CN107715798A - The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure - Google Patents
The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure Download PDFInfo
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- CN107715798A CN107715798A CN201711040835.XA CN201711040835A CN107715798A CN 107715798 A CN107715798 A CN 107715798A CN 201711040835 A CN201711040835 A CN 201711040835A CN 107715798 A CN107715798 A CN 107715798A
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- support frame
- screw rod
- support plate
- anvil
- gas
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Links
- 238000012546 transfer Methods 0.000 claims abstract description 17
- 238000007639 printing Methods 0.000 claims abstract description 12
- 239000010979 ruby Substances 0.000 claims abstract description 10
- 229910001750 ruby Inorganic materials 0.000 claims abstract description 10
- 238000012544 monitoring process Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 230000005684 electric field Effects 0.000 claims abstract description 6
- 238000009738 saturating Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 63
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- 239000010432 diamond Substances 0.000 claims description 25
- 229910003460 diamond Inorganic materials 0.000 claims description 24
- 239000011521 glass Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000428 dust Substances 0.000 claims description 9
- 239000003822 epoxy resin Substances 0.000 claims description 8
- 238000002474 experimental method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229920000647 polyepoxide Polymers 0.000 claims description 8
- 239000013307 optical fiber Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000012495 reaction gas Substances 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 229910001120 nichrome Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000002309 gasification Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000545 Nickel–aluminium alloy Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 238000009156 water cure Methods 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
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
Abstract
The present invention relates to high pressure property fields of measurement, the device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure, supporting table is nonmagnetic, printing opacity, saturating x-ray, it can apply in highfield or high electric field or x ray experimentals, and without in support platform printing opacity, the state no interference signal in ruby fluorescence；Screw rod I, support frame I, screw rod II, support frame II, support screw, screw rod III, screw rod IV form pressing device, support frame I, support frame II are connected into the nested shape that intermeshes by screw rod I, screw rod III, screw rod IV and are from top to bottom support plate on support frame I, support plate under support plate, support frame II under support plate, support frame I on support frame II, rotary screw I can drive support frame II to move, and screw rod IV is through support plate on support frame II；Mobile lower top anvil is only needed to be compressed to realize；Energy video monitoring when gas is introduced close under gas boiling point, is introduced into sample gas and is cooled and liquefies in transfer tube outside device, avoid going out sample room.
Description
Technical field
The present invention relates to the reaction of the superpiezochemistry of high pressure property fields of measurement, particularly gas polymerisation, Neng Gou
Under the conditions of cryogenic high pressure gas polymerization is carried out under the conditions of a kind of cryogenic high pressure of its characteristic of forming gas polymer and in site measurement
The device of reaction.
Background technology
The gas polymerisation that can not be carried out under normal temperature and pressure can be realized under ultra-high pressure condition, current research finds lazy
Property gas super-pressure effect under can also show certain chemism.Simple molecular compound shape under super-pressure effect
Into the polymer of many different structures, such as under 10GPa pressure conditions, methane-hydrogen system can generate CH4(H2)2、
(CH4)2H2、CH4(H2)4、CH4H2Deng polymer.The transfer of electric charge caused by super-pressure acts on of some gas molecules forms
Various polymer, it has now been found that N2O and hydrogen have the polymer of different structure respectively.Find largely exist in ocean depths
Methane hydrate, then be a kind of cage structure material that the lower methane of high pressure effect and water are formed.Current High-Voltage Experimentation is also sent out
The gas hydrate of many new phases, such as Xe-H are showed2O and H2-H2O etc..In addition, great amount of carbon dioxide has been also found on the ocean bottom
Hydrate, this is considered as a kind of feasible method for reducing earth surface GHG carbon dioxide, have it is important should
Use prospect.
Diamond top anvil is the currently the only scientific experiment device that can produce million atmospheric pressure above static pressures, in height
Press irreplaceable in scientific research.Diamond top anvil is mainly made up of two parts, i.e., is directly contacted with sample and produce super-pressure
A pair of diamonds of power and the press for carrying out mechanical pressurization to diamond, and press with a diamond by fixing respectively
Cylindrical drum and piston portion form.The operation principle of diamond top anvil is that have minimum table top (general diameter using a pair
In tens micron dimensions) diamond mechanically extrude sample and produce hyperbaric environment, in two diamond mesa shapes
Into compressive plane between place the metal washer of sample well be pre-machined, sample is placed in sample well, the diameter of sample well
About 1/3rd of diamond mesa diameter.Need to be monitored the pressure that sample is subject in experimentation, current one
As the method composed usually using ruby fluorescence of pressure test method, it is necessary to which one block of ruby is placed in into top anvil together with sample
Sample room in, while collect its fluorescence sent.But prior art defect is as follows, if to reach larger pressure, just need
To use large volume of monoblock diamond, but diamond price, and the tungsten carbide of the substitute inexpensive as its
It is magnetic and light tight, is not suitable for some magnetical or optical related experiments, can be red if alternative materials such as sapphire in addition
Interference signal is produced in gemstone fluorescence spectrum；Need to be introduced into gaseous sample in the experiment of top anvil some, usually using low temperature side
Method and compressed gas method, low temperature method are that gas is cooled to the sample room that top anvil is re-introduced into after liquid or solid-state, its shortcoming
It is that temperature control is required for every kind of gas, once temperature control fails, sample can be changed into gaseous state from liquid rapidly so that sample cavity
Sample cavity is gone out full of bubble, or even by sample；Compressed gas method is first to be re-introduced into top to gas pressurized to 200MPa or so
The sample room of anvil, its shortcoming are to be filled with gases at high pressure in gas loading chamber, have certain danger, the method needs substantial amounts of
For sample gas with the compressed gas under conditions of 200MPa, cost is high, and for some expensive gases such as isotope gas
Body etc., then compressed gas method is not suitable for again, the device energy of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure
Solve the problems, such as.
The content of the invention
In order to solve the above problems, the present invention uses a kind of device of progress gas polymerisation under the conditions of cryogenic high pressure,
Can under the conditions of cryogenic high pressure forming gas polymer and in site measurement its characteristic.
The technical solution adopted in the present invention is：
The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure, mainly includes screw rod I, support frame I, spiral shell
Bar II, support frame II, support screw, piston portion, lower top anvil, upper top anvil, cylindrical drum part, supporting table, screw rod III, screw rod
IV, optical fiber, sample, epoxy resin, diamond dust, metal washer, thermometer, heater, cable, transfer tube and air accumulator,
The metal washer has external meters by cable connection, and support frame as described above I and support frame II are respectively by upper support plate, lower branch
Support plate, connecting rod composition, top anvil, the cylindrical barrel portion are mainly formed by cylindrical drum part, piston portion, upper top anvil and lower top anvil
There are threaded through holes above point, support frame as described above I upper support plate, lower support plate and the supporting table are respectively provided with vertical open-work,
Support frame as described above II upper support plate has screw, and the cylindrical drum is partially attached to supporting table lower surface, and the upper top anvil is consolidated
Due in cylindrical drum part, the upper surface of the lower top anvil connection piston portion, piston portion can be in cylindrical drum part interior edge z
Direction is moved, and the supporting table is connected to the lower section of support plate under support frame as described above I by screw rod II, and the piston portion passes through
Support screw is fixed on support frame as described above II lower support plate, has pad, institute between piston and support frame II lower support plate
State screw rod IV, screw rod III can move down support frame II lower support plate, piston portion is pushed downwards, it is upper top anvil and under
Distance becomes big between pushing up anvil, and so as to unclamp metal washer, the screw rod III and screw rod IV can realize that high accuracy is controllably sample
Room discharges pressure, after introducing liquid reaction gas, removes the screw rod IV and screw rod III, then rotary screw I so that top anvil can
It is compacted, with being respectively provided with pit at the upper surface of lower top anvil, sample exterior is enclosed with epoxy resin successively for the lower surface of upper top anvil
And diamond dust, be placed in a pair of metal washers, a pair of metal washers are truncated cone-shaped structure and its center have it is straight
Footpath 1mm hole, the shape of metal washer can snugly be embedded in the recessed of the lower surface of the upper top anvil and the lower upper surface for pushing up anvil
At hole, material is copper alloy, thickness 0.08mm, and thermometer and heater are respectively arranged in metal washer edge, and thermometer is by nickel
Aluminium alloy and nichrome are made, and the size of diamond dust is 0.2 micron of diameter, and optical fiber sequentially passes through the upper of support frame I
Support plate, support frame II upper support plate, support frame I lower support plate simultaneously connect with supporting table upper surface, transfer tube one end
Connect the cylindrical drum part, other end connection air accumulator, be reacting gas in air accumulator, by transfer tube can push up upwards anvil and
Reacting gas is passed through between the pit of lower top anvil, the top anvil of various configurations can be introduced a gas into, anvil and compressing member are pushed up in experiment
Be placed in a glass Dewar, liquid helium poured into glass Dewar to cool down top anvil, can use ccd video camera or video-frequency monitor or
Lens are by the window of glass Dewar, the situation in the anvil of observation top, and for the supporting table by synthesizing silicon carbide material manufacture, cost is low,
It is nonmagnetic, printing opacity, saturating x-ray, it can apply in highfield or high electric field or x- ray experimentals, and without being opened in supporting table
Mouth printing opacity, the state no interference signal in ruby fluorescence；The screw rod I, support frame I, screw rod II, support frame II, support screw, spiral shell
Bar III, screw rod IV constitute applies stressed pressing device for opposed anvils, and support frame as described above I, support frame II pass through the spiral shell
Bar I, screw rod III, screw rod IV connect into the nested shape to intermesh and are from top to bottom support frame I upper support plate, support frame
II upper support plate, support frame I lower support plate, support frame II lower support plate, the rotary screw I lower ends are articulated with described
Support frame II, upper end are located at support frame as described above I upper support plate, by rotary screw I support frame II can be driven to move up and down,
When support frame II is moved up, piston portion moves up, with can opposed anvils produce pressure, the screw rod IV penetratingly screws in
The screw of support frame as described above II upper support plate, the screw rod III upper ends are connected to below screw rod IV, lower end passes through the support
The open-work of support plate and the supporting table under frame I, and the threaded through holes that penetratingly screw in above cylindrical drum part and with the work
Plug portion upper surface；Device only to need to produce pressure to realize compression, suitable for various pistons by mobile lower top anvil
With the top anvil of cylindrical structure；Can be by video monitoring, to avoid when introducing gas at a temperature of close to gas boiling point
Sample introduces bubble during introducing, and low to the temperature control precise requirements of sample gas, the sample gas of introducing is in device
It is cooled and liquefies in outside transfer tube, sample can be avoided to gasify in the packing ring of top anvil so that being rushed out sample room.
Using under the conditions of a kind of cryogenic high pressure carry out gas polymerisation device tested the step of be：
One, is introduced before gas, and using water as calibration sample, the pressure of calibrating installation, passes through ruby at room temperature
Fluorescent method carries out pressure measxurement, and determines to push up the relation in anvil between pressure and the rotational angle of the screw rod I；
The epoxy resin and diamond dust are placed in metal washer inner surface, the upper top anvil and lower top anvil by two,
Water and a small amount of air are filled between contact surface in pit, and is put into a ruby bead for pressure measurement；
Three, by push up anvil be placed in pressing device, screw rod I described in fine rotation cause push up anvil, it is lower top anvil contact surface it
Between metal washer sealing, by monitor observe the upper top anvil, lower top anvil, the part such as metal washer state；
Device is transferred to glass Dewar by four, and liquid helium is added into glass Dewar；
Five, open air accumulator, and the reacting gas in it is introduced into top anvil by transfer tube, reacting gas is filled with two in pipe
Minute, the air in device is discharged, liquid helium pours into glass Dewar, when the temperature of Dewar is down to 250K, unclamps the screw rod
I, volume increase after the water cure in the metal washer so that metal washer unclamps；
Six, continue to be down to 25K when the temperature in the anvil of top, close to reacting gas boiling point when, the reaction gas in release device
Body, liquefied reacting gas is observed by monitoring, while screw the screw rod I；
After the completion of seven, reacting gas introduce, pressing device and top anvil are taken out from glass Dewar, as temperature rises,
The screw rod I is adjusted, until angle when being calibrated at room temperature in above-mentioned steps one；
Eight, remove the screw rod III and screw rod IV after temperature is raised to room temperature, screw the screw rod I to produce pressure；
Nine, will push up anvil and be taken out from pressing device, and further screw the screw rod I, and so, sample is further compressed,
Gas polymer is generated after the reaction of liquid reaction gas and water；
Ten, carry out in site measurement by connecting the external meters of metal washer, to sample.
The beneficial effects of the invention are as follows：
The present invention is applied to gas polymer for the mechanism of pressure between the anvil of release top, and the metal washer is in light weight,
Thermometer and heater are installed on metal washer edge so that thermometer is not stressed；Use the bortz powder of 0.2 micron-scale
End is placed in top on the outside of sample, can isolate the heat for pushing up anvil with metal washer.Use the less diamond of size and synthesis
The combination of carborundum supporting table, the pressure same with larger diamond top anvil can be reached, cost is low, nonmagnetic, printing opacity, thoroughly
X-ray, it can apply in highfield or high electric field or x- ray experimentals, particularly in x-ray experiment, without in supporting table
Upper shed printing opacity, and signal is not interfered with ruby fluorescence；The special compressing structure of the present apparatus, it is only necessary to pass through movement
The top anvil of side produces pressure, can be used in the top anvil of various piston-cylindrical structures；Because the introducing of gas is to connect
Completed at a temperature of nearly gas boiling point, reduce the waste of under test gas, further, since have video monitoring, can be in sample
Avoid introducing bubble during introducing, so, without there is accurate temperature control to sample gas, furthermore, the sample gas of introducing
Body is cooled and liquefied in the transfer tube outside device, and sample will not gasify so that sample is rushed out sample in the packing ring of top anvil
Product room.
Brief description of the drawings
Further illustrated with reference to the figure of the present invention：
Fig. 1 is schematic structural view of the invention；
Fig. 2 is Fig. 1 schematic top plan view；
Fig. 3 is top anvil contact surface close-up schematic view.
In figure, 1. screw rod I, 2. support frame I, 3. screw rod II, 4. support frame II, 5. support screws, 6. piston portions, 7-1.
Lower top anvil, pushes up anvil on 7-2., 7-3. cylindrical drums part, 8. supporting tables, 9. screw rod III, 10. screw rod IV, 11. optical fiber, 12. samples
Product, 13. epoxy resin, 14. diamond dusts, 15. metal washers, 16. thermometers, 17. heaters.
Embodiment
If Fig. 1 is schematic structural view of the invention, if Fig. 2 is Fig. 1 schematic top plan view, mainly include screw rod I (1), support
Frame I (2), screw rod II (3), support frame II (4), support screw (5), piston portion (6), it is lower top anvil (7-1), it is upper top anvil (7-2),
Cylindrical drum part (7-3), supporting table (8), screw rod III (9), screw rod IV (10), optical fiber (11), sample (12), epoxy resin
(13), diamond dust (14), metal washer (15), thermometer (16), heater (17), cable, transfer tube and air accumulator, institute
State metal washer (15) has external meters by cable connection, and support frame as described above I (2) and support frame II (4) are respectively by upper branch
Support plate, lower support plate, connecting rod composition, mainly by cylindrical drum part (7-3), piston portion (6), upper top anvil (7-2) He Xiading
Anvil (7-1) composition top anvil, the cylindrical drum part (7-3) have a threaded through holes above, support frame as described above I (2) upper support plate,
Lower support plate and the supporting table (8) are respectively provided with vertical open-work, and support frame as described above II (4) upper support plate has screw, described
Cylindrical drum part (7-3) is connected to supporting table (8) lower surface, and the upper top anvil (7-2) is fixed in cylindrical drum part (7-3),
The upper surface of lower top anvil (7-1) the connection piston portion (6), piston portion (6) can be in cylindrical drum part (7-3) interior edge z
Direction is moved, and the supporting table (8) is connected to the lower section of support plate under support frame as described above I (2), the work by screw rod II (3)
Plug portion (6) is fixed on support frame as described above II (4) lower support plate by supporting screw (5), piston with support frame II (4)
There is pad, the screw rod IV (10), screw rod III (9) can make support frame II (4) lower support plate to moving down between support plate
Dynamic, piston portion (6) is pushed downwards, and distance becomes big between upper top anvil (7-2) and lower top anvil (7-1), so as to unclamp metal washer
(15), the screw rod III (9) and screw rod IV (10) can realize that high accuracy controllably discharges pressure for sample room, and it is anti-to introduce liquid
After answering gas, the screw rod IV (10) and screw rod III (9) are removed, then rotary screw I (1) be so that top anvil can be compacted, optical fiber
(11) sequentially pass through support frame I (2) upper support plate, support frame II (4) upper support plate, support frame I (2) lower support plate,
And connect the cylindrical drum part (7-3), other end connection air accumulator, storage with supporting table (8) upper surface, transfer tube one end
It is reacting gas in gas tank, can be upwards pushed up by transfer tube and be passed through reaction gas between anvil (7-2) and the pit of lower top anvil (7-1)
Body, the top anvil of various configurations can be introduced a gas into, push up anvil in experiment and compressing member is placed in a glass Dewar, glass Dewar
In pour into liquid helium to cool down top anvil, ccd video camera or video-frequency monitor or lens can be used to pass through the window of glass Dewar, observation top
Situation in anvil.
For the supporting table (8) by synthesizing silicon carbide material manufacture, cost is low, nonmagnetic, printing opacity, saturating x-ray, can apply
In highfield or high electric field or x- ray experimentals, and without supporting table (8) upper shed printing opacity, in ruby fluorescence without dry
Disturb signal；The screw rod I (1), support frame I (2), screw rod II (3), support frame II (4), support screw (5), screw rod III (9),
Screw rod IV (10) constitutes applies stressed pressing device for opposed anvils, and support frame as described above I (2), support frame II (4) pass through institute
Screw rod I (1), screw rod III (9), screw rod IV (10) is stated to connect into the nested shape to intermesh and be support frame I (2) from top to bottom
Upper support plate, support frame II (4) upper support plate, support frame I (2) lower support plate, support frame II (4) lower support plate,
Rotary screw I (1) lower end is articulated with support frame as described above II (4), upper end is located at support frame as described above I (2) upper support plate, leads to
Crossing rotary screw I (1) can drive support frame II (4) to move up and down, when support frame II (4) is moved up, piston portion (6) to
Upper movement, with can opposed anvils produce pressure, the screw rod IV (10) penetratingly screws in support frame as described above II (4) upper support plate
Screw, screw rod III (9) upper end is connected to below screw rod IV (10), lower end passes through support plate under support frame as described above I (2)
With the open-work of the supporting table (8), and penetratingly screw in cylindrical drum part (7-3) threaded through holes above and with the piston
Partly (6) upper surface；Device only to need to produce pressure to realize compression, suitable for various pistons by mobile lower top anvil
With the top anvil of cylindrical structure；Can be by video monitoring, to avoid when introducing gas at a temperature of close to gas boiling point
Sample introduces bubble during introducing, and low to the temperature control precise requirements of sample gas, the sample gas of introducing is in device
It is cooled and liquefies in outside transfer tube, sample can be avoided to gasify in the packing ring of top anvil so that being rushed out sample room.
As Fig. 3 be top anvil contact surface close-up schematic view, it is upper top anvil (7-2) lower surface with it is lower push up anvil (7-1) it is upper
Pit is respectively provided with surface, epoxy resin (13) and diamond dust (14) is enclosed with successively outside sample (12), is placed in one
To in metal washer (15), a pair of metal washers (15) are the hole that truncated cone-shaped structure and its center have diameter 1mm, golden
The shape of category packing ring (15) can snugly be embedded in the lower surface and the upper surface of lower top anvil (7-1) of the upper top anvil (7-2)
Pit, material are copper alloy, and thickness 0.08mm, thermometer (16) and heater (17) are respectively arranged in metal washer (15) side
Edge, thermometer (16) are made up of nickel alumin(i)um alloy and nichrome, and the size of diamond dust (14) is 0.2 micron of diameter.
The present invention can be reached and larger gold using the combination of the less diamond of size and synthesizing silicon carbide supporting table
The same pressure of hard rock top anvil, cost is low, nonmagnetic, printing opacity, saturating x-ray, can apply and be penetrated in highfield or high electric field or x-
In line experiment, and need not be in support platform printing opacity, and do not interfere with signal in ruby fluorescence spectrum；The present apparatus it is special
Compressing structure, it is only necessary to pressure is produced by the top anvil of mobile side, can be used in the top of various piston-cylindrical structures
In anvil, the preparation of gas polymer samples is particularly suitable for, and reduces the waste of under test gas, and top can be effectively isolated
Heat conduction between anvil and metal washer.Further, since there are video monitoring and the gas quilt in the transfer tube outside device
Cool down and liquefy, avoid the introducing of bubble during sample introduces, and sample will not gasify so that sample in the packing ring of top anvil
Product are rushed out sample room.
Claims (1)
1. carrying out the device of gas polymerisation under the conditions of a kind of cryogenic high pressure, mainly include screw rod I (1), support frame I (2), spiral shell
Bar II (3), support frame II (4), support screw (5), piston portion (6), lower top anvil (7-1), upper top anvil (7-2), cylindrical barrel portion
Divide (7-3), supporting table (8), screw rod III (9), screw rod IV (10), optical fiber (11), sample (12), epoxy resin (13), diamond
Powder (14), metal washer (15), thermometer (16), heater (17), cable, transfer tube and air accumulator, the metal washer
(15) there are external meters by cable connection, support frame as described above I (2) and support frame II (4) are respectively by upper support plate, lower support
Disk, connecting rod composition, mainly it is made up of cylindrical drum part (7-3), piston portion (6), upper top anvil (7-2) and lower top anvil (7-1)
Push up anvil, the cylindrical drum part (7-3) has a threaded through holes above, support frame as described above I (2) upper support plate, lower support plate and
The supporting table (8) is respectively provided with vertical open-work, and support frame as described above II (4) upper support plate has screw, the cylindrical drum part
(7-3) is connected to supporting table (8) lower surface, and the upper top anvil (7-2) is fixed in cylindrical drum part (7-3), the lower top anvil
The upper surface of (7-1) connection piston portion (6), piston portion (6) can be movable in the z-direction in cylindrical drum part (7-3), institute
The lower section that supporting table (8) is connected to support plate under support frame as described above I (2) by screw rod II (3) is stated, the piston portion (6) is logical
The lower support plate that support screw (5) is fixed on support frame as described above II (4) is crossed, between piston and support frame II (4) lower support plate
With pad, the screw rod IV (10), screw rod III (9) can move down support frame II (4) lower support plate, piston portion
(6) are divided to be pushed downwards, distance becomes big between upper top anvil (7-2) and lower top anvil (7-1), described so as to unclamp metal washer (15)
Screw rod III (9) and screw rod IV (10) can realize that high accuracy controllably discharges pressure for sample room, after introducing liquid reaction gas,
Remove the screw rod IV (10) and screw rod III (9), then rotary screw I (1) be so that top anvil can be compacted, upper top anvil (7-2)
Lower surface be respectively provided with pit at the upper surface of lower top anvil (7-1), be enclosed with successively outside sample (12) epoxy resin (13) and
Diamond dust (14), be placed in a pair of metal washers (15), a pair of metal washers (15) be truncated cone-shaped structure and its
Center has a diameter 1mm hole, the shape of metal washer (15) can snugly be embedded in the lower surface of the upper top anvil (7-2) with
The pit of the upper surface of lower top anvil (7-1), material are copper alloy, thickness 0.08mm, thermometer (16) and heater (17) point
Metal washer (15) edge is not installed on, and thermometer (16) is made up of nickel alumin(i)um alloy and nichrome, diamond dust (14)
Size be 0.2 micron of diameter, optical fiber (11) sequentially passes through the upper support of support frame I (2) upper support plate, support frame II (4)
Disk, support frame I (2) lower support plate simultaneously connect the cylindrical drum part with supporting table (8) upper surface, transfer tube one end
(7-3), the other end connect air accumulator, are reacting gas in air accumulator, anvil (7-2) and lower top anvil can be pushed up upwards by transfer tube
Reacting gas is passed through between the pit of (7-1), the top anvil of various configurations can be introduced a gas into, anvil is pushed up in experiment and compressing member is put
In a glass Dewar, liquid helium is poured into glass Dewar to cool down top anvil, ccd video camera or video-frequency monitor or saturating can be used
Mirror is by the window of glass Dewar, the situation in the anvil of observation top, it is characterized in that：The supporting table (8) is by synthesizing silicon carbide material system
Make, nonmagnetic, printing opacity, saturating x-ray, can apply in highfield or high electric field or x- ray experimentals, and without in supporting table
(8) upper shed printing opacity, the state no interference signal in ruby fluorescence；The screw rod I (1), support frame I (2), screw rod II (3), support
Frame II (4), support screw (5), screw rod III (9), screw rod IV (10) are constituted and are applied stressed pressing device for opposed anvils,
Support frame as described above I (2), support frame II (4) are connected into mutually intersecting by the screw rod I (1), screw rod III (9), screw rod IV (10)
Wrong nested shape and be from top to bottom support frame I (2) upper support plate, support frame II (4) upper support plate, support frame I (2)
Lower support plate, support frame II (4) lower support plate, rotary screw I (1) lower end be articulated with support frame as described above II (4), on
End can drive support frame II (4) to move up and down, prop up positioned at support frame as described above I (2) upper support plate by rotary screw I (1)
When support II (4) is moved up, piston portion (6) moves up, with can opposed anvils produce pressure, the screw rod IV (10) passes through
Screw in the screw of support frame as described above II (4) upper support plate with wearing, screw rod III (9) upper end is connected under screw rod IV (10)
Side, lower end pass through the open-work of support plate and the supporting table (8) under support frame as described above I (2), and penetratingly screw in cylindrical drum part
(7-3) threaded through holes above and with the piston portion (6) upper surface；Device only to need by mobile lower top anvil
Produce pressure to compress to realize, suitable for various pistons and the top anvil of cylindrical structure；Draw at a temperature of close to gas boiling point
Can be by video monitoring, to avoid introducing bubble during sample introduces, to the temperature control of sample gas when entering gas
Precise requirements are low, and the sample gas being introduced into is cooled and liquefied in the transfer tube outside device, and sample can be avoided to push up
Gasification is so that be rushed out sample room in the packing ring of anvil.
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| CN201711040835.XA CN107715798A (en) | 2017-10-20 | 2017-10-20 | The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure |
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| CN201711040835.XA CN107715798A (en) | 2017-10-20 | 2017-10-20 | The device of gas polymerisation is carried out under the conditions of a kind of cryogenic high pressure |
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| CN108717064A (en) * | 2018-05-10 | 2018-10-30 | 上海交通大学 | A kind of more outfield material structures of Microfocus X-ray X-ray and performance fibers characterization technique |
| CN109444191A (en) * | 2018-11-27 | 2019-03-08 | 金华职业技术学院 | A kind of high pressure sample test method of pulsed laser heating |
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