CN115672212B - Method for removing silicon mold cores of microporous shell type HDC microspheres - Google Patents
Method for removing silicon mold cores of microporous shell type HDC microspheres Download PDFInfo
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- CN115672212B CN115672212B CN202211029778.6A CN202211029778A CN115672212B CN 115672212 B CN115672212 B CN 115672212B CN 202211029778 A CN202211029778 A CN 202211029778A CN 115672212 B CN115672212 B CN 115672212B
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- 239000004005 microsphere Substances 0.000 title claims abstract description 87
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 34
- 239000010703 silicon Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 86
- 238000005260 corrosion Methods 0.000 claims abstract description 42
- 238000003860 storage Methods 0.000 claims abstract description 36
- 230000007797 corrosion Effects 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 238000005530 etching Methods 0.000 claims description 21
- 239000011261 inert gas Substances 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000006187 pill Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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Abstract
The invention discloses a microporous shell type HDC microsphere silicon mold core corrosion device, which comprises a pressure tank, wherein one side of the top end of the pressure tank is communicated with an air inlet pipe, the other side of the top end of the pressure tank is communicated with an air outlet pipe, and a first electromagnetic valve is arranged on the air inlet pipe; a second electromagnetic valve is arranged on the air outlet pipe; the pressure tank is internally provided with an HDC microsphere storage device for preventing the HDC microsphere from floating upwards, and the HDC microsphere storage device is of a cage-shaped structure. The invention uses pressure difference to accelerate the process of corrosive liquid entering into HDC microspheres and removing products, and has the beneficial effects of improving production efficiency and guaranteeing production quality.
Description
Technical Field
The invention relates to the field of carbon material processing and forming, in particular to a method for removing a silicon mold core of a shell-type HDC microsphere with micropores.
Background
In the research of laser indirect drive Inertial Confinement Fusion (ICF), a target is an important material basis of the ICF research, wherein a target pill is used as a container for loading fusion fuel, and parameters such as materials, diameters, thicknesses and the like of the target pill can influence the results of physical experiments. Compared with other target pills (polymer target pills and glass target pills), the high-density carbon (HDC) target pill has the advantages of high density, high X-ray absorptivity, high thermal conductivity and the like, so that the high-density carbon (HDC) target pill is favored by physical experiments, and the quality is considered as the key of the success of the physical experiments.
The preparation of the HDC target pill comprises five steps of polishing a silicon mandrel, coating a film, polishing the HDC, processing corrosion holes by laser and removing the silicon mandrel. The step of removing the silicon mold core is to remove the silicon mold core in the target ball by adopting a chemical etching method, wherein etching liquid enters from the etching holes to gradually etch away the silicon mold core, and the products are discharged from the etching holes, so that the HDC microspheres are obtained. The diameter of the corrosion hole is 2-20 mu m, so that the corrosion liquid is difficult to enter and the products are discharged, the corrosion rate is very slow, the preparation progress of the HDC target pill is directly influenced, and residues exist in the target pill due to the difficult discharge of the products, so that the quality of the target pill is influenced.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a method for removing a silicon mold core of HDC microsphere with a microporous shell layer, comprising a pressure tank having an air inlet pipe connected through to one side of the top end thereof and an air outlet pipe connected through to the other side of the top end thereof;
the air inlet pipe is provided with a first electromagnetic valve;
a second electromagnetic valve is arranged on the air outlet pipe;
The pressure tank is internally provided with an HDC microsphere storage device for preventing the HDC microsphere from floating upwards, and the HDC microsphere storage device is of a cage-shaped structure.
Preferably, the pressure gauge further comprises a pressure gauge for measuring the pressure inside the pressure tank, the pressure gauge is arranged at the middle position of the top end of the pressure tank, and the pressure gauge is arranged as a corrosion-proof pressure gauge.
Preferably, the manner of disposing the HDC microsphere storage device in the pressure tank is as follows: the inside of the pressure tank is also provided with an etching solution container for storing etching solution, and the HDC microsphere storage device is placed at the bottom in the etching solution container.
Preferably, wherein the pressure tank includes:
A high pressure resistant rigid canister;
and the corrosion-resistant liner is sleeved in the rigid tank body.
Preferably, the air inlet pipe is a corrosion-resistant air inlet pipe, and the air outlet pipe is a corrosion-resistant air outlet pipe.
Preferably, the method further comprises: the anti-corrosion plate is used for separating the inner space of the pressure tank, is arranged in the pressure tank, the peripheral wall of the anti-corrosion plate is in sealing connection with the inner wall of the pressure tank through a sealing ring, a plurality of supporting feet are symmetrically and fixedly connected to the bottom end of the anti-corrosion plate, the bottom ends of the supporting feet are propped against the inner bottom end of the pressure tank, annular protrusions are integrally formed in the middle position of the top end of the anti-corrosion plate in a protruding mode, and the annular protrusions are sleeved on the bottom of the corrosive liquid container and are connected.
A method for removing a silicon mold core of an HDC microsphere with a microporous shell layer comprises the following steps:
firstly, filling HDC microspheres into an HDC microsphere storage device;
placing the HDC microsphere storage device into an etching liquid container, and adding etching liquid into the etching liquid container, wherein the liquid level of the etching liquid is higher than that of the HDC microsphere storage device;
Step three, placing the corrosive liquid container into an inner container, placing the inner container into a rigid tank body, and sealing the rigid tank body;
Step four, closing a second electromagnetic valve and opening a first electromagnetic valve, and injecting inert gas into the pressure tank through an air inlet pipeline to carry out pressurization so that the corrosive liquid enters the HDC microspheres;
Step five, closing the first electromagnetic valve after pressurization is completed, and opening the second electromagnetic valve after 1-30 minutes, wherein the inert gas is naturally discharged from an air outlet pipe, so that a product is discharged from the HDC microspheres;
And step six, after 1 to 30 minutes, closing the second electromagnetic valve again and opening the first electromagnetic valve, injecting inert gas into the pressure tank through the air inlet pipeline for pressurizing, and repeating the operation at intervals of 1 to 30 minutes until the silicon mold cores in the HDC microspheres are completely corroded, and discharging the product.
Preferably, the etching solution comprises a mixed solution of hydrofluoric acid and nitric acid, the volume ratio of the hydrofluoric acid to the nitric acid is 1:3-6:1, and the internal temperature of the pressure tank in the etching process is 20-50 ℃.
Preferably, the inert gas is any one of nitrogen and argon.
Preferably, the pressure of the inert gas for pressurization is 0.2-0.6 mpa.
The invention at least comprises the following beneficial effects:
Firstly, the invention uses the pressure difference to accelerate the process of corrosive liquid entering into the HDC microspheres and removing the products, and has the beneficial effects of improving the production efficiency and guaranteeing the production quality.
Secondly, in the invention, the corrosive liquid is isolated from the pressure tank through the corrosive liquid container, so that other substances generated by reaction between the corrosive liquid and the isolating tank can be effectively avoided, and the method has the advantages of ensuring the production quality, reducing the manufacturing cost and being convenient to control.
Thirdly, in the invention, the rigid tank body is subjected to the pressure generated by injecting inert gas, and the corrosive liquid is isolated from the rigid tank body through the liner, so that the influence of the corrosive liquid on the tightness caused by the corrosion of the rigid tank body is avoided, and the mode has the advantage of prolonging the service life.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a cross-sectional view of the present invention.
Fig. 3 is a schematic view of the corrosion protection plate structure of the present invention.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description. It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof. It should be noted that, in the description of the present invention, the orientation or positional relationship indicated by the term is based on the orientation or positional relationship shown in the drawings, which are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "configured to," "engaged with," "connected to," and the like are to be construed broadly, and for example, "connected" may be a fixed connection, may be a detachable connection, or may be integrally connected, may be mechanically connected, may be electrically connected, may be directly connected, may be indirectly connected through an intermediate medium, may be communication between two members, and may be understood in a specific manner by those skilled in the art. Furthermore, in the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be a direct contact of the first and second features, or an indirect contact of the first and second features through an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
Fig. 1 shows an implementation of the invention comprising: the pressure tank 1, the top one side through connection of pressure tank 1 has intake pipe 11, the top opposite side through connection of pressure tank 1 has outlet duct 12, its characterized in that:
the air inlet pipe 11 is provided with a first electromagnetic valve 13;
The air outlet pipe 12 is provided with a second electromagnetic valve 14;
The pressure tank 1 is internally provided with an HDC microsphere storage device 3 for preventing the HDC microsphere 2 from floating upwards, and the HDC microsphere storage device 3 is of a cage-shaped structure.
Working principle: placing the HDC microspheres 2 into the HDC microsphere storage 3, placing the HDC microsphere storage 3 into the pressure tank 1, injecting the corrosive liquid 6 into the pressure tank 1, completely submerging the corrosive liquid 6 into the HDC microsphere storage 3, closing the first electromagnetic valve 13 and opening the second electromagnetic valve 14 after the corrosive liquid 6 is completely submerged in the HDC microsphere storage 3, discharging the inert gas in the pressure tank 1 through the air outlet pipe 12 after the corrosive liquid 6 is reacted with the silicon mold core for a period of time, removing the generated substances of the corrosive liquid and the silicon in the HDC microsphere 2 under the action of pressure difference, closing the electromagnetic valve 14 after the generated substances are removed under the action of pressure difference, and repeatedly injecting the inert gas into the silicon mold core through the air inlet pipe 11 after the corrosive liquid is completely discharged into the pressure tank 1, and the inert gas is completely injected into the silicon mold core 2 after the corrosive liquid 2 is completely discharged into the pressure tank 1, closing the electromagnetic valve 14 after the air inlet pipe 11 is sealed, and the corrosive liquid 6 is completely injected into the silicon mold core through the pressure tank 1, and the inert gas is completely injected into the silicon mold core after the corrosive liquid is completely discharged into the pressure tank 1, and the corrosive liquid is completely discharged into the silicon mold core after the corrosive liquid is completely submerged in the pressure tank 2. In the technical scheme, the pressure difference is utilized to accelerate the process of the corrosive liquid 6 entering the HDC microspheres 2 and the removal of the products, and the method has the beneficial effects of improving the production efficiency and guaranteeing the production quality.
In the above scheme, the pressure gauge 4 for measuring the pressure inside the pressure tank 1 is further included, and is arranged at the middle position of the top end of the pressure tank 1, and the pressure gauge 4 is arranged as the corrosion-proof pressure gauge 4. Through the manometer 4 that sets up, can be audio-visual to the inside pressure of staff feedback pressure jar 1, the staff of being convenient for is to the accuse to the quantity of injection inert gas in pressure jar 1 to set up manometer 4 into anticorrosive manometer 4, can prevent effectively that evaporation residual corrosive liquid from damaging manometer 4, have guarantee production quality, increase of service life, the advantage of being convenient for control.
In the above-described aspect, the manner of disposing the HDC microsphere storage device 3 in the pressure tank 1 is as follows: the inside of the pressure tank 1 is also provided with an etching solution container 5 for storing etching solution 6, and the HDC microsphere storage device 3 is placed at the bottom in the etching solution container 5. Through the mode of depositing corrosive liquid 6 in corrosive liquid container 5, the staff of being convenient for adds and retrieves corrosive liquid 6 to can effectively control corrosive liquid 6 quantity, reduce unnecessary corrosive liquid 6, keep apart corrosive liquid 6 and overhead tank 1 through corrosive liquid container 5, can effectively avoid producing the reaction between corrosive liquid 6 and overhead tank 1 and produce other substances, have guarantee production quality, reduce manufacturing cost, be convenient for control's advantage.
In the above-described aspect, the pressure tank 1 includes:
A rigid tank 15 resistant to high pressure;
and the corrosion-resistant liner 16 is sleeved in the rigid tank body 15.
Working principle: the rigid tank body 15 bears the pressure generated by injecting inert gas, the corrosive liquid 6 is isolated from the rigid tank body 15 through the liner 16, the influence of the corrosive liquid 6 on the tightness caused by the corrosion of the rigid tank body 15 is avoided, and the mode has the advantage of prolonging the service life.
In the above-mentioned scheme, the air inlet pipe 11 is set as a corrosion-resistant air inlet pipe 11, and the air outlet pipe 12 is set as a corrosion-resistant air outlet pipe 12. Through the corrosion-resistant air inlet pipe 11 and the corrosion-resistant air outlet pipe 12, the corrosion damage of the corrosive liquid 6 can be effectively prevented, and the device has the advantages of prolonging the service life and guaranteeing the working efficiency.
In the above scheme, the method further comprises: the anti-corrosion plate is used for separating the inner space of the pressure tank, is arranged in the pressure tank, the peripheral wall of the anti-corrosion plate is in sealing connection with the inner wall of the pressure tank through a sealing ring, a plurality of supporting feet are symmetrically and fixedly connected to the bottom end of the anti-corrosion plate, the bottom ends of the supporting feet are propped against the inner bottom end of the pressure tank, annular protrusions are integrally formed in the middle position of the top end of the anti-corrosion plate in a protruding mode, and the annular protrusions are sleeved on the bottom of the corrosive liquid container and are connected.
Working principle: when processing HDC microballon 2, put into anticorrosion plate 7 in pressure tank 1, anticorrosion plate 7 passes through sealing washer 72 and pressure tank 1's inner wall sealing connection, separate pressure tank 1 inside into two sealed independent spaces, thereby reach the purpose of reducing inert gas quantity, and support anticorrosion plate 7 in pressure tank 1 through a plurality of supporting legs 71, prevent that anticorrosion plate 7 produces the displacement when pressure tank 1 is inside pressure boost, the position of corrosion solution container 5 is restricted to the rethread annular protrusion 73, prevent that corrosion solution container 5 from turning on one's side and causing the condition that corrosion solution 6 flows out to take place in the operation in-process, and anticorrosion plate 7 all has the corrosion resistance, stable in nature can multiple cycle use, adopt this kind of mode to have the advantage of reduction manufacturing cost, guarantee structural stability.
Example 1:
firstly, loading HDC microspheres 2 with the diameter of 2000 microns and the corrosion aperture of 20 microns into an HDC microsphere storage device 3;
Step two, placing the HDC microsphere storage device 3 into a corrosive liquid container 5, and adding corrosive liquid 6 into the corrosive liquid container 5, wherein the liquid level of the corrosive liquid 6 is higher than the height of the HDC microsphere storage device 3, the corrosive liquid 6 consists of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 1:1;
Step three, placing the corrosive liquid container 5 into an inner container 16, placing the inner container 16 into a rigid tank body 15, and sealing the rigid tank body 15;
step four, closing a second electromagnetic valve 14 and opening a first electromagnetic valve 13, and injecting nitrogen into the pressure tank 1 through the air inlet pipeline 11 to carry out pressurization so that the corrosive liquid 6 enters the HDC microspheres 2;
step five, observing the reading of the pressure gauge 4, closing the first electromagnetic valve 13 when the pressure value reaches 0.35MPa, opening the second electromagnetic valve 14 after 10 minutes, and naturally discharging the nitrogen through the air outlet pipe 12 to discharge the product from the HDC microspheres 2;
Step six, after 10 minutes, the second electromagnetic valve 14 is closed again, the first electromagnetic valve 13 is opened, nitrogen is injected into the pressure tank 1 through the air inlet pipeline 11 to be pressurized to 0.35MPa, the operation is repeated at intervals of 10 minutes, after 120 hours, the silicon mold core inside the HDC microsphere 2 is completely corroded, and the product is completely discharged.
Example 2:
Firstly, loading HDC microspheres 2 with the diameter of 2000 microns and the corrosion aperture of 10 microns into an HDC microsphere storage device 3;
step two, placing the HDC microsphere storage device 3 into a corrosive liquid container 5, and adding corrosive liquid 6 into the corrosive liquid container 5, wherein the liquid level of the corrosive liquid 6 is higher than the height of the HDC microsphere storage device 3, the corrosive liquid 6 consists of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 3:1;
Step three, placing the corrosive liquid container 6 into an inner container 16, then placing the inner container 16 into a rigid tank body 15, sealing the rigid tank body 15, and placing the whole pressure tank 1 into a constant-temperature oven, wherein the temperature is kept at 40 ℃;
step four, closing a second electromagnetic valve 14 and opening a first electromagnetic valve 13, and injecting nitrogen into the pressure tank 1 through the air inlet pipeline 11 to carry out pressurization so that the corrosive liquid 6 enters the HDC microspheres 2;
Step five, observing the reading of the pressure gauge 4, closing the first electromagnetic valve 13 when the pressure value reaches 0.5MPa, opening the second electromagnetic valve 14 after 10 minutes, and naturally discharging the nitrogen through the air outlet pipe 12 to discharge the product from the HDC microspheres 2;
step six, after 10 minutes, the second electromagnetic valve 14 is closed again, the first electromagnetic valve 13 is opened, nitrogen is injected into the pressure tank 1 through the air inlet pipeline 11 to be pressurized to 0.5MPa, the operation is repeated at intervals of 10 minutes, after 72 hours, the silicon mold core inside the HDC microsphere 2 is completely corroded, and the product is completely discharged.
Example 3:
firstly, loading HDC microspheres 2 with the diameter of 900 microns and the corrosion aperture of 10 microns into an HDC microsphere storage device 3;
step two, placing the HDC microsphere storage device 3 into a corrosive liquid container 5, and adding corrosive liquid 6 into the corrosive liquid container 5, wherein the liquid level of the corrosive liquid 6 is higher than the height of the HDC microsphere storage device 3, the corrosive liquid 6 consists of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 3:1;
Step three, placing the corrosive liquid container 5 into an inner container 16, placing the inner container 16 into a rigid tank body 15, and sealing the rigid tank body 15;
step four, closing a second electromagnetic valve 14 and opening a first electromagnetic valve 13, and injecting nitrogen into the pressure tank 1 through the air inlet pipeline 13 to carry out pressurization so that the corrosive liquid 6 enters the HDC microspheres 2;
step five, observing the reading of the pressure gauge 4, closing the first electromagnetic valve 13 when the pressure value reaches 0.35MPa, opening the second electromagnetic valve 14 after 10 minutes, and naturally discharging the nitrogen through the air outlet pipe 12 to discharge the product from the HDC microspheres 2;
Step six, after 10 minutes, the second electromagnetic valve 14 is closed again, the first electromagnetic valve 13 is opened, nitrogen is injected into the pressure tank 1 through the air inlet pipeline 11 to be pressurized to 0.35MPa, the operation is repeated at intervals of 10 minutes, after 72 hours, the silicon mold cores in the HDC microspheres 2 are completely corroded, and the products are completely discharged.
Example 4:
firstly, loading HDC microspheres 2 with the diameter of 900 microns and the corrosion aperture of 3 microns into an HDC microsphere storage device 3;
Step two, placing the HDC microsphere storage device 3 into a corrosive liquid container 5, and adding corrosive liquid 6 into the corrosive liquid container 5, wherein the liquid level of the corrosive liquid 6 is higher than the height of the HDC microsphere storage device 3, the corrosive liquid 6 consists of hydrofluoric acid and nitric acid, and the volume ratio of the hydrofluoric acid to the nitric acid is 6:1;
step three, placing the corrosive liquid container 5 into an inner container 16, then placing the inner container 16 into a rigid tank body 15, sealing the rigid tank body 15, and placing the whole pressure tank 1 into a constant-temperature oven, wherein the temperature is kept at 40 ℃;
Step four, closing a second electromagnetic valve 14 and opening a first electromagnetic valve 13, and injecting argon into the pressure tank 1 through the air inlet pipeline 11 to carry out pressurization so that the corrosive liquid 6 enters the HDC microspheres 2;
Step five, observing the reading of the pressure gauge 4, closing the first electromagnetic valve 13 when the pressure value reaches 0.5MPa, opening the second electromagnetic valve 14 after 5 minutes, and naturally discharging the nitrogen through the air outlet pipe 12 to discharge the product from the HDC microspheres 2;
Step six, after 5 minutes, the second electromagnetic valve 14 is closed again, the first electromagnetic valve 13 is opened, argon is injected into the pressure tank 1 through the air inlet pipeline 11 to be pressurized to 0.5MPa, the operation is repeated at intervals of 5 minutes, after 72 hours, the silicon mold core inside the HDC microsphere 2 is completely corroded, and the product is completely discharged.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (8)
1. The utility model provides a take micropore shell layer formula high density carbon microsphere silicon mold core to get rid of method, is realized through taking micropore shell layer formula high density carbon microsphere silicon mold core to corrode device, take micropore shell layer formula high density carbon microsphere silicon mold core to corrode device includes the overhead tank, overhead tank's top one side through connection has the intake pipe, its characterized in that: the other side of the top end of the pressure tank is connected with an air outlet pipe in a penetrating way;
the air inlet pipe is provided with a first electromagnetic valve;
a second electromagnetic valve is arranged on the air outlet pipe;
a high-density carbon microsphere storage device for preventing the high-density carbon microsphere from floating up is arranged in the pressure tank, and the high-density carbon microsphere storage device is of a cage-shaped structure;
the method for removing the silicon mold core of the microporous shell type high-density carbon microsphere comprises the following steps of:
step one, loading high-density carbon microspheres into a high-density carbon microsphere storage device;
Placing the high-density carbon microsphere storage device into an etching liquid container, and adding etching liquid into the etching liquid container, wherein the liquid level of the etching liquid is higher than that of the high-density carbon microsphere storage device, and the etching liquid comprises mixed solution of hydrofluoric acid and nitric acid;
Step three, placing the corrosive liquid container into an inner container, placing the inner container into a rigid tank body, and sealing the rigid tank body;
Step four, closing a second electromagnetic valve and opening a first electromagnetic valve, injecting inert gas into a pressure tank through an air inlet pipeline to carry out pressurization, so that the corrosive liquid enters the high-density carbon microspheres, wherein the pressure of the inert gas for pressurization is 0.2-0.6 MPa;
Step five, closing the first electromagnetic valve after pressurization is completed, and opening the second electromagnetic valve after 1-30 minutes, wherein the inert gas is naturally discharged from an air outlet pipe, so that a product is discharged from the high-density carbon microsphere;
And step six, after 1 to 30 minutes, closing the second electromagnetic valve again and opening the first electromagnetic valve, injecting inert gas into the pressure tank through the air inlet pipeline for pressurizing, repeating the operation at intervals of 1 to 30 minutes, and discharging the product after the silicon mold core in the high-density carbon microsphere is completely corroded.
2. The method for removing silicon mold cores from microporous shell type high-density carbon microspheres according to claim 1, further comprising a pressure gauge for measuring the pressure inside the pressure tank, wherein the pressure gauge is arranged at the middle position of the top end of the pressure tank and is an anti-corrosion pressure gauge.
3. The method for removing silicon mold cores from microporous shell-type high-density carbon microspheres according to claim 1, wherein the etching apparatus further comprises: the corrosive liquid container is arranged in the pressure tank and used for storing corrosive liquid;
The mode of arranging the high-density carbon microsphere storage device in the pressure tank is as follows: the high-density carbon microsphere storage device is arranged at the bottom of the corrosive liquid container.
4. The method for removing silicon mold cores from microporous shell-type high-density carbon microspheres according to claim 1, wherein the pressure tank comprises:
A high pressure resistant rigid canister;
The corrosion-resistant liner is sleeved in the rigid tank body;
the bearable pressure range of the high-pressure-resistant rigid tank body is 0.2-0.6 MPa.
5. The method for removing the silicon mold cores of the microporous shell type high-density carbon microspheres according to claim 1, wherein the air inlet pipe is a corrosion-resistant air inlet pipe, and the air outlet pipe is a corrosion-resistant air outlet pipe.
6. The method for removing a silicon mold core of a microporous shell-type high-density carbon microsphere according to claim 3, further comprising: the anti-corrosion plate is used for separating the inner space of the pressure tank, is arranged in the pressure tank, the peripheral wall of the anti-corrosion plate is in sealing connection with the inner wall of the pressure tank through a sealing ring, a plurality of supporting feet are symmetrically and fixedly connected to the bottom end of the anti-corrosion plate, the bottom ends of the supporting feet are propped against the inner bottom end of the pressure tank, annular protrusions are integrally formed in the middle position of the top end of the anti-corrosion plate in a protruding mode, and the annular protrusions are sleeved on the bottom of the corrosive liquid container and are connected.
7. The method for removing the silicon mold core of the microporous shell type high-density carbon microsphere according to claim 1, wherein the volume ratio of hydrofluoric acid to nitric acid is 1:3-6:1, and the internal temperature of the pressure tank is 20-50 ℃ in the corrosion process.
8. The method for removing silicon cores from microporous shell type high-density carbon microspheres according to claim 1, wherein the inert gas is either nitrogen or argon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211029778.6A CN115672212B (en) | 2022-08-25 | 2022-08-25 | Method for removing silicon mold cores of microporous shell type HDC microspheres |
Applications Claiming Priority (1)
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| CN104147986A (en) * | 2014-07-23 | 2014-11-19 | 中国人民解放军***南京总医院 | Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof |
| CN113834765A (en) * | 2020-06-08 | 2021-12-24 | 中国石油化工股份有限公司 | Device and method for testing corrosion resistance of material |
| CN112229782A (en) * | 2020-09-01 | 2021-01-15 | 华北电力大学 | Device for simulating corrosion research of liquid metal battery |
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