CN116023169A - Graphite treatment process and graphite structure - Google Patents

Graphite treatment process and graphite structure Download PDF

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Publication number
CN116023169A
CN116023169A CN202211715588.XA CN202211715588A CN116023169A CN 116023169 A CN116023169 A CN 116023169A CN 202211715588 A CN202211715588 A CN 202211715588A CN 116023169 A CN116023169 A CN 116023169A
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China
Prior art keywords
graphite
tantalum
liquid medicine
treatment process
micropores
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CN202211715588.XA
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Chinese (zh)
Inventor
耿安东
刘春艳
周元辉
陈建明
杨洪雨
范子龙
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Suzhou U King Photoelectric Technology Co ltd
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Suzhou U King Photoelectric Technology Co ltd
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Priority to CN202211715588.XA priority Critical patent/CN116023169A/en
Publication of CN116023169A publication Critical patent/CN116023169A/en
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Abstract

A graphite treatment process and a graphite structure relate to the technical field of preparation of anti-corrosion materials. The graphite treatment process comprises the following steps: immersing graphite in the liquid medicine, and enabling the liquid medicine to enter into the inner micropores of the graphite, wherein the liquid medicine is tantalum or tantalum salt solution; and (3) chemically reacting the liquid medicine with the graphite under the first preset temperature condition to form a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite. According to the graphite treatment process, the liquid medicine is immersed into the inner micropores of the graphite through the immersion technology, and the tantalum carbide protective layer is formed on the outer surface and the inner micropore area of the graphite simultaneously through chemical reaction, so that the formed tantalum carbide can effectively prevent the corrosion of the surface and the inner part of the graphite, is good in integrity and not easy to fall off, the corrosion resistance and the service life of the graphite are effectively improved, and impurities in the graphite can be prevented from volatilizing out through the inner micropores of the graphite.

Description

Graphite treatment process and graphite structure
Technical Field
The invention relates to the technical field of preparation of anti-corrosion materials, in particular to a graphite treatment process and a graphite structure.
Background
In the growth process of silicon carbide crystals, the silicon carbide raw material is decomposed, and the raw material decomposed gas component contains silicon vapor which reacts with the graphite crucible. The graphite crucible is continuously corroded by the raw material gas flow, and the porous structure on the graphite crucible becomes more loose and porous and generates graphite fine particles.
Research shows that the tantalum carbide coating can effectively prevent graphite from corroding and prevent impurities in the graphite from volatilizing. However, the tantalum carbide coating prepared on the graphite material in the prior art only exists on the surface of graphite, so that the coating is easy to fall off, once the coating falls off, the graphite can be corroded, impurities in the graphite can volatilize out through air holes of the graphite, and adverse effects are caused on crystal growth.
Disclosure of Invention
The invention aims to provide a graphite treatment process and a graphite structure, wherein a tantalum carbide coating on graphite is not easy to fall off, and the graphite structure is good in corrosion resistance and long in service life.
Embodiments of the present invention are implemented as follows:
the embodiment of the invention provides a graphite treatment process, which comprises the following steps: immersing graphite in the liquid medicine, and enabling the liquid medicine to enter into the inner micropores of the graphite, wherein the liquid medicine is tantalum or tantalum salt solution; and (3) carrying out chemical reaction on the liquid medicine and the graphite under the first preset temperature condition so as to form a tantalum carbide coating on the outer surface of the graphite and the micropore surface inside the graphite.
Optionally, immersing the graphite in a liquid medicine and allowing the liquid medicine to enter the micropores inside the graphite, wherein the liquid medicine is tantalum or tantalum salt solution and comprises: placing graphite to be impregnated in a sealed container; vacuumizing the sealed container to a preset negative pressure to remove air in the inner micropores of the graphite; adding the liquid medicine into a sealed container under the state of maintaining negative pressure, wherein the liquid medicine is tantalum or tantalum salt solution; pressurizing the sealed container to a preset positive pressure to enable the liquid medicine to enter the micropores in the graphite.
Optionally, immersing the graphite in the liquid medicine, and making the liquid medicine enter into the internal micropores of the graphite, wherein after the liquid medicine is tantalum or tantalum salt solution, the graphite treatment process further comprises: and drying the impregnated graphite at a second preset temperature.
Optionally, chemically reacting the medical fluid with the graphite at a first predetermined temperature to form a tantalum carbide coating on the outer surface of the graphite and the inner microporous surface of the graphite comprises: sintering the impregnated graphite to a first preset temperature to enable the chemical liquid to react with the graphite, and forming a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite.
Optionally, the medical solution includes a tantalum salt and an organic solvent capable of dissolving the tantalum salt.
Optionally, sintering the impregnated graphite to a first preset temperature comprises: and placing the impregnated graphite in an atmosphere sintering furnace or a vacuum sintering furnace, and heating to a first preset temperature.
Optionally, the preset negative pressure is 10 -5 Pa~10 -1 Pa, and the preset positive pressure is 1 MPa-10 MPa.
Optionally, the first preset temperature is 500 ℃ to 2000 ℃.
Optionally, the second preset temperature is 80 ℃ to 150 ℃.
The embodiment of the invention also provides a graphite structure which comprises graphite and a tantalum carbide coating, wherein the tantalum carbide coating covers the outer surface of the graphite and the inner micropore surface of the graphite.
The beneficial effects of the embodiment of the invention include:
the graphite treatment process provided by the embodiment of the invention comprises the following steps: immersing graphite in the liquid medicine, and enabling the liquid medicine to enter the micropores in the graphite, wherein the liquid medicine is tantalum or tantalum salt solution; and (3) chemically reacting the liquid medicine with the graphite under the first preset temperature condition to form a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite. According to the graphite treatment process, the liquid medicine is immersed into the inner micropores of the graphite through the immersion technology, and the tantalum carbide protective layer is formed on the outer surface and the inner micropore area of the graphite simultaneously through chemical reaction, so that the formed tantalum carbide can effectively prevent the corrosion of the surface and the inner part of the graphite, is good in integrity and not easy to fall off, the corrosion resistance and the service life of the graphite are effectively improved, and impurities in the graphite can be prevented from volatilizing out through the inner micropores of the graphite.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is one of the flow charts of a graphite treatment process provided by an embodiment of the present invention;
FIG. 2 is a second flowchart of a graphite treatment process according to an embodiment of the present invention;
FIG. 3 is a third flowchart of a graphite treatment process according to an embodiment of the present invention;
FIG. 4 is a flow chart of a graphite treatment process according to an embodiment of the present invention;
FIG. 5 is a flow chart of a graphite treatment process according to an embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, 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 direction, be constructed and operated in a specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Referring to fig. 1, an embodiment of the present application provides a graphite treatment process, including:
s100: immersing graphite in the liquid medicine, and making the liquid medicine enter into the inner micropores of the graphite, wherein the liquid medicine is tantalum or tantalum salt solution.
S200: and (3) chemically reacting the liquid medicine with the graphite under the first preset temperature condition to form a tantalum carbide coating on the outer surface of the graphite and the surface of the inner micropores of the graphite.
The graphite itself has a porous structure, and a plurality of minute pores exist in the graphite itself. Because the internal micropores of the graphite are smaller and air exists, the liquid medicine can not be fully entered into the internal micropores only by placing the graphite in the liquid medicine, and therefore, the liquid medicine can be driven into the internal micropores by adopting a certain means. The liquid medicine used for dipping the graphite is tantalum solution or tantalum salt solution, the liquid medicine is adhered to the surface of the graphite after the graphite is dipped in the liquid medicine, and the condition that the liquid medicine and the graphite are subjected to chemical reaction, namely a first preset temperature condition is provided, so that tantalum ions in the liquid medicine can be subjected to chemical reaction with the graphite to form tantalum carbide. Because the liquid medicine exists in the outer surface and the inner micropores of the graphite, the formed tantalum carbide coating exists in the outer surface and the inner micropores of the graphite at the same time, and the coating has good integrity and is not easy to fall off, so that the corrosion resistance and the service life of the graphite can be effectively improved.
In this embodiment, the graphite is immersed in the liquid, and the liquid chemical liquid is more likely to enter the inner micropores of the graphite. However, in this embodiment, the manner in which the chemical solution is introduced into the internal micropores of the graphite is not limited.
According to the graphite treatment process, the liquid medicine is immersed into the inner micropores of the graphite through the immersion technology, and the tantalum carbide protective layer is formed on the outer surface and the inner micropore area of the graphite simultaneously through chemical reaction, so that the formed tantalum carbide can effectively prevent the corrosion of the surface and the inner part of the graphite, is good in integrity and not easy to fall off, the corrosion resistance and the service life of the graphite are effectively improved, and impurities in the graphite can be prevented from volatilizing out through the inner micropores of the graphite.
Optionally, in one implementation manner of the embodiment of the present invention, the liquid medicine includes a tantalum salt and an organic solvent capable of dissolving the tantalum salt.
The organic solvent can be absolute ethanol, acetone, chloroform, thiophenol, etc.; the tantalum salt may be tantalum pentachloride, tantalum oxalate, or the like. The tantalum salt contains tantalum ions which can react with graphite chemically, and the graphite is immersed in the tantalum salt solution, so that a tantalum carbide coating can be formed on the outer surface of the graphite and in the pores of the graphite.
Preferably, the tantalum salt is tantalum pentachloride, the organic solvent is absolute ethyl alcohol or acetone, and the tantalum pentachloride has high reactivity and is easy to chemically react with graphite.
Optionally, in an implementation manner of the embodiment of the present invention, the first preset temperature is 500 ℃ to 2000 ℃. The tantalum-containing liquid has higher reactivity in the temperature range, smaller activation energy required by chemical reaction with graphite, higher reaction rate and easier generation of tantalum carbide coating on the outer surface and in the air holes of the graphite. The first preset temperature below 500 ℃ or above 2000 ℃ can reduce the reactivity of the tantalum-containing liquid, so that the difficulty of forming the tantalum carbide coating is increased.
Referring to fig. 2, in an alternative implementation manner of the embodiment of the present invention, graphite is immersed in a liquid medicine, and the liquid medicine enters into internal micropores of the graphite, where the liquid medicine is tantalum or a tantalum salt solution, and includes:
s110: the graphite to be impregnated is placed in a sealed container.
S120: and vacuumizing the sealed container to a preset negative pressure to remove air in the inner micropores of the graphite.
S130: and adding the liquid medicine into the sealed container under the state of maintaining negative pressure, wherein the liquid medicine is tantalum or tantalum salt solution.
S140: pressurizing the sealed container to a preset positive pressure to enable the liquid medicine to enter the inner micropores of the graphite.
The graphite to be impregnated is placed in a sealed container, isolated from the outside air. Firstly, vacuumizing the sealed container to enable the interior of the sealed container to be in a negative pressure state, and under the negative pressure state, air in micropores in the graphite can be pumped out so as to facilitate the subsequent liquid medicine to fully fill the micropores in the graphite. And (3) after the air in the inner micropores is pumped out, adding the liquid medicine into the sealed container to impregnate the graphite, and then pressurizing the sealed container to enable the interior of the sealed container to be in a positive pressure state, wherein the liquid medicine can enter the inner micropores under the action of pressure in the positive pressure state, so that the inner micropores are filled.
In this embodiment, the values of the preset negative pressure and the preset positive pressure to be achieved by the sealed container are not limited, and the air in the micropores inside the graphite can be pumped out under the preset negative pressure, and the liquid medicine can be introduced into the micropores inside the graphite under the preset positive pressure.
Optionally, in an achievable manner of the embodiment of the present invention, the preset negative pressure is 10 -5 Pa~10 -1 Pa, and the preset positive pressure is 1 MPa-10 MPa.
The preset negative pressure is within the range, the structure of the graphite is not damaged, and the air in the micropores in the graphite can be rapidly extracted; if the preset negative pressure is greater than 10 -1 Pa, the negative pressure state formed is not obvious enough, and the air in the micropores in the graphite is difficult to be pumped out; if the preset negative pressure is less than 10 -5 Pa may damage the structure of the graphite itself and also increase the impregnation cost. Preferably, the negative pressure is presetIs 10 -3 Pa。
The preset positive pressure is within the range, the structure of the graphite is not damaged, and the liquid medicine can be driven to smoothly enter the inner micropores of the graphite; if the preset positive pressure is less than 1MPa, the formed positive pressure state is not obvious enough, and the liquid medicine is difficult to fully enter the inner micropores of the graphite; if the preset positive pressure is more than 10MPa, the structure of the graphite itself may be damaged, and the impregnation cost may be increased.
Referring to fig. 3, in an alternative implementation manner of the embodiment of the present invention, graphite is immersed in a liquid medicine, and the liquid medicine enters into the internal micropores of the graphite, where after the liquid medicine is tantalum or a tantalum salt solution, the graphite treatment process further includes:
s300: and drying the impregnated graphite at a second preset temperature.
And heating the impregnated graphite to remove the liquid solvent in the liquid medicine on the outer surface and in the micropores of the impregnated graphite, and retaining solid tantalum or tantalum salt so as to prevent liquid components in the liquid medicine, such as organic solvent, water and the like, from affecting the chemical reaction of the tantalum or tantalum salt and the graphite.
Optionally, in an implementation manner of the embodiment of the present invention, the second preset temperature is 80 ℃ to 150 ℃. The drying is carried out within the temperature range, the drying efficiency is higher, the effect is better, and the cost is lower; if the second preset temperature is lower than 80 ℃, the drying is slower, and the condition of insufficient drying may exist; if the second preset temperature is higher than 150 ℃, the drying cost is higher.
Preferably, the second preset temperature is 80 ℃.
Referring to fig. 4, in an alternative implementation manner of the embodiment of the present invention, chemically reacting the chemical solution with graphite under a first preset temperature condition to form a tantalum carbide coating on the outer surface of the graphite and the microporous surface inside the graphite includes:
s210: sintering the impregnated graphite to a first preset temperature to enable the chemical liquid to react with the graphite, and forming a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite.
And providing a first preset temperature condition through sintering, so that graphite and tantalum or tantalum salt in the liquid medicine are subjected to chemical reaction to generate the tantalum carbide coating. Taking the example that the liquid medicine comprises tantalum pentachloride, the tantalum pentachloride can react with graphite as follows:
2TaCl 5 +2C→2TaC+5Cl 2
the tantalum carbide coating generated by the reaction can cover the outer surface of graphite and the surface of the inner micropores, and generated chlorine can be discharged automatically.
Referring to fig. 5, in an alternative implementation manner of the embodiment of the present invention, sintering the impregnated graphite to the first preset temperature includes:
s220: and placing the impregnated graphite in an atmosphere sintering furnace or a vacuum sintering furnace, and heating to a first preset temperature.
The atmosphere sintering furnace and the vacuum sintering furnace can isolate graphite from air, so that the phenomenon that the graphite is oxidized by contact with the air in the sintering process, a tantalum carbide coating cannot be generated in a part of areas, the corrosion resistance and the service life of the graphite cannot be effectively improved, and impurities in the graphite can volatilize through internal micropores of the graphite.
The embodiment also provides a graphite structure comprising graphite and a tantalum carbide coating covering the outer surface of the graphite and the inner microporous surface of the graphite.
The surface and the inside micropore surface of this graphite structure all cover and have the tantalum carbide protective layer, and the existence of tantalum carbide can effectively prevent graphite surface and inside corruption, and the integrality is better, is difficult for droing for this graphite structure has stronger corrosion resistance and higher life-span, can also avoid impurity in the graphite to volatilize out through the inside micropore of graphite.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A graphite treatment process, comprising:
immersing graphite in a liquid medicine, and enabling the liquid medicine to enter into internal micropores of the graphite, wherein the liquid medicine is tantalum or tantalum salt solution;
and (3) carrying out chemical reaction on the liquid medicine and the graphite under the condition of a first preset temperature so as to form a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite.
2. The graphite treatment process according to claim 1, wherein the immersing the graphite in a liquid chemical and causing the liquid chemical to enter the graphite internal micropores, wherein the liquid chemical is tantalum or a tantalum salt solution comprises:
placing graphite to be impregnated in a sealed container;
vacuumizing the sealed container to a preset negative pressure to remove air in micropores in the graphite;
adding the liquid medicine into a sealed container under the state of maintaining negative pressure, wherein the liquid medicine is tantalum or tantalum salt solution;
pressurizing the sealed container to a preset positive pressure to enable the liquid medicine to enter the inner micropores of the graphite.
3. The graphite treatment process according to claim 1, wherein the graphite is immersed in a chemical solution and the chemical solution is introduced into the internal micropores of the graphite, wherein after the chemical solution is tantalum or a tantalum salt solution, the graphite treatment process further comprises:
and drying the impregnated graphite at a second preset temperature.
4. The graphite treatment process of claim 1, wherein chemically reacting the liquid chemical with the graphite at a first predetermined temperature condition to form a tantalum carbide coating on the outer surface of the graphite and the inner microporous surface of the graphite comprises:
sintering the impregnated graphite to a first preset temperature to enable the chemical liquid to react with the graphite, and forming a tantalum carbide coating on the outer surface of the graphite and the inner micropore surface of the graphite.
5. The graphite treatment process according to claim 1, wherein the chemical solution comprises a tantalum salt and an organic solvent capable of dissolving the tantalum salt.
6. The graphite treatment process of claim 4, wherein sintering the impregnated graphite to a first predetermined temperature comprises:
and placing the impregnated graphite in an atmosphere sintering furnace or a vacuum sintering furnace, and heating to a first preset temperature.
7. The graphite treatment process according to claim 2, wherein the preset negative pressure is 10 -5 Pa~10 -1 Pa, wherein the preset positive pressure is 1-10 MPa.
8. The graphite treatment process according to claim 1, wherein the first preset temperature is 500 ℃ to 2000 ℃.
9. A graphite treatment process according to claim 3, wherein the second preset temperature is 80 ℃ to 150 ℃.
10. A graphite structure comprising graphite and a tantalum carbide coating covering the outer surface of said graphite and the inner microporous surface of said graphite.
CN202211715588.XA 2022-12-28 2022-12-28 Graphite treatment process and graphite structure Pending CN116023169A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20200207629A1 (en) * 2018-12-17 2020-07-02 Tokai Carbon Korea Co., Ltd. Carbonated tantalum coating material
JP6849779B1 (en) * 2019-12-06 2021-03-31 國家中山科學研究院 Method of forming tantalum carbide on a graphite substrate
CN113185324A (en) * 2021-06-10 2021-07-30 中电化合物半导体有限公司 Graphite piece and processing method thereof and single crystal growth equipment
CN113549895A (en) * 2021-07-12 2021-10-26 北京钽途新材料科技有限公司 Method for preparing tantalum carbide coating on surface of graphite substrate and graphite device
CN114368984A (en) * 2022-01-27 2022-04-19 中电化合物半导体有限公司 Coating of carbon substrate and preparation method and application thereof
CN115108852A (en) * 2022-07-26 2022-09-27 湖南泰坦未来科技有限公司 Graphite composite material and preparation method and application thereof
CN115198253A (en) * 2022-07-05 2022-10-18 苏州步科斯新材料科技有限公司 Preparation method of graphite matrix surface tantalum carbide coating

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20200207629A1 (en) * 2018-12-17 2020-07-02 Tokai Carbon Korea Co., Ltd. Carbonated tantalum coating material
JP6849779B1 (en) * 2019-12-06 2021-03-31 國家中山科學研究院 Method of forming tantalum carbide on a graphite substrate
CN113185324A (en) * 2021-06-10 2021-07-30 中电化合物半导体有限公司 Graphite piece and processing method thereof and single crystal growth equipment
CN113549895A (en) * 2021-07-12 2021-10-26 北京钽途新材料科技有限公司 Method for preparing tantalum carbide coating on surface of graphite substrate and graphite device
CN114368984A (en) * 2022-01-27 2022-04-19 中电化合物半导体有限公司 Coating of carbon substrate and preparation method and application thereof
CN115198253A (en) * 2022-07-05 2022-10-18 苏州步科斯新材料科技有限公司 Preparation method of graphite matrix surface tantalum carbide coating
CN115108852A (en) * 2022-07-26 2022-09-27 湖南泰坦未来科技有限公司 Graphite composite material and preparation method and application thereof

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