KR101679581B1 - Method for making carbon-carbon composite - Google Patents

Method for making carbon-carbon composite Download PDF

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Publication number
KR101679581B1
KR101679581B1 KR1020150099185A KR20150099185A KR101679581B1 KR 101679581 B1 KR101679581 B1 KR 101679581B1 KR 1020150099185 A KR1020150099185 A KR 1020150099185A KR 20150099185 A KR20150099185 A KR 20150099185A KR 101679581 B1 KR101679581 B1 KR 101679581B1
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South Korea
Prior art keywords
layer
fiber
carbon
product
fiber layer
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KR1020150099185A
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Korean (ko)
Inventor
박종현
구자원
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주식회사 카본티씨지
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Priority to KR1020150099185A priority Critical patent/KR101679581B1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres

Abstract

The method for producing a carbon composite material according to the present invention comprises:
A first step of preparing a base fiber layer;
A second step of infiltrating carbon into the base fiber layer by an isothermal method to form a rough laminar layer surrounding the carbon fibers constituting the base fiber layer;
A third step of heat-treating the base fiber layer on which the rough laminar layer is formed;
A fourth step of roughing the heat-treated base material fiber layer to produce a plurality of product fiber layers;
A smooth laminar layer is formed on the product fibrous layers by a thermal gradient method so as to surround the rough laminar layer or a resin layer is formed by impregnating the product fiber layers with the resin and pyrolyzing the resin to cover the rough laminar layer A fifth step of densifying the product fiber layers;
A sixth step of heat-treating the densified product fiber layers; And
And a seventh step of finishing the heat-treated product fiber layers.

Description

METHOD FOR MAKING CARBON-CARBON COMPOSITE [0001]

The present invention relates to a method for producing a carbon composite material.

Carbon-carbon composites are widely used for aircraft brake discs and heat-resistant materials because of their excellent friction and abrasion characteristics and thermal shock resistance.

The carbon composite material production method can be divided into a step of producing a fiber layer using carbon fiber and a step of densifying the fiber layer.

The process of densifying the fibrous layer is classified into a liquid impregnation method and a chemical vapor infiltration method.

In the liquid phase impregnation method, a fiber layer is impregnated with a resin and the resin is pyrolyzed to form a carbon matrix.

The chemical vapor deposition method is a method of impregnating a hydrocarbon gas into a fiber layer and pyrolyzing the hydrocarbon gas to form a carbon matrix.

The chemical vapor infiltration method is divided into an ISOTHERMAL method and a THERMAL GRADIENT method.

The isothermal method pyrolyzes the hydrocarbon gas in a state in which the inner temperature and the outer temperature of the fiber layer become uniform. Therefore, the carbon composite material produced by the isothermal method has uniform thermal conductivity and uniformity of characteristics of the entire carbon matrix. However, in the isothermal method, pyrolysis reaction of hydrocarbon gas occurs simultaneously at the inside and outside of the fiber layer, so that the carbon which is thermally decomposed from the outside without being diffused into the inside of the fiber layer is deposited on the surface of the fiber layer. As a result, the pores on the surface of the fibrous layer are clogged, preventing the hydrocarbon gas from penetrating into the fibrous layer. Therefore, the surface of the fibrous layer should be ground periodically to pierce the clogged pores. When the surface of the fibrous layer is periodically changed, the size of the fibrous layer that can actually make the product is gradually reduced. Also, it takes a lot of time (2 ~ 3 months) to make the carbon composite because it has to drill periodically clogged pores.

The thermal gradient method gives a temperature gradient from the inside to the outside of the fiber layer so that the thermal decomposition reaction of the hydrocarbon gas progresses gradually from the inside to the outside of the fiber layer. Therefore, the pore clogging does not occur, and the surface of the fibrous layer does not have to be periodically ground, and the time (2 to 3 weeks) required to produce the carbon composite material is shortened. However, the thermal gradient method makes it difficult to linearly and precisely determine the thermal gradient, and when the hydrocarbon gas is pyrolyzed, the temperature inside and outside of the fiber layer becomes unstable as in the isothermal method. Therefore, the carbon composite made by the isothermal method has lower thermal conductivity than the carbon composite made by the isothermal method because the characteristics of the entire carbon matrix are not uniform.

Korean Patent Publication No. 1998-030293

It is an object of the present invention to provide a new method of manufacturing a carbon composite material by taking advantage of merits of isothermal and thermal grading methods.

According to another aspect of the present invention, there is provided a method of manufacturing a carbon composite material,

A first step of preparing a base fiber layer;

A second step of infiltrating carbon into the base fiber layer by an isothermal method to form a rough laminar layer surrounding the carbon fibers constituting the base fiber layer;

A third step of heat-treating the base fiber layer on which the rough laminar layer is formed;

A fourth step of roughing the heat-treated base material fiber layer to produce a plurality of product fiber layers;

A smooth laminar layer is formed on the product fibrous layers by a thermal gradient method so as to surround the rough laminar layer or a resin layer is formed by impregnating the product fiber layers with the resin and pyrolyzing the resin to cover the rough laminar layer A fifth step of densifying the product fiber layers;

A sixth step of heat-treating the densified product fiber layers; And

And finishing the heat-treated product fiber layers.

In the present invention, only the rough laminar layer surrounding the carbon fibers is formed by isothermal method without making the entire fiber layer dense by isothermal method. Due to the rough laminar formed, the thermal conductivity of the carbon composite may be comparable to the thermal conductivity of the carbon composite made by isothermal method.

In the present invention, the entire fibrous layer is not densified by isothermal method, and the pores on the surface of the fibrous layer are not clogged. Therefore, it is not necessary to grind the surface of the fibrous layer to pierce the clogged pores on the surface of the fibrous layer. Therefore, it is possible to prevent the base material fiber layer from becoming smaller in thickness and size. Thus, one large and thick base fiber layer can be roughed to produce a number of fiber layers for a plurality of carbon composites in a predetermined number and size.

In the present invention, a smooth laminar layer is formed by impregnating carbon by a thermal gradient method to enclose the rough laminar layer, or a resin layer is formed by impregnating a resin by resin impregnation method and pyrolyzing the resin to enclose the rough laminar layer, Densify the fiber layer. Therefore, the time for producing the carbon composite material can be significantly shortened compared with the case where the whole fiber layer is densified by the isothermal method.

1 is a flowchart illustrating a method of manufacturing a carbon composite material according to an embodiment of the present invention.
2 is a view showing a base material fiber layer.
FIG. 3 is a view showing a base fiber layer in which a rough laminar layer surrounding carbon fibers is formed.
FIG. 4 is a view showing a state in which a base fiber layer having a rough laminar layer surrounding carbon fibers is roughed to produce various kinds of fiber layers for a carbon composite material.
5 (a), 5 (b), 5 (c) and 5 (d) show a product fiber layer on which a smooth laminar layer is formed to surround a rough laminar layer.
6 is an electron micrograph of a product fiber layer having a smooth laminar layer surrounding a rough laminar layer.
FIG. 7 is another electron micrograph of a product fiber layer formed with a smooth laminar layer surrounding a rough laminar layer.
8 is another electron micrograph of a product fiber layer having a smooth laminar layer surrounding a rough laminar layer.

Hereinafter, a method of manufacturing a carbon composite material according to an embodiment of the present invention will be described in detail.

As shown in FIG. 1, a carbon composite material manufacturing method according to an embodiment of the present invention includes:

A first step S11 of preparing a base fiber layer;

A second step (S12) of infiltrating carbon into the base fiber layer by an isothermal method to form a rough laminar layer surrounding the carbon fibers constituting the base fiber layer;

A third step (S13) of heat-treating the base fiber layer on which the rough laminar layer is formed;

A fourth step (S14) of roughing the heat-treated base material fiber layer to produce a plurality of product fiber layers;

A smooth laminar layer is formed on the product fibrous layers by a thermal gradient method so as to surround the rough laminar layer or a resin layer is formed by impregnating the product fiber layers with the resin and pyrolyzing the resin to cover the rough laminar layer A fifth step (S15) of densifying the product fiber layer;

A sixth step (S16) of heat-treating the densified product fiber layers;

And a seventh step (S17) of finishing the heat-treated product fiber layers.

The first step S11 will be described.

A base fiber layer 10 as shown in Fig. 2 is prepared.

The base material fiber layer 10 refers to one large and thick fiber layer. When the base material fiber layer 10 is used, a plurality of carbon composite materials having various shapes and sizes can be produced from the base material fiber layer 10 at a time. The thickness of the base material fiber layer 10 is 25 to 500 mm. For reference, the thickness of the conventional fiber layer is 20 mm or less. The base material fiber layer 10 is made by laminating carbon fiber fabrics and a carbon fiber web therebetween and needle punching in a lamination (vertical) direction. The density of the base material fiber layer 10 is 0.2 to 1.0 g / cm < 3 > to be.

The second step S12 will be described.

The base fiber layer (10) is impregnated with carbon by an isothermal method. 6 to 8, a rough laminar layer RL surrounding the carbon fiber Cf constituting the base material fiber layer 10 is formed. A reference symbol BR denotes a boundary line drawn in an electron microscope photograph to distinguish between a carbon fiber (Cf) and a rough laminar layer (RL), a rough laminar layer (RL) and a smooth laminar layer (SL).

The base fiber layer 10 'shown in FIG. 3 represents a base fiber layer in which a rough laminar layer RL is formed. In order to distinguish the base fiber layer 10 'from the base fiber layer 10 before the rough laminar layer RL is formed, a superscript (') is attached to the reference numeral 10 and a base fiber layer 10 ' Respectively.

The thickness of the rough laminar layer (RL) is 10 nm to 10 탆. Due to the rough laminar layer (RL), the thermal conductivity of the carbon composite increases from 10 to 40 w / mk to 30 to 120 w / mk. In addition, the density of the fibrous base material (10) 0.2 ~ 1.0 g / cm 3 0.3 to 1.5 g / cm < 3 > .

The time for forming the rough laminar layer RL is several hours to one week. The surface pores of the base material fiber layer 10 are not clogged to such an extent that a rough laminar layer (RL) having a thickness of 10 nm to 10 탆 is formed by an isothermal method. Therefore, it is not necessary to grind the surface of the base material fiber layer 10 to pierce the clogged surface pores.

However, if the isothermal method is used to make the thickness of the rough laminar layer (RL) thicker than 10 μm, the surface pores may be clogged. On the other hand, if the thickness of the rough laminar layer (RL) is made smaller than 10 nm, the thermal conductivity decreases because the surface pores are clogged. Therefore, in the present invention, the thickness of the rough laminar layer (RL) is in the range of 10 nm to 10 μm, which is an important thickness range having a critical meaning.

The third step S13 will be described.

the base fiber layer 10 'on which the rough laminar layer RL is formed is heat-treated at 1500 ° C or higher. When the base material fiber layer 10 'is heat-treated, it becomes soft enough to be roughed in the fourth step S14.

The fourth step S14 will be described.

Roughing refers to the work of cutting and cutting the base fiber layer to make the fiber layer of the carbon composite material into approximate shape and size.

The heat-treated base material fiber layer 10 'is roughed to produce plate-like product fiber layers 11 and 12 for carbon composite material and disc-shaped product fiber layers 13 and 14 for carbon composite material as shown in FIG. 3 . Of course, the heat treated base material fiber layer 10 'may be roughed to produce more product fiber layers in various shapes and sizes.

In the present invention, the surface pores of the base material fiber layer 10 are not clogged even though the isothermal method for forming the rough laminar layer (RL) is used. Therefore, it is not necessary to grind the surface of the base fiber layer 10 in order to drill the surface pores, and the shape and size of the base fiber layer 10 'are maintained at the roughing stage. Accordingly, the product fiber layers 11, 12, 13 and 14 for the carbon composite material can be formed in a predetermined number and size from the base fiber layer 10 '.

The fifth step S15 will be described.

5 (a), 5 (b), 5 (c) and 5 (d) show the densified product fiber layers 11 ', 12', 13 'and 14'. 12, 13, and 14 are distinguished from the product fiber layers 11, 12, 13, and 14 shown in FIG. 4 by the superscripts (' , 13 ', 14') are denoted more sharply than the product fiber layers (11, 12, 13, 14) before being densified.

Referring to Figs. 4 and 5 (a), (b), (c) and (d), carbon is infiltrated into each of the product fibrous layers 11, 12, 13 and 14 by a thermal gradient method. Then, as shown in FIGS. 6 to 8, a smooth laminar layer SL surrounding the rough laminar layer RL is formed. As the smooth laminar layer SL is diffused, the product fiber layers 11, 12, 13 and 14 are densified.

Alternatively, each of the product fibrous layers 11, 12, 13, and 14 is impregnated with a resin, and the resin is thermally decomposed to form a resin layer surrounding the rough laminar layer RL. As the resin layer is diffused, the product fiber layers 11, 12, 13, and 14 are densified.

In this way, since the final fiber density of the product fiber layer is reduced by a thermal gradient method or a resin impregnation method other than the isothermal method, the time for producing the carbon composite material can be reduced.

The density of the densified product fiber layers 11 ', 12', 13 ', 14' is 1.7 g / cm 3 Or more.

The sixth step S16 will be described.

The dense product fiber layers 11 ', 12', 13 'and 14' are heat treated at 1500 ° C. or higher.

When the densified product fiber layers 11 ', 12', 13 ', and 14' are heat-treated, they are softened enough to finish finishing in the seventh step S17.

The seventh step S17 will be described.

Finishing refers to the final production of a carbon composite material having a predetermined shape and size by precisely processing and polishing the product fiber layer.

The thermally treated product fibrous layers 11 ', 12', 13 ', and 14' are finely finished to finally produce a carbon composite having a predetermined shape and size.

10: base material fiber layer
10 ': base fiber layer formed with rough laminar layer
11, 12, 13, 14: Before the density is reduced,
11 ', 12', 13 ', 14': dense product fiber layer

Claims (4)

A first step of preparing a base fiber layer made by laminating carbon fiber fabrics and a carbon fiber web therebetween and needle punching in a stacking (vertical) direction;
A rough laminar layer having a thickness of 10 nm to 10 占 퐉 is formed by thermally decomposing hydrocarbon gas to penetrate carbon to enclose the carbon fibers constituting the base fiber layer in a state where the inner temperature and the outer temperature of the base material fiber layer are in a uniform state A second step of forming by an isothermal method;
A third step of heat-treating the base fiber layer on which the rough laminar layer is formed;
A fourth step of roughing the heat-treated base material fiber layer to produce a plurality of product fiber layers;
The thermal decomposition reaction of the hydrocarbon gas progresses gradually from the inside to the outside of each of the fibrous layers by giving a temperature gradient from the inside to the outside of each of the product fibrous layers so that the pore clogging does not occur so that the surface of the fibrous layer needs to be periodically polished A fifth step of densifying the product fiber layers by forming a smooth laminar layer by impregnating carbon without impregnating the rough laminar layer by a thermal gradient method;
A sixth step of heat-treating the densified product fiber layers; And
And finishing the heat-treated product fiber layers. delete delete delete
KR1020150099185A 2015-07-13 2015-07-13 Method for making carbon-carbon composite KR101679581B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190005305A (en) * 2017-07-06 2019-01-16 주식회사 카본티씨지 Method for manufacturing pump impeller having uniform rigidity
KR20190049132A (en) * 2017-11-01 2019-05-09 국방과학연구소 Fabrication Method of Carbon Fiber Preform Using In-Situ Coupling

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190005305A (en) * 2017-07-06 2019-01-16 주식회사 카본티씨지 Method for manufacturing pump impeller having uniform rigidity
KR102006737B1 (en) * 2017-07-06 2019-08-02 주식회사 카본티씨지 Method for manufacturing pump impeller having uniform rigidity
KR20190049132A (en) * 2017-11-01 2019-05-09 국방과학연구소 Fabrication Method of Carbon Fiber Preform Using In-Situ Coupling
KR102046783B1 (en) 2017-11-01 2019-11-20 국방과학연구소 Fabrication Method of Carbon Fiber Preform Using In-Situ Coupling

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