KR920005409B1 - Preparing method of carbon/ceramic composite - Google Patents

Preparing method of carbon/ceramic composite Download PDF

Info

Publication number
KR920005409B1
KR920005409B1 KR1019890020181A KR890020181A KR920005409B1 KR 920005409 B1 KR920005409 B1 KR 920005409B1 KR 1019890020181 A KR1019890020181 A KR 1019890020181A KR 890020181 A KR890020181 A KR 890020181A KR 920005409 B1 KR920005409 B1 KR 920005409B1
Authority
KR
South Korea
Prior art keywords
carbon
ceramic composite
less
pitch
composite material
Prior art date
Application number
KR1019890020181A
Other languages
Korean (ko)
Other versions
KR910011703A (en
Inventor
박양덕
이성영
Original Assignee
포항종합제철 주식회사
정명식
재단법인 산업과학기술연구소
박태준
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 포항종합제철 주식회사, 정명식, 재단법인 산업과학기술연구소, 박태준 filed Critical 포항종합제철 주식회사
Priority to KR1019890020181A priority Critical patent/KR920005409B1/en
Publication of KR910011703A publication Critical patent/KR910011703A/en
Application granted granted Critical
Publication of KR920005409B1 publication Critical patent/KR920005409B1/en

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/653Processes involving a melting step
    • C04B35/657Processes involving a melting step for manufacturing refractories

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

A carbon-ceramics composite is produced by (1) adding pitch system (isotropic and/or anisotropic) 10-40 wt.% with more than 300 deg.C of melting temperature as a carbon source, into a blast furnace water granulating slag 60-90 wt.% as a ceramic source, (the size of the mixed powder of the above pitch and slag is less than 0.074 mm), (2) pressure molding under the range of 100-500 kg/cm2 G, (3) heating the above molding material at a rate of less than 10 deg.C/ min in inert gas atmosphere, and (4) sintering the above (3) for 1 hour in the temperature range of 1,050-1,150 deg.C.

Description

핏치류와 고로수쇄슬래그를 이용한 탄소/세라믹 복합재료 제조방법Manufacturing method of carbon / ceramic composite using pitch and blast furnace slag

제1도는 본 발명의 방법에 의해 1050℃에서 소성한 탄소/세라믹 복합체의 탄소함량에 따른 압축강도의 변화를 나타내는 그래프.1 is a graph showing the change in compressive strength according to the carbon content of the carbon / ceramic composites calcined at 1050 ℃ by the method of the present invention.

제2도는 본 발명의 방법에 의해 1150℃에서 소성한 탄소/세라믹 복합체의 탄소함량에 따른 압축강도의 변화를 나타내는 그래프.2 is a graph showing the change in compressive strength according to the carbon content of the carbon / ceramic composites fired at 1150 ℃ by the method of the present invention.

본 발명은 탄소/세라믹 복합재료의 제조방법에 관한 것이며, 특히 핏치류와 고로수쇄슬래그를 이용한 탄소/세라믹복합재료의 제조방법에 관한 것이다. 탄소/세라믹 복합재료는 탄소재료의 특징인 경량, 내열성, 내열충격성, 전도성과 세라믹재료의 특징인 내산화성, 기계적강도등의 특성을 겸비한 재료로서 기계, 장치등의 내열구조재료, 고부하.고온용섭동재, 내식재, 전극재등의 다양한 용도로 활용된다. 통상 탄소/세라믹복합재료를 제조하기 위한 공급원료로는 탄소의 경우, 위스커(Whisker) 강화형의 탄소, 흑연 및 생코크스 또는 가소코크스등이 사용되어지고 있으며, 세라믹의 경우, 산화물(Al2O3, Y2O3, SiO2), 탄화물(SiC, B4C) 및 질화물(Si3N4)등이 사용되고 있다.The present invention relates to a method for producing a carbon / ceramic composite material, and more particularly to a method for producing a carbon / ceramic composite material using pitches and blast furnace slag. Carbon / ceramic composite material combines the characteristics of carbon materials such as light weight, heat resistance, thermal shock resistance, conductivity and ceramic material characteristics such as oxidation resistance, mechanical strength, and so on. It is used for various purposes such as perturbation, corrosion resistance, and electrode. In general, as a feedstock for the production of carbon / ceramic composites, carbon, graphite and raw coke or plastic coke of Whisker-reinforced type are used for carbon, and in the case of ceramics, oxide (Al 2 O) is used. 3 , Y 2 O 3 , SiO 2 ), carbides (SiC, B 4 C), nitrides (Si 3 N 4 ), and the like are used.

탄소/세라믹 복합재료는 다양한 구조를 갖고있으며, 섬유를 포함하는 복합재료와 포함하지않는 복합재료로 대별할 수 있다. 또한, 제조방법에 있어서는 복합재료의 구조에 따라 여러가지 제조법이 개발되었으나, 섬유를 사용하지 않는 경우에는 분말혼합소결방법과 성형체 함침방법등이 있다. 분말혼합소결방법으로서는 1) 생코크스 분말과 SiC 및 B4C 분말을 혼합하여 가압성형한후 불활성분위기하에서 소결하는 방법(일 특개공보 소59-131576, 59-213674), 2) 가소코크스분말과 금속산화물을 혼합하여 가열가압성형하는 방법(일 특개공보 소56-37192, 58-6711, 61-27352)등이 있으나, 이러한 제조방법은 사용되는 원료가 SiC, B4C, Si3N4, Al2O3, Y2O3등과같은 고순도의 원료를 사용함으로써 복합재료의 제조원가를 상승시키는 요인이 되는 것이다.Carbon / ceramic composites have a variety of structures and can be roughly classified into composite materials including fibers and composite materials without. In addition, in the manufacturing method, various manufacturing methods have been developed according to the structure of the composite material. However, when the fiber is not used, there are a powder mixed sintering method and a molding impregnation method. Powder mixing and sintering methods include: 1) mixing raw coke powder, SiC and B 4 C powder, and pressing them for sintering under inert atmosphere (Japanese Patent Publication No. 59-131576, 59-213674), 2) There is a method of heating and pressing a metal oxide mixture (Japanese Patent Laid-Open Publication No. 56-37192, 58-6711, 61-27352), but the raw materials used are SiC, B 4 C, Si 3 N 4 , and the like. By using high purity raw materials such as Al 2 O 3 , Y 2 O 3, etc., the manufacturing cost of the composite material is increased.

본 발명의 목적은 탄소/세라믹 복합재료를 제조함에 있어서 종래의 고순도원료를 사용하지 않고, 탄소원료로서 융점이 300℃ 이상인 핏치류를, 세라믹원료로서 제철부산물인 고로수쇄슬래그를 사용하여 탄소/세라믹 복합재료 제조방법을 제공하는데 있다.It is an object of the present invention to produce carbon / ceramic composite materials without using conventional high-purity raw materials, but with pitches having a melting point of 300 ° C. or higher as carbon raw materials, and blast furnace chain slag as steel by-products as ceramic raw materials. It is to provide a method for manufacturing a composite material.

본 발명에 의하면 세라믹원료로서 고로수쇄슬래그 60-90중량%에 탄소원료로서 융점 300℃ 이상의 핏치류 40-10중량% 첨가하여 100-500Kg/cm2의 압력하에 가압성형한후, 불활성 분위기하에서 승온속도 10℃/min 이하로 승온하여 1050-1150℃에서 1시간 유지시켜 소성시키는 탄소/세라믹 복합재료 제조방법이 제공된다.According to the present invention, 60-90 wt% of blast furnace slag slag as a ceramic raw material is added as a carbon raw material, and 40-10 wt% of pitches having a melting point of 300 ° C. or higher is formed under pressure under a pressure of 100-500 Kg / cm 2 and then heated in an inert atmosphere. Provided is a method for producing a carbon / ceramic composite material which is heated at a rate of 10 ° C./min or less and maintained at 1050-1150 ° C. for 1 hour to be fired.

본 발명에 사용되는 핏치류는 등방성 혹은 이방성 액정핏치를 다함께 사용가능하며 융점이 300℃ 이상인 것이 적합하다. 융점이 300℃ 이하인 경우 소성시 핏치의 용융으로 인한 변형이 야기될 우려가 있으며 휘발 성분의 방출에 따른 성형체의 강도저하를 일으키게된다.Pitches used in the present invention can be used together with isotropic or anisotropic liquid crystal pitch, and the melting point is preferably 300 ° C or higher. If the melting point is 300 ℃ or less, there is a fear that the deformation due to the melting of the pitch during firing, and the strength of the molded body due to the release of the volatile component is caused.

핏치의 함유량은 핏치 및 수쇄슬래그 전체중량의 약 10-40중량%가 바람직하며, 10중량% 이하 함유된 경우 탄소함유량이 지나치게 낮아 탄소/세라믹 복합재료로서의 효과를 기대하기 어렵게되며, 40중량% 이상 함유된 경우 성형체의 휨현상(Warping) 및 변형이 일어날 우려가 있는 것이다.Pitch content is preferably about 10 to 40% by weight of the total weight of the pitch and crushed slag, when less than 10% by weight of the carbon content is too low, it is difficult to expect the effect as a carbon / ceramic composite material, more than 40% by weight If contained, warping and deformation of the molded body may occur.

한편 본 발명에서의 핏치와 수쇄슬래그의 혼합분말의 입도는 0.074mm 이하가 바람직하며, 이는 입도가 0.074mm보다 큰 경우 충진율이 저하될뿐만 아니라 서형시 강도를 유지못하는 문제점이 있기때문이다.On the other hand, the particle size of the mixed powder of the pitch and the crushed slag in the present invention is preferably 0.074mm or less, because when the particle size is larger than 0.074mm, not only the filling rate is lowered but also the strength of the moldability is not maintained.

성형압력은 100-500Kg/cm2G가 바람직한바, 이는 500Kg/cm2G보다 높을경우에는 성형체 제조시 압축결함(pressing flaw)이 발생되기때문이고 100Kg/cm2G 이하에서는 성형체의 취급가능한 강도를 유지못하기 때문이다/승온속도를 10℃/min 이하로 한정한 이유는 그이상에서는 급송승온에 의한 핏치성분의 분해가 촉진되므로 분해성분의 과도한 휘발로인해 소결후 변형이 일어나기 때문이다. 소결온도를 1050℃-1150℃로 한정한 이유는 1050℃ 이하에서는 소결체로서의 충분한 강도를 유지못하기 때문이며 1150℃ 이상에서는 자화(Vitrification)가 일어나므로 변형을 일으키기 쉽다.Molding pressure is 100-500Kg / cm 2 G are preferred bars, which 500Kg / cm 2 G higher than the case has a defect, because the compression-molded article during manufacture (pressing flaw) caused 100Kg / cm 2 G or less in the treated possible strength of the molded article The reason for limiting the temperature increase rate to 10 ° C./min or less is that since the decomposition of the pitch component is accelerated by rapid temperature increase, the deformation occurs after sintering due to excessive volatilization of the decomposition component. The reason for limiting the sintering temperature to 1050 ° C. to 1150 ° C. is that it does not maintain sufficient strength as a sintered body at 1050 ° C. or lower, and it is susceptible to deformation since magnetization occurs at 1150 ° C. or higher.

이하 본 발명을 실시예에 따라 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

[실시예 1]Example 1

고로수쇄슬래그 분말과 핏치분말의 혼합비를 중량%로 90/10, 85/15, 80/20, 70/30, 60/40으로 변화시켜 0.074mm 이하의 입도를 갖도록 12시간 이상 혼합기를 이용 혼합분쇄한후, 성형압 100-500Kg/cm2G로 성형하여 성형체를 제조하였다. 제조된 성형체는 불활성분위기하에서 승온속도 10℃/min으로 승온하여 1050℃에서 1시간 소성하였다. 본 실시예에 사용된 고로수쇄 슬래그의 조성을 표 1에, 함량변화에 따른 복합재료의 비저항을 표 2에 압축강도를 제1도에 나타내었다.Mixing pulverization using a mixer for 12 hours or more to change the mixing ratio of blast furnace slag powder and pitch powder to 90/10, 85/15, 80/20, 70/30, 60/40 by weight% to have a particle size of 0.074 mm or less After that, the molded body was manufactured by molding at a molding pressure of 100-500 Kg / cm 2 G. The prepared molded article was heated at a heating rate of 10 ° C./min under an inert atmosphere and calcined at 1050 ° C. for 1 hour. The composition of the blast furnace slag used in this example is shown in Table 1, and the specific resistance of the composite material according to the content change is shown in Table 2 in the compressive strength in FIG.

[표 1]TABLE 1

Figure kpo00001
Figure kpo00001

[표 2]TABLE 2

Figure kpo00002
Figure kpo00002

상기 표 2 및 제1도에 의하면, 핏치함량이 증가할수록 압축강도는 증가하는 반면, 비저항은 감소함을 알 수 있다.According to Table 2 and FIG. 1, as the pitch content increases, the compressive strength increases, while the specific resistance decreases.

[실시예 2]Example 2

실시예1과 동일한 혼합성형방법으로 성형체를 제조한후, 불활성 분위기하에서 승온속도 5℃/min로 승온하여 1150℃에서 1시간 소성하였다. 제조된 복합재료의 압축강도를 제2도에, 비저항을 표 3에 나타내었다. 제2도 및 표 3에서 알수 있는 바와같이 1150℃에서 소성한 결과 1050℃에서 소성한 실시예 1에 비하여 압축강도가 3배이상 증가하였으며 전기 비저항은 1/10 이하로 감소하였다.After the molded product was produced by the same mixing molding method as in Example 1, the resultant was heated at a temperature increase rate of 5 ° C / min in an inert atmosphere and calcined at 1150 ° C for 1 hour. The compressive strength of the manufactured composite material is shown in FIG. 2 and the specific resistance is shown in Table 3. As can be seen from FIG. 2 and Table 3, as a result of firing at 1150 ° C., the compressive strength increased more than three times compared to Example 1 baked at 1050 ° C., and the electrical resistivity decreased to 1/10 or less.

[표 3]TABLE 3

Figure kpo00003
Figure kpo00003

상기한 바와같이, 본 발명은 제철부산물인 고로수쇄슬래그와 화석원료의 잔사인 핏치류를 사용하여 탄소/세라믹 복합재료를 제조함으로써 제철 부산물의 고부가가치화는 물론 탄소/세라믹 복합재료의 제조원가절감을 도모할 수 있는 것이다.As described above, the present invention provides a carbon / ceramic composite material by using blast furnace slag as a by-product of iron and pitch as a residue of fossil raw material, thereby achieving high added value of steel by-products as well as manufacturing cost reduction of carbon / ceramic composite. You can do it.

Claims (1)

탄소/세라믹복합재료를 제조하는 방법에 있어서, 고로수쇄슬래그 60-90중량%에 융점 300℃ 이상의 핏치류 40-10중량%를 첨가하여 100-500Kg/cm2G의 압력하에서 가압성형한후, 불활성분위기하에서 승온속도 10℃/min 이하로 승온하여 1050-1150℃에서 1시간 유지시켜 소성시킴을 특징으로 하는 탄소/세라믹 복합재료제조방법.In the method for producing a carbon / ceramic composite material, 60-90% by weight of blast furnace slag is added under pressure of 100-500 Kg / cm 2 G by adding 40-10% by weight of pitches having a melting point of 300 ° C. or higher, and A method of producing a carbon / ceramic composite material, wherein the temperature is raised to 10 ° C./min or less in an inert atmosphere and maintained at 1050-1150 ° C. for 1 hour for baking.
KR1019890020181A 1989-12-29 1989-12-29 Preparing method of carbon/ceramic composite KR920005409B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019890020181A KR920005409B1 (en) 1989-12-29 1989-12-29 Preparing method of carbon/ceramic composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019890020181A KR920005409B1 (en) 1989-12-29 1989-12-29 Preparing method of carbon/ceramic composite

Publications (2)

Publication Number Publication Date
KR910011703A KR910011703A (en) 1991-08-07
KR920005409B1 true KR920005409B1 (en) 1992-07-03

Family

ID=19294219

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1019890020181A KR920005409B1 (en) 1989-12-29 1989-12-29 Preparing method of carbon/ceramic composite

Country Status (1)

Country Link
KR (1) KR920005409B1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2384774A (en) * 2002-02-01 2003-08-06 Carbon Applic Technology Ltd Refractory article comprising particulate pitch

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR970042374A (en) * 1995-12-30 1997-07-24 석진철 Method for manufacturing primary carbides of carbon / carbon composites

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2384774A (en) * 2002-02-01 2003-08-06 Carbon Applic Technology Ltd Refractory article comprising particulate pitch

Also Published As

Publication number Publication date
KR910011703A (en) 1991-08-07

Similar Documents

Publication Publication Date Title
KR940011452B1 (en) Silicon carbide refractories having modified silicon nitride bond
US3250832A (en) Process for making refractory articles
US4224073A (en) Active silicon carbide powder containing a boron component and process for producing the same
CN101798222A (en) Al2O3-Ni-C-B4C composite ceramic and preparation method thereof
EP2527773B1 (en) Refractory for an inner lining of a blast furnace, obtained by semi-graphitization of a mixture comprising C and Si.
KR920005409B1 (en) Preparing method of carbon/ceramic composite
DE3229701A1 (en) METHOD FOR PRODUCING A Sintered Shaped Body From Refractory Material
JP3765840B2 (en) Carbon material manufacturing method
US4770825A (en) Process for producing electrodes from carbonaceous particles and a boron source
KR100310050B1 (en) method for forming canbon brick with fire resistance and corrosion resestance
KR900005513B1 (en) Carbon containing refractories
US4788168A (en) Method for producing carbon-ceramic composite material
DE2232719A1 (en) Refractory stones - contg refractory oxide and/or carbide grains and silicon carbide binder
JPS605550B2 (en) Manufacturing method of silicon carbide sintered body
JPH0881706A (en) Production of carbon refractories for blast furnace
EP0109839A2 (en) Method of making graphite electrodes
CN100376509C (en) Use of a silicon carbide-based ceramic material in aggressive environments
KR940006428B1 (en) Process for the preparation of firebrick
JPS5919073B2 (en) Method for manufacturing sintered compacts
JP3966911B2 (en) In-furnace members and jigs
JPS6374978A (en) Ceramic composite body
RU2084426C1 (en) Method of preparing blend for moldings containing silicon carbide
KR100638447B1 (en) Method for preparing carbonaceous material by using wasted cordress tire powder and fine graphite powder
JP2697482B2 (en) Method for producing pitch-based material and method for producing carbon material using the same as raw material
KR100752918B1 (en) Method of preparing carbonaceous material by using wasted cordless tire power and coke dust

Legal Events

Date Code Title Description
A201 Request for examination
G160 Decision to publish patent application
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20000704

Year of fee payment: 9

LAPS Lapse due to unpaid annual fee