CN110018221A - A kind of test device of the metal cluster of chemical modification - Google Patents

A kind of test device of the metal cluster of chemical modification Download PDF

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Publication number
CN110018221A
CN110018221A CN201910196771.5A CN201910196771A CN110018221A CN 110018221 A CN110018221 A CN 110018221A CN 201910196771 A CN201910196771 A CN 201910196771A CN 110018221 A CN110018221 A CN 110018221A
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heater
sample
reaction chamber
pulse valve
ring electrode
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张珊珊
黄亚玲
高晴
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Jinhua Polytechnic
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Jinhua Polytechnic
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

The present invention relates to new material research and development technology fields, a kind of test device of the metal cluster of chemical modification, including rotating base, cluster generator, specimen holder, sample, pulse valve, air accumulator, droplet ejection source, laser, quadrupole rod mass spectrum, ion trap, detector, vacuum chamber and computer, rotating base and specimen holder all have magnetism, and rotating base is able to drive specimen holder and rotates around x axis;Ring electrode and heater are respectively positioned in reaction chamber, and ring electrode is ring-type, can apply the voltage of highest 5000V on ring electrode, and heater is cylindrical shape, and the potential of heater remains 0V, and the central axis of ring electrode, the central axis of heater and tubule are coaxial;There is reaction chamber outlet and outlet to be located in vacuum chamber, and the laser of laser transmitting can enter reaction chamber by the outlet, and enter sample cavity by tubule, to be mapped on sample;Droplet ejection source has jet port, and jet port can eject superfluid helium droplet, and the superfluid helium droplet temperature is lower than 2.8K.

Description

A kind of test device of the metal cluster of chemical modification
Technical field
It is especially a kind of for generating the metal of chemical modification under gas phase the present invention relates to new material research and development technology field The test device of cluster and a kind of metal cluster for the chemical modification tested.
Background technique
The metal cluster as made of tens or several hundred a metallic atom aggregations is that one in current new material research is important Aspect, can be applied to many technical fields, such as environmental protection, new energy, new material, pulse-laser deposition method is to prepare metal group A kind of common method of cluster, and further chemical modification is carried out to metal cluster and generallys use reaction gas and metal cluster The method of interaction is so that certain chemical groups in reaction gas are combined with metal cluster.Prior art defect be During pulse-laser deposition forms metal cluster, since the heat that laser light incident to metal sample target surface generates can unevenly be led Cause the size difference of the metal cluster generated larger, furthermore, in the process for needing to carry out metal cluster subsequent chemical modification In, if during reaction gas has participated in pulse-laser deposition, will lead to and generate other products, in addition, passing through pulse-laser deposition The internal temperature that method forms metal cluster is higher to be not sufficiently stable, and is easy to decompose during follow-up test, therefore need Follow-up test, a kind of metal group of chemical modification are carried out again after wanting the carrier of external low temperature to carry out certain cooling to it The test device of cluster is able to solve problem.
Summary of the invention
To solve the above-mentioned problems, the present invention is using rotatable specimen holder and the confession of special carrier gas and reaction gas Gas method, and metal cluster is embedded into low temperature superfluid helium droplet in carry out subsequent measurement experiment.
The technical scheme adopted by the invention is that:
A kind of test device of the metal cluster of chemical modification includes rotating base, cluster generator, specimen holder, sample Product, pulse valve I, air accumulator I, pulse valve II, air accumulator II, droplet ejection source, laser, quadrupole rod mass spectrum, ion trap, detection Device, vacuum chamber and computer, pulse valve I, pulse valve II and the equal cable connection computer of detector, can be controlled by computer Pulse valve I is opened or closed with pulse valve II's, and cluster generator includes cavity, sample cavity, air inlet pipe I, tubule, air inlet pipe II, reaction chamber, ring electrode and heater, xy z are three-dimensional coordinate system, and ring electrode is circumscribed with voltage source, and heater is circumscribed with One end of current source, cluster generator has rotating base, and the sample cavity, tubule and reaction chamber are sequentially connected and are respectively positioned on chamber In vivo, one end of air inlet pipe I is connected to sample cavity, the other end is located at the outside of cavity and is connected to pulse valve I, and pulse valve I is logical It crosses tracheae and is connected to air accumulator I, store carrier gas in air accumulator I;One end of air inlet pipe II is connected to the side of tubule, the other end Positioned at cavity outside and be connected to pulse valve II, pulse valve II is connected to air accumulator II by tracheae, stores in air accumulator II There is reaction gas;Sample is fixed on specimen holder and is respectively positioned in sample cavity;Vacuum chamber has the window that can penetrate laser;Rotation Turn pedestal and specimen holder all has magnetism, rotating base is able to drive specimen holder and rotates around x axis;Ring electrode and heater are respectively positioned on In reaction chamber, ring electrode is ring-type, and heater is cylindrical shape, and the central axis of ring electrode, the central axis of heater and tubule are coaxial And in the x-direction, 5000 volts of highest of voltage can be applied on ring electrode, the potential of heater remains zero volt;Reaction chamber tool There is outlet, the outlet is located in vacuum chamber and the outlet towards x positive direction, ring electrode and heater apart from reaction chamber is respectively 10 centimetres and 2 centimetres, the laser of laser transmitting can enter reaction chamber by the outlet, and enter sample by tubule Chamber, to be mapped on sample;Droplet ejection source, quadrupole rod mass spectrum, ion trap and detector are arranged successively along y negative direction and equal position In in vacuum chamber, droplet ejection source has jet port, and it is micro- to eject superfluid helium to y negative direction by the jet port Drop, the superfluid helium droplet temperature are lower than 2.8K, and the helium atom number for including in each superfluid helium droplet arrives for 10000 20000, jet port of the axis of reaction chamber outlet between droplet ejection source and quadrupole rod mass spectrum and with droplet ejection source Axis in x/y plane be in an angle of 90 degrees.Sample is metal;The internal diameter of air inlet pipe I is 2mm, and the internal diameter of air inlet pipe II is 1.6mm; The internal diameter of tubule is 2mm, length 15mm;The internal diameter of heater is 6mm, and the diameter of the outlet of reaction chamber is 2mm.
The step of preparing the metal cluster of chemical modification and it measured:
Step 1 controls opening or closing for pulse valve I and pulse valve II by computer, so that carrier gas and reaction gas It is filled with sample cavity and tubule respectively, and the air pressure in sample cavity is made to be consistently greater than the air pressure in reaction chamber;
Step 2 makes rotating base that specimen holder and sample be driven to rotate around x axis, and applies voltage to ring electrode, opens heating Device;
The laser of step 3, laser transmitting passes sequentially through vacuum chamber, reaction chamber and tubule, into sample cavity and is mapped to sample On product, so that sample surfaces partial melting, sample atoms form metal cluster and move with carrier gas into tubule;
Step 4, metal cluster move in reaction chamber with carrier gas, and interact with reaction gas, generate chemical modification Metal cluster, and with carrier gas from reaction chamber outlet enter vacuum chamber;
Step 5, droplet ejection source eject superfluid helium droplet to y negative direction, into the part chemical modification of vacuum chamber Metal cluster and part superfluid helium droplet mutually collide and are embedded into superfluid helium droplet, so that the metal cluster of chemical modification Temperature decline;
Step 6, the metal cluster for being embedded into the chemical modification in superfluid helium droplet are transported with superfluid helium droplet to y negative direction It is dynamic, and quality selection is carried out by quadrupole rod mass spectrum, meet the metal cluster of the chemical modification of mass number needed for experiment measures after Continue and moved to y negative direction, and by eventually entering into detector after ion trap;
Collected related data is inputted computer by step 7, detector, and computer obtains chemistry after treatment and repairs The relevant information of the metal cluster of decorations.
The beneficial effects of the present invention are:
Apparatus of the present invention metal sample when carrying out laser and melting steaming is heated evenly under laser, the ruler of the metal cluster of generation Very little difference is smaller, and the gas-supplying structure with special carrier gas and reaction gas, avoids generating other products, moreover, using low The superfluid helium droplet of temperature is cooling to metal cluster, so that metal cluster structure in subsequent measurement experiment is more stable.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic top plan view of the present invention.
In figure, 1. rotating bases, 2. cluster generators, 2-1. cavity, 2-2. sample cavity, 2-3. air inlet pipe I, 2-4. be thin Pipe, 2-5. air inlet pipe II, 2-6. reaction chamber, 2-7. ring electrode, 2-8. heater, 3. specimen holders, 4. samples, 5. pulse valve I, 6. Air accumulator I, 7. pulse valve II, 8. air accumulator II, 9. droplet ejection sources, 10. lasers, 11. quadrupole rod mass spectrums, 12. ion traps, 13. detector, 14. vacuum chambers.
Specific embodiment
If Fig. 1 is schematic top plan view of the present invention, including rotating base (1), cluster generator (2), specimen holder (3), sample (4), pulse valve I (5), air accumulator I (6), pulse valve II (7), air accumulator II (8), droplet ejection source (9), laser (10), four Pole bar mass spectrum (11), ion trap (12), detector (13), vacuum chamber (14) and computer, pulse valve I (5), pulse valve II (7) With detector (13) cable connection computer, the unlatching of pulse valve I (5) Yu pulse valve II (7) can be controlled by computer Or close, cluster generator (2) includes cavity (2-1), sample cavity (2-2), air inlet pipe I (2-3), tubule (2-4), air inlet pipe II (2-5), reaction chamber (2-6), ring electrode (2-7) and heater (2-8), xy z are three-dimensional coordinate system, and ring electrode (2-7) is outside It is connected to voltage source, heater (2-8) is circumscribed with current source, and one end of cluster generator (2) has rotating base (1), rotates bottom Seat (1) and specimen holder (3) all have magnetism, and rotating base (1) is able to drive specimen holder (3) and rotates around x axis;The sample cavity (2-2), tubule (2-4) and reaction chamber (2-6) are sequentially connected and are respectively positioned in cavity (2-1), the internal diameter of tubule (2-4) be 2mm, Length is 15mm, and the internal diameter of air inlet pipe I (2-3) is 2mm, and one end of air inlet pipe I (2-3) is connected to sample cavity (2-2), the other end Positioned at cavity (2-1) outside and be connected to pulse valve I (5), pulse valve I (5) is connected to air accumulator I (6), gas storage by tracheae Tank I stores carrier gas in (6);The internal diameter of air inlet pipe II (2-5) is 1.6mm, and one end of air inlet pipe II (2-5) is connected to tubule The side of (2-4), the other end are located at the outside of cavity (2-1) and are connected to pulse valve II (7), and pulse valve II (7) passes through tracheae It is connected to air accumulator II (8), air accumulator II stores reaction gas in (8);Sample (4) is metal, and sample (4) is fixed on sample On seat (3) and it is respectively positioned in sample cavity (2-2);Vacuum chamber (14) has the window that can penetrate laser;Ring electrode (2-7) and add Hot device (2-8) is respectively positioned in reaction chamber (2-6), and ring electrode (2-7) is ring-type, and heater (2-8) is cylindrical shape, ring electrode (2- 7) central axis and tubule (2-4) of central axis, heater (2-8) are coaxial and in the x-direction, can apply on ring electrode (2-7) Add 5000 volts of highest of voltage, the internal diameter of heater (2-8) is 6mm, and the potential of heater (2-8) remains zero volt;Reaction chamber (2-6) has outlet, and the diameter of the outlet of reaction chamber (2-6) is 2mm, and the outlet is located in vacuum chamber (14) and towards x just Direction, the outlet of ring electrode (2-7) and heater (2-8) apart from reaction chamber (2-6) is respectively 10 centimetres and 2 centimetres, laser (10) laser emitted can enter reaction chamber (2-6) by the outlet, and enter sample cavity (2-2) by tubule (2-4), To be mapped on sample (4);Droplet ejection source (9), quadrupole rod mass spectrum (11), ion trap (12) and detector (13) are along y losing side To being arranged successively and be respectively positioned in vacuum chamber (14), droplet ejection source (9) have a jet port, and can by the jet port to Y negative direction ejects superfluid helium droplet, and the superfluid helium droplet temperature is lower than 2.8K, includes in each superfluid helium droplet Helium atom number is 10000 to 20000, and the axis of reaction chamber (2-6) outlet is located at droplet ejection source (9) and quadrupole rod mass spectrum It (11) is in an angle of 90 degrees in x/y plane between and with the axis of the jet port of droplet ejection source (9).
A kind of test device of the metal cluster of chemical modification includes rotating base (1), cluster generator (2), sample Product seat (3), sample (4), pulse valve I (5), air accumulator I (6), pulse valve II (7), air accumulator II (8), droplet ejection source (9), Laser (10), quadrupole rod mass spectrum (11), ion trap (12), detector (13), vacuum chamber (14) and computer, pulse valve I (5), pulse valve II (7) and detector (13) cable connection computer, can control pulse valve I (5) and arteries and veins by computer Rush opening or closing for valve II (7), cluster generator (2) includes cavity (2-1), sample cavity (2-2), air inlet pipe I (2-3), thin (2-4), air inlet pipe II (2-5), reaction chamber (2-6), ring electrode (2-7) and heater (2-8) are managed, xy z is three dimensional space coordinate System, ring electrode (2-7) are circumscribed with voltage source, and heater (2-8) is circumscribed with current source, and one end of cluster generator (2) has rotation Turning pedestal (1), the sample cavity (2-2), tubule (2-4) and reaction chamber (2-6) are sequentially connected and are respectively positioned in cavity (2-1), One end of air inlet pipe I (2-3) is connected to sample cavity (2-2), the other end is located at the outside of cavity (2-1) and is connected to pulse valve I (5), pulse valve I (5) is connected to air accumulator I (6) by tracheae, and air accumulator I stores carrier gas in (6);Air inlet pipe II's (2-5) One end is connected to the side of tubule (2-4), the other end is located at the outside of cavity (2-1) and is connected to pulse valve II (7), pulse valve II (7) is connected to air accumulator II (8) by tracheae, and air accumulator II stores reaction gas in (8);Sample (4) is fixed on sample On seat (3) and it is respectively positioned in sample cavity (2-2);Vacuum chamber (14) has the window that can penetrate laser;Rotating base (1) and sample Product seat (3) all has magnetism, and rotating base (1) is able to drive specimen holder (3) and rotates around x axis;Ring electrode (2-7) and heater (2-8) is respectively positioned in reaction chamber (2-6), and ring electrode (2-7) is ring-type, and heater (2-8) is cylindrical shape, ring electrode (2-7) Central axis, the central axis of heater (2-8) and tubule (2-4) are coaxial and in the x-direction, can apply most on ring electrode (2-7) The potential of high 5000 volts of voltage, heater (2-8) remains zero volt;Reaction chamber (2-6) has outlet, and the outlet is located at true In cavity (14) and towards x positive direction, the outlet of ring electrode (2-7) and heater (2-8) apart from reaction chamber (2-6) is respectively 10 Centimetre and 2 centimetres, laser (10) transmitting laser can by it is described outlet enter reaction chamber (2-6), and pass through tubule (2- 4) enter sample cavity (2-2), to be mapped on sample (4);Droplet ejection source (9), quadrupole rod mass spectrum (11), ion trap (12) and Detector (13) is arranged successively along y negative direction and is respectively positioned in vacuum chamber (14), and droplet ejection source (9) have jet port, and energy Superfluid helium droplet is enough ejected to y negative direction by the jet port, the superfluid helium droplet temperature is lower than 2.8K, each described The helium atom number for including in superfluid helium droplet is 10000 to 20000, and the axis of reaction chamber (2-6) outlet is located at droplet spray It penetrates between source (9) and quadrupole rod mass spectrum (11) and is in 90 degree in x/y plane with the axis of the jet port of droplet ejection source (9) Angle.Sample (4) is metal;The internal diameter of air inlet pipe I (2-3) is 2mm, and the internal diameter of air inlet pipe II (2-5) is 1.6mm;Tubule (2-4) Internal diameter be 2mm, length 15mm;The internal diameter of heater (2-8) is 6mm, and the diameter of the outlet of reaction chamber (2-6) is 2mm.
Embodiment, sample (4) are titanium, and carrier gas is nitrogen, and the pressure of nitrogen is 0.25kPa, reaction in air inlet pipe I (2-3) Gas is oxygen, and the pressure of oxygen is 0.1kPa in air inlet pipe II (2-5), the unlatching of pulse valve I (5) and pulse valve II (7) close The closed cycle phase is 1500 microseconds, and pulse valve I (5) opens 300 microseconds every 1500 gsecs, and pulse valve II (7) is every 1500 Gsec opens 200 microseconds, and the start-up time of pulse valve II (7) delays 200 microseconds, rotating base relative to pulse valve I (5) (1) swing circle is 10 seconds, and the pulse laser wavelength of laser (10) transmitting is 532 nanometers, power is 5 watts, pulse period It is 100 microseconds for 1500 microseconds, burst length, applying voltage to ring electrode (2-7) is 1000V.
Apparatus of the present invention have magnetic rotating base, contactlessly specimen holder can be driven to rotate, so that metal sample exists It is heated evenly under laser, and uses the air supply method of special carrier gas and reaction gas, reduce the probability of other products generation, Moreover, using the superfluid helium droplet of low temperature cooling to metal cluster to carry out subsequent measurement.

Claims (6)

1. a kind of test device of the metal cluster of chemical modification, including rotating base (1), cluster generator (2), specimen holder (3), sample (4), pulse valve I (5), air accumulator I (6), pulse valve II (7), air accumulator II (8), droplet ejection source (9), laser Device (10), quadrupole rod mass spectrum (11), ion trap (12), detector (13), vacuum chamber (14) and computer, pulse valve I (5), arteries and veins Valve II (7) and detector (13) cable connection computer are rushed, pulse valve I (5) and pulse valve II can be controlled by computer (7) open or close, cluster generator (2) includes cavity (2-1), sample cavity (2-2), air inlet pipe I (2-3), tubule (2- 4), air inlet pipe II (2-5), reaction chamber (2-6), ring electrode (2-7) and heater (2-8), xyz are three-dimensional coordinate system, ring Electrode (2-7) is circumscribed with voltage source, and heater (2-8) is circumscribed with current source, and one end of cluster generator (2) has rotating base (1), the sample cavity (2-2), tubule (2-4) and reaction chamber (2-6) are sequentially connected and are respectively positioned in cavity (2-1), air inlet pipe I The one end of (2-3) is connected to sample cavity (2-2), the other end is located at the outside of cavity (2-1) and is connected to pulse valve I (5), pulse Valve I (5) is connected to air accumulator I (6) by tracheae, and air accumulator I stores carrier gas in (6);One end of air inlet pipe II (2-5) connects It is located at the outside of cavity (2-1) in the side of tubule (2-4), the other end and is connected to pulse valve II (7), pulse valve II (7) is logical It crosses tracheae to be connected to air accumulator II (8), air accumulator II stores reaction gas in (8);Sample (4) is fixed on specimen holder (3) And it is respectively positioned in sample cavity (2-2);Vacuum chamber (14) has the window that can penetrate laser,
It is characterized in that: rotating base (1) and specimen holder (3) all have magnetism, rotating base (1) is able to drive specimen holder (3) around x Axis rotation;Ring electrode (2-7) and heater (2-8) are respectively positioned in reaction chamber (2-6), and ring electrode (2-7) is ring-type, heater (2-8) is cylindrical shape, and the central axis of ring electrode (2-7), the central axis of heater (2-8) and tubule (2-4) are coaxial and along the side x To 5000 volts of highest of voltage can be applied on ring electrode (2-7), and the potential of heater (2-8) remains zero volt;Reaction chamber (2-6) has outlet, and the outlet is located in vacuum chamber (14) and towards x positive direction, ring electrode (2-7) and heater (2-8) Outlet apart from reaction chamber (2-6) is respectively 10 centimetres and 2 centimetres, and the laser of laser (10) transmitting can pass through the outlet Enter sample cavity (2-2) into reaction chamber (2-6), and by tubule (2-4), to be mapped on sample (4);Droplet ejection source (9), quadrupole rod mass spectrum (11), ion trap (12) and detector (13) are arranged successively along y negative direction and are respectively positioned on vacuum chamber (14) Interior, droplet ejection source (9) have jet port, and can eject superfluid helium droplet to y negative direction by the jet port, described Superfluid helium droplet temperature is lower than 2.8K, and the helium atom number for including in each superfluid helium droplet is 10000 to 20000, Reaction chamber (2-6) outlet axis be located between droplet ejection source (9) and quadrupole rod mass spectrum (11) and with droplet ejection source (9) Jet port axis in x/y plane be in an angle of 90 degrees.
2. the test device of the metal cluster of a kind of chemical modification according to claim 1, it is characterized in that: sample (4) is Metal.
3. the test device of the metal cluster of a kind of chemical modification according to claim 1, it is characterized in that: air inlet pipe I (2- 3) internal diameter is 2mm, and the internal diameter of air inlet pipe II (2-5) is 1.6mm.
4. the test device of the metal cluster of a kind of chemical modification according to claim 1, it is characterized in that: tubule (2-4) Internal diameter be 2mm, length 15mm.
5. the test device of the metal cluster of a kind of chemical modification according to claim 1, it is characterized in that: heater (2- 8) internal diameter is 6mm.
6. the test device of the metal cluster of a kind of chemical modification according to claim 1, it is characterized in that: reaction chamber (2- 6) diameter of outlet is 2mm.
CN201910196771.5A 2019-03-02 2019-03-02 A kind of test device of the metal cluster of chemical modification Pending CN110018221A (en)

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CN110961039A (en) * 2018-09-28 2020-04-07 铠柏科技有限公司 Laser heating cavity system
CN112683801A (en) * 2021-01-21 2021-04-20 上海菁一科技有限公司 Spectrophotometry test method sample treatment test capsule

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Publication number Priority date Publication date Assignee Title
CN110961039A (en) * 2018-09-28 2020-04-07 铠柏科技有限公司 Laser heating cavity system
CN112683801A (en) * 2021-01-21 2021-04-20 上海菁一科技有限公司 Spectrophotometry test method sample treatment test capsule

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