CN109580717B - Electrical measurement method for sample after vacuum chemical reaction - Google Patents
Electrical measurement method for sample after vacuum chemical reaction Download PDFInfo
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- CN109580717B CN109580717B CN201811431995.1A CN201811431995A CN109580717B CN 109580717 B CN109580717 B CN 109580717B CN 201811431995 A CN201811431995 A CN 201811431995A CN 109580717 B CN109580717 B CN 109580717B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
Abstract
The invention relates to the field of chemistry, and discloses an electrical measurement method for a sample after a vacuum chemical reaction, wherein a vacuum reaction and test device comprises a reaction cavity, an observation window, a liquid container, a linear driver, a cooling rod, a sample seat, a sample table, a metal rod, a gas inlet, a vacuum pump I, a corrugated pipe I, a gate valve, a corrugated pipe II, a test cavity, a sample rack, a transmission rod, a vacuum pump II and a test circuit.
Description
Technical Field
The invention relates to the field of chemistry, in particular to an electrical measurement method for a vacuum chemical reaction post-sample of a film sample, which is used for carrying out the chemical reaction in vacuum.
Background
Many chemical reactions, such as some gas-phase catalytic reactions, need to be performed in a vacuum environment, that is, the chemical reactions and subsequent property tests of the reactants are all located in a vacuum cavity, and some special reaction processes need to be performed in an ultra-high vacuum environment to directly drop a liquid reagent on the surface of a solid sample, which has the following drawbacks: in the prior art, a solid sample is usually required to be transferred outside a vacuum environment or protective gas is introduced into a vacuum cavity, the operation process is complicated, impurities can be introduced, and in addition, in some experiments, no permanent electrical connection between the sample and a sample transmission rod and between the sample transmission rod and the vacuum cavity is required, and a simple fixing structure is required to implement an electrical test; the defects of the prior art are as follows: the sample holder connection mode in the prior art is complex, and the electrical measurement method of the sample after the vacuum chemical reaction can solve the problem.
Disclosure of Invention
In order to solve the problems, the method of the invention directly drops gaseous reagent molecules on the surface of a solid sample through the steps of freezing, heating and melting in a vacuum environment, and in addition, the method of the invention adopts a specially designed sample holder transmission and fixing method to electrically measure the reacted sample in the vacuum environment.
The technical scheme adopted by the invention is as follows:
the vacuum reaction and test device comprises a reaction cavity, an observation window, a liquid container, a linear driver, a cooling rod, a sample seat, a sample table, a metal rod, a gas inlet, a vacuum pump I, a corrugated pipe I, a gate valve, a corrugated pipe II, a test cavity, a sample frame, a conveying rod, a vacuum pump II and a test circuit, wherein xyz is a three-dimensional space coordinate system, and the vacuum pump II and the test circuit are connected outside the test cavity; the reaction chamber, the corrugated pipe I, the gate valve, the corrugated pipe II and the test chamber are sequentially connected, when the gate valve is opened, the vacuum pump II can simultaneously vacuumize the reaction chamber and the test chamber, the reaction chamber is provided with an observation window, a liquid container, a metal rod, a gas inlet and the vacuum pump I, a liquid reagent is filled in the liquid container, the temperature of the liquid container is adjustable, an outlet of the liquid container is positioned in the reaction chamber, a pulse electromagnetic valve is arranged at an outlet of the liquid container, and the quantity of the reagent entering the reaction chamber can be controlled; the cooling rod is installed and connected on the reaction cavity through a linear driver, the lower end of the cooling rod penetrates into the reaction cavity, and the cooling rod can move up and down relative to the reaction cavity in the y direction through the linear driver; the metal rod is arranged below the reaction cavity, the upper end of the metal rod is positioned in the reaction cavity, air tightness is provided between the metal rod and the reaction cavity, the metal rod can move up and down relative to the reaction cavity in the y direction, the upper end of the metal rod is sequentially connected with a sample table, a sample seat and a sample, and the sample seat is provided with a small hole; the conveying rod can penetrate through the test cavity, the corrugated pipe II, the gate valve and the corrugated pipe I, the front end of the conveying rod can enter the reaction cavity, the rear end of the conveying rod is positioned outside the test cavity, the conveying rod can move along the z direction and can rotate 360 degrees around the axis of the conveying rod, the front end of the conveying rod is provided with a pincer mechanism, the pincer mechanism can clamp two sides of the sample seat, the sample seat can be installed on or removed from the sample table through the conveying rod in the state that the gate valve is opened, the sample seat can be conveyed between the reaction cavity and the test cavity, and the position of the sample table can be adjusted; the cooling rod comprises a liquid nitrogen container, an inner pipe, an outer pipe, a sleeve, a heater, a cold head, an outlet and a cylindrical pipe, wherein the inner pipe is coaxially nested in the outer pipe and is placed along the y direction, the upper end of the inner pipe is connected with the liquid nitrogen container, the upper end of the outer pipe is provided with the outlet, the outlet is provided with a flow rate control valve, the lower end of the outer pipe is connected with the cold head, the cold head is a cone with the radius of the bottom surface of three millimeters, the height of four millimeters and the vertex of the cold head facing downwards, the cylindrical pipe is coaxially nested outside the outer pipe, the sleeve is coaxially nested outside the cylindrical pipe, the distance between the lower part of the sleeve and the cold head is 40 millimeters, the heater is arranged inside the sleeve, a vacuum layer is arranged between the inner pipe, the outer pipe and the cylindrical pipe, and a thermocouple is arranged between the cold head and the lower end of the inner pipe; the sample rack is positioned in the test cavity, the sample rack comprises a substrate, an operating rod, a limiting piece, a supporting piece, a front clamping piece and a rear clamping piece, the substrate is connected to the upper side surface in the test cavity, the operating rod can move up and down relative to the test cavity along the y direction, the upper end of the operating rod is positioned outside the test cavity and is mutually airtight, the lower end of the operating rod is provided with a barb, when the sample seat is taken down from the sample table by the conveying rod and is transmitted to the test cavity, the barb can be inserted into a small hole on the sample seat, so that the movement of the sample seat can be controlled, the limiting piece is fixed on the substrate through a screw, the distance between the limiting piece and the substrate is five millimeters, the supporting piece is positioned below the limiting piece and is fixed on the substrate through the screw, the distance between the supporting piece and the substrate is eight millimeters, two rear clamping pieces and two front clamping pieces are respectively elastic, and the front clamping piece and the rear clamping pieces are respectively connected to a test circuit outside the test cavity through cables, and the upper end of the sample seat can be inserted between the front clamping piece and the rear clamping piece through the operating rod and the sample seat is clamped; the vacuum pump I is a liquid nitrogen cooling absorption pump; the cold head is made of stainless steel; the inner diameter of the inner tube is two millimeters, the inner diameter of the outer tube is six millimeters, the inner diameter of the cylindrical tube is ten millimeters, the length of the cylindrical tube is 100 millimeters, the inner diameter of the sleeve is 24 millimeters, and the length of the sleeve is 40 millimeters; the diameter of the operating rod is three millimeters; the front clamping piece and the rear clamping piece are both made of metal tantalum.
The steps of the chemical reaction in vacuum are as follows:
step 1, opening a gate valve, and vacuumizing a reaction cavity and a test cavity by adopting a vacuum pump II to ensure that the vacuum of the reaction cavity reaches 1 multiplied by 10 -8 mbar；
Step 2. According to the kind of the reagent in the liquid container, the temperature in the liquid container is adjusted so that the vapor pressure of the reagent in the liquid container is 3X 10 -10 The typical value of the temperature of the liquid container is zero degrees celsius;
step 3, by controlling the opening and closing of a pulse electromagnetic valve of the liquid container, enabling the reagent to enter the reaction cavity so as to discharge other impurity molecules adsorbed on the inner wall of the reaction cavity in advance;
step 4, adding liquid nitrogen into a liquid nitrogen container, regulating a flow rate control valve at an outlet to control the flow rate of the liquid nitrogen in the inner tube, and simultaneously regulating the temperature of a heater to 30 ℃ to ensure that the temperature of a cold head reaches 77K and the temperature of the outer wall of a cylindrical tube ranges from 100K to 120K, wherein the aim is to ensure that the vapor pressure of reagent molecules in a reaction cavity is less than 1 multiplied by 10 -10 mbar, and the reagent molecules freeze-solidify only in the region outside the coldhead;
step 5, closing a gate valve between the reaction cavity and the test cavity, adjusting the linear driver to enable the cold head to be opposite to the outlet of the liquid container, enabling gaseous reagent molecules to enter the reaction cavity by controlling the opening and closing of a pulse electromagnetic valve of the liquid container, and keeping the vacuum degree of the reaction cavity to be better than 1 multiplied by 10 -6 mbar；
Step 6, most reagent molecules entering the reaction cavity are adsorbed by the outer wall of the cylindrical tube, and a small part of reagent molecules are frozen and solidified in the area outside the cold head;
step 7, opening a gate valve between the reaction cavity and the test cavity, transferring a sample seat with a sample into the reaction cavity through a transfer rod and installing the sample seat on the sample table, and closing the gate valve between the reaction cavity and the test cavity;
step 8, after an obvious solidified reagent layer appears on the outer side of the cold head, closing a pulse electromagnetic valve of the liquid container, adjusting the position of the sample stage to enable the sample stage to be positioned at a position which is one cm below the cold head, and adjusting the position of the metal rod to enable the upper end of the metal rod to be in contact with the lower side surface of the sample stage;
step 9, adjusting a flow rate control valve at the outlet to reduce the flow rate of liquid nitrogen in the inner tube, so that the cold head is heated, the solidified reagent layer is slowly melted, and finally the solidified reagent layer is dripped on the surface of a sample in the form of liquid drops, wherein the vacuum range of the reaction cavity is 1 multiplied by 10 -5 Typical values for the rate of change of temperature of the coldhead are 0.2K/min, with drop volumes ranging from 30 microliters to 100 microliters;
and 10, after the reagent liquid drops are dripped on the surface of the sample for two minutes, starting a vacuum pump I to pump out reagent molecules in the reaction cavity.
Immediately after the preceding chemical reaction in vacuo, electrical testing of the following samples can follow:
the method for electrically measuring the sample after the vacuum chemical reaction comprises the following steps:
step one, the vacuum degree of the reaction cavity and the test cavity is better than 5 multiplied by 10 -8 The method comprises the steps of mbar, opening a gate valve between a reaction cavity and a test cavity, clamping edges of two sides of a sample seat by a pincer mechanism at the front end of a conveying rod, then moving the conveying rod in the positive z direction, taking the sample seat and a sample off a sample table, and conveying the sample seat and the sample to the test cavity;
step two, the conveying rod rotates 90 degrees around the axis of the conveying rod, the position of the operating rod is adjusted, so that barbs at the lower end of the conveying rod are inserted into small holes in the sample seat, then the pincer mechanism at the front end of the conveying rod is separated from the edges of the two sides of the sample seat, finally the sample seat is hooked by the operating rod, and at the moment, the sample seat is contacted with the operating rod only through the small holes;
step three, adjusting the position of the operating rod, so that the sample seat is inserted between the front clamping piece and the rear clamping piece from bottom to top, the front clamping piece is only contacted with the sample, the rear clamping piece is only contacted with the sample seat, the sample seat can be stably clamped by the front clamping piece and the rear clamping piece and cannot fall down, and then the operating rod is separated from the sample seat;
and fourthly, testing the electrical property of the sample through a testing circuit outside the testing cavity.
The beneficial effects of the invention are as follows:
the method can directly drop the liquid reagent onto the surface of the sample in vacuum to carry out chemical reaction, avoids sudden deterioration of the vacuum degree around the sample, has simple operation steps and can not introduce impurities.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic view of a sample holder of the present invention in a reaction chamber;
FIG. 2 is a schematic view of a sample holder of the present invention in a test chamber;
FIG. 3 is an enlarged schematic view of a cooling rod;
FIG. 4 is an enlarged schematic view of a sample holder;
fig. 5 is a left side view of fig. 4.
In the drawings, 1, reaction chamber, 2, observation window, 3, liquid container, 4, linear drive, 5, cooling rod, 5-1, liquid nitrogen container, 5-2, inner tube, 5-3, outer tube, 5-4, sleeve, 5-5, heater, 5-6, cold head, 5-7, outlet, 5-8, cylindrical tube, 6, sample, 7, sample holder, 8, sample stage, 9, metal rod, 10, gas inlet, 11, vacuum pump I,12, bellows I,13, gate valve, 14, bellows II,15, test chamber, 16, sample holder, 16-1, base plate, 16-2, operating rod, 16-3, limiting piece, 16-4, support piece, 16-5, front clamping piece, 16-6, rear clamping piece, 17, transfer rod, 18, vacuum pump II.
Detailed Description
Fig. 1 is a schematic diagram of a sample holder in a reaction chamber, fig. 2 is a schematic diagram of a sample holder in a test chamber in the invention, the sample holder comprises a reaction chamber (1), an observation window (2), a liquid container (3), a linear driver (4), a cooling rod (5), a sample (6), a sample holder (7), a sample table (8), a metal rod (9), a gas inlet (10), a vacuum pump I (11), a corrugated pipe I (12), a gate valve (13), a corrugated pipe II (14), a test chamber (15), a sample rack (16), a transmission rod (17), a vacuum pump II (18) and a test circuit, xyz is a three-dimensional space coordinate system, the outside of the test chamber (15) is connected with the vacuum pump II (18) and the test circuit, the vacuum pump I (11) is a liquid nitrogen cooled absorption pump, the reaction chamber (1), the corrugated pipe I (12), a gate valve (13), the corrugated pipe II (14) and the test chamber (15) are sequentially connected, when the gate valve (13) is opened, the vacuum pump II (18) can simultaneously pump the reaction chamber (1) and the test chamber (15), the vacuum pump (3) is installed with the liquid container (3), the liquid container (10) is installed, the liquid container (3) is installed in the vacuum pump (3) and the liquid container (3), the temperature of the liquid container (3) can be adjusted, the outlet of the liquid container (3) is positioned in the reaction cavity (1), and the outlet of the liquid container (3) is provided with a pulse electromagnetic valve which can control the amount of the reagent entering the reaction cavity (1); the cooling rod (5) is installed and connected on the reaction cavity (1) through the linear driver (4), the lower end of the cooling rod (5) penetrates into the reaction cavity (1), and the cooling rod (5) can move up and down in the y direction relative to the reaction cavity (1) through the linear driver (4); the metal rod (9) is arranged below the reaction cavity (1), the upper end of the metal rod (9) is positioned in the reaction cavity (1), air tightness is provided between the metal rod (9) and the reaction cavity (1), the metal rod (9) can move up and down in the y direction relative to the reaction cavity (1), the upper end of the metal rod (9) is sequentially connected with the sample table (8), the sample seat (7) and the sample (6), and the sample seat (7) is provided with a small hole; the conveying rod (17) can penetrate through the test cavity (15), the corrugated pipe II (14), the door valve (13) and the corrugated pipe I (12), the front end of the conveying rod (17) can enter the reaction cavity (1), the rear end of the conveying rod (17) is located outside the test cavity (15), the conveying rod (17) can move along the z direction and can rotate around the axis of the conveying rod (17) by 360 degrees, the front end of the conveying rod (17) is provided with a clamp-shaped mechanism, two sides of the sample seat (7) can be clamped, the sample seat (7) can be installed on the sample table (8) or taken down from the sample table (8) through the conveying rod (17) under the state that the door valve (13) is opened, the sample seat (7) can be conveyed between the reaction cavity (1) and the test cavity (15), and the position of the sample table (8) can be adjusted.
As shown in fig. 3, the cooling rod (5) comprises a liquid nitrogen container (5-1), an inner tube (5-2), an outer tube (5-3), a sleeve (5-4), a heater (5-5), a cold head (5-6), an outlet (5-7) and a cylindrical tube (5-8), wherein the cold head (5-6) is made of stainless steel, the inner tube (5-2) is coaxially nested in the outer tube (5-3) and is placed along the y direction, the upper end of the inner tube (5-2) is connected with the liquid nitrogen container (5-1), the upper end of the outer tube (5-3) is provided with the outlet (5-7), the outlet (5-7) is provided with a flow rate control valve, the lower end of the outer tube (5-3) is connected with the cold head (5-6), the cold head (5-6) is a cone with the bottom radius of three millimeters and the height of which is four millimeters and the top point downward, the cylindrical tube (5-8) is coaxially nested outside the outer tube (5-3), the sleeve (5-4) is coaxially nested outside the cylindrical tube (5-8), the sleeve (5-4) is arranged below the inner tube (5-4) and is arranged at the inner diameter of the inner tube (5-4) from the inner tube (5-5), the inner diameter of the outer tube (5-3) is six millimeters, the inner diameter of the cylindrical tube (5-8) is ten millimeters, the length of the cylindrical tube is 100 millimeters, the inner diameter of the sleeve (5-4) is 24 millimeters, the length of the sleeve is 40 millimeters, vacuum layers are arranged between the inner tube (5-2), the outer tube (5-3) and the cylindrical tube (5-8), and a thermocouple is arranged between the cold head (5-6) and the lower end of the inner tube (5-2).
Referring to fig. 4, which is an enlarged schematic view of the sample holder, and to fig. 4, which is a left side view of fig. 4, the sample holder (16) is located in the test chamber (15), the sample holder (16) includes a base plate (16-1), a lever (16-2), a limiting plate (16-3), a supporting plate (16-4), a front clamping piece (16-5) and a rear clamping piece (16-6), the base plate (16-1) is connected to an upper side surface in the test chamber (15), the lever (16-2) can move up and down in a y direction relative to the test chamber (15), the diameter of the lever (16-2) is three millimeters, the upper end of the lever (16-2) is located outside the test chamber (15) and has air tightness with each other, the lower end of the lever (16-2) has barbs, when the transfer lever (17) removes the sample holder (7) from the sample holder (8) and transfers the test chamber (15), the barbs can be inserted into small holes on the sample holder (7), thereby controlling movement of the sample holder (7), the limiting plate (16-3) is fixed to the base plate (16-1) by a screw (16-3) and the base plate (16-1) is fixed between the base plate (16-1) and the base plate (16-1) by a screw (16-3), the distance between the supporting piece (16-4) and the substrate (16-1) is eight millimeters, two rear clamping pieces (16-6) and two front clamping pieces (16-5) are arranged on the supporting piece (16-4), as shown in figures 4 and 5, the positive x direction of the supporting piece (16-4) is two rear clamping pieces (16-6), the negative x direction of the supporting piece (16-4) is two front clamping pieces (16-5), the front clamping pieces (16-5) and the rear clamping pieces (16-6) are elastic, the front clamping pieces (16-5) and the rear clamping pieces (16-6) are all made of metal tantalum, the front clamping pieces (16-5) and the rear clamping pieces (16-6) are all connected to a test circuit outside the test cavity (15) through cables, and the upper end of the sample seat (7) can be inserted between the front clamping pieces (16-5) and the rear clamping pieces (16-6) through the operating rod (16-2) and clamp the sample seat (7).
Principle of chemical reaction in vacuum:
adjusting the temperature in the liquid container (3) so that the vapor pressure of the reagent in the liquid container (3) is 3X 10 - 10 mbar and opening pulse electromagnetic valve of liquid container (3) to make reagent molecule enter reaction cavity (1), regulating heater (5-5) temperature to 30deg.C to make cold head (5-6) temperature reach 77K, and the external wall of cylindrical tube (5-8) temperature range is 100K to 120K, meshIs that the vapor pressure of the reagent in the reaction chamber (1) is less than 1×10 -10 The reagent freezes and solidifies only in the region outside the cold head (5-6), most reagent molecules entering the reaction cavity (1) are adsorbed by the outer wall of the cylindrical tube (5-8), a small part of reagent molecules freezes and solidifies in the region outside the cold head (5-6), the thickness of the frozen and solidified solid reagent layer in the region outside the cold head (5-6) depends on the opening time of the pulse electromagnetic valve, the vapor pressure and the temperature of the reagent in the liquid container (3), the flow rate control valve at the outlet (5-7) is adjusted to reduce the liquid nitrogen flow rate in the inner tube (5-2), so that the cold head (5-6) is heated, the solidified reagent layer slowly melts, and finally drops to the surface of the sample (6) in the form of liquid drops.
The vacuum reaction and test device comprises a reaction cavity (1), an observation window (2), a liquid container (3), a linear driver (4), a cooling rod (5), a sample (6), a sample seat (7), a sample table (8), a metal rod (9), a gas inlet (10), a vacuum pump I (11), a corrugated pipe I (12), a gate valve (13), a corrugated pipe II (14), a test cavity (15), a sample frame (16), a transmission rod (17), a vacuum pump II (18) and a test circuit, xyz is a three-dimensional space coordinate system, and the vacuum pump II (18) and the test circuit are connected outside the test cavity (15); the reaction chamber (1), the corrugated pipe I (12), the gate valve (13), the corrugated pipe II (14) and the test chamber (15) are sequentially connected, when the gate valve (13) is opened, the vacuum pump II (18) can simultaneously vacuumize the reaction chamber (1) and the test chamber (15), the reaction chamber (1) is provided with an observation window (2), a liquid container (3), a metal rod (9), a gas inlet (10) and a vacuum pump I (11), liquid reagents are filled in the liquid container (3), the temperature of the liquid container (3) is adjustable, an outlet of the liquid container (3) is positioned in the reaction chamber (1), and a pulse electromagnetic valve is arranged at an outlet of the liquid container (3) so as to control the quantity of the reagents entering the reaction chamber (1); the cooling rod (5) is installed and connected on the reaction cavity (1) through the linear driver (4), the lower end of the cooling rod (5) penetrates into the reaction cavity (1), and the cooling rod (5) can move up and down in the y direction relative to the reaction cavity (1) through the linear driver (4); the metal rod (9) is arranged below the reaction cavity (1), the upper end of the metal rod (9) is positioned in the reaction cavity (1), air tightness is provided between the metal rod (9) and the reaction cavity (1), the metal rod (9) can move up and down in the y direction relative to the reaction cavity (1), the upper end of the metal rod (9) is sequentially connected with the sample table (8), the sample seat (7) and the sample (6), and the sample seat (7) is provided with a small hole; the conveying rod (17) can penetrate through the test cavity (15), the corrugated pipe II (14), the door valve (13) and the corrugated pipe I (12), the front end of the conveying rod (17) can enter the reaction cavity (1), the rear end of the conveying rod (17) is located outside the test cavity (15), the conveying rod (17) can move along the z direction and can rotate around the axis of the conveying rod (17) by 360 degrees, the front end of the conveying rod (17) is provided with a clamp-shaped mechanism, the clamp-shaped mechanism can clamp two sides of the sample seat (7), the sample seat (7) can be installed on the sample table (8) or removed from the sample table (8) through the conveying rod (17) under the state that the door valve (13) is opened, the sample seat (7) can be conveyed between the reaction cavity (1) and the test cavity (15), and the position of the sample table (8) can be adjusted; the cooling rod (5) comprises a liquid nitrogen container (5-1), an inner tube (5-2), an outer tube (5-3), a sleeve (5-4), a heater (5-5), a cold head (5-6), an outlet (5-7) and a cylindrical tube (5-8), wherein the inner tube (5-2) is coaxially nested in the outer tube (5-3) and is placed along the y direction, the upper end of the inner tube (5-2) is connected with the liquid nitrogen container (5-1), the upper end of the outer tube (5-3) is provided with the outlet (5-7), the outlet (5-7) is provided with a flow rate control valve, the lower end of the outer tube (5-3) is connected with the cold head (5-6), the cold head (5-6) is a cone with the bottom radius of three millimeters and the height of four millimeters and the vertex of which is downward, the cylindrical tube (5-8) is coaxially nested outside the outer tube (5-3), the sleeve (5-4) is coaxially nested outside the cylindrical tube (5-8), the lower part of the sleeve (5-4) is 40 millimeters from the cold head (5-6), the inner side of the sleeve (5-4) is separated from the inner tube (5-3), the inner tube (5-3) is arranged between the heat-layer and the outer tube (5-2), a thermocouple is arranged between the cold head (5-6) and the lower end of the inner pipe (5-2); the sample rack (16) is positioned in the test cavity (15), the sample rack (16) comprises a substrate (16-1), an operating rod (16-2), a limiting plate (16-3), a supporting plate (16-4), a front clamping plate (16-5) and a rear clamping plate (16-6), the substrate (16-1) is connected to the upper side surface in the test cavity (15), the operating rod (16-2) can move up and down along the y direction relative to the test cavity (15), the upper end of the operating rod (16-2) is positioned outside the test cavity (15) and is mutually airtight, the lower end of the operating rod (16-2) is provided with a barb, when the conveying rod (17) removes the sample seat (7) from the sample table (8) and transmits the sample seat (7) to the test cavity (15), the barb can be inserted into a small hole on the sample seat (7), so that the movement of the sample seat (7) can be controlled, the limiting plate (16-3) is fixed on the substrate (16-1) through a screw, the distance between the limiting plate (16-3) and the substrate (16-1) is five, the supporting plate (16-3) is positioned on the lower side of the substrate (16-1) through the screw, the supporting plate (16-4) is positioned between the limiting plate (16-1) and the supporting plate (16-4) and the sample seat (16-1), two rear clamping pieces (16-6) and two front clamping pieces (16-5) are arranged on the supporting piece (16-4), the front clamping pieces (16-5) and the rear clamping pieces (16-6) are elastic, the front clamping pieces (16-5) and the rear clamping pieces (16-6) are respectively connected to a test circuit outside the test cavity (15) through cables, and the upper end of the sample seat (7) can be inserted between the front clamping pieces (16-5) and the rear clamping pieces (16-6) through the operating rod (16-2) and clamp the sample seat (7); the vacuum pump I (11) is a liquid nitrogen cooling absorption pump; the cold head (5-6) is made of stainless steel; the inner diameter of the inner tube (5-2) is two millimeters, the inner diameter of the outer tube (5-3) is six millimeters, the inner diameter of the cylindrical tube (5-8) is ten millimeters, the length is 100 millimeters, the inner diameter of the sleeve (5-4) is 24 millimeters, and the length is 40 millimeters; the diameter of the operating rod (16-2) is three millimeters; the front clamping piece (16-5) and the rear clamping piece (16-6) are both made of metallic tantalum.
The steps of the chemical reaction in vacuum are as follows:
step 1, opening a gate valve (13), and vacuumizing the reaction cavity (1) and the test cavity (15) by adopting a vacuum pump II (18) to ensure that the vacuum of the reaction cavity (1) reaches 1 multiplied by 10 -8 mbar；
Step 2. According to the kind of the reagent in the liquid container (3), the temperature in the liquid container (3) is adjusted so that the vapor pressure of the reagent in the liquid container (3) is 3X 10 -10 The typical value of the temperature of the liquid container (3) is zero degrees celsius;
step 3, by controlling the opening and closing of the pulse electromagnetic valve of the liquid container (3), enabling the reagent to enter the reaction cavity (1) so as to discharge other impurity molecules adsorbed on the inner wall of the reaction cavity (1) in advance;
step 4. Adding liquid nitrogen into the liquid nitrogen container (5-1), adjusting a flow rate control valve at an outlet (5-7) to control the flow rate of liquid nitrogen in the inner tube (5-2), and simultaneously adjusting the temperature of the heater (5-5) to 30 ℃ to ensure that the temperature of the cold head (5-6) reaches 77K and the temperature of the outer wall of the cylindrical tube (5-8) ranges from 100K to 120K, so that the vapor pressure of reagent molecules in the reaction cavity (1) is less than 1 multiplied by 10 -10 mbar, and the reagent molecules freeze-solidify only in the region outside the cold head (5-6);
step 5. Closing the gate valve (13) between the reaction chamber (1) and the test chamber (15), adjusting the linear driver (4) to enable the cold head (5-6) to be opposite to the outlet of the liquid container (3), controlling the opening and closing of the pulse electromagnetic valve of the liquid container (3) to enable gaseous reagent molecules to enter the reaction chamber (1), and keeping the vacuum degree of the reaction chamber (1) to be better than 1 multiplied by 10 -6 mbar；
Step 6, most reagent molecules entering the reaction cavity (1) are adsorbed by the outer wall of the cylindrical tube (5-8), and a small part of reagent molecules are frozen and solidified in the area outside the cold head (5-6);
step 7, opening a gate valve (13) between the reaction cavity (1) and the test cavity (15), transferring a sample seat (7) with a sample (6) into the reaction cavity (1) through a transfer rod (17) and installing the sample seat on a sample table (8), and closing the gate valve (13) between the reaction cavity (1) and the test cavity (15);
step 8, after obvious solidified reagent layers appear on the outer side of the cold head (5-6), closing a pulse electromagnetic valve of the liquid container (3), adjusting the position of the sample stage (8) to be positioned at a position which is one cm right below the cold head (5-6), and adjusting the position of the metal rod (9) to enable the upper end of the metal rod (9) to be in contact with the lower side surface of the sample stage (8);
step 9. Adjusting the flow rate control valve at the outlet (5-7) to reduce the flow rate of liquid nitrogen in the inner tube (5-2) so that the cold head (5-6) is heated, the solidified reagent layer slowly melts and finally drops onto the surface of the sample (6) in the form of liquid drops, wherein the vacuum range of the reaction chamber (1) is 1X 10 -5 Typical values for the rate of temperature change of the coldhead (5-6) are 0.2K/min, dripping in drop volumes ranging from 30 microliter to 100 microliter;
and 10, after the reagent liquid drops are dripped on the surface of the sample (6) for two minutes, starting a vacuum pump I (11) to pump out reagent molecules in the reaction cavity (1).
Immediately after the preceding chemical reaction in vacuo, electrical testing of the following samples can follow:
the method for electrically measuring the sample after the vacuum chemical reaction comprises the following steps:
step one, the vacuum degree of the reaction cavity (1) and the test cavity (15) is better than 5 multiplied by 10 -8 mbar, opening the door between the reaction chamber (1) and the test chamber (15)A valve (13) which clamps the edges of both sides of the sample holder (7) by a pincerlike mechanism at the front end of the transmission rod (17), then moves the transmission rod (17) towards the positive z direction, and removes the sample holder (7) together with the sample (6) from the sample table (8) and transmits the sample to the test cavity (15);
step two, the conveying rod (17) rotates 90 degrees around the axis of the conveying rod, the position of the operating rod (16-2) is adjusted, so that barbs at the lower end of the conveying rod are inserted into small holes in the sample seat (7), then the pincer-shaped mechanism at the front end of the conveying rod (17) is separated from two side edges of the sample seat (7), finally the sample seat (7) is hooked by the operating rod (16-2), and at the moment, the sample seat (7) is contacted with the operating rod (16-2) only through the small holes;
adjusting the position of the operating rod (16-2) so that the sample seat (7) is inserted between the front clamping piece (16-5) and the rear clamping piece (16-6) from bottom to top, enabling the front clamping piece (16-5) to be only in contact with the sample (6), enabling the rear clamping piece (16-6) to be only in contact with the sample seat (7), enabling the sample seat (7) to be stably clamped by the front clamping piece (16-5) and the rear clamping piece (16-6) and not to fall down, and then separating the operating rod (16-2) from the sample seat (7);
and fourthly, testing the electrical property of the sample through a testing circuit outside the testing cavity (15).
The method can directly drop liquid reagent molecules on the surface of the solid sample in a vacuum environment, avoids sudden vacuum degree deterioration in the reaction cavity, has simple operation process and no impurity introduction, and in addition, the sample seat transferring and fixing method adopted by the method can be used for measuring the electrical properties of the sample in the vacuum cavity, has simple sample seat fixing structure and simple sample transferring step, and is particularly suitable for experiments requiring immediate subsequent measurement of the electrical properties of the sample after chemical reaction.
Claims (1)
1. The utility model provides an electricity measuring method of sample after vacuum chemical reaction, vacuum reaction and testing arrangement includes reaction chamber (1), observation window (2), liquid container (3), linear drive (4), cooling pole (5), sample (6), sample seat (7), sample platform (8), metal pole (9), gas inlet (10), vacuum pump I (11), bellows I (12), gate valve (13), bellows II (14), test chamber (15), sample frame (16), transfer line (17), vacuum pump II (18) and test circuit, xyz is three-dimensional space coordinate system, be connected with vacuum pump II (18) and test circuit outside test chamber (15); the reaction chamber (1), the corrugated pipe I (12), the gate valve (13), the corrugated pipe II (14) and the test chamber (15) are sequentially connected, when the gate valve (13) is opened, the vacuum pump II (18) can simultaneously vacuumize the reaction chamber (1) and the test chamber (15), the reaction chamber (1) is provided with an observation window (2), a liquid container (3), a metal rod (9), a gas inlet (10) and a vacuum pump I (11), liquid reagents are filled in the liquid container (3), the temperature of the liquid container (3) is adjustable, an outlet of the liquid container (3) is positioned in the reaction chamber (1), and a pulse electromagnetic valve is arranged at an outlet of the liquid container (3) so as to control the quantity of the reagents entering the reaction chamber (1); the cooling rod (5) is installed and connected on the reaction cavity (1) through the linear driver (4), the lower end of the cooling rod (5) penetrates into the reaction cavity (1), and the cooling rod (5) can move up and down in the y direction relative to the reaction cavity (1) through the linear driver (4); the metal rod (9) is arranged below the reaction cavity (1), the upper end of the metal rod (9) is positioned in the reaction cavity (1), air tightness is provided between the metal rod (9) and the reaction cavity (1), the metal rod (9) can move up and down in the y direction relative to the reaction cavity (1), the upper end of the metal rod (9) is sequentially connected with the sample table (8), the sample seat (7) and the sample (6), and the sample seat (7) is provided with a small hole; the conveying rod (17) can penetrate through the test cavity (15), the corrugated pipe II (14), the door valve (13) and the corrugated pipe I (12), the front end of the conveying rod (17) can enter the reaction cavity (1), the rear end of the conveying rod (17) is located outside the test cavity (15), the conveying rod (17) can move along the z direction and can rotate around the axis of the conveying rod (17) by 360 degrees, the front end of the conveying rod (17) is provided with a clamp-shaped mechanism, the clamp-shaped mechanism can clamp two sides of the sample seat (7), the sample seat (7) can be installed on the sample table (8) or removed from the sample table (8) through the conveying rod (17) under the state that the door valve (13) is opened, the sample seat (7) can be conveyed between the reaction cavity (1) and the test cavity (15), and the position of the sample table (8) can be adjusted; the cooling rod (5) comprises a liquid nitrogen container (5-1), an inner tube (5-2), an outer tube (5-3), a sleeve (5-4), a heater (5-5), a cold head (5-6), an outlet (5-7) and a cylindrical tube (5-8), wherein the inner tube (5-2) is coaxially nested in the outer tube (5-3) and is placed along the y direction, the upper end of the inner tube (5-2) is connected with the liquid nitrogen container (5-1), the upper end of the outer tube (5-3) is provided with the outlet (5-7), the outlet (5-7) is provided with a flow rate control valve, the lower end of the outer tube (5-3) is connected with the cold head (5-6), the cold head (5-6) is a cone with the bottom radius of three millimeters and the height of four millimeters and the vertex of which is downward, the cylindrical tube (5-8) is coaxially nested outside the outer tube (5-3), the sleeve (5-4) is coaxially nested outside the cylindrical tube (5-8), the lower part of the sleeve (5-4) is 40 millimeters from the cold head (5-6), the inner side of the sleeve (5-4) is separated from the inner tube (5-3), the inner tube (5-3) is arranged between the heat-layer and the outer tube (5-2), a thermocouple is arranged between the cold head (5-6) and the lower end of the inner pipe (5-2); the sample rack (16) is positioned in the test cavity (15), the sample rack (16) comprises a substrate (16-1), an operating rod (16-2), a limiting plate (16-3), a supporting plate (16-4), a front clamping plate (16-5) and a rear clamping plate (16-6), the substrate (16-1) is connected to the upper side surface in the test cavity (15), the operating rod (16-2) can move up and down along the y direction relative to the test cavity (15), the upper end of the operating rod (16-2) is positioned outside the test cavity (15) and is mutually airtight, the lower end of the operating rod (16-2) is provided with a barb, when the conveying rod (17) removes the sample seat (7) from the sample table (8) and transmits the sample seat (7) to the test cavity (15), the barb can be inserted into a small hole on the sample seat (7), so that the movement of the sample seat (7) can be controlled, the limiting plate (16-3) is fixed on the substrate (16-1) through a screw, the distance between the limiting plate (16-3) and the substrate (16-1) is five, the supporting plate (16-3) is positioned on the lower side of the substrate (16-1) through the screw, the supporting plate (16-4) is positioned between the limiting plate (16-1) and the supporting plate (16-4) and the sample seat (16-1), two rear clamping pieces (16-6) and two front clamping pieces (16-5) are arranged on the supporting piece (16-4), the front clamping pieces (16-5) and the rear clamping pieces (16-6) are elastic, the front clamping pieces (16-5) and the rear clamping pieces (16-6) are respectively connected to a test circuit outside the test cavity (15) through cables, and the upper end of the sample seat (7) can be inserted between the front clamping pieces (16-5) and the rear clamping pieces (16-6) through the operating rod (16-2) and clamp the sample seat (7); the vacuum pump I (11) is a liquid nitrogen cooling absorption pump; the cold head (5-6) is made of stainless steel; the inner diameter of the inner tube (5-2) is two millimeters, the inner diameter of the outer tube (5-3) is six millimeters, the inner diameter of the cylindrical tube (5-8) is ten millimeters, the length is 100 millimeters, the inner diameter of the sleeve (5-4) is 24 millimeters, and the length is 40 millimeters; the diameter of the operating rod (16-2) is three millimeters; the front clamping piece (16-5) and the rear clamping piece (16-6) are both made of metal tantalum,
the steps of the chemical reaction in vacuum are as follows:
step 1. Opening the door valve (13) andvacuum pump II (18) is adopted to vacuumize the reaction cavity (1) and the test cavity (15) so that the vacuum of the reaction cavity (1) reaches 1 multiplied by 10 -8 mbar；
Step 2. According to the kind of the reagent in the liquid container (3), the temperature in the liquid container (3) is adjusted so that the vapor pressure of the reagent in the liquid container (3) is 3X 10 -10 The typical value of the temperature of the liquid container (3) is zero degrees celsius;
step 3, by controlling the opening and closing of the pulse electromagnetic valve of the liquid container (3), enabling the reagent to enter the reaction cavity (1) so as to discharge other impurity molecules adsorbed on the inner wall of the reaction cavity (1) in advance;
step 4. Adding liquid nitrogen into the liquid nitrogen container (5-1), adjusting a flow rate control valve at an outlet (5-7) to control the flow rate of liquid nitrogen in the inner tube (5-2), and simultaneously adjusting the temperature of the heater (5-5) to 30 ℃ to ensure that the temperature of the cold head (5-6) reaches 77K and the temperature of the outer wall of the cylindrical tube (5-8) ranges from 100K to 120K, so that the vapor pressure of reagent molecules in the reaction cavity (1) is less than 1 multiplied by 10 -10 mbar, and the reagent molecules freeze-solidify only in the region outside the cold head (5-6);
step 5. Closing the gate valve (13) between the reaction chamber (1) and the test chamber (15), adjusting the linear driver (4) to enable the cold head (5-6) to be opposite to the outlet of the liquid container (3), controlling the opening and closing of the pulse electromagnetic valve of the liquid container (3) to enable gaseous reagent molecules to enter the reaction chamber (1), and keeping the vacuum degree of the reaction chamber (1) to be better than 1 multiplied by 10 -6 mbar；
Step 6, most reagent molecules entering the reaction cavity (1) are adsorbed by the outer wall of the cylindrical tube (5-8), and a small part of reagent molecules are frozen and solidified in the area outside the cold head (5-6);
step 7, opening a gate valve (13) between the reaction cavity (1) and the test cavity (15), transferring a sample seat (7) with a sample (6) into the reaction cavity (1) through a transfer rod (17) and installing the sample seat on a sample table (8), and closing the gate valve (13) between the reaction cavity (1) and the test cavity (15);
step 8, after obvious solidified reagent layers appear on the outer side of the cold head (5-6), closing a pulse electromagnetic valve of the liquid container (3), adjusting the position of the sample stage (8) to be positioned at a position which is one cm right below the cold head (5-6), and adjusting the position of the metal rod (9) to enable the upper end of the metal rod (9) to be in contact with the lower side surface of the sample stage (8);
step 9. Adjusting the flow rate control valve at the outlet (5-7) to reduce the flow rate of liquid nitrogen in the inner tube (5-2) so that the cold head (5-6) is heated, the solidified reagent layer slowly melts and finally drops onto the surface of the sample (6) in the form of liquid drops, wherein the vacuum range of the reaction chamber (1) is 1X 10 -5 Typical values for the rate of temperature change of the coldhead (5-6) are 0.2K/min, dripping in drop volumes ranging from 30 microliter to 100 microliter;
step 10, after the reagent liquid drops are dripped on the surface of the sample (6) for two minutes, starting a vacuum pump I (11) to pump out reagent molecules in the reaction cavity (1),
the above-described chemical reaction in vacuo can be immediately followed by electrical testing of the following samples:
the method is characterized in that: the method for electrically measuring the sample after the vacuum chemical reaction comprises the following steps:
step one, the vacuum degree of the reaction cavity (1) and the test cavity (15) is better than 5 multiplied by 10 -8 The method comprises the steps of (1) opening a gate valve (13) between a reaction cavity (1) and a test cavity (15), clamping two side edges of a sample seat (7) by adopting a clamp mechanism at the front end of a conveying rod (17), then moving the conveying rod (17) in the positive z direction, taking the sample seat (7) together with a sample (6) from a sample table (8), and conveying the sample seat to the test cavity (15);
step two, the conveying rod (17) rotates 90 degrees around the axis of the conveying rod, the position of the operating rod (16-2) is adjusted, so that barbs at the lower end of the conveying rod are inserted into small holes in the sample seat (7), then the pincer-shaped mechanism at the front end of the conveying rod (17) is separated from two side edges of the sample seat (7), finally the sample seat (7) is hooked by the operating rod (16-2), and at the moment, the sample seat (7) is contacted with the operating rod (16-2) only through the small holes;
adjusting the position of the operating rod (16-2) so that the sample seat (7) is inserted between the front clamping piece (16-5) and the rear clamping piece (16-6) from bottom to top, enabling the front clamping piece (16-5) to be only in contact with the sample (6), enabling the rear clamping piece (16-6) to be only in contact with the sample seat (7), enabling the sample seat (7) to be stably clamped by the front clamping piece (16-5) and the rear clamping piece (16-6) and not to fall down, and then separating the operating rod (16-2) from the sample seat (7);
and fourthly, testing the electrical property of the sample through a testing circuit outside the testing cavity (15).
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