KR101759280B1 - Method for preparing porous carbon materials using polymer - Google Patents
Method for preparing porous carbon materials using polymer Download PDFInfo
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- KR101759280B1 KR101759280B1 KR1020150085751A KR20150085751A KR101759280B1 KR 101759280 B1 KR101759280 B1 KR 101759280B1 KR 1020150085751 A KR1020150085751 A KR 1020150085751A KR 20150085751 A KR20150085751 A KR 20150085751A KR 101759280 B1 KR101759280 B1 KR 101759280B1
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- South Korea
- Prior art keywords
- polymer particles
- carbon material
- porous carbon
- manufacturing
- necked
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 229920000642 polymer Polymers 0.000 title claims abstract description 47
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 51
- 238000005530 etching Methods 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 20
- 238000001125 extrusion Methods 0.000 claims abstract description 14
- 239000004065 semiconductor Substances 0.000 claims abstract description 14
- 238000010000 carbonizing Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003763 carbonization Methods 0.000 claims description 17
- 239000005011 phenolic resin Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011300 coal pitch Substances 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 239000011301 petroleum pitch Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229920001187 thermosetting polymer Polymers 0.000 claims description 2
- 239000004634 thermosetting polymer Substances 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract 2
- 238000000465 moulding Methods 0.000 description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 5
- 229920001568 phenolic resin Polymers 0.000 description 5
- 239000000758 substrate Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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Classifications
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- C01B31/02—
-
- 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
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/008—Pyrolysis reactions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02115—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material being carbon, e.g. alpha-C, diamond or hydrogen doped carbon
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Thermal Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a process for producing a molded article having a structure in which polymer particles are necked together by extrusion molding of polymer particles; Curing the molded body; And carbonizing the cured molded article, and to a porous carbon material produced by the method. According to this technology, carbon material having a uniform micropore structure is formed and corrosive gas can be uniformly permeated, so that it can be applied as a cathode in a semiconductor etching process, thereby improving the efficiency of the etching process. In addition, the porous carbon material manufactured according to the present technology has excellent corrosion resistance and strength, and can maintain a fine pore structure for a long period of time even though it is applied to etching, thereby improving the life and economical efficiency.
Description
More particularly, the present invention relates to a method of manufacturing a porous carbonaceous material that can uniformly form pores by using a polymer, and is particularly useful as a cathode in a semiconductor etching process to improve etching efficiency. And a manufacturing method thereof.
In a semiconductor manufacturing process, an etching process can be divided into a wet etching process and a dry etching process, in which a corrosive gas is injected into a substrate and a plasma is formed simultaneously to form a circuit on the substrate.
At this time, the porous part used as a gas mask for etching gas permeation is etched by a corrosive gas in the etching process to form a plasma by acting as a cathode by forming a circuit by forming an electric conductivity. In addition, the porous component also permeates the corrosive gas uniformly and spreads the gas evenly over the substrate.
Generally, a porous component used as a cathode in an etching process is mainly manufactured by processing a ceramic material such as alumina or silicon carbide into a predetermined shape, and then forming pores of uniform size at regular intervals by punching.
However, since the cathode formed of the porous ceramic material is etched, the permeation amount of the etching gas differs between the portion where the pores are formed and the portion where the pores are not formed. Therefore, there is a difference in the degree of etching, do. Further, as the etching progresses, corrosion is caused by the corrosive gas and the pore size is changed to increase the defect rate, and the life is shortened, which is not economical.
Thus, there is a demand for a material having a strong corrosion resistance that can be used as a cathode in the etching process, an excellent electrical conductivity, and a porous microstructure.
On the other hand, carbon materials are known as materials excellent in corrosion resistance and electrical conductivity. Porous carbon materials are manufactured by modifying pitch as a starting material and carbonizing under high temperature and high pressure, or by carbonizing a polymer foamed with a foaming agent, To form pores, thereby forming a pore, is known.
However, since the carbonization process is performed under high temperature and high pressure, the process itself is complicated and difficult, and therefore, it is difficult to apply the process to mass production. In addition, the method of producing a porous carbon material by using a foaming agent is difficult to apply as a cathode in a semiconductor etching process because the produced carbon material does not exhibit sufficient strength. Furthermore, the method of manufacturing a porous carbon material by forming a template and corroding the material is also not mass-producible because it is difficult to process and economical.
A problem to be solved by the present invention is to provide a method of manufacturing a semiconductor device, which is excellent in corrosion resistance and electrical conductivity and which can uniformly form a fine porous structure to uniformly transmit corrosive gas in a semiconductor etching process and can be efficiently applied as a cathode having excellent corrosion resistance To provide a method for manufacturing porous carbon materials.
According to an aspect of the present invention, there is provided a method of manufacturing a molded article, the method including: preparing a molded article having a structure in which polymer particles are necked together by extrusion molding polymer particles; Curing the molded body; And a step of carbonizing the cured molded article.
Further, another embodiment of the present invention relates to a porous carbonaceous material produced by the above method.
In addition, the porous carbon material according to another embodiment of the present invention can be used as a cathode of a semiconductor etching process.
According to the present invention, since a carbon material having a uniform micropore structure is formed using a polymer, the corrosive gas can be uniformly permeated, so that it can be applied as a cathode in a semiconductor etching process, thereby improving the efficiency of the etching process.
In addition, the porous carbon material produced according to the present invention has excellent corrosion resistance and strength, and can maintain a fine pore structure for a long period of time even though it is applied to etching, thereby improving the life and economical efficiency.
In addition, according to the present invention, since a final cathode is formed by extrusion molding, the post-processing can be omitted, which is economical and efficient.
1 is a photograph of a spherical polymer particle used in an embodiment of the present invention.
2 is a photograph of a molded article extruded according to an embodiment of the present invention.
3 is a photograph showing a microstructure of a formed body formed by extrusion molding according to an embodiment of the present invention.
4 is a photograph of a carbonized porous carbon material according to an embodiment of the present invention.
5 is a photograph showing the microstructure of a porous carbon material produced according to an embodiment of the present invention.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings, so that those skilled in the art can easily carry out the technical idea of the present invention. In the following description, numerous specific details are set forth, such as specific elements, which are provided to aid a more thorough understanding of the present invention, and it is to be understood that the present invention may be practiced without these specific details, It will be obvious to those who have. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
According to an embodiment of the present invention, there is provided a method of manufacturing a porous carbon material, comprising: preparing a molded body having a structure in which polymer particles are necked together by extrusion molding polymer particles; Curing the molded body; And carbonizing the cured shaped body.
The polymer particles may be spherical thermosetting polymer particles that are solid at room temperature. For example, it may be at least one selected from the group consisting of a polyurethane resin, an epoxy resin, a silicone resin, a furan resin, a phenol resin, a coal pitch and a petroleum pitch.
The size of the polymer particles may range from 10 to 500 mu m. When the particle size is less than 10 탆, the pores of the formed body become too small in the molding process of applying the temperature and the pressure, and porous carbon materials having desired pores can not be produced. When the particle size exceeds 500 탆, The pore becomes too large to exhibit a value equal to or higher than a desired fluid permeability, so that too much fluid can pass therethrough, resulting in product defects and shortening the service life of the component.
The forming of the molded body can be carried out by extrusion using a final product, for example a metal mold having the shape of a cathode of a semiconductor etching process. By using the mold in this way, the final product can be produced only by molding once without a subsequent processing step, which is economical advantage.
During extrusion molding in the molding step, the polymer particles are heated to a softening point to soften the polymer particles, and the pressure applied is controlled so that the polymer particles are necked with each other.
In the context of the present invention, the term "necked structure" means a structure in which the polymer particles are not completely clumped and densely clustered but the polymer particles are partially contacted to each other and have a uniform microspace between the polymer particles .
The forming step may be performed at a temperature in the range of 50 to 200 ° C. When the temperature is lower than 50 ° C, the polymer particles are not sufficiently softened to cause the polymer particles to cling to each other, making it difficult to form a necking structure. When the temperature exceeds 200 ° C, the polymer particles become close to the melting point and have high fluidity, The porous carbon material having uniform pores due to inter-particle necking can not be formed.
The pressure applied in the molding step is adjusted so that the polymer particles have a necked structure with each other. If the pressure is excessively high during molding, the polymer particles will not stop in the necked state, but will clump together and become united, making it impossible to form a porous carbon material having uniform pores. In addition, when the pressure is too low, physical strength may be lowered because a very weak necking structure is formed between the polymer particles.
Specifically, the pressure applied in the molding step may vary depending on the characteristics of the particles of the polymer used, that is, the softening point, the flowability, the density, etc., and the polymer particles may be adjusted to have a necked structure by confirming the characteristics of the different raw materials. have.
By controlling the pressure in this manner, the formed body can form a necking structure having a uniform space between spherical polymer particles, and this uniform space can be converted into a uniform microporous structure through the subsequent curing reaction step and carbonization step have.
Then, the molded article having the structure in which the polymer particles are necked in the curing reaction step can be completely cured.
The curing reaction step can be carried out at a temperature ranging from 50 to 200 DEG C for 1 to 72 hours. If the temperature of the curing reaction is less than 50 ° C, the curing reaction may not be performed at all. If the temperature exceeds 200 ° C, the molded product is broken due to high fluidity, so that the molded body is damaged and at the same time, Can not be. If the time of the curing reaction is less than 1 hour, the curing reaction is insignificant and the curing reaction can not be completed. If the time exceeds 72 hours, the curing reaction may be completed, none.
If the curing reaction is not completely completed in the curing reaction step, the polymer may be softened when heat-treated in the subsequent carbonization step, and the shape of the molded body may be deformed. To prevent this, the curing reaction step should completely cure the polymer.
Subsequently, in the carbonization step, the fully cured molded body can be carbonized.
The carbonization step can be carried out under an inert atmosphere at a temperature in the range of 1000 to 1350 ° C. When the temperature of the carbonization step is less than 1000 ° C, carbonization does not occur completely and the strength of the obtained carbon material is weak. When the temperature is more than 1350 ° C, further carbonization reaction is completed and the property improvement can not be described.
Also, the carbonization step can be performed by heat-treating the formed body at a heating rate of 1 to 30 DEG C / min. The rate of temperature rise during carbonization can be appropriately controlled in consideration of the thermal decomposition behavior of the polymer forming the formed body.
The carbon material formed through the carbonization step only has electrical conductivity and corrosion resistance. Further, since the space between the necked polymer particles formed on the formed article by carbonization is converted into uniform micropores, the carbon material has a uniform porous structure.
According to another embodiment of the present invention, there is provided a method of manufacturing a porous carbon material, comprising: preparing a molded body having a structure in which polymer particles are necked together by extrusion molding polymer particles; Curing the molded body; And a step of carbonizing the cured molded body. The porous carbonaceous material is produced by a method of producing a porous carbonaceous material.
The porous carbon material according to the present embodiment has a uniform microporous structure and is characterized by excellent electrical conductivity and corrosion resistance.
Accordingly, the porous carbon material according to the embodiment can be applied to the cathode of the semiconductor etching process. When applied as a cathode of a semiconductor etching process, the etching gas is uniformly permeated by a uniform microporous structure and is transferred to the substrate, thereby improving the etching efficiency and maintaining the pore structure for a long period of time due to high electrical conductivity and corrosion resistance The occurrence of defects in the etching process can be reduced, and the lifetime of the cathode can be increased.
Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are illustrative of the present invention, and the scope of the present invention is not limited to the following examples.
[Example]
(1) Extrusion molding step
The spherical phenolic resin particles shown in Fig. 1 were placed in a mold for extrusion molding and heated at 180 캜 to cause the phenolic resin particles to be entangled with each other. At this time, the pressure was applied to adjust the degree of clumping of the polymer particles, so that the polymer particles were not tightly adhered to each other and necked together. Thereby forming a molded article having a structure in which the phenolic resin particles are necked with each other. Fig. 2 shows a molded body formed by extrusion molding, and Fig. 3 shows a microstructure photograph of the molded body.
As shown in Fig. 3, the molded article formed according to the present invention has a structure in which spherical phenol resin particles are necked together and a small and uniform space is formed between the necked phenolic resin particles.
(2) Curing reaction step
The molded body formed in the extrusion molding step was placed in an oven and held at a temperature of 200 DEG C for 72 hours to perform a curing reaction so as to be completely cured.
(3) Carbonization step
In the curing reaction step, the cured molded article was subjected to heat treatment to carbonize it. The pyrolysis reaction of the phenolic resin was carried out by heat treatment at 1100 ° C while controlling the heating rate at 5 ° C / min. The carbon material thus formed is shown in Fig. 4, and a microstructure photograph of the carbon material is shown in Fig.
It can be confirmed that deformation on the outer appearance of the molded body after carbonization does not occur as compared with the molded body formed by the extrusion molding shown in Fig.
Further, as shown in Fig. 5, it can be seen that the porous carbon material has a structure in which spherical particles are necked with each other, and uniform fine pores are formed between necked particles. Such a microporous structure is formed by converting a small and uniform space between necked polymer particles present in an extruded molded article into pores after carbonization.
The porous carbon material thus formed is excellent in electrical conductivity and corrosion resistance and has a uniform micro pore structure. In particular, it is possible to uniformly permeate the corrosive gas in the semiconductor etching process and maintain the pore structure for a long period of time even if the etching proceeds , The performance of the porous cathode used in the semiconductor etching process can be further improved.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments or constructions. Various changes, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention. It will be clear to those who have knowledge.
Claims (10)
Curing the molded body; And
Carbonizing the cured shaped body,
The molded article manufacturing step is performed so that the polymer particles are necked with each other by heating and softening the polymer particles and controlling the pressure,
The necked structure is a structure in which the polymer particles are in partial contact with each other and have uniform pores between the polymer particles
A method for manufacturing a porous carbon material.
The polymer particles are spherical thermosetting polymer particles having a solid state at room temperature, and the particle size is 10 to 500 mu m
A method for manufacturing a porous carbon material.
Wherein the polymer particles are at least one selected from the group consisting of a polyurethane resin, an epoxy resin, a silicone resin, a furan resin, a phenol resin, a coal pitch, and a petroleum pitch
A method for manufacturing a porous carbon material.
Wherein the step of preparing the molded article is carried out at a temperature in the range of 50 to 200 ° C
A method for manufacturing a porous carbon material.
Wherein the curing reaction step is carried out at a temperature ranging from 50 to 200 DEG C for 1 to 72 hours
A method for manufacturing a porous carbon material.
Characterized in that the carbonization step is carried out in an inert atmosphere at a temperature in the range of 1000 to 1350 ° C
A method for manufacturing a porous carbon material.
Wherein the carbonization step is performed by heat treatment at a heating rate of 1 to 30 DEG C / min
A method for manufacturing a porous carbon material.
Characterized in that it is used as a cathode in a semiconductor etching process
Porous carbon material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150085751A KR101759280B1 (en) | 2015-06-17 | 2015-06-17 | Method for preparing porous carbon materials using polymer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150085751A KR101759280B1 (en) | 2015-06-17 | 2015-06-17 | Method for preparing porous carbon materials using polymer |
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| Publication Number | Publication Date |
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| KR20160148935A KR20160148935A (en) | 2016-12-27 |
| KR101759280B1 true KR101759280B1 (en) | 2017-07-19 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102462754B1 (en) | 2018-03-09 | 2022-11-02 | 주식회사 엘지화학 | Electrode of secondary battery and secondary battery comprising the same |
| CN108675791A (en) * | 2018-08-17 | 2018-10-19 | 苏州宏久航空防热材料科技有限公司 | It is a kind of using foam waste as the preparation method of the carbon foam of raw material |
| KR102382237B1 (en) * | 2019-12-27 | 2022-04-05 | 한국세라믹기술원 | Manufacturing method of carbon form shaped by mold |
| KR102512058B1 (en) * | 2020-10-06 | 2023-03-21 | 한국세라믹기술원 | Manufacturing method of porous carbon having ultra-high strength and macro pore size |
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