CN109499478B - Vacuum reaction and testing device - Google Patents
Vacuum reaction and testing device Download PDFInfo
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- CN109499478B CN109499478B CN201811431994.7A CN201811431994A CN109499478B CN 109499478 B CN109499478 B CN 109499478B CN 201811431994 A CN201811431994 A CN 201811431994A CN 109499478 B CN109499478 B CN 109499478B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 109
- 238000012360 testing method Methods 0.000 title claims abstract description 98
- 239000007788 liquid Substances 0.000 claims abstract description 67
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000003153 chemical reaction reagent Substances 0.000 claims description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- 238000012546 transfer Methods 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 5
- 210000000080 chela (arthropods) Anatomy 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
Classifications
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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
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
Abstract
The invention relates to the chemical field, in particular to a vacuum reaction and test device which 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 transmission rod, a vacuum pump II and a test circuit.
Description
Technical Field
The invention relates to the field of chemistry, in particular to a vacuum reaction and testing device for performing chemical reaction on a film sample 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 seat connection mode in the prior art is complex, and the vacuum reaction and testing device can solve the problem.
Disclosure of Invention
In order to solve the above problems, the present invention adopts a method of melting a previously frozen reagent in a vacuum environment to directly drop a liquid reagent on a solid sample surface, and adopts a simple sample transfer and installation method.
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 frame is located the test chamber, and the sample frame includes base plate, control lever, spacing piece, backing sheet, preceding clamping piece and back clamping piece, and the base plate is connected in the upside of test chamber, and the control lever can reciprocate along y direction for the test chamber, and control lever upper end is located the test chamber and each other has the gas tightness, and the control lever lower extreme has the barb, when the transfer lever takes off the sample seat from the sample platform and transmits to the test chamber, the aperture on the sample seat can be inserted to the barb to can control the removal of sample seat, the spacing piece passes through the screw fixation in the base plate, and the distance between spacing piece and the base plate is five millimeters, and the backing sheet is located spacing piece below and is fixed in the base plate through the screw, and the distance between backing sheet and the base plate is eight millimeters, installs two back clamping pieces and two preceding clamping pieces on the backing sheet, and preceding clamping piece and back clamping piece all have elasticity, and preceding clamping piece and back clamping piece all are connected to the test circuit outside the test chamber through the cable respectively, can make sample seat upper end insert between preceding clamping piece and the back clamping piece through the control lever, and the clamping piece clamp sample seat.
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 vacuum reaction and testing device is adopted to carry out the vacuum chemical reaction process, which comprises the following steps:
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 steps of the electrical test process of the sample by adopting the vacuum reaction and test device are as follows:
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 device does not need to transfer a solid sample out of a vacuum environment or introduce protective gas into a vacuum cavity in the reaction requiring a liquid reagent, does not cause the sudden deterioration of the vacuum degree around the sample, has simple operation process and avoids introducing impurities, and in addition, the device has a simple sample seat transferring and fixing method and can be immediately used for electrical measurement after the sample is subjected to chemical reaction.
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 a pulse solenoid valve of the liquid container (3) to enable reagent molecules to enter the reaction cavity (1), regulating the temperature of the heater (5-5) to 30 ℃ to enable the temperature of the cold head (5-6) to reach 77K and the temperature of the outer wall of the cylindrical tube (5-8) to be in a range of 100K to 120K, wherein the aim is to enable the vapor pressure of the reagent in the reaction cavity (1) to be less than 1 multiplied by 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 conveying rod (17), a vacuum pump II (18) and a test circuit, wherein xyz is a three-dimensional space coordinate system, and a vacuum pump H (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 device provided by the invention is provided with the specially designed cooling rod, can freeze and solidify gaseous reagent molecules in a vacuum environment, and adopts a slow heating method to enable the reagent to drop on the surface of a sample for chemical reaction after being melted, so that the vacuum degree in the reaction cavity is not suddenly reduced, the operation is simple, no impurities are introduced, and in addition, the device provided by the invention is provided with a simple sample transferring and fixing method, and the chemical reaction and the electrical measurement of the sample can be completed in the cavity.
Claims (6)
1. The utility model provides a vacuum reaction and testing arrangement, including reaction chamber (1), observation window (2), liquid container (3), linear drive ware (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, test chamber (15) external connection has vacuum pump II (18) and test circuit, characterized by:
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).
2. The vacuum reaction and testing apparatus of claim 1, wherein: the vacuum pump I (11) is a liquid nitrogen cooled absorption pump.
3. The vacuum reaction and testing apparatus of claim 1, wherein: the cold head (5-6) is made of stainless steel.
4. The vacuum reaction and testing apparatus of claim 1, wherein: 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, and the inner diameter of the sleeve (5-4) is 24 millimeters, and the length is 40 millimeters.
5. The vacuum reaction and testing apparatus of claim 1, wherein: the diameter of the operating rod (16-2) is three millimeters.
6. The vacuum reaction and testing apparatus of claim 1, wherein: the front clamping piece (16-5) and the rear clamping piece (16-6) are both made of metallic tantalum.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH051665A (en) * | 1991-06-27 | 1993-01-08 | Fujitsu Ltd | Vacuum pump |
| JP2000260839A (en) * | 1999-03-11 | 2000-09-22 | Mitsubishi Electric Corp | Low-temperature testing device |
| JP2002372483A (en) * | 2001-04-09 | 2002-12-26 | Toshiba Microelectronics Corp | Elimination gas analysis apparatus and method |
| JPWO2011102320A1 (en) * | 2010-02-17 | 2013-06-17 | 株式会社アルバック | Electron beam irradiation apparatus and electron beam irradiation method |
| KR20130113104A (en) * | 2012-04-05 | 2013-10-15 | 한국에너지기술연구원 | Poly silicon manufacturing apparatus having oxidation source inputting part or plasma inputting part and manufacturing method using the same |
| CN105642206A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院合肥物质科学研究院 | Beryllium-water reaction device |
| CN105842042A (en) * | 2016-05-31 | 2016-08-10 | 中国科学院理化技术研究所 | Low temperature sample cavity |
| JP2017003337A (en) * | 2015-06-08 | 2017-01-05 | 大同特殊鋼株式会社 | Wettability test device |
| CN106568794A (en) * | 2016-11-04 | 2017-04-19 | 上海交通大学 | Low temperature refrigerating machine-based visual experiment observation apparatus of controlled liquefaction and solidification process of fluid |
| CN107389498A (en) * | 2017-07-07 | 2017-11-24 | 金华职业技术学院 | A kind of method for measuring methane transmitance |
| CN209378953U (en) * | 2018-11-17 | 2019-09-13 | 金华职业技术学院 | A kind of vacuum reaction and test device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011102320A (en) * | 2011-01-18 | 2011-05-26 | Seoul National Univ Industry Foundation | B cell-mediated vaccine loaded with ligand of natural killer t cell and antigen |
-
2018
- 2018-11-17 CN CN201811431994.7A patent/CN109499478B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH051665A (en) * | 1991-06-27 | 1993-01-08 | Fujitsu Ltd | Vacuum pump |
| JP2000260839A (en) * | 1999-03-11 | 2000-09-22 | Mitsubishi Electric Corp | Low-temperature testing device |
| JP2002372483A (en) * | 2001-04-09 | 2002-12-26 | Toshiba Microelectronics Corp | Elimination gas analysis apparatus and method |
| JPWO2011102320A1 (en) * | 2010-02-17 | 2013-06-17 | 株式会社アルバック | Electron beam irradiation apparatus and electron beam irradiation method |
| KR20130113104A (en) * | 2012-04-05 | 2013-10-15 | 한국에너지기술연구원 | Poly silicon manufacturing apparatus having oxidation source inputting part or plasma inputting part and manufacturing method using the same |
| JP2017003337A (en) * | 2015-06-08 | 2017-01-05 | 大同特殊鋼株式会社 | Wettability test device |
| CN105642206A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院合肥物质科学研究院 | Beryllium-water reaction device |
| CN105842042A (en) * | 2016-05-31 | 2016-08-10 | 中国科学院理化技术研究所 | Low temperature sample cavity |
| CN106568794A (en) * | 2016-11-04 | 2017-04-19 | 上海交通大学 | Low temperature refrigerating machine-based visual experiment observation apparatus of controlled liquefaction and solidification process of fluid |
| CN107389498A (en) * | 2017-07-07 | 2017-11-24 | 金华职业技术学院 | A kind of method for measuring methane transmitance |
| CN209378953U (en) * | 2018-11-17 | 2019-09-13 | 金华职业技术学院 | A kind of vacuum reaction and test device |
Non-Patent Citations (1)
| Title |
|---|
| 真空环境熔融金属成分检测的激光诱导击穿光谱系统;潘从元;杜学维;安宁;韩振宇;王声波;尉伟;王秋平;;光谱学与光谱分析(12);3388-3391 * |
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