CN109499478A - A kind of vacuum reaction and test device - Google Patents
A kind of vacuum reaction and test device Download PDFInfo
- Publication number
- CN109499478A CN109499478A CN201811431994.7A CN201811431994A CN109499478A CN 109499478 A CN109499478 A CN 109499478A CN 201811431994 A CN201811431994 A CN 201811431994A CN 109499478 A CN109499478 A CN 109499478A
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- specimen holder
- reaction chamber
- chamber
- vacuum
- test
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 105
- 238000012360 testing method Methods 0.000 title claims abstract description 96
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000000758 substrate Substances 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 13
- 238000009434 installation Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 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
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 8
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 241000656145 Thyrsites atun Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
Classifications
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Electrochemistry (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
Abstract
The present invention relates to chemical fields, a kind of vacuum reaction and test device, including reaction chamber, observation window, liquid container, linear actuator, cooling rod, sample, specimen holder, sample stage, metallic rod, gas feed, vacuum pump I, bellows I, gate valve, bellows II, test chamber, specimen holder, driven rod, vacuum pump II and test circuit, it is a kind of vacuum reaction chemically reacted in a vacuum for film sample and test device, the reagent of liquid is directly dripped on solid sample surface using the method for melting the reagent freezed in advance, it is not necessary that solid sample to be transferred to outside vacuum environment or to being passed through protective gas in vacuum chamber in the reaction for needing liquid reagent, the vacuum degree that not will lead to around sample is deteriorated suddenly, operating process is simple and avoids introducing impurity, apparatus of the present invention tool There are simple specimen holder transfer and fixing means, electrical measurement can be immediately available for after sample is chemically reacted.
Description
Technical field
The present invention relates to chemical field, especially a kind of one kind chemically reacted in a vacuum for film sample is true
Sky reaction and test device.
Background technique
Such as certain gas phase catalytic reaction needs of many chemical reactions carry out in vacuum environment, i.e. the chemistry of reactant is anti-
It answers and subsequent characteristic test is all located in vacuum cavity, certain special reaction process needs carry out in ultra-high vacuum environment
The reagent of liquid is directly dripped on solid sample surface, prior art defect one: in the prior art it is generally necessary to by solid sample
It is transferred to outside vacuum environment or to protective gas is passed through in vacuum chamber, operating process is cumbersome and can introduce impurity, in addition, certain
It needs to be electrically connected between sample and sample driven rod and vacuum cavity without permanent in experiment, and needs simple fixed structure
To implement electrical testing；Prior art defect two: specimen holder connection type in the prior art is complex, a kind of vacuum
Reaction and test device are able to solve problem.
Summary of the invention
To solve the above-mentioned problems, the present invention using make in vacuum environment the reagent freezed in advance melt method come
The reagent of liquid is directly dripped on solid sample surface, and uses simple sample transfer and installation method.
The technical scheme adopted by the invention is that:
A kind of vacuum reaction and test device include reaction chamber, observation window, liquid container, linear actuator, cooling
Bar, sample, specimen holder, sample stage, metallic rod, gas feed, vacuum pump I, bellows I, gate valve, bellows II, test chamber, sample
Product frame, driven rod, vacuum pump II and test circuit, xyz is three-dimensional coordinate system, and test chamber is externally connected with vacuum pump II and survey
Try circuit；Reaction chamber, bellows I, gate valve, bellows II and test chamber are sequentially connected, and when gate valve is opened, vacuum pump II can
Simultaneously reaction chamber and test chamber are vacuumized, reaction chamber installation be connected with observation window, liquid container, metallic rod, gas feed and
Vacuum pump I is equipped with the reagent of liquid in liquid container, and the temperature of liquid container is adjustable, and liquid container outlet is located at reaction chamber
Interior, the outlet of liquid container has impulse electromagnetic valve, can control the amount into the reagent of reaction chamber；Cooling rod is driven by straight line
Dynamic device is installed and connected in above reaction chamber and cooling rod lower end penetrates reaction chamber, enables to cooling rod by linear actuator
Relative to reaction chamber lower movement in y-direction；Metallic rod is installed below reaction chamber and metallic rod upper end is located in reaction chamber,
There is air-tightness, metallic rod can be relative to reaction chamber lower movement in y-direction, metallic rod upper end between metallic rod and reaction chamber
It is connected with sample stage, specimen holder and sample in turn, there is aperture on specimen holder；Driven rod can pass through test chamber, bellows II,
Gate valve and bellows I, driven rod front end is able to enter in reaction chamber, rear end is located at outside test chamber, and driven rod can move in the z-direction
It moves and can be rotated around 360 degree of its axis, driven rod front end has pincerlike mechanism, and pincerlike mechanism can block specimen holder two sides,
In the state that gate valve is opened, specimen holder can be installed on sample stage by driven rod or be removed from sample stage, and energy
Enough that specimen holder is transmitted between reaction chamber and test chamber, sample stage position can be adjusted；Cooling rod include liquid nitrogen container, inner tube,
Outer tube, sleeve, heater, cold head, outlet and cylindrical tube, inner tube are coaxially nested in outer tube and place in the y-direction, upper end of inner tube
Liquid nitrogen container is connected, outer tube upper end has outlet, and exit has flow control valve, and outer tube lower end is connected with cold head, described cold
Head is that bottom surface radius is three millimeters, is highly four millimeters and vertex cone directed downwardly, cylindrical tube are coaxially nested on the outside of outer tube,
Sleeve is coaxially nested on the outside of cylindrical tube, apart from cold head is 40 millimeters below sleeve, installs having heaters on the inside of sleeve, inner tube,
Vacuum layer is all had between outer tube and cylindrical tube, and thermocouple is installed between cold head and the lower end of inner tube；Specimen holder is located at test chamber
Interior, specimen holder includes substrate, control stick, limit film, support chip, preceding intermediate plate and rear jaw, and substrate is connected to upper in test chamber
Side, control stick can move up and down in the y-direction relative to test chamber, and control stick upper end is located at outside test chamber and mutually has gas
Close property, control stick lower end have barb, when specimen holder is removed from sample stage and is transmitted to test chamber by driven rod, it is described fall
Hook is inserted into the aperture on specimen holder, and so as to control the movement of specimen holder, limit film is screwed in substrate, limit
Distance is five millimeters between bit slice and substrate, and support chip is located at below limit film and is screwed in substrate, support chip and
Distance is eight millimeters between substrate, intermediate plate before two pieces of rear jaws and two pieces is equipped on support chip, preceding intermediate plate and rear jaw have
Flexible, preceding intermediate plate and rear jaw can be made respectively by the test circuit outside cable connection to test chamber by control stick
It obtains specimen holder upper end to be inserted between the preceding intermediate plate and rear jaw, and clamps specimen holder.
Vacuum pump I is the cooling absorption pump of liquid nitrogen；Cold head is made of stainless steel；Inner tube diameter is two millimeters, outer tube diameter
It is six millimeters, cylinder bore is ten millimeters, length is 100 millimeters, and sleeve diameter is 24 millimeters, length is 40 millimeters；Manipulation
Shank diameter is three millimeters；Preceding intermediate plate and rear jaw are made of metal tantalum.
The step of chemical reaction process in vacuum is carried out using a kind of vacuum reaction and test device are as follows:
Step 1. opens gate valve, and is vacuumized using vacuum pump II to reaction chamber and test chamber, so that reaction chamber
Vacuum reaches 1 × 10-8mbar；
Step 2. adjusts the temperature in liquid container so that reagent holds in liquid according to the type of reagent in liquid container
Vapour pressure in device is 3 × 10-10Mbar, the temperature representative value of liquid container are zero degrees celsius；
Step 3. passes through the opening and closing of the impulse electromagnetic valve of control liquid container, so that reagent enters reaction chamber with pre-
The other impurities molecule of first discharge reaction cavity wall absorption；
Liquid nitrogen container is added in liquid nitrogen by step 4., adjusts the flow control valve in exit to control the liquid nitrogen stream in inner tube
Speed, while heter temperature is adjusted to 30 degrees Celsius, so that cold head temperature reaches 77K, and the temperature range of cylinder pipe outer wall exists
100K to 120K, it is therefore an objective to so that the vapour pressure of the reagent molecule in reaction chamber is less than 1 × 10-10Mbar, and reagent molecule only exists
Region cryocoagulation on the outside of cold head；
Step 5. closes the gate valve between reaction chamber and test chamber, adjusts linear actuator and makes cold head face liquid container
Outlet, the opening and closing of the impulse electromagnetic valve by controlling liquid container so that gaseous reagent molecule enters reaction chamber,
And keep the vacuum degree of reaction chamber better than 1 × 10-6mbar；
Most of reagent molecule that step 6. enters reaction chamber is adsorbed by cylinder pipe outer wall, and small part reagent molecule is in cold head
The region cryocoagulation in outside；
Step 7. opens the gate valve between reaction chamber and test chamber, by driven rod that the specimen holder with sample is incoming anti-
It answers chamber and is installed on sample stage, close the gate valve between reaction chamber and test chamber；
After the reagent layer significantly solidified occurs on the outside of cold head in step 8., the impulse electromagnetic valve of closing liquid container is adjusted
Sample stage position is saved, a centimeters immediately below cold head are located at, metallic rod position is adjusted, so that metallic rod upper end and sample stage
Downside face contact；
Step 9. adjusts the flow control valve in exit to reduce the liquid nitrogen flow velocity in inner tube, so that cold head heats up, solidification
Reagent layer slowly melt, finally drip to sample surfaces in droplets, during this vacuum range of reaction chamber be 1 ×
10-5Mbar to 50mbar, the rate temperature change representative value of cold head are 0.2K/ minutes, and the droplet size range dripped is 30 micro-
It is raised to 100 microlitres；
After step 10. candidate agent drop drips to sample surfaces two minutes, vacuum pump I is opened by the reagent molecule in reaction chamber
Extraction.
It formerly carries out in above-mentioned vacuum after chemical reaction process, can then carry out the electrical testing of following sample immediately:
The step of electrical testing process of sample is carried out using a kind of vacuum reaction and test device are as follows:
Step 1 waits for that the vacuum degree of reaction chamber and test chamber is better than 5 × 10-8Mbar is opened between reaction chamber and test chamber
Gate valve, specimen holder both sides of the edge are blocked using the pincerlike mechanism of driven rod front end, will then to the mobile driven rod of positive z direction
Specimen holder is removed from sample stage together with sample, and is transmitted to test chamber；
90 degree rotatable around its axis of step 2 driven rod, and stick position is adjusted, so that the barb of its lower end is inserted into sample
Then the pincerlike mechanism of driven rod front end is separated with the both sides of the edge of specimen holder, finally makes specimen holder by the aperture on product seat
It is manipulated pike pole to rise, specimen holder only passes through aperture and contacts with control stick at this time；
Step 3 adjusts stick position, so that specimen holder is inserted into from bottom to top between preceding intermediate plate and rear jaw, and makes
Preceding intermediate plate is only contacted with sample, and rear jaw is only contacted with specimen holder, and enables specimen holder steady by preceding intermediate plate and rear jaw
Clamp is lived without falling, and then separates control stick with specimen holder；
Step 4 by test chamber outside test circuit the electrical properties of sample are tested.
The beneficial effects of the present invention are:
Apparatus of the present invention are outside vacuum environment or right it is not necessary that solid sample to be transferred in the reaction for needing liquid reagent
Protective gas is passed through in vacuum chamber, the vacuum degree that not will lead to around sample is deteriorated suddenly, and operating process is simple and avoids introducing
Impurity can be stood in addition, apparatus of the present invention have the transfer of simple specimen holder and fixing means after sample is chemically reacted
It is used for electrical measurement.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram when specimen holder of the present invention is located at reaction chamber；
Fig. 2 is schematic diagram when specimen holder of the present invention is located at test chamber；
Fig. 3 is cooling rod enlarged diagram；
Fig. 4 is specimen holder enlarged diagram；
Fig. 5 is the left view of Fig. 4.
In figure, 1. reaction chambers, 2. observation windows, 3. liquid containers, 4. linear actuators, 5. cooling rods, 5-1. liquid nitrogen container,
5-2. inner tube, 5-3. outer tube, 5-4. sleeve, 5-5. heater, 5-6. cold head, the outlet 5-7., 5-8. cylindrical tube, 6. samples, 7.
Specimen holder, 8. sample stages, 9. metallic rods, 10. gas feeds, 11. vacuum pump I, 12. bellows I, 13. gate valves, 14. bellowss
II, 15. test chambers, 16. specimen holders, 16-1. substrate, 16-2. control stick, 16-3. limit film, 16-4. support chip, before 16-5.
Intermediate plate, 16-6. rear jaw, 17. driven rods, 18. vacuum pump II.
Specific embodiment
If Fig. 1 is schematic diagram when specimen holder of the present invention is located at reaction chamber, when such as Fig. 2 being that specimen holder of the present invention is located at test chamber
Schematic diagram, including reaction chamber (1), observation window (2), liquid container (3), linear actuator (4), cooling rod (5), sample (6), sample
Product seat (7), sample stage (8), metallic rod (9), gas feed (10), vacuum pump I (11), bellows I (12), gate valve (13), wave
Line pipe II (14), test chamber (15), specimen holder (16), driven rod (17), vacuum pump II (18) and test circuit, xyz are three-dimensional
Space coordinates, test chamber (15) are externally connected with vacuum pump II (18) and test circuit, and vacuum pump I (11) is the cooling suction of liquid nitrogen
Pump is received, reaction chamber (1), bellows I (12), gate valve (13), bellows II (14) and test chamber (15) are sequentially connected, and work as gate valve
(13) when opening, vacuum pump II (18) can simultaneously be vacuumized reaction chamber (1) and test chamber (15), and reaction chamber (1) installation connects
It is connected to observation window (2), liquid container (3), metallic rod (9), gas feed (10) and vacuum pump I (11), dress in liquid container (3)
There is the reagent of liquid, the temperature of liquid container (3) is adjustable, and liquid container (3) outlet is located in reaction chamber (1), liquid container
(3) outlet has impulse electromagnetic valve, can control the amount of the reagent into reaction chamber (1)；Cooling rod (5) passes through linear drives
Device (4) is installed and connected in reaction chamber (1) above and cooling rod (5) lower end penetrates reaction chamber (1), passes through linear actuator (4) energy
Enough so that cooling rod (5) is relative to reaction chamber (1) lower movement in y-direction；Metallic rod (9) be installed on reaction chamber (1) below and
Metallic rod (9) upper end is located in reaction chamber (1), has air-tightness between metallic rod (9) and reaction chamber (1), metallic rod (9) can
Relative to reaction chamber (1) lower movement in y-direction, metallic rod (9) upper end is connected with sample stage (8), specimen holder (7) and sample in turn
Product (6) have aperture on specimen holder (7)；Driven rod (17) can pass through test chamber (15), bellows II (14), gate valve (13)
With bellows I (12), driven rod (17) front end is able to enter in reaction chamber (1), rear end is located at test chamber (15) outside, driven rod
(17) it can be movable in the z-direction and can be rotated around 360 degree of its axis, driven rod (17) front end has pincerlike mechanism, pincerlike machine
Structure can block specimen holder (7) two sides, can be by specimen holder (7) by driven rod (17) in the state that gate valve (13) are opened
It is installed on sample stage (8) or is removed from sample stage (8), and sample can be transmitted between reaction chamber (1) and test chamber (15)
Product seat (7), sample stage (8) position can be adjusted.
If Fig. 3 is cooling rod enlarged diagram, cooling rod (5) includes liquid nitrogen container (5-1), inner tube (5-2), outer tube (5-
3), sleeve (5-4), heater (5-5), cold head (5-6), outlet (5-7) and cylindrical tube (5-8), cold head (5-6) is by stainless steel
At inner tube (5-2) is coaxially nested in outer tube (5-3) and places in the y-direction, and the inner tube upper end (5-2) connects liquid nitrogen container (5-
1), the outer tube upper end (5-3) has outlet (5-7), has flow control valve at outlet (5-7), the lower end outer tube (5-3) is connected with cold
Head (5-6), the cold head (5-6) are that bottom surface radius is three millimeters, is highly four millimeters and vertex cone directed downwardly, cylindrical tube
(5-8) is coaxially nested on the outside of outer tube (5-3), and sleeve (5-4) is coaxially nested on the outside of cylindrical tube (5-8), and sleeve (5-4) is below
It is 40 millimeters apart from cold head (5-6), having heaters (5-5) is installed on the inside of sleeve (5-4), inner tube (5-2) internal diameter is two millimeters, outside
Managing (5-3) internal diameter is six millimeters, and cylindrical tube (5-8) internal diameter is ten millimeters, length is 100 millimeters, and sleeve (5-4) internal diameter is 24 millis
Rice, length are 40 millimeters, all have vacuum layer between inner tube (5-2), outer tube (5-3) and cylindrical tube (5-8), cold head (5-6) and
Thermocouple is installed between the lower end of inner tube (5-2).
If Fig. 4 is specimen holder enlarged diagram, if Fig. 5 is the left view of Fig. 4, specimen holder (16) is located at test chamber (15)
Interior, specimen holder (16) includes substrate (16-1), control stick (16-2), limit film (16-3), support chip (16-4), preceding intermediate plate (16-
5) and rear jaw (16-6), substrate (16-1) is connected to the upper side in test chamber (15), and control stick (16-2) can be relative to
Test chamber (15) moves up and down in the y-direction, and control stick (16-2) diameter is three millimeters, and the control stick upper end (16-2) is located at test chamber
(15) outside and mutually there is air-tightness, the control stick lower end (16-2) has barb, when driven rod (17) by specimen holder (7) from sample
When removing on platform (8) and being transmitted to test chamber (15), the barb is inserted into the aperture on specimen holder (7), so as to control
The movement of specimen holder (7) processed, limit film (16-3) are screwed in substrate (16-1), limit film (16-3) and substrate (16-
1) distance is five millimeters between, and support chip (16-4) is located at below limit film (16-3) and is screwed in substrate (16-
1), distance is eight millimeters between support chip (16-4) and substrate (16-1), is equipped with two pieces of rear jaws on support chip (16-4)
Intermediate plate (16-5) before (16-6) and two pieces, such as Fig. 4,5, the positive x direction of support chip (16-4) is two pieces of rear jaws (16-6), support
The negative x-direction of piece (16-4) is intermediate plate (16-5) before two pieces, and preceding intermediate plate (16-5) and rear jaw (16-6) all have elasticity, fore-clamp
Piece (16-5) and rear jaw (16-6) are made of metal tantalum, and preceding intermediate plate (16-5) and rear jaw (16-6) pass through cable respectively
It is connected to the test circuit of test chamber (15) outside, before enabling to the insertion of specimen holder (7) upper end described by control stick (16-2)
Between intermediate plate (16-5) and rear jaw (16-6), and clamp specimen holder (7).
The principle chemically reacted in vacuum:
The temperature in liquid container (3) is adjusted so that vapour pressure of the reagent in liquid container (3) is 3 × 10- 10Mbar, and the impulse electromagnetic valve for opening liquid container (3) enters reagent molecule reaction chamber (1), adjusts heater (5-5)
Temperature is to 30 degrees Celsius, so that cold head (5-6) temperature reaches 77K, and the temperature range of cylindrical tube (5-8) outer wall is arrived in 100K
120K, it is therefore an objective to so that the vapour pressure of the reagent in reaction chamber (1) is less than 1 × 10-10Mbar, and reagent only cold head (5-6) outside
The region cryocoagulation of side, most of reagent molecule into reaction chamber (1) are adsorbed by cylindrical tube (5-8) outer wall, small part examination
Region cryocoagulation of the agent molecule on the outside of cold head (5-6), the solid state reagents layer of the region cryocoagulation on the outside of cold head (5-6)
The vapour pressure and temperature of reagent of the thickness depending on the time of impulse electromagnetic valve unlatching, in liquid container (3), adjust outlet (5-
7) flow control valve at place is to reduce the liquid nitrogen flow velocity in inner tube (5-2), so that cold head (5-6) heats up, the reagent layer of solidification is slow
It is slow to melt, sample (6) surface is finally dripped in droplets.
A kind of vacuum reaction and test device include reaction chamber (1), observation window (2), liquid container (3), straight line drive
Dynamic device (4), cooling rod (5), sample (6), specimen holder (7), sample stage (8), metallic rod (9), gas feed (10), vacuum pump I
(11), bellows I (12), gate valve (13), bellows II (14), test chamber (15), specimen holder (16), driven rod (17), vacuum
II (18) and test circuit are pumped, xyz is three-dimensional coordinate system, and test chamber (15) is externally connected with vacuum pump H (18) and test electricity
Road；Reaction chamber (1), bellows I (12), gate valve (13), bellows II (14) and test chamber (15) are sequentially connected, when gate valve (13)
When unlatching, vacuum pump II (18) can simultaneously be vacuumized reaction chamber (1) and test chamber (15), and reaction chamber (1) installation is connected with
Observation window (2), liquid container (3), metallic rod (9), gas feed (10) and vacuum pump I (11) are equipped with liquid in liquid container (3)
The temperature of the reagent of state, liquid container (3) is adjustable, and liquid container (3) outlet is located in reaction chamber (1), liquid container (3)
Outlet has impulse electromagnetic valve, can control the amount of the reagent into reaction chamber (1)；Cooling rod (5) passes through linear actuator (4)
It is installed and connected in reaction chamber (1) above and cooling rod (5) lower end penetrates reaction chamber (1), can be made by linear actuator (4)
Cooling rod (5) are obtained relative to reaction chamber (1) lower movement in y-direction；Metallic rod (9) is installed on reaction chamber (1) below and metal
Bar (9) upper end is located in reaction chamber (1), has air-tightness between metallic rod (9) and reaction chamber (1), metallic rod (9) can be opposite
In reaction chamber (1) lower movement in y-direction, metallic rod (9) upper end is connected with sample stage (8), specimen holder (7) and sample in turn
(6), there is aperture on specimen holder (7)；Driven rod (17) can pass through test chamber (15), bellows II (14), gate valve (13) and
Bellows I (12), driven rod (17) front end is able to enter in reaction chamber (1), rear end is located at test chamber (15) outside, driven rod (17)
It can be movable in the z-direction and can be rotated around 360 degree of its axis, driven rod (17) front end has pincerlike mechanism, pincerlike mechanism energy
Specimen holder (7) two sides are enough blocked, in the state that gate valve (13) are opened, specimen holder (7) can be installed by driven rod (17)
It is removed on sample stage (8) or from sample stage (8), and specimen holder can be transmitted between reaction chamber (1) and test chamber (15)
(7), sample stage (8) position can be adjusted；Cooling rod (5) includes liquid nitrogen container (5-1), inner tube (5-2), outer tube (5-3), sleeve
(5-4), heater (5-5), cold head (5-6), outlet (5-7) and cylindrical tube (5-8), inner tube (5-2) are coaxially nested in outer tube (5-
3) it places in and in the y-direction, the inner tube upper end (5-2) connects liquid nitrogen container (5-1), and the outer tube upper end (5-3) has outlet (5-7),
Exporting has flow control valve at (5-7), the lower end outer tube (5-3) is connected with cold head (5-6), and the cold head (5-6) is bottom surface half
Diameter is three millimeters, is highly four millimeters and vertex cone directed downwardly, and cylindrical tube (5-8) is coaxially nested on the outside of outer tube (5-3),
Sleeve (5-4) is coaxially nested on the outside of cylindrical tube (5-8), and sleeve (5-4) is below 40 millimeters apart from cold head (5-6), sleeve (5-
4) having heaters (5-5) is installed in inside, all has vacuum layer, cold head between inner tube (5-2), outer tube (5-3) and cylindrical tube (5-8)
Thermocouple is installed between (5-6) and the lower end of inner tube (5-2)；Specimen holder (16) is located in test chamber (15), specimen holder (16) packet
Include substrate (16-1), control stick (16-2), limit film (16-3), support chip (16-4), preceding intermediate plate (16-5) and rear jaw (16-
6), substrate (16-1) is connected to the upper side in test chamber (15), and control stick (16-2) can be relative to test chamber (15) along the side y
It moves up and down, the control stick upper end (16-2) is located at test chamber (15) outside and mutually has air-tightness, the lower end control stick (16-2)
With barb, when specimen holder (7) is removed from sample stage (8) and is transmitted to test chamber (15) by driven rod (17), it is described fall
Hook is inserted into the aperture on specimen holder (7), and so as to control the movement of specimen holder (7), limit film (16-3) passes through screw
It is fixed on substrate (16-1), distance is five millimeters between limit film (16-3) and substrate (16-1), and support chip (16-4) is located at limit
Below bit slice (16-3) and to be screwed the distance between substrate (16-1), support chip (16-4) and substrate (16-1) be eight
Millimeter, is equipped with intermediate plate (16-5) before two pieces of rear jaws (16-6) and two pieces on support chip (16-4), preceding intermediate plate (16-5) and after
Intermediate plate (16-6) all has elasticity, and preceding intermediate plate (16-5) and rear jaw (16-6) pass through cable connection to test chamber (15) respectively
Outer test circuit enables to specimen holder (7) upper end to be inserted into the preceding intermediate plate (16-5) and rear folder by control stick (16-2)
Between piece (16-6), and clamp specimen holder (7).
Vacuum pump I (11) is the cooling absorption pump of liquid nitrogen；Cold head (5-6) is made of stainless steel；Inner tube (5-2) internal diameter is two
Millimeter, outer tube (5-3) internal diameter are six millimeters, and cylindrical tube (5-8) internal diameter is ten millimeters, length is 100 millimeters, in sleeve (5-4)
Diameter is 24 millimeters, length is 40 millimeters；Control stick (16-2) diameter is three millimeters；Preceding intermediate plate (16-5) and rear jaw (16-6) are equal
It is made of metal tantalum.
Apparatus of the present invention have the cooling rod of special designing, and gaseous reagent molecule can be made to freeze in vacuum environment
Solidification, and drip in sample surfaces after using the method slowly to heat up that reagent is melted to be chemically reacted, it not will lead to anti-
Intracavitary vacuum degree is answered to be deteriorated suddenly, it is easy to operate and impurity will not be introduced, in addition, apparatus of the present invention turn with simple sample
Shifting and fixing means, can be in the intracavitary chemical reaction and electrical measurement for completing sample.
Claims (6)
1. a kind of vacuum reaction and test device, including reaction chamber (1), observation window (2), liquid container (3), linear actuator
(4), cooling rod (5), sample (6), specimen holder (7), sample stage (8), metallic rod (9), gas feed (10), vacuum pump I (11),
Bellows I (12), gate valve (13), bellows II (14), test chamber (15), specimen holder (16), driven rod (17), vacuum pump II
(18) and test circuit, xyz are three-dimensional coordinate system, and test chamber (15) is externally connected with vacuum pump II (18) and test circuit,
It is characterized in that:
Reaction chamber (1), bellows I (12), gate valve (13), bellows II (14) and test chamber (15) are sequentially connected, and work as gate valve
(13) when opening, vacuum pump II (18) can simultaneously be vacuumized reaction chamber (1) and test chamber (15), and reaction chamber (1) installation connects
It is connected to observation window (2), liquid container (3), metallic rod (9), gas feed (10) and vacuum pump I (11), dress in liquid container (3)
There is the reagent of liquid, the temperature of liquid container (3) is adjustable, and liquid container (3) outlet is located in reaction chamber (1), liquid container
(3) outlet has impulse electromagnetic valve, can control the amount of the reagent into reaction chamber (1)；Cooling rod (5) passes through linear drives
Device (4) is installed and connected in reaction chamber (1) above and cooling rod (5) lower end penetrates reaction chamber (1), passes through linear actuator (4) energy
Enough so that cooling rod (5) is relative to reaction chamber (1) lower movement in y-direction；Metallic rod (9) be installed on reaction chamber (1) below and
Metallic rod (9) upper end is located in reaction chamber (1), has air-tightness between metallic rod (9) and reaction chamber (1), metallic rod (9) can
Relative to reaction chamber (1) lower movement in y-direction, metallic rod (9) upper end is connected with sample stage (8), specimen holder (7) and sample in turn
Product (6) have aperture on specimen holder (7)；Driven rod (17) can pass through test chamber (15), bellows II (14), gate valve (13)
With bellows I (12), driven rod (17) front end is able to enter in reaction chamber (1), rear end is located at test chamber (15) outside, driven rod
(17) it can be movable in the z-direction and can be rotated around 360 degree of its axis, driven rod (17) front end has pincerlike mechanism, pincerlike machine
Structure can block specimen holder (7) two sides, can be by specimen holder (7) by driven rod (17) in the state that gate valve (13) are opened
It is installed on sample stage (8) or is removed from sample stage (8), and sample can be transmitted between reaction chamber (1) and test chamber (15)
Product seat (7), sample stage (8) position can be adjusted；
Cooling rod (5) includes liquid nitrogen container (5-1), inner tube (5-2), outer tube (5-3), sleeve (5-4), heater (5-5), cold head
(5-6), outlet (5-7) and cylindrical tube (5-8), inner tube (5-2) are coaxially nested in outer tube (5-3) and place in the y-direction, inner tube
The upper end (5-2) connects liquid nitrogen container (5-1), and the outer tube upper end (5-3) has outlet (5-7), has flow control at outlet (5-7)
Valve, the lower end outer tube (5-3) are connected with cold head (5-6), and the cold head (5-6) is that bottom surface radius is three millimeters, is highly four millimeters
And vertex cone directed downwardly, cylindrical tube (5-8) are coaxially nested on the outside of outer tube (5-3), sleeve (5-4) is coaxially nested in cylinder
It manages on the outside of (5-8), sleeve (5-4) is below 40 millimeters apart from cold head (5-6), installs having heaters (5- on the inside of sleeve (5-4)
5) vacuum layer, is all had between inner tube (5-2), outer tube (5-3) and cylindrical tube (5-8), under cold head (5-6) and inner tube (5-2)
Thermocouple is installed between end；
Specimen holder (16) is located in test chamber (15), and specimen holder (16) includes substrate (16-1), control stick (16-2), limit film
(16-3), support chip (16-4), preceding intermediate plate (16-5) and rear jaw (16-6), substrate (16-1) are connected in test chamber (15)
Upper side, control stick (16-2) can move up and down in the y-direction relative to test chamber (15), and the control stick upper end (16-2), which is located at, to be surveyed
Trying chamber (15) outside and mutually has air-tightness, and the control stick lower end (16-2) has barb, when driven rod (17) by specimen holder (7) from
When removing on sample stage (8) and being transmitted to test chamber (15), the barb is inserted into the aperture on specimen holder (7), so as to
The movement of specimen holder (7) is enough controlled, limit film (16-3) is screwed in substrate (16-1), limit film (16-3) and substrate
Distance is five millimeters between (16-1), and support chip (16-4) is located at below limit film (16-3) and is screwed in substrate
(16-1), distance is eight millimeters between support chip (16-4) and substrate (16-1), is pressed from both sides after being equipped with two pieces on support chip (16-4)
Intermediate plate (16-5) before piece (16-6) and two pieces, preceding intermediate plate (16-5) and rear jaw (16-6) all have elasticity, preceding intermediate plate (16-5)
It, can by control stick (16-2) with rear jaw (16-6) respectively by test circuit of the cable connection to test chamber (15) outside
So that specimen holder (7) upper end is inserted between the preceding intermediate plate (16-5) and rear jaw (16-6), and clamp specimen holder (7).
2. a kind of vacuum reaction according to claim 1 and test device, it is characterized in that: vacuum pump I (11) is that liquid nitrogen is cold
But absorption pump.
3. a kind of vacuum reaction according to claim 1 and test device, it is characterized in that: cold head (5-6) is by stainless steel
At.
4. a kind of vacuum reaction according to claim 1 and test device, it is characterized in that: inner tube (5-2) internal diameter is two millis
Rice, outer tube (5-3) internal diameter are six millimeters, and cylindrical tube (5-8) internal diameter is ten millimeters, length is 100 millimeters, sleeve (5-4) internal diameter
It is 40 millimeters for 24 millimeters, length.
5. a kind of vacuum reaction according to claim 1 and test device, it is characterized in that: control stick (16-2) diameter is three
Millimeter.
6. a kind of vacuum reaction according to claim 1 and test device, it is characterized in that: preceding intermediate plate (16-5) and rear jaw
(16-6) is made of metal tantalum.
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| CN201811431994.7A CN109499478B (en) | 2018-11-17 | 2018-11-17 | Vacuum reaction and testing device |
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| CN201811431994.7A CN109499478B (en) | 2018-11-17 | 2018-11-17 | Vacuum reaction and testing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112034150A (en) * | 2019-06-03 | 2020-12-04 | 杭州安旭科技有限公司 | Sample collection and detection device and method |
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