounted on at least one of the middle portion and the bottom portion. Conduits are connected to the probe for transferring materials into and out of the reaction cavity.
  • embodiment of the present invention provides a reactor for testing samples, comprises a reaction cavity for testing samples therein.
  • the reaction cavity has a first opening.
  • a first light source is disposed outside the reaction cavity to generate a first light beam.
  • a second light source is disposed outside the reaction cavity to generate a second light beam, wherein the reactor is configured to select among the group consisting of (1) the first light source, (2) the second light source, and (3) both of the first and the second light sources, to illuminate the reaction cavity through the first opening.
  • FIG. 1 is a schematic diagram of a testing system with a substrate located in a first region in accordance with one embodiment of the present invention
  • FIG. 2 is a schematic diagram of the testing system shown in Fig. 1 with the substrate located in a second region;
  • FIG. 3 is schematic diagrams of the substrate, and the substrate and a sample in accordance with the present invention.
  • FIG. 4 is a schematic diagram of a testing system with a probe located in the first region in accordance with another embodiment of the present invention.
  • FIG. 5 is a schematic diagram of the testing system shown in Fig. 4 with the probe located in the second region;
  • FIG. 6 is a schematic diagram of a testing system in accordance with yet another embodiment of the present invention.
  • FIG. 7 is a schematic diagram of a testing system in accordance with yet another embodiment of the present invention, with a substrate holder located in a first position;
  • FIG. 8 is a schematic diagram of the testing system shown in Fig. 7, with the substrate holder located in a second position;
  • Fig. 9 is a perspective view of a testing system comprising a reactor and a pretreatment device in accordance with a preferred embodiment of the present invention;
  • Fig. 10 is a perspective view of the pretreatment device shown in Fig. 9;
  • Fig. 11 is a cross- sectional perspective view of the pretreatment device shown in Fig. 10, with the substrate holder located in the second position;
  • Fig. 12 is a cross-sectional perspective view of the substrate holder and a shielding setup
  • Fig. 13 is an assembled perspective view of the substrate holder and the shielding setup shown in Fig. 12;
  • Fig. 14 is a cross-sectional plane view of an upper portion of the pretreatment device shown in Fig. 10, with the substrate holder located in the first position;
  • Fig. 15 is a cross-sectional plan view of the pretreatment device shown in Fig. 10;
  • Fig. 16 is a view similar to Fig. 15, but the substrate holder located in the first position;
  • Fig. 17 is an assembled perspective view of a reactor in accordance with one embodiment of the present invention.
  • Fig. 18 is a schematic diagram of the system of the reactor in accordance with the present invention.
  • Fig. 19 is a partially assembled perspective view of the reactor shown in Fig. 17;
  • Fig. 20 is an enlarged perspective view of part A shown in Fig. 19;
  • Fig. 21 is a cross-sectional view of a probe of the reactor in accordance with the present invention.
  • Fig. 22 is an enlarged view of part B shown in Fig. 21 ;
  • Fig. 23 is a cross-sectional perspective view of a covering element of the probe.
  • Fig. 24 is a perspective view of a guiding portion of the probe
  • Fig. 25 is a schematic diagram of a pressure control in the reactor.
  • Fig. 26 is a schematic diagram of another pressure control in the reactor.
  • Fig. 27 is a schematic diagram of system modules of the reactor.
  • Fig. 28 is a schematic diagram of an experiment flow chart to use the reactor.
  • Fig. 29 is a schematic diagram of an opening of a bottom of the reactor, light sources and the substrate in accordance with one embodiment of the present invention.
  • Fig. 30 is another schematic diagram of the opening, the light sources and the substrate shown in Fig. 29;
  • Fig. 31 is a yet another schematic diagram of the opening, the light sources and the substrate shown in Fig. 29;
  • Fig. 32 is a schematic diagram of the openings, the light sources and the substrate in accordance with another embodiment of the present invention.
  • Fig. 33 is another schematic diagram of the openings, the light sources and the substrate shown in Fig. 32;
  • Fig. 34 is a planform of the openings of the reactor of in accordance with yet another embodiment of the present invention.
  • Fig. 35 is a cross-sectional perspective view of the openings shown in Fig. 34;
  • Fig. 36 is a side view of the openings shown in Fig. 34;
  • Fig. 37 is a second cross-sectional plan view of the openings in accordance with yet another embodiment of the present invention.
  • Fig. 38 is a cross-sectional plan view of the openings in accordance with yet another embodiment of the present invention.
  • Fig. 39 is a schematic diagram of a heating system of the reactor in accordance with the present invention.
  • a system 1000 for testing samples in accordance with one embodiment of the present invention comprises an enclosed cavity 100 having a first region 1020, a second region 1010 and a channel 1030 between the first region 1020 and the second region 1010.
  • the system 1000 further comprises a pretreatment unit 102 to pretreat the samples in the first region 1020, and a test unit 101 is to test the samples in the second region 1010 after the samples are pretreated.
  • a substrate (sample carrier) 300 is provided to carry the samples.
  • the samples include catalysts for catalyzing reactions.
  • the pretreatment process may be a reduction of the samples.
  • oxygenated samples may be pretreated by a pretreating mechanism that introduces hydrogen into the pretreatment unit 102 through a passage and heats the samples using a heating device (heating mechanism) 208.
  • the temperature of the samples may be controlled so that the oxygenated samples are reduced in a temperature-controlled condition.
  • unreacted hydrogen and water produced in the reaction can be discharged from the pretreatment unit 102.
  • the pretreatment process may involve drying the samples. For example, some samples may become damp by being exposed to moisture. So, when drying the damp samples, the heating device 208 can be used to dry the samples with a controlled temperature, while an inert gas is introduced into the pretreatment unit 102 to carry the steam from the heated samples out of the pretreatment unit 102.
  • the substrate 300 can be made of quartz or silica.
  • surfaces of each carrying areas 301 can be treated to increase its roughness in order to fix the samples thereon. Meanwhile, the substrate 300 can be formed with recesses to load the samples, such as those known in the art.
  • the test unit 101 includes a test platform (substrate holder) 15 for holding the substrate 300.
  • the test platform 15 may need to move precisely and is susceptible to temperature, especially to high temperature, which can debase its operation precision and influence its service effectiveness.
  • the test unit 101 further comprises a test mechanism, such as including a probe 109.
  • the probe 109 is formed with a sampling configuration, such as including a sampling passage 105 for sampling testing products and sending the testing products to an analysis device (not shown) for analyzing.
  • the probe 109 and the test platform 15 can move with respect to each other.
  • the sampling passage 105 of the probe 109 can be positioned precisely by moving the substrate holder 15 so that the sampling passage 105 can face the corresponding carrying area exactly.
  • the sampling passage 105 can sample the testing product(s) from a particular carrying area.
  • the substrate holder 15 should be protected from exposure to high temperatures, which may cause deformation or malfunction of its positional mechanism.
  • the probe 109 of the test unit 101 is designed with an input passage 106 and an output passage 107 for one or more materials (generally gaseous materials) to flow in/out of the test unit 101.
  • the input passage 106 and the output passage 107 are not installed in the probe 109.
  • the test unit 101 further comprises a temperature control device 108 for controlling the temperature of the samples during testing.
  • the temperature control device 108 may include a laser heating system, infrared heating system, heating ring or other heating devices.
  • the temperature control device 108 can heat multiple samples on the substrate 300 collectively or individually.
  • the temperature control device 108 is installed on the test unit 101, and the device 108 can also be a separate unit from the test unit 101.
  • the pretreatment unit 102 can also comprise a substrate holder (pretreatment platform) 25 for holding the substrate 300 and a cover 204 opposite to the substrate holder 25.
  • the substrate holder 25 and the cover 204 can move with respect to each other.
  • a gap may exist between the cover 204 and the substrate 300 placed on the substrate holder 25, and the gap therebetween can be about 0.5-lmm.
  • the substrate holder 25 and the cover 204 can both move, or the substrate holder 25 is stationary, while the cover 204 moves relative to the substrate holder 25, or vice versa.
  • the heating device 208 can be disposed on the cover 204.
  • the pretreatment unit 102 can also comprise an input passage 206 and an output passage 207 so that a gas may flow through the gap.
  • the gas flowing from the input passage 206 to the output passage 207 may become a stable concentrated gas stream flowing through the samples.
  • Figs. 4-5 illustrate one embodiment of the present invention wherein elements similar to those shown in Figs. 1-2 are numbered similarly.
  • the test unit 101 and the pretreatment unit 102 share the same input/output passages 106 and 107.
  • the input passage 106 and the output passage 107 are disposed in the probe 109 and the probe 109 can move between the first region and the second region.
  • the input passage 106 and the output passage 107 can provide a flow of gas for pretreating
  • the input/output passages 106 and 107 can provide a flow of gas for testing.
  • a bottom 1040 of the probe 109 can be used as the cover 204 shown in Fig. 1.
  • Figs. 6-8 illustrate other embodiments of the invention wherein elements similar to those shown in Figs.1-2 and 4-5 are numbered similarly.
  • the system according to illustrated embodiments shown in Figs. 6-8 comprise a reactor (test unit) 1 and a pretreatment device (pretreatment unit) 2 coupled to the reactor 1 through a passage (channel) 24.
  • the passage 24 is shaped to have a different height from the first and second region.
  • the reactor 1 defines a reaction cavity (the second region) 10 and the pretreatment device 2 defines a pretreatment cavity (the first region) 20.
  • the reaction cavity 10, the pretreatment cavity 20, and the passage 24 together form an enclosed cavity of the system.
  • the first region 20 and the second region 10 are connected with each other by the passage 24.
  • the system can be made by coupling a testing unit to a pretreatment unit through an enclose channel or a passage.
  • a substrate handling element 28 is disposed in the pretreatment device 2 to transfer the pretreated samples into the second region 10 from the first region 20.
  • the substrate handling element 28 may be disposed in the testing system shown in Fig. 1.
  • a gate 210 can be disposed in the passage 24 to open/close the communication between the first region 20 and the second region 10.
  • the gate 210 can be a brake valve or any other gating elements which can control the opening/closing of the passage 24.
  • the gate 210 can also be disposed in a system shown in Figs. 7-8.
  • the cover 204 is stationary and the substrate holder 25 is moveable.
  • the substrate handling element 28 can push the substrate 300 into the second region 10 from the first region 20.
  • the cover 204 may also be moveable.
  • a driving device 4 may be positioned under the pretreatment device 2 to drive the substrate holder 25 to move up and down.
  • the testing system 1000 comprises a sample reactor (test unit) 1, a pretreatment device (pretreatment unit) 2 coupled to the sample reactor 1 through a mating portion 23, a driving device 4 (shown in Fig. 10) and a substrate handling element 28.
  • the pretreatment device 2 comprises an upper body 21 and a lower body 22.
  • the upper and lower bodies 21 and 22 can be mounted together in virtue of fixing elements 201 to form a pretreatment cavity (first region) 20.
  • a gasket ring 202 may be disposed between the upper and lower bodies 21 and 22 for sealing.
  • the mating portion 23 may be unitary with the pretreatment device 2 and defines a passage 24 to communicate with the pretreatment cavity 20.
  • the substrate holder 25 is located in the pretreatment cavity 20 and has an upper surface 250 to hold the substrate 300.
  • a sample plate 30 is placed on the upper face 250 of the substrate holder 25 and has a recess thereon for carrying the substrate 300.
  • the substrate 300 can move with movement of the sample plate 30.
  • the driving device 4 such as including a gas cylinder connects to the substrate holder 25 through a bottom 221 of the cavity 20.
  • the gas cylinder 4 can drive the substrate holder 25 to move between a first position (shown in Fig. 14) and a second position (shown in Fig. 15) by an output axis 41 thereof.
  • the output axis 41 of the gas cylinder 4 is prevented from rotating in order to avoid rotation of the substrate holder 25.
  • the pretreatment device 2 can also include four holding members 29 mounted on the lower body 22 for sustaining the pretreatment device 2.
  • the pretreatment device 2 comprises a pretreating mechanism which includes a ring heating device (not shown), the input passage 206 and the output passage 207.
  • the ring heating device is mounted in a ring recess 212 recessed downwardly from a top 211 of the device 2.
  • a gap may exist among the input passage 206, the output passage 207, the substrate holder 25 and the top 211 of the cavity 20, and height of the gap may be about 0.5-lmm. So, the samples can locate in the gap.
  • a pretreatment gas is fed into the gap to contact the samples from the input passage 206. Unreacted gas and product gases are discharged out of the gap from the output passage 207.
  • the gap can limit heat and the pretreatment gas therein to avoid the heat and the pretreatment gas to diffuse outside the gap.
  • the samples on the substrate 300 can not contact the top 211 of the cavity 20.
  • the ring heating device heats the top 211 of the device 2 so that the samples can be heated by heat radiation and heat convection.
  • the pretreatment device 2 can form a hole 200 in a front end thereof.
  • a seal cover 203 covers the hole 200.
  • the substrate handling element 28 is mounted to the seal cover moveably. Shown in Fig. 15, the sample plate 30 carrying the samples can be placed on the substrate holder 25 from the hole 200.
  • the substrate handling element 28 extends into the pretreatment cavity 20 from an exterior of the pretreatment device 2 and can move horizontally to push the sample plate 30 into the reactor 1 through the passage 24 of the mating portion 23.
  • a heat insulation element 213, such as including a fiberglass heat retaining wool is mounted on an outside of the top 211 of the pretreatment device 2 to reduce the heat dissipation.
  • a stainless steel shell 214 can cover the heat retaining wool 213 in order to assemble conveniently and enhance an appearance of the pretreatment device 2.
  • the samples are carried in different carrying areas of the substrate 300.
  • the pretreatment gas introduced from the input passage 206 is relatively concentrated because limitation of the input passage 206. So, in this situation, it is preferred to disperse the gas so that the gas can flow through all the samples uniformly. Therefore, referring to Figs. 11-13, a guiding plate 26 formed with a plurality of guiding recesses 260 is disposed on the substrate holder 25 adjacent to the input passage 206. The guiding recesses 260 can disperse the pretreatment gas to the samples uniformly.
  • another guiding plate 27 can also be disposed on the substrate holder 25 adjacent to the output passage 207.
  • a plurality of guiding recesses 270 are also formed to guide the unreacted gas and the production gases to flow to the output passage 207.
  • the input passage 206 and the output passage 207 face each other and are located approximately in a straight line.
  • An extending direction of the substrate handling element 28 is perpendicular to the straight line.
  • two ends of each of the guiding plates 26 and 27 along the extending direction are formed with chamfer angles 261 , 271, 262 and 272 separately.
  • a method for pretreating the samples comprises:
  • Pretreating the samples driving the substrate holder 25 by the gas cylinder 4 to the first position, feeding a pretreatment gas, such as including hydrogen in this embodiment until the gas has a stable flow, then, setting heating temperature and pretreatment time to pretreat the samples;
  • a pretreatment gas such as including hydrogen in this embodiment
  • the pretreatment gas fed into the pretreatment device 2 may penetrate into the reactor 1 so as to disturb the subsequent tests in the reactor 1. Therefore, after the samples are moved into the reactor 1 , it may need to vacuum the testing system. Subsequently, a testing gas can be introduced into the reactor 1 to carry out the tests.
  • the gate 210 shown in Fig. 6
  • the gate 210 such as including a brake valve can be disposed in the mating portion 23 for controlling the communication of the pretreatment device 2 and the reactor 1. When the gate exists, only the reactor 1 may need to be vacuumed after closing the gate.
  • a shielding setup 5 including three layers of mirror plates may be mounted under the substrate holder 25. Distances between edges of the mirror plates 5 and the sidewalls of the upper body 21 are so small that the pretreatment gas or the heat can be prevented from diffusing to a lower portion of the pretreatment cavity 20. Thus, elements in the lower portion of the cavity 20 can be avoided chemical changes or losses effectiveness. For example, it can prevent the gasket ring 202 from losing effectiveness.
  • the upper surface 250 of the substrate holder 25 for placing the substrate 300 can also be used as a shielding setup to limit the heat radiation in the gap by polishing or spreading some materials which can reduce the heat radiation on the upper surface.
  • a water cooling tube 209 is disposed at a middle portion of the upper body 21 to forcibly decrease the heat conduction so as to improve security of the system.
  • a flexible metal conduit connects the substrate holder 25 and the mirror plates 5.
  • the substrate holder 25 can move with movement of the mirror plates 5. Because of flexibility of the metal conduit 205, the substrate holder 25 can attach the top 211 better in the first position.
  • a gas flow and pressure controller (not shown) may be disposed at a front end of the input passage 206.
  • a thermocouple can be inserted into the gap from the output passage 207 to measure temperature of the pretreatment.
  • Figs. 17-28 illustrate diagrams of the reactor 1 in accordance with the preferred embodiment shown in Fig. 9.
  • the reactor 1 can also have other configurations known in the arts.
  • the reactor 1 is approximate in a cuboid shape.
  • the reactor 1 comprises a top portion 150, a bottom portion 151 and a middle portion 152 locating between the top portion 150 and the bottom portion 151.
  • the top, middle and bottom portions together define a reaction cavity (second region) 153 (shown in Figs. 18-19).
  • a first, second and third driving devices 155,157 and 156 are installed on three sidewalls of the middle portion 152 separately.
  • the driving devices 155, 157 and 156 are provided with step motors separately to drive relevant elements to move.
  • one side of the middle portion 152 on which the third driving device 156 is installed defines a window 11.
  • a charge coupled device (CCD) 158 can be disposed outside the window 11.
  • Other two opposite sides of the middle portion 152 are formed with a group of holes separately to accommodate some conduits 159.
  • the conduits 159 may be used for controlling pressure, providing reactants, sampling products or connecting external electrical devices etc. Referring to Fig. 18, all the conduits 159 can be disposed at the middle portion 152. Alternatively, a part or all of the conduits 159 can also be disposed at the top portion 150 or the bottom portion 151.
  • Fig. 18 illustrates a schematic diagram of a reaction system including the reactor 1.
  • the reactor 1 is the core of the reaction system.
  • the reactor 1 comprises a probe 109 located in the reaction cavity 153 and a platform (substrate holder) 8 for holding the substrate 300 which carries the pretreated samples.
  • the probe 109 and the platform 8 can move with respect to each other. In this embodiment, the probe 109 can move up and down, and the platform 8 can move along X, Y directions.
  • the reactants flow along a gaseous stop valve (not shown) and a filter (not shown) in turn to a mass flow controller (MFC) 160.
  • MFC mass flow controller
  • the reactants are introduced into the probe 109 via input conduits 118 disposed on the middle portion 152.
  • the reactants and the pretreated samples participate in reactions, while reaction products are sampled and sent to a vacuum chamber 6 via a sampling conduit 123.
  • a measuring device 161 analyses the reaction products to get desired information.
  • the sampling conduit 123 may need to be heated.
  • the measuring device 161 is a QMS, and distance between ionization filaments of the QMS and end of the sampling conduits can be adjusted.
  • PFC pressure flow controller
  • the reaction cavity 153 and the vacuum chamber 6 can have independent pumps and valves (not shown) in order to satisfy their desired vacuum degree.
  • a primary mechanical pump (not shown) and a molecular pump (not shown) can both be installed in the vacuum chamber 6 to satisfy higher vacuum degree.
  • a primary mechanical pump (not shown) can be installed in the reaction cavity 153 to satisfy lower vacuum degree.
  • the input conduits 118 can be mainly used to feed reactants (generally gaseous reactants), while the reactants may be mixed with some impurities.
  • the sampling conduit 123 can be mainly used to sample the reaction products, while the reaction products may be mixed with unreacted reactants etc.
  • the output conduits 124 can be mainly used to discharge the unreacted reactants, while the unreacted reactants may be mixed with other gases.
  • the bottom portion 151 of the reactor 1 is formed with a guiding portion 114 protruding upwardly and extending along the X direction.
  • the platform 8 is installed on the guiding portion 114 moveably and comprises an upper/lower platforms moveably mounted together.
  • a stainless steel shaft (not shown) connects the second driving device 157 to the lower platform of the platform 8. So, the second driving device 157 can drive the lower platform to move along the Y direction on the guiding portion 114 by driving the steel shaft.
  • a shaft 119 connects the second driving device 156 to the upper platform. So, the third driving device 156 can drive the upper platform to move along the X direction on the lower platform.
  • the reactor 1 defines an opening 112 on one side of the middle portion 152 opposite to the side on which the driving device 156 is installed. Referring to Fig. 9, the mating portion 23 of the pretreatment device 2 connects with the opening 112 so that the substrate 300 can be sent on the platform 8 from the opening 112.
  • the reactor 1 is formed with a mounting portion 113.
  • the mounting portion 113 can be in a shaft shape and two ends thereof may be separately installed on the two opposite sides of the middle portion 152.
  • a connecting portion connecting the two ends of the mounting portion 113 is suspended in the reaction cavity 153.
  • the mounting portion 113 may be mounted on other positions of the middle portion 152 or be mounted on the bottom portion 151, or be mounted on both of the bottom portion 151 and the middle portion 152.
  • the mounting portion 113 can form a lead rail 115 in a middle position thereof.
  • the lead rail 115 is formed with two rows of ball bearing (not shown).
  • a supporting element 116 is moveably assembled on the lead rail 115.
  • the probe 109 is installed on the supporting element 116.
  • the supporting element 116 may be adiabatic.
  • the probe 109 can also be installed on the lead rail 115 directly.
  • a pair of hooks 1160 can be disposed at two sides of the supporting element 116 along the X direction separately. One ends of a pair of elastic elements 117, such as including springs connect the corresponding hooks 1160 and the other ends thereof connect the mounting portion 113. Alternatively, the hooks 1160 can also be disposed on the probe 109.
  • the driving device 155 drives a contacting portion 111 by a connecting shaft 110, which connects the driving device 155 and the contacting portion 111.
  • the contacting portion 111 contacts an upper surface of the probe 109.
  • the connecting shaft 110 and the contacting portion 111 connect and are independent with each other. Alternatively, they also can be unitary.
  • the driving device 155 drives the contacting portion 111 to press the probe 109 downwardly, while the pair of springs 117 are stretched.
  • the driving device 155 returns, the contacting portion 111 releases the probe 109 and the probe 109 is pulled upwardly by restoring forces of the springs 117.
  • the CCD 158 located outside the window 11 is used to adjust distance between the probe 109 and the substrate 300 on the platform 8 so as to determine precise position between the probe 109 and the substrate 300.
  • FIG. 21 there illustrates a cross-sectional view of the probe 109 in accordance with the preferred embodiment of the present invention.
  • the probe 109 is a critical element of the reactor 1 and has functions of feeding the reactants, sampling the products, balancing pressure and preventing impurities entering into a reaction room 133 (shown in Fig. 22).
  • the probe 109 comprises a main body 125, a covering element 126 assembled under the main body 125 and a guiding portion 137.
  • the main body 125 defines a pair of horizontal output passageways 127 arranged symmetrically. Two vertical output passageways 128 extend downwardly and run through the main body 125 from ends of the corresponding passageways 127 separately.
  • the main body 125 further defines a sampling passageway 129 at an upper part thereof and a cut 1250 coaxial and connecting with the sampling passageway 129 at a lower part thereof.
  • the covering element 126 has a concave 140 recessed downwardly from a middle portion of an upper surface thereof. A bottom surface of the concave 140 may be approximately cone-shaped.
  • a column hole 139 is recessed from a middle portion of the bottom surface of the concave 140 to connect with the reaction room 133 defined upwardly from a bottom surface of the covering element 126.
  • the reaction room has a larger diameter than that of the column hole 139.
  • the covering element 126 can have output holes 130 recessed from the upper surface thereof and input holes 131 recessed from a lateral of the bottom surface of the concave 140.
  • a first groove 141 and a second groove 142 are defined upwardly from the bottom surface of the covering element 126 to connect with the input holes 131 and the output holes 130 separately.
  • the input holes 131 and the output holes 130 can be arranged annularly around the reaction room 133.
  • the input holes 131 and the output holes 130 also can be arranged in a square configuration or a triangle configuration around the reaction room 133.
  • the guiding portion 137 has an axial hole 138.
  • Semicircle guiding passages 134 are formed on an exterior surface of the guiding portion 137 and extend along an axial direction.
  • the guiding passages 134 can also be other configurations and extend along a curved-shaped.
  • the output passageways 127, 128 communicate with the output holes 130.
  • the concave 140 and the cut 1250 of the main body 125 both define a receiving cavity. Because an end of the guiding portion 137 protrudes downwardly and fits well with the cone-shaped bottom surface of the concave 140, the guiding portion 137 can position in the receiving cavity easily without additional aiding methods.
  • the guiding portion 137 fits with the receiving cavity loosely, or it can also interfere with each other.
  • the axial hole 138 of the guiding portion 137, the column hole 139 of the covering element 126, the reaction room 133 and the sampling passageway 129 of the main body are arranged coaxially and communicated.
  • the receiving chamber has a mixing chamber 136 above the guiding portion 137 and a sidewall of the mixing chamber 136 defines feeding passageways 135.
  • the input conduits 118 are received in the corresponding passageways 135.
  • the sampling conduit 123 passes through the sampling passageway 129, the axial hole 138 and the column hole 139 so as to communicate with the reaction room 133.
  • the output conduits 124 are received in the corresponding output passageways 127.
  • the sampling conduit 123 can be capillary which has a diameter of 10-lOOum to adapt pressure difference between the reaction cavity 153 and the vacuum chamber 6. Meanwhile, a length of the capillary can be adjusted according to specific reactions.
  • the pressure of the reaction cavity 153 may need to reach demand of reaction pressure, and the reactants are provided stably. Then, the driving devices 155, 156 and 157 drive the platform 8 and the probe 109 to reach a predetermined position. The CCD 158 monitors the distance between the probe 109 and the substrate 300 so as to adjust it. Next, the reactants are fed into the mixing chamber 136 from the input conduits 118 to be mixed. The mixed reactants flow through the guiding passages 134 of the guiding portion 137 to get into the input holes 131, wherein the input holes 131 has a function of distributing the reactants. Subsequently, the reactants enter into the first groove 141 and are mixed again.
  • reaction room 133 a small part of reactants enter into the reaction room 133 to contact with the samples for testing.
  • the reaction products are sampled by the sampling conduit 123 and are sent into the vacuum chamber 6 to analyze by the QMS 161.
  • QMS 161 a large part of the reactants flow into the second groove 142 and are discharged through the output holes 130, the output passageway 128 and the output conduit 124 in turn.
  • the reaction cavity 153 may need to be full of an environment gas, which is normally an inert gas, such as Ar to reach a predetermined pressure in the reaction cavity 153.
  • an environment gas which is normally an inert gas, such as Ar to reach a predetermined pressure in the reaction cavity 153.
  • the MFC 160 is disposed on the input conduits 118 to control flow capacity of the reactants.
  • a MFC 163 controls flow capacity of the environment gas.
  • the PFC 162 is disposed on the output conduits 124 to control the pressure in the reaction cavity 153.
  • entrances of the output holes 130 are defined in the probe 109 and are near the reaction room 133.
  • the distance between the probe 109 and substrate 300 is in a micrometer lever, such as including 10-20um.
  • Exhaust of the unreacted reactants is mainly controlled by the PFC 162.
  • the flow capacity of the reactants is small, such as l-2ml/m, the pressure balance in the reaction room 133 may not be controlled easily because flow capacity of the PFC 162 is normally large, such as 500ml/m. Therefore, another pressure control system may need to be provided when the pressure balance is not controlled yet by adjusting controlling parameters of the PFC 162.
  • Fig. 26 illustrates a schematic diagram of another pressure control system, which can solve the pressure control problem when the flow capacity of the reactants is small.
  • the PFC 162 can control the pressure of the environment gas in the reaction cavity 153.
  • a MFC 163 controls a flow rate of the environment gas in the reaction cavity 153.
  • the pressure balance and the exhaust of the unreacted reactants are controlled by a MFC 164.
  • Flow capacity Q of the MFC 164 is approximate to the flow capacity Qresource of the reactants controlled by the MFC 160.
  • Q IO* Qresource.
  • the MFC 164 can be substituted by a conduit having a larger flow resistance, such as including a capillary.
  • a value of the flow capacity of the MFC 164, and a diameter and a length of the capillary are related to parameters, such as including the environment pressure in the reaction cavity 153 and the height of the probe 109 etc.
  • the reaction system comprises a controlling system module 40, a motion/position module 49, a heating module 42, a pump/valve module 45, a source distributing module 46, the reactor 1, a product analysis module 43 and a data manipulation module 44.
  • the controlling system module 40 can control operation of the reactor 1 by controlling the motion/position module 49, the heating module 42, the pump/valve module 45 and the source distributing module 46.
  • the products in the reactor 1 are sent into the analysis module 43 to get data.
  • the data are sent to the date manipulation module 44 to be manipulated to get desired information.
  • a flow chart of the test in the reactor 1 comprises
  • Initialization 50 which includes loading initializing files of the reaction system, inspecting/starting up the vacuum system, inspecting the gas source, inspecting and heating the capillary etc.;
  • Cleanout 52 which includes charging the environment gas into the reactor 1 to reach the predetermined pressure and then vacuumizing the reactor 1 some times to clean the reactor 1 ;
  • Positioning 53 which includes setting the pressure in the reactor 1 and original position of the probe 109 and the platform 8;
  • Setting testing processes 54 which includes setting parameters of the reactant gas, the reaction cavity and the flow controllers separately, setting heating curves, reaction routes, inspecting the flow capacity of the gas source, a heating system (shown in Fig. 39) and a cooling system etc.;
  • a selected usage of the reactor 1 is provided to test activities of different amounts of CuO during oxygenation of CO: Test conditions: 1. CO : 4.7 %
  • the substrate is calcined at 650 "C .
  • a reactor in accordance with one embodiment of the present invention, comprises a top portion, a bottom portion opposite to the top portion and a middle portion connecting the top portion and the bottom portion, commonly defining a reaction cavity. Wherein at least a reactant input conduit is disposed in the middle portion of the reactor.
  • reactant gases are fed into the reaction cavity to contact with the samples located in the reactor.
  • the products are kept in the reactor and an exterior spectrometric detector can be used to measure the characteristics of the products, such as described in PCT/CN2006/000945 of the same applicants.
  • light sources may need to be used to illuminate the tests, for example illumination during heating, lighting, inspecting or measuring etc.
  • the light sources are used on a reactor.
  • the light sources can also be used on the pretreatment device under certain conditions.
  • the reactor 1 comprises a reaction cavity 153 in which the samples are tested.
  • the reaction cavity 153 has a first opening 60.
  • a first light source 71 is disposed outside the reaction cavity 153 to generate a first light beam.
  • a second light source 72 is disposed outside the reaction cavity 153 to generate a second light beam.
  • the reactor 1 is configured to select among the group consisting of (1) the first light source, (2) the second light source, and (3) both of the first and the second light sources 71 and 72 to illuminate the reaction cavity 153 through the first opening.
  • the bottom 151 of the reactor 1 defines a first opening 60.
  • the sentence of "either or both of the first and the second light sources 71 and 72 to illuminate the reaction cavity 153 through the first opening 60" means: a), only the first light beam passes through the first opening; b) only the second light beam passes through the first opening; c) the first light beam and the second light beam both pass through the first opening simultaneously or asynchronously.
  • the substrate 300 carries the sample 302, 303 and 304.
  • the first light beam generated from the first light source 71 or only the second light beam generated from the second light source 72 passes through the opening 60 to handle the sample 302, such as including heating, lighting or inspecting etc.
  • the light beams generated from the first/second light sources 71 and 72 can handle different samples 303 and 304, or can handle the same one sample.
  • light routes of the first light beam and the second light beam can be independent or be coincident partly with each other.
  • the first light beam and the second light beam can enter into the reaction cavity 153 directly.
  • an additional element such as including a reflecting mirror or a convex mirror etc. is disposed to adjust the light route.
  • the mirror is made of different materials.
  • Figs. 32-33 illustrate the light sources and the reactor 1 in accordance with another embodiment of the present invention.
  • the reactor 1 defines the first opening 60 and a second opening 61 on the bottom portion 151 thereof.
  • the first light source 71 and the second light source 72 can illuminate the reaction cavity 153 through the first opening 60 and the second opening 61 separately.
  • the first light source 71 and the second light source 72 handle the samples selectively:
  • the first light beam of the first light source 71 and the second light beam of the second light source 72 handle the different samples 303 and 304 from the openings 60 and 60 separately.
  • the first light beam and the second light beam can handle the same sample 302 from the different openings.
  • the first light source 71 and the second light source 72 can handle the same one/two sample(s) simultaneously or asynchronously. Or one light source works, another light source does not work.
  • the first light beam and the second light beam can includes laser or infrared lights for heating the sample.
  • a light emitting diode (LED) can also be used to illuminate.
  • Materials for generating the laser have some types, such as including solids, gases, semiconductors and free electrons etc.
  • the solid laser is generated by a material bar selected specially, such as including a ruby laser or a sapphire laser etc.
  • the gas laser such as including CO 2 Laser whose wavelength is 1036nm is emitted by activating gas atoms which have discharge properties.
  • the semiconductor laser such as a diode laser whose wavelength is 808nm is generated by a laser generator.
  • the laser generator is formed by connecting two pieces of semiconductor materials. The two semiconductor materials are treated in different processes to contain different impurities. When a great deal of electricity passes this generator, the laser is emitting from connection of the two semiconductor materials.
  • the free electrons are derived from a specific accelerator or other energy devices. Then, they are accelerated to light velocity by an undulator which is formed by linearity electromagnetic. Thus, the free electrons can emit energy in a fashion of a synchronous acceleration ray so that the free electron laser is formed. Additionally, a density and a wavelength of the ray can be adjusted by changing a girth of its magnetic field. A range of the wavelength of the ray can be adjusted from the microwave to the ultraviolet.
  • the substrates are made of different materials because of different light beams.
  • appropriate light beams can be selected after determining the substrate.
  • the different light beams with different wavelengths can be selected as long as the selected light beams can not damage the substrate and ensure the operations of the tests.
  • the substrate may be made of silica or quartz.
  • the diode laser or the LED can be used.
  • the substrate is silica, the CO 2 laser or light beams whose wavelength are small than 1036nm, such as including the diode laser or the LED etc. can be used.
  • the reactor may need to be sealed when the tests are operating. Therefore, a first light transmission element and a second light transmission element can be accommodated in the first opening 60 and the second opening 61 separately.
  • the light transmission elements may be made of glass or other materials. It is preferred that the light transmission are made of the glass, and the first/second light transmission elements are the same or different. In one embodiment, glass materials of the first/second light transmission elements are different to adapt the first/second light beams with different wavelengths.
  • glass materials can comprise: a), a silicate glass whose main composition includes SiO 2 ; b). an oxide glass whose main composition may includes B 2 O 3 ⁇ P 2 O 5 ⁇ Al 2 O 3 ⁇ GeO 2 ⁇ TeO 2 or V 2 O 5 etc.; c). a non-oxide glass whose main composition can be sulphur series compounds or a halide etc.; d). a metal glass formed by quickly cooling some alloys.
  • the first opening and the second opening can accommodate a SiO 2 glass sheet or a ZnSe glass sheet.
  • the light beam is CO 2 laser
  • the ZnSe glass sheet can be used.
  • the light beam is the diode laser or the LED
  • the SiO 2 and the ZnSe glass sheets can both be used.
  • the reactor 1 may define a third opening for a third light beam passing through. Positions of the first opening, the second opening or the third opening can be the same or different. The same position means the first opening, the second opening and the third opening are all defined on the same one of the top, middle and bottom portions.
  • handling situations comprise:
  • the three light beams handle the same one sample simultaneously;
  • the phrase “every time” means all of the light beams which are working complete to handle the sample(s) one time. For example, when there are two working light beams, the phrase “every time” means the two light beams both complete to handle the corresponding sample(s).
  • the first, second, third light beams can be the diode laser, the CO 2 laser or the LED.
  • the first light beam may be the diode laser
  • the second light beam may be the CO 2 laser
  • the third light beam may be the LED.
  • the reactor can also define a fourth opening or a fifth opening etc. for a fourth light beam and a fifth light beam passing through.
  • there may be different combinations of the light beams and the openings to handle the samples such as including the combination of the three light beams and the three openings described above.
  • the glass sheets may be coated with antireflection coatings.
  • the openings may be coated with a black color or machined coarsely to absorb a part of reflected lights.
  • a seal groove shown in Fig. 35 can be disposed in the corresponding opening to accommodate a seal element including an O- shaped gasket.
  • FIGs. 34-37 there illustrate schematic diagrams of openings of the reactor 1 in accordance with a preferred embodiment of the present invention. Additionally, configurations of any one of the openings shown in Figs. 29-33 can be the same as/similar to configurations of the openings shown in Figs. 34-37.
  • the reactor 1 defines a first opening 81 , a second opening 82 and a third opening 80 which downwardly run through the bottom portion 151 thereof from an inner surface of the bottom portion 151.
  • the first, second and third openings 81, 82 and 80 comprise a first opening portions 811, 821 and 801 recessed downwardly from the inner surface, a third opening portions 813, 823 and 803, and a second opening portions 812, 822 and 802 connecting the first opening portions and the second opening portions separately.
  • the first, second and third opening portions 801, 802 and 803 of the third opening 80 extend downwardly along a direction perpendicular to the inner surface.
  • the first, second and third opening portions 811, 821, 812, 822, 813 and 823 extend slopingly from the inner surface.
  • the inner surface of the bottom portion 151 is a horizontal surface.
  • the first opening portions of the openings can be recessed downwardly from the inner surface or from an outer surface opposite to the inner surface.
  • the reactor has a mounting surface which can be the inner surface or the outer surface from which the first opening portions are recessed directly.
  • the light transmission elements, such as including the glass sheets are placed into the corresponding openings from the mounting surface.
  • the mounting surface is the inner surface of the reactor 1.
  • the size of the reactor 1 may be relatively small.
  • the openings may be so compact that the first opening portions 811 and 801 or 821 and 801 may interfere with each other.
  • directions of fixing forces for fixing seal gaskets and the glass sheets are generally perpendicular to the inner surface of the bottom surface.
  • the seal gaskets or the glass sheets are placed slopingly in the first opening portions 811 and 821. So, the fixing forces exerting on the seal gaskets or the glass sheets may not balance so as to influence the tests in the reactor 1.
  • the reactor 1 defines a first opening 91, a second opening 92 and a third opening 90 which run through the bottom portion 151 thereof.
  • the first opening 91 and the second opening 92 are located at two sides of the third opening 90.
  • the first, second and third openings 91, 92 and 90 comprise a first opening portions 911, 921 and 901 recessed downwardly from the inner surface of the bottom portion 151, a third opening portions 913, 923 and 903, and a second opening portions 912, 922 and 902 connecting the first opening portions and the second opening portions separately.
  • the first, second and third opening portions 901, 902 and 903 have the same extending direction E. That is, angles among the extending directions of the first, second and third opening portions 901, 902 and 903 are zero degree.
  • the direction E is perpendicular to the inner surface of the bottom portion 151.
  • An extending direction A of the first opening portion 911 of the first opening 91 is parallel to the extending direction E of the third opening 90.
  • the second and third opening portions 912 and 913 have the same extending direction B.
  • the extending direction B has an acute angle, such as including 30 degrees with the extending direction A.
  • An extending direction C of the first opening portion 921 of the second opening 92 is also parallel to the extending direction E of the third opening 90.
  • the second and third opening portions 922 and 923 have the same extending direction D.
  • the extending direction D has an acute angle with the extending direction C.
  • the seal grooves for receiving the O-shaped gaskets 33 are recessed downwardly from laterals of the first opening portions 911 , 921 and 901.
  • the glass sheets (not shown) may be placed in the first opening portions 911 , 921 and 901. In this situation, the distances from every spots of each of the bottom surfaces of the openings to the inner surface of the bottom portion 151 are the same. So the fixing forces exerting on the glass sheets and the gaskets 33 are balance and uniform so that leakage can be avoided.
  • Fig. 38 illustrates a configuration similar as the diagram shown in Fig. 37. The difference is that the second opening 92 further defines a fourth opening portion 924 connecting the second opening portion 922 and the third opening portion 923.
  • the testing system may have a laser heating system to generate a laser to heat the samples on the substrate 300.
  • a temperature control loop of the laser heating system comprises an infrared thermometer 62, a PID controller 63, a laser controller 64 and a laser generator 65.
  • the infrared thermometer 62 inspects temperatures of the tests and converts temperature signals to electrical signals which are 4-2OmA. The electrical signals are sent into the PID controller 63.
  • a CCD 66 transmits figures of the carrying areas of the substrate 300 to a computer 67 to determine heating positions.
  • the computer 67 controls the PID controller 63.
  • the PID controller 63 sends its output signals to the laser controller 64 to control power of the laser generator 65, which is 0-95%.
  • An electrical source module 68 controls the opening/closing of the laser generator 65.
  • the chilling system 69 is for cooling the laser generator 65.
  • heating systems can selectively heat the samples from the first openings 81, 91, the second openings 82, 92 or the third openings 80, 90.
  • the CO 2 laser passes through the third openings 80, 90 to heat the samples.
  • the diode laser passes through the first openings 81, 91 to heat the samples.
  • the light emitting diode is disposed near the second openings 82, 92 for illuminating the reaction cavity 153 of the reactor 1. Either or both of the diode laser and the CO 2 laser can be opened. In the meantime, the light emitting diode may work or not work.

Abstract

A testing system (1000) for testing a plurality of samples on a substrate (300) comprises an enclosed cavity (100) having a first region (1020) and a second region (1010). A pretreatment unit (102) is provided to pretreat the samples while the substrate (300) is in the first region. A test unit (101) is provided to receive the substrate (300) after the samples are pretreated and to test the samples while the substrate is in the second region. The test unit (101) includes a test mechanism for determining characteristics of the samples while the substrate (300) is in the second region.

Description

System and method for sample testing
FIELD OF INVENTION
[0001] The invention relates to a system and a method for testing samples, especially catalyst samples.
BACKGROUND OF THE INVENTION
[0002] In recent years, new materials with excellent properties and wide usage have been developed. Research works to discover the properties of such new material are not only beneficial to the developments of these materials but also provide information to the production and applications of these materials.
[0003] Using combinatorial chemistry methods on material research, researchers can make a large quantity of material samples at the same time. It is often difficult and costly, however, to test the properties of a large quantity of samples and to screen the samples in a short time using traditional methods.
[0004] The emergence of micro-reaction technology solves this difficult problem by conducting chemical reactions in micro-reactors each requiring only a small volume of reactants. Compared to traditional chemical reactions, the micro-reaction technology can reduce research costs, improve work efficiency, and make better use of materials and resources because of its associated high heat transfer, high mass transfer, high security, and rapid response time. Moreover, combined with advanced process automation technology, transduce technology, measurement technology and software data analysis, the micro-reaction technology can lead to high throughput micro-reaction systems.
[0005] In a high throughput micro-reaction system, sample preparation is a complex process that may comprise steps of screening, grinding, resolving and/or heating. During such sample preparation processes, as well as transfer and preservation of prepared samples, sample contamination may occur, such as by steam or oxygen from the air, so that the samples may be oxygenated or otherwise reacted with to possess undesired variations.
[0006] Therefore, it is desired to provide a system and a method for testing samples without worrying about sample contamination during sample preparation, transfer, and preservation.
SUMMARY OF THE INVENTION
[0007] A testing system for testing a plurality of samples on a substrate, according to one embodiment, comprises an enclosed cavity having a first region and a second region. A pretreatment unit is provided to pretreat the samples while the substrate is in the first region. A test unit is provided to receive the substrate after the samples are pretreated and to test the samples while the substrate is in the second region. The test unit includes a test mechanism for determining characteristics of the samples while the substrate is in the second region.
[0008] A sample testing system, according to another embodiment, comprises a pretreatment unit including a substrate holder to hold a substrate carrying a plurality of samples and a pretreating mechanism to pretreat the samples. A test unit is coupled to the pretreatment unit and to receive the substrate from the pretreatment unit. The test unit includes a test mechanism to determine characteristics of the samples while the substrate is situated in the test unit.
[0009] Embodiment of the present invention further provides a sample testing method for testing samples on a substrate. The method comprises pretreating the samples in a pretreatment unit; moving the substrate from the pretreatment unit to a testing unit through a channel coupling the pretreatment unit to the testing unit such that the samples are not exposed to the atmosphere after being pretreated in the pretreatment unit and before being tested in the testing unit; and testing samples in the testing unit, wherein testing sample includes determining characteristics of the samples while the substrate is in the testing unit.
[0010] Embodiment of the present invention further provides a reactor for testing samples, comprises a top portion, a bottom portion for holding a substrate carrying a plurality of samples, and a middle portion disposed between the top portion and the bottom portion. The top, middle and bottom portions together define a reaction cavity. A probe is disposed in the reaction cavity and mounted on at least one of the middle portion and the bottom portion. Conduits are connected to the probe for transferring materials into and out of the reaction cavity.
[0011] Furthermore, embodiment of the present invention provides a reactor for testing samples, comprises a reaction cavity for testing samples therein. The reaction cavity has a first opening. A first light source is disposed outside the reaction cavity to generate a first light beam. A second light source is disposed outside the reaction cavity to generate a second light beam, wherein the reactor is configured to select among the group consisting of (1) the first light source, (2) the second light source, and (3) both of the first and the second light sources, to illuminate the reaction cavity through the first opening.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Fig. 1 is a schematic diagram of a testing system with a substrate located in a first region in accordance with one embodiment of the present invention;
[0013] Fig. 2 is a schematic diagram of the testing system shown in Fig. 1 with the substrate located in a second region;
[0014] Fig. 3 is schematic diagrams of the substrate, and the substrate and a sample in accordance with the present invention;
[0015] Fig. 4 is a schematic diagram of a testing system with a probe located in the first region in accordance with another embodiment of the present invention;
[0016] Fig. 5 is a schematic diagram of the testing system shown in Fig. 4 with the probe located in the second region;
[0017] Fig. 6 is a schematic diagram of a testing system in accordance with yet another embodiment of the present invention;
[0018] Fig. 7 is a schematic diagram of a testing system in accordance with yet another embodiment of the present invention, with a substrate holder located in a first position;
[0019] Fig. 8 is a schematic diagram of the testing system shown in Fig. 7, with the substrate holder located in a second position; [0020] Fig. 9 is a perspective view of a testing system comprising a reactor and a pretreatment device in accordance with a preferred embodiment of the present invention;
[0021] Fig. 10 is a perspective view of the pretreatment device shown in Fig. 9;
[0022] Fig. 11 is a cross- sectional perspective view of the pretreatment device shown in Fig. 10, with the substrate holder located in the second position;
[0023] Fig. 12 is a cross-sectional perspective view of the substrate holder and a shielding setup;
[0024] Fig. 13 is an assembled perspective view of the substrate holder and the shielding setup shown in Fig. 12;
[0025] Fig. 14 is a cross-sectional plane view of an upper portion of the pretreatment device shown in Fig. 10, with the substrate holder located in the first position;
[0026] Fig. 15 is a cross-sectional plan view of the pretreatment device shown in Fig. 10;
[0027] Fig. 16 is a view similar to Fig. 15, but the substrate holder located in the first position;
[0028] Fig. 17 is an assembled perspective view of a reactor in accordance with one embodiment of the present invention;
[0029] Fig. 18 is a schematic diagram of the system of the reactor in accordance with the present invention;
[0030] Fig. 19 is a partially assembled perspective view of the reactor shown in Fig. 17; [0031] Fig. 20 is an enlarged perspective view of part A shown in Fig. 19;
[0032] Fig. 21 is a cross-sectional view of a probe of the reactor in accordance with the present invention;
[0033] Fig. 22 is an enlarged view of part B shown in Fig. 21 ;
[0034] Fig. 23 is a cross-sectional perspective view of a covering element of the probe;
[0035] Fig. 24 is a perspective view of a guiding portion of the probe;
[0036] Fig. 25 is a schematic diagram of a pressure control in the reactor;
[0037] Fig. 26 is a schematic diagram of another pressure control in the reactor;
[0038] Fig. 27 is a schematic diagram of system modules of the reactor;
[0039] Fig. 28 is a schematic diagram of an experiment flow chart to use the reactor;
[0040] Fig. 29 is a schematic diagram of an opening of a bottom of the reactor, light sources and the substrate in accordance with one embodiment of the present invention;
[0041] Fig. 30 is another schematic diagram of the opening, the light sources and the substrate shown in Fig. 29;
[0042] Fig. 31 is a yet another schematic diagram of the opening, the light sources and the substrate shown in Fig. 29; [0043] Fig. 32 is a schematic diagram of the openings, the light sources and the substrate in accordance with another embodiment of the present invention;
[0044] Fig. 33 is another schematic diagram of the openings, the light sources and the substrate shown in Fig. 32;
[0045] Fig. 34 is a planform of the openings of the reactor of in accordance with yet another embodiment of the present invention;
[0046] Fig. 35 is a cross-sectional perspective view of the openings shown in Fig. 34;
[0047] Fig. 36 is a side view of the openings shown in Fig. 34;
[0048] Fig. 37 is a second cross-sectional plan view of the openings in accordance with yet another embodiment of the present invention;
[0049] Fig. 38 is a cross-sectional plan view of the openings in accordance with yet another embodiment of the present invention; and
[0050] Fig. 39 is a schematic diagram of a heating system of the reactor in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0051] Referring to Figs. 1-2, a system 1000 for testing samples in accordance with one embodiment of the present invention comprises an enclosed cavity 100 having a first region 1020, a second region 1010 and a channel 1030 between the first region 1020 and the second region 1010. The system 1000 further comprises a pretreatment unit 102 to pretreat the samples in the first region 1020, and a test unit 101 is to test the samples in the second region 1010 after the samples are pretreated. A substrate (sample carrier) 300 is provided to carry the samples.
[0052] The samples include catalysts for catalyzing reactions. The pretreatment process may be a reduction of the samples. For example, oxygenated samples may be pretreated by a pretreating mechanism that introduces hydrogen into the pretreatment unit 102 through a passage and heats the samples using a heating device (heating mechanism) 208. The temperature of the samples may be controlled so that the oxygenated samples are reduced in a temperature-controlled condition. At the meantime, unreacted hydrogen and water produced in the reaction can be discharged from the pretreatment unit 102. Alternatively or additionally, the pretreatment process may involve drying the samples. For example, some samples may become damp by being exposed to moisture. So, when drying the damp samples, the heating device 208 can be used to dry the samples with a controlled temperature, while an inert gas is introduced into the pretreatment unit 102 to carry the steam from the heated samples out of the pretreatment unit 102.
[0053] Referring to Fig. 3, the substrate 300 has n*n carrying areas 301, wherein n is an integer larger than 1. In one example, n = 20. In many cases, Kn<=100. The substrate 300 can be made of quartz or silica. The carrying areas 301 can carry the same or different samples 302. A height h of the sample 302 on the substrate 300 can be different based on specific tests (reactions) involved. Generally, h=10-300um. In order to attach the samples on the substrate 300 firmly, surfaces of each carrying areas 301 can be treated to increase its roughness in order to fix the samples thereon. Meanwhile, the substrate 300 can be formed with recesses to load the samples, such as those known in the art. [0054] As shown in Figs. 1-2, the test unit 101 includes a test platform (substrate holder) 15 for holding the substrate 300. In this embodiment, the test platform 15 may need to move precisely and is susceptible to temperature, especially to high temperature, which can debase its operation precision and influence its service effectiveness. The test unit 101 further comprises a test mechanism, such as including a probe 109. In one embodiment, the probe 109 is formed with a sampling configuration, such as including a sampling passage 105 for sampling testing products and sending the testing products to an analysis device (not shown) for analyzing. In this embodiment, the probe 109 and the test platform 15 can move with respect to each other. The sampling passage 105 of the probe 109 can be positioned precisely by moving the substrate holder 15 so that the sampling passage 105 can face the corresponding carrying area exactly. Thus, the sampling passage 105 can sample the testing product(s) from a particular carrying area. In order to obtain precise positioning of the sampling passage 105 with respect to the corresponding carrying area 301 of the substrate 300, the substrate holder 15 should be protected from exposure to high temperatures, which may cause deformation or malfunction of its positional mechanism.
[0055] Moreover, the probe 109 of the test unit 101 is designed with an input passage 106 and an output passage 107 for one or more materials (generally gaseous materials) to flow in/out of the test unit 101. Alternatively, the input passage 106 and the output passage 107 are not installed in the probe 109.
[0056] The test unit 101 further comprises a temperature control device 108 for controlling the temperature of the samples during testing. The temperature control device 108 may include a laser heating system, infrared heating system, heating ring or other heating devices. The temperature control device 108 can heat multiple samples on the substrate 300 collectively or individually. In this embodiment, the temperature control device 108 is installed on the test unit 101, and the device 108 can also be a separate unit from the test unit 101.
[0057] Furthermore, the pretreatment unit 102 can also comprise a substrate holder (pretreatment platform) 25 for holding the substrate 300 and a cover 204 opposite to the substrate holder 25. The substrate holder 25 and the cover 204 can move with respect to each other. A gap may exist between the cover 204 and the substrate 300 placed on the substrate holder 25, and the gap therebetween can be about 0.5-lmm. The substrate holder 25 and the cover 204 can both move, or the substrate holder 25 is stationary, while the cover 204 moves relative to the substrate holder 25, or vice versa. The heating device 208 can be disposed on the cover 204.
[0058] The pretreatment unit 102 can also comprise an input passage 206 and an output passage 207 so that a gas may flow through the gap. The gas flowing from the input passage 206 to the output passage 207 may become a stable concentrated gas stream flowing through the samples.
[0059] Figs. 4-5 illustrate one embodiment of the present invention wherein elements similar to those shown in Figs. 1-2 are numbered similarly. In this embodiment, the test unit 101 and the pretreatment unit 102 share the same input/output passages 106 and 107. The input passage 106 and the output passage 107 are disposed in the probe 109 and the probe 109 can move between the first region and the second region. When the probe 109 is in the first region (shown in Fig. 4), the input passage 106 and the output passage 107 can provide a flow of gas for pretreating, and when the probe is in the second region (shown in Fig. 5), the input/output passages 106 and 107 can provide a flow of gas for testing. In certain situations, a bottom 1040 of the probe 109 can be used as the cover 204 shown in Fig. 1.
[0060] Figs. 6-8 illustrate other embodiments of the invention wherein elements similar to those shown in Figs.1-2 and 4-5 are numbered similarly. The system according to illustrated embodiments shown in Figs. 6-8 comprise a reactor (test unit) 1 and a pretreatment device (pretreatment unit) 2 coupled to the reactor 1 through a passage (channel) 24. The passage 24 is shaped to have a different height from the first and second region. The reactor 1 defines a reaction cavity (the second region) 10 and the pretreatment device 2 defines a pretreatment cavity (the first region) 20. The reaction cavity 10, the pretreatment cavity 20, and the passage 24 together form an enclosed cavity of the system. The first region 20 and the second region 10 are connected with each other by the passage 24. Thus, the system can be made by coupling a testing unit to a pretreatment unit through an enclose channel or a passage. A substrate handling element 28 is disposed in the pretreatment device 2 to transfer the pretreated samples into the second region 10 from the first region 20. Alternatively, the substrate handling element 28 may be disposed in the testing system shown in Fig. 1.
[0061] Referring to Fig. 6, a gate 210 can be disposed in the passage 24 to open/close the communication between the first region 20 and the second region 10. The gate 210 can be a brake valve or any other gating elements which can control the opening/closing of the passage 24. The gate 210 can also be disposed in a system shown in Figs. 7-8.
[0062] Referring to Figs. 7-8, in this embodiment, the cover 204 is stationary and the substrate holder 25 is moveable. When the substrate holder 25 moves from a first position (shown in Fig. 7) to a second position (shown in Fig. 8), the substrate handling element 28 can push the substrate 300 into the second region 10 from the first region 20. The cover 204 may also be moveable. Alternatively or additionally, a driving device 4 may be positioned under the pretreatment device 2 to drive the substrate holder 25 to move up and down.
[0063] Referring to Fig. 9, there illustrates a preferred embodiment of the present invention wherein elements similar to those shown in the above Figures are numbered similarly. The samples include catalysts containing noble metals, such as including Pt etc. In this embodiment, the testing system 1000 comprises a sample reactor (test unit) 1, a pretreatment device (pretreatment unit) 2 coupled to the sample reactor 1 through a mating portion 23, a driving device 4 (shown in Fig. 10) and a substrate handling element 28.
[0064] Referring to Figs. 10-16, there illustrate diagrams of the pretreatment device 2 in accordance with the preferred embodiment shown in Fig. 9. Referring to Figs. 10-11, the pretreatment device 2 comprises an upper body 21 and a lower body 22. The upper and lower bodies 21 and 22 can be mounted together in virtue of fixing elements 201 to form a pretreatment cavity (first region) 20. A gasket ring 202 may be disposed between the upper and lower bodies 21 and 22 for sealing. The mating portion 23 may be unitary with the pretreatment device 2 and defines a passage 24 to communicate with the pretreatment cavity 20.
[0065] The substrate holder 25 is located in the pretreatment cavity 20 and has an upper surface 250 to hold the substrate 300. In this embodiment, a sample plate 30 is placed on the upper face 250 of the substrate holder 25 and has a recess thereon for carrying the substrate 300. The substrate 300 can move with movement of the sample plate 30.
[0066] Referring to Figs. 14-16, in this embodiment, the driving device 4, such as including a gas cylinder connects to the substrate holder 25 through a bottom 221 of the cavity 20. The gas cylinder 4 can drive the substrate holder 25 to move between a first position (shown in Fig. 14) and a second position (shown in Fig. 15) by an output axis 41 thereof. In the meantime, the output axis 41 of the gas cylinder 4 is prevented from rotating in order to avoid rotation of the substrate holder 25. The pretreatment device 2 can also include four holding members 29 mounted on the lower body 22 for sustaining the pretreatment device 2.
[0067] Referring to Figs. 10, 14 and 16, the pretreatment device 2 comprises a pretreating mechanism which includes a ring heating device (not shown), the input passage 206 and the output passage 207. The ring heating device is mounted in a ring recess 212 recessed downwardly from a top 211 of the device 2. A gap may exist among the input passage 206, the output passage 207, the substrate holder 25 and the top 211 of the cavity 20, and height of the gap may be about 0.5-lmm. So, the samples can locate in the gap. A pretreatment gas is fed into the gap to contact the samples from the input passage 206. Unreacted gas and product gases are discharged out of the gap from the output passage 207.
[0068] In one embodiment, because the substrate holder 25 can attach to two sides of the top 211, so, the gap can limit heat and the pretreatment gas therein to avoid the heat and the pretreatment gas to diffuse outside the gap. In order to ensure the pretreatment gas flows through the gap, the samples on the substrate 300 can not contact the top 211 of the cavity 20. The ring heating device heats the top 211 of the device 2 so that the samples can be heated by heat radiation and heat convection.
[0069] The pretreatment device 2 can form a hole 200 in a front end thereof. A seal cover 203 covers the hole 200. The substrate handling element 28 is mounted to the seal cover moveably. Shown in Fig. 15, the sample plate 30 carrying the samples can be placed on the substrate holder 25 from the hole 200. The substrate handling element 28 extends into the pretreatment cavity 20 from an exterior of the pretreatment device 2 and can move horizontally to push the sample plate 30 into the reactor 1 through the passage 24 of the mating portion 23.
[0070] In one embodiment, a heat insulation element 213, such as including a fiberglass heat retaining wool is mounted on an outside of the top 211 of the pretreatment device 2 to reduce the heat dissipation. At the meantime, a stainless steel shell 214 can cover the heat retaining wool 213 in order to assemble conveniently and enhance an appearance of the pretreatment device 2.
[0071] Additionally, the samples are carried in different carrying areas of the substrate 300. The pretreatment gas introduced from the input passage 206 is relatively concentrated because limitation of the input passage 206. So, in this situation, it is preferred to disperse the gas so that the gas can flow through all the samples uniformly. Therefore, referring to Figs. 11-13, a guiding plate 26 formed with a plurality of guiding recesses 260 is disposed on the substrate holder 25 adjacent to the input passage 206. The guiding recesses 260 can disperse the pretreatment gas to the samples uniformly.
[0072] Accordingly, another guiding plate 27 can also be disposed on the substrate holder 25 adjacent to the output passage 207. A plurality of guiding recesses 270 are also formed to guide the unreacted gas and the production gases to flow to the output passage 207.
[0073] The input passage 206 and the output passage 207 face each other and are located approximately in a straight line. An extending direction of the substrate handling element 28 is perpendicular to the straight line. In order to push the sample plate 30 in/out of a position between the two guiding plates 26 and 27, two ends of each of the guiding plates 26 and 27 along the extending direction are formed with chamfer angles 261 , 271, 262 and 272 separately.
[0074] A method for pretreating the samples comprises:
(1). Positioning the samples: pushing the sample plate 30 carrying the substrate 300 into the pretreatment cavity 20 so that the sample plate 30 reaches an appropriate position between the two guiding plates 26 and 27 on the substrate holder 25, wherein position of the sample plate 30 is determined by movement of the substrate handling element 28;
(2). Pretreating the samples: driving the substrate holder 25 by the gas cylinder 4 to the first position, feeding a pretreatment gas, such as including hydrogen in this embodiment until the gas has a stable flow, then, setting heating temperature and pretreatment time to pretreat the samples;
(3). Transferring the samples: after the samples are pretreated, and driving the substrate holder 25 back to the second position by the gas cylinder 4; then, the substrate handling element 28 pushes the sample plate 30 into the reactor 1 through the passage 24 of the mating portion 23 for testing.
[0075] Because the pretreatment device 2 and the reactor 1 can communicate with each other, the pretreatment gas fed into the pretreatment device 2 may penetrate into the reactor 1 so as to disturb the subsequent tests in the reactor 1. Therefore, after the samples are moved into the reactor 1 , it may need to vacuum the testing system. Subsequently, a testing gas can be introduced into the reactor 1 to carry out the tests. Alternatively, the gate 210 (shown in Fig. 6), such as including a brake valve can be disposed in the mating portion 23 for controlling the communication of the pretreatment device 2 and the reactor 1. When the gate exists, only the reactor 1 may need to be vacuumed after closing the gate.
[0076] In this embodiment, a shielding setup 5 including three layers of mirror plates may be mounted under the substrate holder 25. Distances between edges of the mirror plates 5 and the sidewalls of the upper body 21 are so small that the pretreatment gas or the heat can be prevented from diffusing to a lower portion of the pretreatment cavity 20. Thus, elements in the lower portion of the cavity 20 can be avoided chemical changes or losses effectiveness. For example, it can prevent the gasket ring 202 from losing effectiveness.
[0077] Alternatively, the upper surface 250 of the substrate holder 25 for placing the substrate 300 can also be used as a shielding setup to limit the heat radiation in the gap by polishing or spreading some materials which can reduce the heat radiation on the upper surface. Additionally, referring to Fig. 11 , a water cooling tube 209 is disposed at a middle portion of the upper body 21 to forcibly decrease the heat conduction so as to improve security of the system.
[0078] Referring to Figs. 11 , 12 and 14, a flexible metal conduit connects the substrate holder 25 and the mirror plates 5. The substrate holder 25 can move with movement of the mirror plates 5. Because of flexibility of the metal conduit 205, the substrate holder 25 can attach the top 211 better in the first position. In one embodiment, a gas flow and pressure controller (not shown) may be disposed at a front end of the input passage 206. A thermocouple can be inserted into the gap from the output passage 207 to measure temperature of the pretreatment.
[0079] Figs. 17-28 illustrate diagrams of the reactor 1 in accordance with the preferred embodiment shown in Fig. 9. The reactor 1 can also have other configurations known in the arts.
[0080] Referring to Figs. 17-28, the reactor 1 is approximate in a cuboid shape. The reactor 1 comprises a top portion 150, a bottom portion 151 and a middle portion 152 locating between the top portion 150 and the bottom portion 151. The top, middle and bottom portions together define a reaction cavity (second region) 153 (shown in Figs. 18-19). A first, second and third driving devices 155,157 and 156 are installed on three sidewalls of the middle portion 152 separately. The driving devices 155, 157 and 156 are provided with step motors separately to drive relevant elements to move. In this embodiment, one side of the middle portion 152 on which the third driving device 156 is installed defines a window 11. A charge coupled device (CCD) 158 can be disposed outside the window 11. Other two opposite sides of the middle portion 152 are formed with a group of holes separately to accommodate some conduits 159. The conduits 159 may be used for controlling pressure, providing reactants, sampling products or connecting external electrical devices etc. Referring to Fig. 18, all the conduits 159 can be disposed at the middle portion 152. Alternatively, a part or all of the conduits 159 can also be disposed at the top portion 150 or the bottom portion 151.
[0081] Fig. 18 illustrates a schematic diagram of a reaction system including the reactor 1. The reactor 1 is the core of the reaction system. The reactor 1 comprises a probe 109 located in the reaction cavity 153 and a platform (substrate holder) 8 for holding the substrate 300 which carries the pretreated samples. The probe 109 and the platform 8 can move with respect to each other. In this embodiment, the probe 109 can move up and down, and the platform 8 can move along X, Y directions. As shown in Fig. 18, the reactants flow along a gaseous stop valve (not shown) and a filter (not shown) in turn to a mass flow controller (MFC) 160. Then, the reactants are introduced into the probe 109 via input conduits 118 disposed on the middle portion 152. Next, the reactants and the pretreated samples participate in reactions, while reaction products are sampled and sent to a vacuum chamber 6 via a sampling conduit 123. Finally, a measuring device 161 analyses the reaction products to get desired information. In order to prevent the product samples from blocking the sampling conduit 123, the sampling conduit 123 may need to be heated. In this embodiment, the measuring device 161 is a QMS, and distance between ionization filaments of the QMS and end of the sampling conduits can be adjusted. [0082] Meanwhile, unreacted reactants are discharged through the probe 109, output conduits 124 and a pressure flow controller (PFC) 162 in turn. The reaction cavity 153 and the vacuum chamber 6 can have independent pumps and valves (not shown) in order to satisfy their desired vacuum degree. A primary mechanical pump (not shown) and a molecular pump (not shown) can both be installed in the vacuum chamber 6 to satisfy higher vacuum degree. A primary mechanical pump (not shown) can be installed in the reaction cavity 153 to satisfy lower vacuum degree. In this embodiment, the input conduits 118 can be mainly used to feed reactants (generally gaseous reactants), while the reactants may be mixed with some impurities. The sampling conduit 123 can be mainly used to sample the reaction products, while the reaction products may be mixed with unreacted reactants etc. The output conduits 124 can be mainly used to discharge the unreacted reactants, while the unreacted reactants may be mixed with other gases.
[0083] Referring to Figs. 17 and 19, the bottom portion 151 of the reactor 1 is formed with a guiding portion 114 protruding upwardly and extending along the X direction. The platform 8 is installed on the guiding portion 114 moveably and comprises an upper/lower platforms moveably mounted together. Referring to Fig. 20, a stainless steel shaft (not shown) connects the second driving device 157 to the lower platform of the platform 8. So, the second driving device 157 can drive the lower platform to move along the Y direction on the guiding portion 114 by driving the steel shaft. A shaft 119 connects the second driving device 156 to the upper platform. So, the third driving device 156 can drive the upper platform to move along the X direction on the lower platform. Therefore, the driving devices 156 and 157 can cooperate with each other to drive the platform 8 to move along the X, Y directions. The reactor 1 defines an opening 112 on one side of the middle portion 152 opposite to the side on which the driving device 156 is installed. Referring to Fig. 9, the mating portion 23 of the pretreatment device 2 connects with the opening 112 so that the substrate 300 can be sent on the platform 8 from the opening 112.
[0084] Referring to Figs. 19-20, the reactor 1 is formed with a mounting portion 113. In this embodiment, the mounting portion 113 can be in a shaft shape and two ends thereof may be separately installed on the two opposite sides of the middle portion 152. A connecting portion connecting the two ends of the mounting portion 113 is suspended in the reaction cavity 153. Alternatively, the mounting portion 113 may be mounted on other positions of the middle portion 152 or be mounted on the bottom portion 151, or be mounted on both of the bottom portion 151 and the middle portion 152. In this embodiment, the mounting portion 113 can form a lead rail 115 in a middle position thereof. The lead rail 115 is formed with two rows of ball bearing (not shown). A supporting element 116 is moveably assembled on the lead rail 115. The probe 109 is installed on the supporting element 116. In this embodiment, the supporting element 116 may be adiabatic. Alternatively, the probe 109 can also be installed on the lead rail 115 directly.
[0085] A pair of hooks 1160 can be disposed at two sides of the supporting element 116 along the X direction separately. One ends of a pair of elastic elements 117, such as including springs connect the corresponding hooks 1160 and the other ends thereof connect the mounting portion 113. Alternatively, the hooks 1160 can also be disposed on the probe 109. The driving device 155 drives a contacting portion 111 by a connecting shaft 110, which connects the driving device 155 and the contacting portion 111. The contacting portion 111 contacts an upper surface of the probe 109. In this embodiment, the connecting shaft 110 and the contacting portion 111 connect and are independent with each other. Alternatively, they also can be unitary. The driving device 155 drives the contacting portion 111 to press the probe 109 downwardly, while the pair of springs 117 are stretched. When the driving device 155 returns, the contacting portion 111 releases the probe 109 and the probe 109 is pulled upwardly by restoring forces of the springs 117. Referring to Fig. 17, the CCD 158 located outside the window 11 is used to adjust distance between the probe 109 and the substrate 300 on the platform 8 so as to determine precise position between the probe 109 and the substrate 300.
[0086] Referring to Fig. 21, there illustrates a cross-sectional view of the probe 109 in accordance with the preferred embodiment of the present invention. The probe 109 is a critical element of the reactor 1 and has functions of feeding the reactants, sampling the products, balancing pressure and preventing impurities entering into a reaction room 133 (shown in Fig. 22).
[0087] Referring to Fig. 22-24, the probe 109 comprises a main body 125, a covering element 126 assembled under the main body 125 and a guiding portion 137. The main body 125 defines a pair of horizontal output passageways 127 arranged symmetrically. Two vertical output passageways 128 extend downwardly and run through the main body 125 from ends of the corresponding passageways 127 separately. The main body 125 further defines a sampling passageway 129 at an upper part thereof and a cut 1250 coaxial and connecting with the sampling passageway 129 at a lower part thereof. As shown in Fig. 23, the covering element 126 has a concave 140 recessed downwardly from a middle portion of an upper surface thereof. A bottom surface of the concave 140 may be approximately cone-shaped. A column hole 139 is recessed from a middle portion of the bottom surface of the concave 140 to connect with the reaction room 133 defined upwardly from a bottom surface of the covering element 126. The reaction room has a larger diameter than that of the column hole 139. In the meantime, the covering element 126 can have output holes 130 recessed from the upper surface thereof and input holes 131 recessed from a lateral of the bottom surface of the concave 140. A first groove 141 and a second groove 142 are defined upwardly from the bottom surface of the covering element 126 to connect with the input holes 131 and the output holes 130 separately. In this embodiment, the input holes 131 and the output holes 130 can be arranged annularly around the reaction room 133. Alternatively, the input holes 131 and the output holes 130 also can be arranged in a square configuration or a triangle configuration around the reaction room 133.
[0088] Referring to Fig. 24, the guiding portion 137 has an axial hole 138. Semicircle guiding passages 134 are formed on an exterior surface of the guiding portion 137 and extend along an axial direction. Alternatively, the guiding passages 134 can also be other configurations and extend along a curved-shaped. Combined with Fig. 21, the output passageways 127, 128 communicate with the output holes 130. The concave 140 and the cut 1250 of the main body 125 both define a receiving cavity. Because an end of the guiding portion 137 protrudes downwardly and fits well with the cone-shaped bottom surface of the concave 140, the guiding portion 137 can position in the receiving cavity easily without additional aiding methods. In this embodiment, the guiding portion 137 fits with the receiving cavity loosely, or it can also interfere with each other. The axial hole 138 of the guiding portion 137, the column hole 139 of the covering element 126, the reaction room 133 and the sampling passageway 129 of the main body are arranged coaxially and communicated. Meanwhile, the receiving chamber has a mixing chamber 136 above the guiding portion 137 and a sidewall of the mixing chamber 136 defines feeding passageways 135.
[0089] Referring to Figs. 20-21, the input conduits 118 are received in the corresponding passageways 135. The sampling conduit 123 passes through the sampling passageway 129, the axial hole 138 and the column hole 139 so as to communicate with the reaction room 133. The output conduits 124 are received in the corresponding output passageways 127. Alternatively, the sampling conduit 123 can be capillary which has a diameter of 10-lOOum to adapt pressure difference between the reaction cavity 153 and the vacuum chamber 6. Meanwhile, a length of the capillary can be adjusted according to specific reactions.
[0090] When testing, the pressure of the reaction cavity 153 may need to reach demand of reaction pressure, and the reactants are provided stably. Then, the driving devices 155, 156 and 157 drive the platform 8 and the probe 109 to reach a predetermined position. The CCD 158 monitors the distance between the probe 109 and the substrate 300 so as to adjust it. Next, the reactants are fed into the mixing chamber 136 from the input conduits 118 to be mixed. The mixed reactants flow through the guiding passages 134 of the guiding portion 137 to get into the input holes 131, wherein the input holes 131 has a function of distributing the reactants. Subsequently, the reactants enter into the first groove 141 and are mixed again. Finally, a small part of reactants enter into the reaction room 133 to contact with the samples for testing. The reaction products are sampled by the sampling conduit 123 and are sent into the vacuum chamber 6 to analyze by the QMS 161. In the meantime, a large part of the reactants flow into the second groove 142 and are discharged through the output holes 130, the output passageway 128 and the output conduit 124 in turn.
[0091] In the reactor 1, the reaction cavity 153 may need to be full of an environment gas, which is normally an inert gas, such as Ar to reach a predetermined pressure in the reaction cavity 153. Referring to Fig. 25, the MFC 160 is disposed on the input conduits 118 to control flow capacity of the reactants. A MFC 163 controls flow capacity of the environment gas. The PFC 162 is disposed on the output conduits 124 to control the pressure in the reaction cavity 153.
[0092] During the tests, when partial pressure of the reactants is equal to the pressure of the environment gas in the reaction cavity 153, pressure in the reaction room 133 and the pressure in the cavity 153 can reach a balance so that effect of the environment gas on the reactants in the reaction room 133 is minished. In the meantime, the reactants flowing out of the first groove 141 can form a gas barrier to prevent the environment gas from influencing the reactions reacted in the reaction room 133. Obviously, pressure balance between the reaction room 133 and the cavity 153 is important.
[0093] Referring to Fig. 25, entrances of the output holes 130 are defined in the probe 109 and are near the reaction room 133. Generally, because of limitations of machining process, inspecting, controlling and system cost, the distance between the probe 109 and substrate 300 is in a micrometer lever, such as including 10-20um. Exhaust of the unreacted reactants is mainly controlled by the PFC 162. When the flow capacity of the reactants is small, such as l-2ml/m, the pressure balance in the reaction room 133 may not be controlled easily because flow capacity of the PFC 162 is normally large, such as 500ml/m. Therefore, another pressure control system may need to be provided when the pressure balance is not controlled yet by adjusting controlling parameters of the PFC 162.
[0094] Fig. 26 illustrates a schematic diagram of another pressure control system, which can solve the pressure control problem when the flow capacity of the reactants is small. In this embodiment, the PFC 162 can control the pressure of the environment gas in the reaction cavity 153. A MFC 163 controls a flow rate of the environment gas in the reaction cavity 153. The pressure balance and the exhaust of the unreacted reactants are controlled by a MFC 164. Flow capacity Q of the MFC 164 is approximate to the flow capacity Qresource of the reactants controlled by the MFC 160. Generally, Q=IO* Qresource. Alternatively, the MFC 164 can be substituted by a conduit having a larger flow resistance, such as including a capillary. A value of the flow capacity of the MFC 164, and a diameter and a length of the capillary are related to parameters, such as including the environment pressure in the reaction cavity 153 and the height of the probe 109 etc.
[0095] In the reaction system in which the reactor 1 locates, there are several subsystems to cooperate to ensure successful operation of the reaction system. Referring to Fig. 27, there illustrates a schematic diagram of functional modules (subsystems) of the reaction system. The reaction system comprises a controlling system module 40, a motion/position module 49, a heating module 42, a pump/valve module 45, a source distributing module 46, the reactor 1, a product analysis module 43 and a data manipulation module 44. The controlling system module 40 can control operation of the reactor 1 by controlling the motion/position module 49, the heating module 42, the pump/valve module 45 and the source distributing module 46. The products in the reactor 1 are sent into the analysis module 43 to get data. The data are sent to the date manipulation module 44 to be manipulated to get desired information.
[0096] Referring to Fig. 28, a flow chart of the test in the reactor 1, comprises
a). Initialization 50, which includes loading initializing files of the reaction system, inspecting/starting up the vacuum system, inspecting the gas source, inspecting and heating the capillary etc.;
b). Loading the substrate 51, which includes sending the substrate 300 carrying the pretreated samples into the reactor 1 ;
c). Cleanout 52, which includes charging the environment gas into the reactor 1 to reach the predetermined pressure and then vacuumizing the reactor 1 some times to clean the reactor 1 ;
d). Positioning 53, which includes setting the pressure in the reactor 1 and original position of the probe 109 and the platform 8;
e). Setting testing processes 54, which includes setting parameters of the reactant gas, the reaction cavity and the flow controllers separately, setting heating curves, reaction routes, inspecting the flow capacity of the gas source, a heating system (shown in Fig. 39) and a cooling system etc.;
f). Monitoring in real time 55, which includes monitoring reaction conditions, figures from the CCD and status of the substrate, and examining reaction results etc.; g). Ending the test; and
h). Unloading the samples.
[0097] A selected usage of the reactor 1 is provided to test activities of different amounts of CuO during oxygenation of CO: Test conditions: 1. CO : 4.7 %
2. 02: 7.1 %
3. Ar: 88.2 %
4. Overall flow rate : 17 ml/min
5. Heating the catalyst CuO to 400 "C from a room temperature.
6. the substrate is calcined at 650 "C .
Test results: different amounts of the CuO have important effects on conversions of the CO. The activities of CuO increase with the incremental amount of the CuO.
[0098] Alternatively, a reactor (not shown) in accordance with one embodiment of the present invention, comprises a top portion, a bottom portion opposite to the top portion and a middle portion connecting the top portion and the bottom portion, commonly defining a reaction cavity. Wherein at least a reactant input conduit is disposed in the middle portion of the reactor.
[0099] Thus, reactant gases are fed into the reaction cavity to contact with the samples located in the reactor. The products are kept in the reactor and an exterior spectrometric detector can be used to measure the characteristics of the products, such as described in PCT/CN2006/000945 of the same applicants.
[0100] In the test system, light sources may need to be used to illuminate the tests, for example illumination during heating, lighting, inspecting or measuring etc. Referring to Figs. 29-33, in a preferred embodiment of the present invention, the light sources are used on a reactor. Alternatively, the light sources can also be used on the pretreatment device under certain conditions.
[0101] Referring to Figs. 29-31, there illustrate a schematic diagram of the light sources and the reactor, such as including the preferred reactor 1 shown in Fig. 18. The reactor 1 comprises a reaction cavity 153 in which the samples are tested. The reaction cavity 153 has a first opening 60. A first light source 71 is disposed outside the reaction cavity 153 to generate a first light beam. A second light source 72 is disposed outside the reaction cavity 153 to generate a second light beam. The reactor 1 is configured to select among the group consisting of (1) the first light source, (2) the second light source, and (3) both of the first and the second light sources 71 and 72 to illuminate the reaction cavity 153 through the first opening. In this embodiment, the bottom 151 of the reactor 1 defines a first opening 60. The sentence of "either or both of the first and the second light sources 71 and 72 to illuminate the reaction cavity 153 through the first opening 60" means: a), only the first light beam passes through the first opening; b) only the second light beam passes through the first opening; c) the first light beam and the second light beam both pass through the first opening simultaneously or asynchronously.
[0102] The substrate 300 carries the sample 302, 303 and 304. Referring to Figs. 29-31, In situations a) and b), only the first light beam generated from the first light source 71 or only the second light beam generated from the second light source 72 passes through the opening 60 to handle the sample 302, such as including heating, lighting or inspecting etc. In situation c), the light beams generated from the first/second light sources 71 and 72 can handle different samples 303 and 304, or can handle the same one sample.
[0103] Additionally, referring to Figs. 29 and 30, light routes of the first light beam and the second light beam can be independent or be coincident partly with each other. The first light beam and the second light beam can enter into the reaction cavity 153 directly. Or an additional element, such as including a reflecting mirror or a convex mirror etc. is disposed to adjust the light route. According to different light beams, the mirror is made of different materials.
[0104] Figs. 32-33 illustrate the light sources and the reactor 1 in accordance with another embodiment of the present invention. The reactor 1 defines the first opening 60 and a second opening 61 on the bottom portion 151 thereof. The first light source 71 and the second light source 72 can illuminate the reaction cavity 153 through the first opening 60 and the second opening 61 separately. Thus, there are two situations that the first light source 71 and the second light source 72 handle the samples selectively:
a). Referring to Fig. 32, the first light beam of the first light source 71 and the second light beam of the second light source 72 handle the different samples 303 and 304 from the openings 60 and 60 separately.
b). Referring to Fig. 33, the first light beam and the second light beam can handle the same sample 302 from the different openings.
[0105] In above situations, the first light source 71 and the second light source 72 can handle the same one/two sample(s) simultaneously or asynchronously. Or one light source works, another light source does not work.
[0106] In one embodiment, the first light beam and the second light beam can includes laser or infrared lights for heating the sample. Alternatively, a light emitting diode (LED) can also be used to illuminate.
[0107] Materials for generating the laser have some types, such as including solids, gases, semiconductors and free electrons etc. The solid laser is generated by a material bar selected specially, such as including a ruby laser or a sapphire laser etc. The gas laser, such as including CO2 Laser whose wavelength is 1036nm is emitted by activating gas atoms which have discharge properties. The semiconductor laser, such as a diode laser whose wavelength is 808nm is generated by a laser generator. The laser generator is formed by connecting two pieces of semiconductor materials. The two semiconductor materials are treated in different processes to contain different impurities. When a great deal of electricity passes this generator, the laser is emitting from connection of the two semiconductor materials.
[0108] To free electron laser, firstly, the free electrons are derived from a specific accelerator or other energy devices. Then, they are accelerated to light velocity by an undulator which is formed by linearity electromagnetic. Thus, the free electrons can emit energy in a fashion of a synchronous acceleration ray so that the free electron laser is formed. Additionally, a density and a wavelength of the ray can be adjusted by changing a girth of its magnetic field. A range of the wavelength of the ray can be adjusted from the microwave to the ultraviolet.
[0109] Based on different tests, different types of light beams may be used. In one embodiment, the substrates are made of different materials because of different light beams. Or appropriate light beams can be selected after determining the substrate. The different light beams with different wavelengths can be selected as long as the selected light beams can not damage the substrate and ensure the operations of the tests.
[0110] In one embodiment, the substrate may be made of silica or quartz. When the substrate is quartz, the diode laser or the LED can be used. When the substrate is silica, the CO2 laser or light beams whose wavelength are small than 1036nm, such as including the diode laser or the LED etc. can be used.
[0111] Generally, the reactor may need to be sealed when the tests are operating. Therefore, a first light transmission element and a second light transmission element can be accommodated in the first opening 60 and the second opening 61 separately. The light transmission elements may be made of glass or other materials. It is preferred that the light transmission are made of the glass, and the first/second light transmission elements are the same or different. In one embodiment, glass materials of the first/second light transmission elements are different to adapt the first/second light beams with different wavelengths.
[0112] There are many different glass materials, which can comprise: a), a silicate glass whose main composition includes SiO2; b). an oxide glass whose main composition may includes B2O3 ^ P2O5^ Al2O3 ^ GeO2^ TeO2 or V2O5 etc.; c). a non-oxide glass whose main composition can be sulphur series compounds or a halide etc.; d). a metal glass formed by quickly cooling some alloys.
[0113] In one embodiment, the first opening and the second opening can accommodate a SiO2 glass sheet or a ZnSe glass sheet. When the light beam is CO2 laser, the ZnSe glass sheet can be used. When the light beam is the diode laser or the LED, the SiO2 and the ZnSe glass sheets can both be used.
[0114] Additionally, the reactor 1 may define a third opening for a third light beam passing through. Positions of the first opening, the second opening or the third opening can be the same or different. The same position means the first opening, the second opening and the third opening are all defined on the same one of the top, middle and bottom portions.
[0115] When operating, the first, second and third beams can pass through the first opening, the second opening and the third opening separately to handle the sample(s) on the carrying area(s). Thus, handling situations comprise:
a), the three light beams handle the same one sample simultaneously;
b). when handling every time, two of the three light beams handle the same one sample simultaneously, and the remaining one beams handles another sample which is at the same time or asynchronous with the former two light beams;
c). when handling every time, three light beams handle the samples on three different carrying areas simultaneously or asynchronously.
[0116] The phrase "every time" means all of the light beams which are working complete to handle the sample(s) one time. For example, when there are two working light beams, the phrase "every time" means the two light beams both complete to handle the corresponding sample(s).
[0117] In one embodiment, the first, second, third light beams can be the diode laser, the CO2 laser or the LED. For example, the first light beam may be the diode laser, the second light beam may be the CO2 laser and the third light beam may be the LED. Alternatively, the reactor can also define a fourth opening or a fifth opening etc. for a fourth light beam and a fifth light beam passing through. Thus, there may be different combinations of the light beams and the openings to handle the samples, such as including the combination of the three light beams and the three openings described above.
[0118] In order to prevent the light beams from reflecting so as to weaken the incident light beams, the glass sheets may be coated with antireflection coatings. Meanwhile, the openings may be coated with a black color or machined coarsely to absorb a part of reflected lights. Additionally, a seal groove (shown in Fig. 35) can be disposed in the corresponding opening to accommodate a seal element including an O- shaped gasket.
[0119] Referring to Figs. 34-37, there illustrate schematic diagrams of openings of the reactor 1 in accordance with a preferred embodiment of the present invention. Additionally, configurations of any one of the openings shown in Figs. 29-33 can be the same as/similar to configurations of the openings shown in Figs. 34-37.
[0120] Referring to Figs. 34-36, the reactor 1 defines a first opening 81 , a second opening 82 and a third opening 80 which downwardly run through the bottom portion 151 thereof from an inner surface of the bottom portion 151. The first, second and third openings 81, 82 and 80 comprise a first opening portions 811, 821 and 801 recessed downwardly from the inner surface, a third opening portions 813, 823 and 803, and a second opening portions 812, 822 and 802 connecting the first opening portions and the second opening portions separately. The first, second and third opening portions 801, 802 and 803 of the third opening 80 extend downwardly along a direction perpendicular to the inner surface. The first, second and third opening portions 811, 821, 812, 822, 813 and 823 extend slopingly from the inner surface. In one embodiment, the inner surface of the bottom portion 151 is a horizontal surface.
[0121] The first opening portions of the openings can be recessed downwardly from the inner surface or from an outer surface opposite to the inner surface. The reactor has a mounting surface which can be the inner surface or the outer surface from which the first opening portions are recessed directly. The light transmission elements, such as including the glass sheets are placed into the corresponding openings from the mounting surface. In one embodiment, the mounting surface is the inner surface of the reactor 1.
[0122] Generally, the size of the reactor 1 may be relatively small. When the three light beams pass through the three openings to handle the same one sample, the openings may be so compact that the first opening portions 811 and 801 or 821 and 801 may interfere with each other. Additionally, directions of fixing forces for fixing seal gaskets and the glass sheets are generally perpendicular to the inner surface of the bottom surface. However, in this embodiment, the seal gaskets or the glass sheets are placed slopingly in the first opening portions 811 and 821. So, the fixing forces exerting on the seal gaskets or the glass sheets may not balance so as to influence the tests in the reactor 1.
[0123] Therefore, referring to Figs. 37-38, the reactor 1 defines a first opening 91, a second opening 92 and a third opening 90 which run through the bottom portion 151 thereof. The first opening 91 and the second opening 92 are located at two sides of the third opening 90. The first, second and third openings 91, 92 and 90 comprise a first opening portions 911, 921 and 901 recessed downwardly from the inner surface of the bottom portion 151, a third opening portions 913, 923 and 903, and a second opening portions 912, 922 and 902 connecting the first opening portions and the second opening portions separately. In the meantime, the first, second and third opening portions 901, 902 and 903 have the same extending direction E. That is, angles among the extending directions of the first, second and third opening portions 901, 902 and 903 are zero degree. In this embodiment, the direction E is perpendicular to the inner surface of the bottom portion 151.
[0124] An extending direction A of the first opening portion 911 of the first opening 91 is parallel to the extending direction E of the third opening 90. The second and third opening portions 912 and 913 have the same extending direction B. The extending direction B has an acute angle, such as including 30 degrees with the extending direction A. An extending direction C of the first opening portion 921 of the second opening 92 is also parallel to the extending direction E of the third opening 90. The second and third opening portions 922 and 923 have the same extending direction D. The extending direction D has an acute angle with the extending direction C. Distances from every spots of bottom surfaces of the first opening portions 911, 921 and 901 to the inner surface of the bottom portion 153 are dl, d2 and d3. It is preferred that dl=d2=d3.
[0125] The seal grooves for receiving the O-shaped gaskets 33 are recessed downwardly from laterals of the first opening portions 911 , 921 and 901. The glass sheets (not shown) may be placed in the first opening portions 911 , 921 and 901. In this situation, the distances from every spots of each of the bottom surfaces of the openings to the inner surface of the bottom portion 151 are the same. So the fixing forces exerting on the glass sheets and the gaskets 33 are balance and uniform so that leakage can be avoided.
[0126] Fig. 38 illustrates a configuration similar as the diagram shown in Fig. 37. The difference is that the second opening 92 further defines a fourth opening portion 924 connecting the second opening portion 922 and the third opening portion 923.
[0127] In one embodiment, the testing system may have a laser heating system to generate a laser to heat the samples on the substrate 300. Referring to Fig. 39, a temperature control loop of the laser heating system comprises an infrared thermometer 62, a PID controller 63, a laser controller 64 and a laser generator 65. The infrared thermometer 62 inspects temperatures of the tests and converts temperature signals to electrical signals which are 4-2OmA. The electrical signals are sent into the PID controller 63. Meanwhile, a CCD 66 transmits figures of the carrying areas of the substrate 300 to a computer 67 to determine heating positions. The computer 67 controls the PID controller 63. The PID controller 63 sends its output signals to the laser controller 64 to control power of the laser generator 65, which is 0-95%. An electrical source module 68 controls the opening/closing of the laser generator 65. The chilling system 69 is for cooling the laser generator 65.
[0128] As shown in Figs. 35 and 37, heating systems can selectively heat the samples from the first openings 81, 91, the second openings 82, 92 or the third openings 80, 90. In one embodiment, the CO2 laser passes through the third openings 80, 90 to heat the samples. The diode laser passes through the first openings 81, 91 to heat the samples. The light emitting diode is disposed near the second openings 82, 92 for illuminating the reaction cavity 153 of the reactor 1. Either or both of the diode laser and the CO2 laser can be opened. In the meantime, the light emitting diode may work or not work.
[0129] While the present invention has been illustrated and described with reference to some preferred embodiments, the present invention is not limited to these. Those skilled in the art should recognize that various variations and modifications can be made without departing from the spirit and scope of the present invention as defined by the accompanying claims.

Claims

1. A testing system for testing a plurality of samples on a substrate comprising: an enclosed cavity having a first region and a second region; a pretreatment unit provided to pretreat the samples while the substrate is in the first region; and a test unit provided to receive the substrate after the samples are pretreated and to test the samples while the substrate is in the second region, the test unit including a test mechanism for determining characteristics of the samples while the substrate is in the second region.
2. The testing system as described in claim 1, wherein the pretreatment unit includes a heating mechanism to heat the samples.
3. The testing system as described in claim 2, wherein the pretreatment unit further comprises a substrate holder for holding the substrate, the substrate holder is moveable.
4. The testing system as described in claim 3, wherein the pretreatment unit further comprises a shielding setup for keeping the heat generated by the heating device in the first region.
5. The testing system as described in claim 1 , wherein the test mechanism includes a probe to test the samples on the substrate.
6. The testing system as described in claim 5, wherein the samples are catalyst samples and the probe is a probe for testing catalysts samples.
7. The testing system as described in claim 1, further comprising a substrate handling element to move the samples from the first region to the second region.
8. The testing system as described in claim 1 , wherein the sample testing system further comprises a gate to control communication between the first region and the second region
9. A sample testing system comprising: a pretreatment unit including a substrate holder to hold a substrate carrying a plurality of samples and a pretreating mechanism to pretreat the samples; and a test unit coupled to the pretreatment unit, the test unit to receive the substrate from the pretreatment unit, the test unit including a test mechanism to determine characteristics of the samples while the substrate is situated in the test unit.
10. A sample testing system as described in claim 9, wherein the pretreating mechanism includes a passage for introducing a pretreatment gas into the pretreatment unit and a heating device to heat the samples, and wherein the test mechanism includes a probe.
11. A sample testing method for testing samples on a substrate, comprising: pretreating the samples in a pretreatment unit; moving the substrate from the pretreatment unit to a testing unit through a channel coupling the pretreatment unit to the testing unit such that the samples are not exposed to the atmosphere after being pretreated in the pretreatment unit and before being tested in the testing unit; and testing samples in the testing unit, wherein testing sample includes determining characteristics of the samples while the substrate is in the testing unit.
12. A reactor for testing samples, comprising: a top portion, a bottom portion for holding a substrate carrying a plurality of samples, and a middle portion disposed between the top portion and the bottom portion, the top, middle and bottom portions together defining a reaction cavity; a probe disposed in the reaction cavity and mounted on at least one of the middle portion and the bottom portion; and conduits connected to the probe for transferring materials into and out of the reaction cavity.
13. The reactor as described in claim 12, wherein the reactor has a mounting portion disposed on the middle portion thereof and the probe is installed on the mounting portion.
14. The reactor as described in claim 13, wherein two ends of the mounting portion are installed on the middle portion and a connecting portion connecting the two ends is suspended in the reaction cavity, the probe is installed in the connection portion of the mounting portion.
15. The reactor as described in claim 13, wherein the bottom portion includes a substrate holder for holding the substrate, and wherein the probe is configured to move with respect to the substrate holder to test the plurality of samples in succession.
16. The reactor as described in claim 12, wherein the samples are catalysts and the probe is a probe for testing catalysts.
17. The reactor as described in claim 12, wherein the conduits include at least two of an input passage, an output passage and a sampling passage, and wherein the conduits run through the middle portion.
18. A reactor for testing samples, comprising: a reaction cavity for testing samples therein, the reaction cavity having a first opening; a first light source disposed outside the reaction cavity to generate a first light beam; and a second light source disposed outside the reaction cavity to generate a second light beam, wherein the reactor is configured to select among the group consisting of (1) the first light source, (2) the second light source, and (3) both of the first and the second light sources, to illuminate the reaction cavity through the first opening.
19. The reactor as described in claim 18, wherein the reaction cavity has a second opening, and the reactor is further configured to select both of the first and second light sources to illuminate the reaction cavity through the first and second openings respectively.
20. The reactor as described in claim 19, wherein the reaction cavity has a third opening, and a third light source is disposed outside the reaction cavity to generate a third light beam to pass through the third opening, the first, second and third light sources are a diode laser, a CO2 laser and a light emitting diode, respectively.
21. The reactor as described in claim 18, wherein a SiO2 glass sheet and a ZnSe glass sheet are installed in the first and second openings, respectively.
PCT/CN2007/070824 2006-09-30 2007-09-29 System and method for sample testing WO2008043303A1 (en)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
CN200610139043 2006-09-30
CN200610139043.3 2006-09-30
CN200610173356.0 2006-12-29
CN200610173356 2006-12-29
CN200610130890 2006-12-29
CN200610130890.3 2006-12-29

Publications (1)

Publication Number Publication Date
WO2008043303A1 true WO2008043303A1 (en) 2008-04-17

Family

ID=39282427

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2007/070824 WO2008043303A1 (en) 2006-09-30 2007-09-29 System and method for sample testing

Country Status (1)

Country Link
WO (1) WO2008043303A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140373642A1 (en) * 2011-12-28 2014-12-25 Hitachi High-Technologies Corporation Sample pretreatment system that supports multisystem configuration

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030003017A1 (en) * 2001-06-29 2003-01-02 Symyx Technologies, Inc. In-situ injection and materials screening device
US6689613B1 (en) * 1999-03-31 2004-02-10 General Electric Company Method for preparing and screening catalysts
US7078164B1 (en) * 2000-06-19 2006-07-18 Symyx Technologies, Inc. High throughput screen for identifying polymerization catalysts from potential catalysts
WO2006119708A1 (en) * 2005-05-11 2006-11-16 Accelergy Shanghai R & D Center Co., Ltd A combinatorial screening method for formulating processes and the apparatus thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6689613B1 (en) * 1999-03-31 2004-02-10 General Electric Company Method for preparing and screening catalysts
US7078164B1 (en) * 2000-06-19 2006-07-18 Symyx Technologies, Inc. High throughput screen for identifying polymerization catalysts from potential catalysts
US20030003017A1 (en) * 2001-06-29 2003-01-02 Symyx Technologies, Inc. In-situ injection and materials screening device
WO2006119708A1 (en) * 2005-05-11 2006-11-16 Accelergy Shanghai R & D Center Co., Ltd A combinatorial screening method for formulating processes and the apparatus thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140373642A1 (en) * 2011-12-28 2014-12-25 Hitachi High-Technologies Corporation Sample pretreatment system that supports multisystem configuration
US9632100B2 (en) * 2011-12-28 2017-04-25 Hitachi High-Technologies Corporation Sample pretreatment system that supports multisystem configuration

Similar Documents

Publication Publication Date Title
US6602714B1 (en) Viscosity and mass sensor for the high-throughput synthesis, screening and characterization of combinatorial libraries
CA2679733C (en) Automated analyzer using light diffraction
EP0446859B1 (en) Chemical luminescence-detecting apparatus
Van Rijn et al. Ultrahigh vacuum/high-pressure flow reactor for surface x-ray diffraction and grazing incidence small angle x-ray scattering studies close to conditions for industrial catalysis
TWI385715B (en) Advanced mixing system for integrated tool having site-isolated reactors
US7033840B1 (en) Reaction calorimeter and differential scanning calorimeter for the high-throughput synthesis, screening and characterization of combinatorial libraries
CN101173953A (en) System and method for sampling tests
CA2562838A1 (en) Smart combinatorial operando spectroscopy catalytic system
CN112226350A (en) Centrifugal nuclear extraction and amplification integrated system and detection method
AU1064200A (en) Method and apparatus for screening catalyst libraries
US20220373524A1 (en) Device and Method for Determination of a Catalyst State in a Chemical Reactor
EP4010679A1 (en) High throughput radiochemistry system
WO2008043303A1 (en) System and method for sample testing
KR20170005401A (en) Analysis device
US7052914B2 (en) Automated method for examining catalytic and spectroscopic properties of the components of combinatorial libraries
CN105823820A (en) Catalyst evaluating apparatus
US7255474B2 (en) Parallel infrared spectroscopy apparatus and method
CN214735762U (en) Centrifugal nuclear extraction and amplification integrated system
CN101769907B (en) Differential automatic test system for photocatalytic reaction
WO2019118369A1 (en) Systems for a modular multi-wavelength absorbance detector
KR20040039172A (en) Device for performing catalytic screening
CN109682847B (en) High-flux material synthesis and synchrotron radiation light source high-flux characterization method of combined material chip
TWI751412B (en) Inline chamber metrology
CN108261991A (en) Reactor
Maier et al. Combinatorial chemistry of materials, polymers, and catalysts

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 07817015

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 07817015

Country of ref document: EP

Kind code of ref document: A1