KR101626335B1 - Manufacturing method for Self-lubricated SiC ceramic disk - Google Patents

Manufacturing method for Self-lubricated SiC ceramic disk Download PDF

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KR101626335B1
KR101626335B1 KR1020160028437A KR20160028437A KR101626335B1 KR 101626335 B1 KR101626335 B1 KR 101626335B1 KR 1020160028437 A KR1020160028437 A KR 1020160028437A KR 20160028437 A KR20160028437 A KR 20160028437A KR 101626335 B1 KR101626335 B1 KR 101626335B1
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sic
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강성호
김인섭
이진욱
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주식회사 신한세라믹
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/005Control means for lapping machines or devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/20Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B24B7/22Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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    • 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
    • C04B35/64Burning or sintering processes

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Abstract

The present invention relates to a manufacturing method for a self-lubricated SiC ceramic disk, and more specifically, to a self-lubricated SiC ceramic composition and a manufacturing method of a ceramic disk using the same, in which the self-lubricated SiC ceramic composition is mounted in a faucet for reducing frictional resistance of the ceramic disk which is a module functioning as a valve with respect to hot and cold water to provide the ceramic disk with self-lubricated property. The present invention includes: 75-95 parts by weight of SiC having an average particle size of 0.3-2 μm; 5-20 parts by weight of carbon powder having an average particle size of 0.1-50 μm; 0.5-1.5 parts by weight of boron carbide (B_4C); 1.0-5.0 parts by weight of carbon black; 0.1-1.0 parts by weight of triethanolamine (TEA); 0.5-4.0 parts by weight of polyvinyl alcohol (PVA); and 0.5-4.0 parts by weight of polyethylene glycol (PEG).

Description

자기윤활성 SiC 세라믹디스크 제조방법{Manufacturing method for Self-lubricated SiC ceramic disk}Technical Field [0001] The present invention relates to a self-lubricating SiC ceramic disk,

본 발명은 자기윤활성 SiC 세라믹디스크의 제조방법에 관한 것으로서, 보다 상세하게는 수전금구에 내장되어 냉·온수에 대한 밸브기능을 하는 모듈인 세라믹카트리지내의 세라믹디스크의 접동(sliding)시 마찰저항을 감소시켜 자기윤활성을 부여할 수 있는 자기윤활성 SiC 세라믹디스크의 제조방법에 관한 것이다.The present invention relates to a method of manufacturing a self-lubricating SiC ceramic disk, and more particularly, to a method of manufacturing a self-lubricating SiC ceramic disk by reducing a frictional resistance during sliding of a ceramic disk in a ceramic cartridge which is built in a water- To a self-lubricating SiC ceramic disk which is capable of imparting self-lubricating properties to the self-lubricating SiC ceramic disk.

수전금구에 내장되어 냉·온수에 대한 밸브기능을 하는 세라믹카트리지 모듈은 냉·온수의 온도환경에 대한 열팽창특성 및 열충격특성, 워터해머 등의 높은 수압환경에 견디는 내수압특성, 장기사용에 대한 구성부품의 장기내구특성, 물속에 포함되어 있는 각종 고형분 또는 화학적 작용에 대한 내구특성, 장기사용에 대한 누수 및 레버 토크의 일정성 등 가혹한 환경에서의 고신뢰성을 요하는 정밀 제품이어야 한다. The ceramic cartridge module, which is built into the faucet and functions as a valve for cold and hot water, has the thermal expansion and thermal shock characteristics against the temperature environment of cold and hot water, the water pressure characteristics to withstand the high water pressure environment such as water hammer, The product must be a precision product requiring high reliability in a harsh environment, such as long-term durability of water, durability against various solid contents or chemical action contained in water, lean water for long-term use, and uniformity of lever torque.

기존의 세라믹카트리지는 열충격으로 인한 세라믹크랙 및 파단, 플라스틱부품의 저강도, 알루미나세라믹디스크의 낮은 마모 특성으로 인한 장기 사용 시 스틱킹 현상, 설계사상 및 부품간 치수정밀성 부족 등으로 인하여 다양한 고장요인이 있다. Conventional ceramic cartridges have various failures due to ceramic cracks and fractures due to thermal shock, low strength of plastic parts, sticking phenomenon due to long wear due to characteristics of alumina ceramic disc, have.

세라믹카트리지의 구성부품들 중에서 가장 핵심적인 부품이 세라믹디스크인데, 기존에는 96%알루미나 성분으로 구성된 알루미나 세라믹디스크가 주로 사용되었으며, 또 하나의 종류로 96%알루미나 세라믹디스크의 폴리싱 표면에 DLC(Diamond Like Carbon)층을 코팅한 DLC디스크가 사용되고 있다. The most important component of the ceramic cartridge is a ceramic disk. In the past, an alumina ceramic disk composed of 96% alumina was mainly used. Another type of disk was a DLC (Diamond Like Carbon layer coated DLC disc is used.

기존의 알루미나 세라믹디스크의 단점은 장시간 사용 시 낮은 내마모 특성으로 인한 디스크 마모와 디스크 사이에 도포된 그리스의 소실로 인해 누수 고장율이 높고, 상·하 디스크간의 고착현상(Sticking)이 발생하여 핸들토크가 증가하는 문제점이 있다. The disadvantage of the conventional alumina ceramic disc is that the leakage of the lubricant between the disc and the disc due to wear of the disc due to low abrasion resistance is high and the sticking phenomenon between the upper and lower discs occurs, Is increased.

또한, DLC디스크의 단점은 DLC코팅비용이 고가(알루미나디스크의 3~4배 가격)라는 문제점, 코팅층의 두께가 불과 1㎛ 정도로 얇아 장기사용 시 코팅층의 이탈로 인한 누수 발생이라는 문제점, 그리고 PVD 및 CVD코팅공정에서 코팅표면에 형성되는 DLC의 작은 덩어리(droplet)로 인한 평탄도 변화로 인한 누수발생의 문제점 등이 있다. The disadvantage of the DLC disc is that the DLC coating cost is high (3 to 4 times the price of the alumina disk), the thickness of the coating layer is as thin as 1 占 퐉, There is a problem of leakage due to a change in flatness due to a small droplet of DLC formed on the coating surface in the CVD coating process.

대한민국 등록특허공보 제10-0471662호.Korean Patent Registration No. 10-0471662. 대한민국공개특허공보 제10-1996-0013530호.Korean Patent Publication No. 10-1996-0013530. 대한민국공개특허공보 제10-1989-0001908호.Korean Patent Publication No. 10-1989-0001908. 대한민국공개특허공보 제10-2014-0096282호.Korean Patent Publication No. 10-2014-0096282.

따라서, 본 발명에서는 상기한 종래 기술의 문제점을 해결하고자 안출한 것으로, 종래의 알루미나디스크 및 DLC디스크의 여러 가지 문제점을 해소하고, 다음과 같은 장점을 가진 자기윤활성 SiC세라믹디스크를 제조할 수 있는 방법을 제공하는 것을 그 해결과제로 한다. SUMMARY OF THE INVENTION Accordingly, the present invention has been made in order to solve the problems of the prior art described above, and it is an object of the present invention to provide a method of manufacturing a self-lubricating SiC ceramic disk having the following merits and solving various problems of conventional alumina disks and DLC disks As a solution to the problem.

1. 내마모성이 우수하여 장기 사용 시에도 마모로 인한 누수고장과 디스크간의 스틱킹 현상의 문제점을 해결한 경도가 매우 높은 SiC세라믹을 이용한 자기윤활성 SiC세라믹디스크를 제조할 수 있는 방법의 제공.1. Providing a method for manufacturing a self-lubricating SiC ceramic disk using SiC ceramics which solves the problems of water leakage due to abrasion and sticking phenomenon due to abrasion even when using for a long time due to excellent abrasion resistance.

2. 마찰계수가 매우 낮은 SiC세라믹을 사용하여 카트리지의 핸들 토크저항이 낮아 카트리지 구성부품에 무리한 힘을 가하지 않으며 사용자의 레버 조작감이 부드러워질 수 있는 이점을 갖는 자기윤활성 SiC세라믹디스크를 제조할 수 있는 방법의 제공.2. It is possible to manufacture a self-lubricating SiC ceramic disk with a low friction coefficient of SiC ceramics which has a low handle torque resistance of the cartridge and does not exert unnecessary force on the cartridge components and has an advantage that the user can feel the lever operation smoothly Providing a method.

3. DLC디스크와 같은 코팅층이 없는 SiC세라믹디스크를 제공함으로써, 코팅층으로 인해 발생하는 얇은 DLC코팅층의 내구성, DLC코팅공정의 droplet으로 인한 평탄도 변화에서 발생되는 미세누수의 문제점을 근본적으로 해결한 자기윤활성 SiC세라믹디스크의 제공.3. By providing a SiC ceramic disk without a coating layer such as a DLC disk, it is possible to improve the durability of the thin DLC coating layer caused by the coating layer and the problem of micro leakage caused by the flatness change due to the droplet of the DLC coating process. Providing of lubricous SiC ceramic disc.

4. 고가의 grease를 사용하지 않아도 되어 grease 도포공정 비용 및 grease 비용을 절감할 수 있고, 사용 중 소실되는 grease로 인한 인체 및 환경에 대한 영향을 완전히 배제할 수 있는 자기윤활성 SiC세라믹디스크를 제조할 수 있는 방법의 제공.4. Manufacture self-lubricating SiC ceramic discs which can reduce the cost of grease coating process and grease cost by eliminating expensive grease and completely eliminate human and environmental influences due to lost grease Provide a way of being able.

5. 고신뢰성 고급제품에 적용이 가능한 자기윤활성 SiC세라믹디스크를 제조할 수 있는 방법의 제공과 또한, 본 발명에서는 상기한 자기윤활성 SiC세라믹디스크를 제공하기 위하여, 자기윤활성을 부여할 수 있는 상압소결용 SiC세라믹 조성물을 제공하는 것을 다른 해결과제로 한다 5. Providing a method of manufacturing a self-lubricating SiC ceramic disk which can be applied to a high-reliability high-grade product. In addition, in order to provide the self-lubricating SiC ceramic disk described above, Another object of the present invention is to provide a SiC ceramic composition

상기한 과제를 해결한 본 발명의 자기윤활성을 부여할 수 있는 상압소결용 SiC세라믹 조성물은 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에타놀아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하는 것을 특징으로 한다. The SiC ceramic composition for atmospheric pressure sintering according to the present invention which solves the above problems has 75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 탆, 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1 to 1.0 part by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); And 0.5 to 4.0 parts by weight of polyethylene glycol (PEG).

여기서, 상기 카본블랙은 평균입도크기 10~90㎚인 것을 사용하는 것을 특징으로 한다. Here, the carbon black having an average particle size of 10 to 90 nm is used.

또한, 본 발명에서는 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도분포 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에탄올아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하도록 볼밀링장치에 투입하고, 회전수 15~20rpm 조건으로 20~24시간 볼밀링하여 혼합하는 상압소결용 SiC세라믹 슬러리를 준비하는 혼합공정;Also, in the present invention, 75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 탆, 5 to 20 parts by weight of a carbon powder having an average particle size distribution of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1-1.0 parts by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); 0.5 to 4.0 parts by weight of polyethylene glycol (PEG) is put into a ball milling apparatus and ball milling is performed for 20 to 24 hours at a rotation speed of 15 to 20 rpm to prepare a SiC ceramic slurry for pressure-sintering;

상기 혼합공정의 슬러리를 분무건조기에 투입하여 과립화하는 과립공정;A granulation step of granulating the slurry of the mixing step into a spray dryer;

상기 과립공정에서 얻어지는 과립을 금형에 투입하여 성형하는 성형공정;A molding step in which the granules obtained in the granulation process are put into a mold and molded;

상기 성형공정에서 얻어진 성형체를 진공상태에서 첨가된 유기물을 제거하기 위한 탈지공정;A degreasing step of removing the organic material added in the vacuum state of the formed body obtained in the forming step;

상기 탈지공정이 완료된 후, 그 성형체를 진공분위기에서 10℃/min의 승온속도로 0~1500℃까지 승온하고, 아르곤(Ar) 가스분위기에서 4℃/min의 승온속도로 1500~2100℃까지 승온하여 2~3시간 유지하여 SiC디스크를 소결하는 소결공정;After the degreasing step is completed, the formed body is heated in a vacuum atmosphere at a temperature raising rate of 10 DEG C / min to a temperature of 0 to 1500 DEG C and heated to a temperature of 1500 to 2100 DEG C at a temperature raising rate of 4 DEG C / min in an argon And sintering the SiC disk by holding it for 2 to 3 hours;

상기 소결공정에서 소결된 SiC디스크를 래핑기에서 래핑가공하고, 상기 래핑가공이 완료된 SiC디스크를 폴리싱 장비에 투입하여 폴리싱 가공을 포함하여 이루어지는 자기윤활성 SiC 세라믹디스크 제조방법을 제공한다. There is provided a self-lubricating SiC ceramic disk manufacturing method comprising lapping a SiC disk sintered in the sintering process in a lapping machine, and polishing the SiC disk having been subjected to the lapping process to a polishing machine.

여기서, 상기 과립공정은 쳄버온도(Chamber Temp.) 80~120℃, 인렛온도(Inlet Temp.) 180~200℃, 아토마이져디스크(atomizer disc)의 회전수 4000~12000rpm의 건조조건으로 과립화하는 것을 특징으로 한다.Here, the granulation process is granulated at a chamber temperature of 80 to 120 ° C, an inlet temperature of 180 to 200 ° C, and an atomizer disc at 4000 to 12000 rpm, .

여기서, 상기 탈지공정은 진공상태에서 승온속도 1℃/min의 속도로 탈지최고온도 800℃까지 승온한 후, 1.5~2시간동안 유지하는 것을 특징으로 한다.Here, the degreasing process is characterized in that the temperature is raised to a degreasing maximum temperature of 800 ° C at a rate of 1 ° C / min in a vacuum state, and then maintained for 1.5 to 2 hours.

여기서, 상기 가공공정의 래핑기에서 래핑은 회전수 5~100rpm의 조건으로 1~5분 동안 래핑가공하고, 상기 폴리싱가공은 폴리싱 장비에서 다이야몬드 연마입자의 크기가 1~5㎛를 포함하는 슬러리를 분무하여 폴리싱 가공하는 것을 특징으로 한다. Here, the lapping in the lapping machine of the working step is performed by lapping for 1-5 minutes under the condition of 5 to 100 rpm of rotation, and the polishing is performed in a polishing machine in a slurry containing diamine abrasive grains of 1 to 5 탆 Is sprayed and polished.

또한, 본 발명에서는 상기한 제조방법에 의해 제조되는 것으로, 밀도 2.4~3.1(g/㎤), 경도(Hv0.5) 2,400~2,600kgf/㎟, 표면조도 0.02~0.15㎛의 물성을 가지는 자기윤활성 SiC세라믹디스크를 제공한다.In the present invention, it is produced by the above-mentioned manufacturing method and has self-lubricating properties having physical properties of a density of 2.4 to 3.1 (g / cm3), a hardness (Hv0.5) of 2,400 to 2,600 kgf / SiC ceramic disk.

본 발명에 따라 제공되는 자기윤활성을 부여할 수 있는 자기윤활성 SiC 세라믹디스크의 제조방법에 의해 제조되는 SiC세라믹디스크는 다음과 같은 효과를 얻을 수 있다.The SiC ceramic disk manufactured by the method of manufacturing a self-lubricating SiC ceramic disk which can provide self-lubricating provided according to the present invention can obtain the following effects.

1. 자기윤활성 SiC세라믹디스크는 경도가 매우 높아 내마모성이 우수하여 장기 사용 시에도 마모로 인한 누수고장과 디스크간의 스틱킹 현상의 문제점을 해결할 수 있다. 1. Self-lubricating SiC ceramics discs have very high hardness, so they have excellent abrasion resistance, which can solve problems of water leakage due to wear and sticking phenomenon between discs even in long-term use.

2. 자기윤활성 SiC세라믹디스크는 마찰계수가 매우 낮아 세라믹카트리지의 핸들 토크저항이 낮아 카트리지 구성부품에 무리한 힘을 가하지 않으며 사용자의 레버 조작감이 부드러워지는 장점이 있다. 2. The self-lubricating SiC ceramic disc has a very low coefficient of friction so that the handle torque resistance of the ceramic cartridge is low, so that it does not exert excessive force on the cartridge components and softens the user's levers.

3. 자기윤활성 SiC세라믹디스크는 DLC디스크와 같은 코팅층이 없기 때문에 코팅층으로 인해 발생하는 얇은 DLC코팅층의 내구성, DLC코팅공정의 droplet으로 인한 평탄도 변화에서 발생되는 미세누수의 문제점을 근본적으로 해결할 수 있다. 3. Because the self-lubricating SiC ceramic disk does not have the same coating layer as the DLC disk, it can fundamentally solve the problems of the durability of the thin DLC coating layer caused by the coating layer and the micro leakage caused by the flatness change due to the droplet of the DLC coating process .

4. 자기윤활성 SiC세라믹디스크를 사용함으로써 고가의 grease를 사용하지 않아도 되어 grease 도포공정 비용 및 grease 비용을 절감할 수 있고, 사용 중 소실되는 grease로 인한 인체 및 환경에 대한 영향을 완전히 배제할 수 있는 장점이 있다. 4. By using self-lubricating SiC ceramics disk, it is possible to reduce the cost of grease coating process and grease cost because it does not need to use expensive grease, and it is possible to completely eliminate the influence on human body and environment due to lost grease There are advantages.

도 1 내지 3은 본 발명의 조성물에 적용되는 SiC원료의 그레이드(grade)별 전자현미경 사진이다.
도 4는 본 발명의 조성물에 사용되는 최적조건인 A-grade의 입도분석결과를 도시한 표 및 그래프이다.
도 5는 본 발명의 조성물의 부원료로 사용되는 카본파우더의 입도분석결과를 도시한 표 및 그래프이다.
도 6은 본 발명의 일실험예에 따른 분무과립조건에서의 이상과립 형상의 전자현미경 사진이다.
도 7은 본 발명의 일실험예에 따른 최적 분무과립조건에서 제조된 과립형상의 전자현미경사진이다.
도 8은 본 발명의 일실험예에 따라 제조된 SiC세라믹디스크의 폴리싱 면의 표면조도 측정 결과를 도시한 그래프이다.
도 9는 본 발명의 일실험예에 따라 제조된 소결체 SiC디스크의 파단면 SEM분석결과를 도시한 SEM사진이다.
도 10은 본 발명의 일실험예에 따라 제조된 소결체인 SiC디스크의 파단면의 EDS분석결과를 나타낸 사진이다.
도 11은 본 발명의 일실험예에 따른 SiC세라믹카트리지의 내압시험결과를 도시한 사진이다.
1 to 3 are electron micrographs of grade of SiC raw materials applied to the composition of the present invention.
4 is a table and a graph showing the results of particle size analysis of A-grade which is an optimum condition used in the composition of the present invention.
FIG. 5 is a table and a graph showing the results of particle size analysis of carbon powder used as a sub ingredient of the composition of the present invention.
6 is an electron micrograph of an abnormal granule shape under spray granulation conditions according to an experimental example of the present invention.
7 is an electron micrograph of a granular shape prepared under optimum spray granulation conditions according to an experimental example of the present invention.
8 is a graph showing surface roughness measurement results of a polishing surface of a SiC ceramic disk manufactured according to an experimental example of the present invention.
9 is a SEM photograph showing a SEM analysis result of a fracture surface of a sintered SiC disk manufactured according to an experimental example of the present invention.
10 is a photograph showing the result of EDS analysis of the fracture surface of a SiC disk, which is a sintered body manufactured according to an experimental example of the present invention.
11 is a photograph showing the result of the pressure resistance test of the SiC ceramic cartridge according to one experimental example of the present invention.

이하, 본 발명을 첨부된 도면을 참조하여 보다 상세히 설명하기로 한다. BRIEF DESCRIPTION OF THE DRAWINGS The present invention will be described in more detail with reference to the accompanying drawings.

본 발명은 수전금구에 내장되어 냉·온수에 대한 밸브기능을 하는 모듈인 세라믹카트리지를 구성하는 상·하판으로 구성된 세라믹디스크의 표면에 도포하던 그리스를 사용하지 않고 그 세라믹디스크에 자기윤활성을 부여할 수 있는 자기윤활성 SiC세라믹 조성물 및 이를 이용한 세라믹디스크의 제조방법에 관한 것이다.The present invention relates to a ceramic disk, which is built in a water-receiving metal fitting and functions as a valve for cold and hot water, is self-lubricating the ceramic disk without using grease applied to the surface of the ceramic disk constituted by the upper and lower plates constituting the ceramic cartridge To a self-lubricating SiC ceramic composition and a method of manufacturing a ceramic disk using the same.

본 발명에 따른 자기윤활성을 부여할 수 있는 상압소결용 SiC세라믹 조성물은 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에타놀아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하는 것에 그 기술적 특징이 있다. The SiC ceramic composition for pressureless sintering according to the present invention, which can impart self-lubricating properties, comprises 75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 占 퐉; 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1 to 1.0 part by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); And 0.5 to 4.0 parts by weight of polyethylene glycol (PEG).

이때, 상기 카본블랙은 평균입도크기 10~90㎚인 것을 사용하는 것이 바람직하다. 그 이유는 카본블랙의 입도가 미세할수록 비표면적이 높아 반응속도가 빠르고 미반응 카본으로 잔류하는 것이 적어지기 때문이다. At this time, the carbon black preferably has an average particle size of 10 to 90 nm. The reason is that the finer the particle size of the carbon black, the higher the specific surface area, the faster the reaction rate and the less the unreacted carbon remains.

본 발명에 따른 자기윤활성 SiC 세라믹디스크 제조방법은 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에타놀아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하도록 볼밀링장치에 투입하고, 회전수 15~20rpm 조건으로 20~24시간 볼밀링하여 혼합하는 상압소결용 SiC세라믹 슬러리를 준비하는 혼합공정;A method of manufacturing a self-lubricating SiC ceramic disk according to the present invention comprises: 75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 탆; 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1 to 1.0 part by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); 0.5 to 4.0 parts by weight of polyethylene glycol (PEG) is put into a ball milling apparatus and ball milling is performed for 20 to 24 hours at a rotation speed of 15 to 20 rpm to prepare a SiC ceramic slurry for pressure-sintering;

상기 혼합공정의 슬러리를 분무건조기에 투입하여 과립화하는 과립공정;A granulation step of granulating the slurry of the mixing step into a spray dryer;

상기 과립공정에서 얻어지 과립을 금형에 투입하여 성형하는 성형공정;A molding step of molding the granules obtained in the granulation process into a mold;

상기 성형공정에서 얻어진 성형체를 진공상태에서 첨가된 유기물을 제거하기 위한 탈지공정;A degreasing step of removing the organic material added in the vacuum state of the formed body obtained in the forming step;

상기 탈지공정이 완료된 후, 그 성형체를 진공분위기에서 10℃/min의 승온속도로 0~1500℃까지 승온하고, 아르곤(Ar) 가스분위기에서 4℃/min의 승온속도로 1500~2100℃까지 승온하여 2~3시간 유지하여 SiC디스크를 소결하는 소결공정; After the degreasing step is completed, the formed body is heated in a vacuum atmosphere at a temperature raising rate of 10 DEG C / min to a temperature of 0 to 1500 DEG C and heated to a temperature of 1500 to 2100 DEG C at a temperature raising rate of 4 DEG C / min in an argon And sintering the SiC disk by holding it for 2 to 3 hours;

상기 소결공정에서 소성된 SiC디스크를 래핑기에서 래핑가공하고, 상기 래핑가공이 완료된 SiC디스크를 폴리싱 장비에 투입하여 폴리싱 가공을 포함하여 이루어지는 자기윤활성 SiC 세라믹디스크 제조방법을 제공한다. The present invention also provides a self-lubricating SiC ceramic disk manufacturing method comprising lapping a sintered SiC disk in a sintering process and polishing the sintered SiC disk into a polishing machine.

여기서, 상기 과립공정은 쳄버온도(Chamber Temp.) 80~120℃, 인렛온도(Inlet Temp.) 180~200℃, 아토마이져디스크(atomiser disc)의 회전수 4000~12000rpm의 건조조건으로 과립화하는 것을 특징으로 한다.Herein, the granulation process is granulated at a chamber temperature of 80 to 120 DEG C, an inlet temperature of 180 to 200 DEG C, and an atomizer disc at 4000 to 12000 rpm, .

여기서, 상기 탈지공정은 진공상태에서 승온속도 1℃/min의 속도로 탈지최고온도 800℃까지 승온한 후, 1.5~2시간동안 유지하는 것을 특징으로 한다.Here, the degreasing process is characterized in that the temperature is raised to a degreasing maximum temperature of 800 ° C at a rate of 1 ° C / min in a vacuum state, and then maintained for 1.5 to 2 hours.

여기서, 상기 가공공정의 래핑기에서 래핑은 회전수 5~100rpm의 조건으로 1~5분 동안 래핑가공하고, 상기 폴리싱가공은 폴리싱 장비에서 다이야몬드 연마입자의 크기가 1~5㎛를 포함하는 슬러리를 분무하여 폴리싱 가공하는 것을 특징으로 한다. Here, the lapping in the lapping machine of the working step is performed by lapping for 1-5 minutes under the condition of 5 to 100 rpm of rotation, and the polishing is performed in a polishing machine in a slurry containing diamine abrasive grains of 1 to 5 탆 Is sprayed and polished.

또한, 본 발명에서는 상기한 제조방법에 의해 제조되는 것으로, 밀도 2.4~3.1(g/㎤), 경도(Hv0.5) 2,400~2,600kgf/㎟, 표면조도 0.02~0.15㎛의 물성을 가지는 가지는 자기윤활성 SiC세라믹디스크를 제공할 수 있으며, 그 제공된 자기윤활성 SiC세라믹디스크를 적용함으로써 고신뢰성 SiC세라믹카트리지를 제공할 수 있는 것이다. In the present invention, it is produced by the above-mentioned production method, and has a property of having a physical property of a density of 2.4 to 3.1 (g / cm3), a hardness (Hv0.5) of 2,400 to 2,600 kgf / A lubricating SiC ceramic disk can be provided, and a highly reliable SiC ceramic cartridge can be provided by applying the self-lubricating SiC ceramic disk provided.

이상에서 설명되는 본 발명을 완성하기 위하여 실험예를 통해 보다 상세히 설명하여 보면,  In order to complete the present invention described above,

1. 출발원료의 선정1. Selection of starting materials

<주원료 선정><Main ingredient selection>

자기윤활성을 부여할 수 있는 출발원료의 선정과 출발원료에 대한 조성을 설계하기 위해서 주원료, 부원료, 유기첨가원료 등에 대하여 검토하고 선정하기 위하여 시험하여 보았다. In order to select the starting materials that can impart self-lubricating properties and to design the ingredients for the starting materials, the main ingredients, additives, and organic additives were tested and selected.

주원료는 SiC(Silicon Carbide)로서 상압소결용 원료로 주로 사용되는 것은 α type 6H 결정을 사용한다. The main raw material is SiC (Silicon Carbide), which is mainly used as a raw material for pressureless sintering. Α type 6H crystal is used.

상압소결용 SiC 출발원료 선정을 위해서는 순도, 평균입자크기, 입도분포, 입자형상 등이 중요한 판단요소로, 이러한 여러 가지 요인을 염두에 두고 평균입도크기가 0.3~2㎛ 정도의 범위에 있는 원료들을 도 1 내지 3에 도시된 바와 같이, grade별로 검토하였으며, 그 결과, A-grade의 원료를 선정하여 입도를 분석하여 보았으며, 그 결과는 도 4에 도시하였다. 도 4에 따르면, A-grade는 평균입도분포가 0.78㎛인 것을 확인할 수 있었다. Purity, average particle size, particle size distribution, particle shape, etc. are important factors for selecting SiC starting material for pressureless sintering. Considering these various factors, raw materials having an average particle size in the range of about 0.3 to 2 μm As shown in FIGS. 1 to 3, the grades were examined by grades. As a result, raw materials of A-grade were selected and the particle size was analyzed. The results are shown in FIG. According to Fig. 4, it was confirmed that the A-grade had an average particle size distribution of 0.78 mu m.

<부원료 선정><Selection of sub materials>

SiC는 원료자체 만으로는 상압소결이 어렵다는 것이 널리 알려진 사실로서 통상 B계와 C계의 원료를 소결조제로 사용하는 것이 가장 많이 알려져 있다. It is widely known that SiC is difficult to sinter at normal pressure only by the raw material itself, and it is generally known to use raw materials of B and C systems as sintering additives.

본 발명에서도 소결조제로 B계와 C계의 원료인 탄화붕소 및 카본블랙 원료를 선정하였다.In the present invention, boron carbide and carbon black raw materials of raw materials B and C were selected as sintering auxiliary agents.

또한, 자기윤활성을 나타낼 수 있는 부원료인 Carbon계 출발원료의 입도를 분석하여 보았고, 그 분석결과는 도 5에 도시한 바와 같다. 그 분석결과에 평균입도분포 21㎛를 나타내었다. In addition, the particle size of the carbon-based starting material, which is a subordinate material capable of exhibiting self-lubricating property, was analyzed, and the analysis result is as shown in FIG. The results of the analysis show an average particle size distribution of 21 mu m.

이 외에 부원료로 유기첨가원료들은 프레스 성형시 성형강도와 가소성을 부여하기 위한 결합제, 분말혼합시 균일 분산을 하기 위한 분산제 등이 있으며, 적정한 종류와 첨가량을 결정하기 위하여 시험하여 보았으며, 그 시험 중 온도에 따른 유기첨가제의 거동 시험을 실시하여 보았으며, 그 시험결과는 하기 표 1에 나타낸바와 같다. 상기 유기첨가제의 온도에 따른 거동을 살펴보기 위하여 dry oven에서 온도별로 시험하였고, 그 결과 무게 감량을 측정하여 표 1에 나타내었다. In addition to these, the organic additives as additives are classified into a binder for imparting molding strength and plasticity during press molding, a dispersing agent for uniform dispersion during powder mixing and the like, and it has been tested to determine appropriate kinds and amounts of additives. The behavior of organic additives according to temperature was tested. The test results are shown in Table 1 below. In order to examine the behavior of the organic additives according to temperature, they were tested in dry oven by temperature, and the weight loss was measured and shown in Table 1.

Figure 112016022962002-pat00001
Figure 112016022962002-pat00001

상기 표 1의 결과, 분무과립 건조온도 범위 160℃ 이내에서는 PVA는 90%, PEG, TEA는 변화가 거의 없었음을 알 수 있었다. As a result of the above Table 1, it was found that the PVA was 90% and the PEG and TEA were not substantially changed within the spray granulation drying temperature range of 160 ° C.

2. SiC 조성 선정2. Selection of SiC composition

상기한 출발원료 및 부원료들의 선정을 위한 예비시험결과에 따라, 상압소결용 SiC세라믹 조성은 8종의 조성을 선정하였으며, 그 조성비는 α type 6H 결정을 가지는 A-grade의 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1 ~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에타놀아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하도록 하여 상압소결용 SiC세라믹 조성물을 준비하였다. According to the preliminary test results for the selection of the starting materials and additive materials described above, the composition of the SiC ceramics for pressureless sintering was selected from 8 kinds of composition, and the composition ratio thereof was 0.3 ~ 2 ㎛ in the average grain size of the A- 75 to 95 parts by weight of SiC; 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1 to 1.0 part by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); And 0.5 to 4.0 parts by weight of polyethylene glycol (PEG), to prepare a SiC ceramic composition for pressureless sintering.

3. 혼합공정 시험3. Mixing process test

<볼 밀링 시험><Ball milling test>

최적의 볼밀링 조건을 선정하기 위하여 볼 밀링의 회전수 및 시간에 따른 평균입도분석 시험을 진행하였으며, 그 결과는 하기 표 2에 나타내었다. In order to select the optimum ball milling conditions, the average particle size analysis was performed according to the number of revolutions and the time of the ball milling, and the results are shown in Table 2 below.

Figure 112016022962002-pat00002
Figure 112016022962002-pat00002

위 표 2의 결과, 최적 회전수는 15~20rpm에서 20~24시간 동안 볼밀링 한 후에 평균입도가 1.5㎛ 이하를 나타내어 최적 볼밀링 조건으로 선정하였다. As a result of Table 2, the optimal number of revolutions was selected as the optimum ball milling condition with an average particle size of 1.5 μm or less after ball milling for 20 to 24 hours at 15 to 20 rpm.

4. 과립공정 시험4. Granulation process test

상기와 같이 적정한 원료혼합 공정조건이 선정되어 제조된 슬러리를 최적의 분무건조 조건을 선정하기 위한 시험으로 원료의 흐름성, 수분함량, bulk density 분석을 진행하여 최적 분무과립화 공정조건을 선정하였다. The optimal spray granulation conditions were selected by conducting flow rate, moisture content and bulk density analysis of the raw materials by selecting the optimal spray drying conditions for the slurry prepared by selecting appropriate raw material mixing process conditions as described above.

최적 과립공정 조건을 선정하기 위하여 하기 표 3과 같이 시험을 진행하였으며, 그 조건에 따른 과립의 특성치를 측정하였다. In order to select optimal granulation process conditions, the test was carried out as shown in Table 3 below, and the granule characteristics were measured according to the conditions.

Figure 112016022962002-pat00003
Figure 112016022962002-pat00003

상기 표 3의 결과, 챔버온도 80℃ 이하에서는 수분함량이 너무 높고, 105℃ 이상에서는 과립의 형상이 도 6에 도시된 바와 같이, dimple type이 많이 발생하였으며, Inlet 온도는 160~200℃, Feed Rate는 2~4, atomizer disc의 회전수는 6000~9000 범위 내에서 조건시험을 진행한 결과 최적의 스프레이드라잉 공정 조건은 챔버온도 95~100℃, Inlet온도 200℃, Feed rate 4, Disc rpm 8000의 조건에서 B/D 0.85~0.86g/㎤, 수분함량 0.3~0.4%, 흐름도 10.5~10.8로 우수한 과립특성을 얻을 수 있었다. 이때의 과립을 확인한 결과, 도 7에 도시된 바와 같이, 구형의 과립이 형성됨을 알 수 있었다.As a result of the above Table 3, the moisture content was too high at a chamber temperature of 80 ° C or less, and the granule shape was more dimple type at 105 ° C or higher as shown in FIG. 6. The inlet temperature was 160-200 ° C, The optimum spray drying conditions were chamber temperature of 95 ~ 100 ℃, inlet temperature of 200 ℃, feed rate of 4, Disc rpm of 2 ~ 4 and atomizer disc rotation speed of 6000 ~ 9000. 8000, B / D of 0.85 ~ 0.86g / ㎤, water content of 0.3 ~ 0.4% and flow rate of 10.5 ~ 10.8. As a result of checking the granules at this time, it was found that spherical granules were formed as shown in Fig.

5. 성형공정 시험5. Molding process test

SiC 디스크 금형 설계 및 제작: 최적의 과립분말을 제조한 후, 디스크의 금형을 제작하기 위하여는 수축율을 결정하여야 하는데 시험금형으로 성형한 후 소결수축율을 측정한 결과 선수축율이 19.5%이었다. Design and fabrication of SiC disk mold: After manufacturing the optimum granular powder, the shrinkage ratio should be determined in order to fabricate the disk mold. The sintering shrinkage rate after molding with the test mold was 19.5%.

따라서, 상기 측정결과에 따라 선정된 소결수축율에 의하여 SiC디스크용 금형을 설계하고 제작한 다음, 제작된 SiC디스크 성형용 금형으로 성형시험을 진행하여 최적의 성형조건으로 성형체 두께 및 성형체 무게를 결정하였다.Therefore, the mold for SiC disk was designed and manufactured by the selected sintering shrinkage ratio according to the above measurement results, and the molding test was conducted with the manufactured mold for molding the SiC disk to determine the thickness of the molded body and the weight of the molded body under the optimum molding conditions .

6. 탈지공정 시험6. Degreasing process test

탈지조건 선정: 분산과 성형을 위해 첨가된 유기물을 서서히 제거하기 우한 탈지공정의 승온속도, 최고온도, 탈지율 등에 대하여 시험하고 최적 조건을 선정하였다. 최적의 진공탈지 조건을 선정한 결과 다음과 같다. Selection of the degreasing condition: Gradually remove the added organic materials for dispersion and molding. The temperature raising rate, the maximum temperature and the degreasing rate of the degreasing process were tested and the optimal conditions were selected. The optimum vacuum degreasing conditions were selected as follows.

승온속도: 1℃/minHeating rate: 1 캜 / min

탈지최고온도: 800℃Degreasing maximum temperature: 800 ℃

최고온도 유지시간: 1.5~2hrMaximum temperature holding time: 1.5 to 2 hr

분위기: 진공 조건Atmosphere: Vacuum condition

7. 소결공정 시험7. Sintering Process Test

소성조건 선정: 탈지처리가 된 디스크제품을 2100℃ 정도의 고온에서 소결열처리시의 승온속도, 소결온도, 소결시간을 선정하였다. Selection of firing conditions: The rate of temperature rise, sintering temperature and sintering time at sintering heat treatment at 2100 ℃ were selected for the degreased disc products.

그 결과, 최적의 승온조건은 다음과 같다. As a result, the optimum temperature rise condition is as follows.

0~1500℃: 10℃/min: 진공분위기0 to 1500 占 폚: 10 占 폚 / min: Vacuum atmosphere

1500~2100: 4℃/min: Ar 가스분위기1500 to 2100: 4 DEG C / min: Ar gas atmosphere

2100℃: 2~3시간 유지2100 ℃: Maintain for 2 ~ 3 hours

8. 가공공정 시험8. Processing test

소성된 SiC디스크를 폴리싱 공정 전에 래핑공정으로 최적 두께와 표면조도를 달성할 수 있는 래핑기의 회전수, 시간 등을 선정하였다. 그 선정 결과, 회전수 (5)~(100)rpm, 시간 (1)~(5)분의 조건을 선정하였다. The number of revolutions and time of the lapping machine which can achieve the optimum thickness and surface roughness by the lapping process before the polishing process of the fired SiC disk were selected. As a result of the selection, conditions for rpm (5) to (100) rpm and time (1) to (5) were selected.

래핑 가공이 끝난 제품을 폴리싱 장비에 투입하여 다이아몬드 연마입자의 크기가 1~5㎛를 포함하는 슬러리를 회전정반에 분무하여 최종 폴리싱 면의 특성이 표면조도 0.02~0.15㎛ 값을 갖는 최적 폴리싱 조건을 선정하였다. After the lapping process is completed, the slurry containing 1 to 5 탆 of diamond abrasive grains is sprayed on the rotating platen by the application to the polishing machine, and the characteristics of the final polishing surface is adjusted to the optimum polishing condition having a surface roughness of 0.02 to 0.15 탆 Respectively.

9. SiC디스크의 특성평가9. Characterization of SiC disk

상기와 같이 선정된 최적 조건에 따라, SiC디스크 예비시험편을 제작하고, 밀도와 표면조도 특성을 평가하여 본 결과 다음과 같았으며, 이때 측정된 표면조도 측정결과는 도 8에 도시하였다. The SiC disk preliminary test specimen was prepared according to the optimum conditions as described above, and the density and the surface roughness characteristics were evaluated. The results were as follows. The measurement results of the surface roughness were shown in FIG.

- 밀도: 2.80(g/㎤)- Density: 2.80 (g / cm3)

- 표면조도: 0.05㎛- Surface roughness: 0.05 탆

또한, 상기 예비시험편의 소결체 파단면 SEM 분석결과를 도 9에 도시하였으며, 그 결과 SiC입자와 Carbon입자가 균일하게 분포하고 있음을 확인할 수 있었다. Also, FIG. 9 shows the SEM analysis results of the sintered body of the preliminary test piece. As a result, it can be confirmed that the SiC particles and the carbon particles are uniformly distributed.

한편, 상기 소결체의 EDS분석결과, SiC grain과 grain 사이에 존재하는 카본 입자로 추정하는 것이 맞는 지를 확인하기 위하여 EDS분석을 표 4와 같은 조건으로 분석한 결과 카본입자임을 확인할 수 있었다. (도 10 참조)On the other hand, as a result of EDS analysis of the sintered body, it was confirmed that the carbon particles are the carbon particles by analyzing the EDS analysis under the conditions as shown in Table 4 in order to confirm whether or not the carbon particles existing between the SiC grain and the grain are correct. (See Fig. 10)

ElementElement Weight%Weight% Atomic%Atomic% C KC K 82.6782.67 91.7791.77 Si KSi K 17.3317.33 8.238.23 TotalsTotals 100.00100.00

10. SiC세라믹카트리지 시제품 성능시험10. SiC Ceramic Cartridge Prototype Test

상기와 같이, 확립된 최적공정조건에 따라, SiC세라믹디스크를 제조하고, 그 디스크를 사용하여 SiC세라믹카트리지를 준비하여 그 성능을 시험하여 보았다. As described above, a SiC ceramic disk was manufactured according to the established optimum process conditions, and the performance of the SiC ceramic cartridge was prepared using the disk.

<SiC세라믹디스크의 제조>&Lt; Production of SiC ceramic disk >

평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에탄올아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하도록 볼밀링장치에 투입하고, 회전수 15~20rpm 조건으로 20~24시간 볼밀링하여 상압소결용 SiC세라믹 슬러리를 준비하고; 상기 슬러리를 분부건조기에 투입하여 쳄버온도(Chamber Temp.) 90~105℃, 인렛온도(Inlet Temp.) 200℃, 피드레이트(Feed rate) 3~4, 아토마이져 디스크(Atomizer disc)의 회전수 8,000~9,000rpm의 건조조건으로 과립화하였다. 75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 탆; 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1-1.0 parts by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); 0.5 to 4.0 parts by weight of polyethylene glycol (PEG), and the resulting mixture is ball milled for 20 to 24 hours at a rotation speed of 15 to 20 rpm to prepare a SiC ceramic slurry for pressure-sintering; The slurry was put into a weft dryer to adjust the chamber temperature to 90 to 105 ° C., the inlet temperature to 200 ° C., the feed rate to 3 to 4, the rotation of the atomizer disc And granulation was carried out under a drying condition of 8,000 to 9,000 rpm.

상기 과립을 금형에 투입하여 성형체를 성형하고; 상기 성형공정에서 얻어진 성형체를 진공상태에서 승온속도 1℃/min의 속도로 탈지최고온도 800℃까지 승온한 후, 1.5~2시간 동안 유지하여 첨가된 유기물을 제거하고, 그 성형체를 진공분위기에서 10℃/min의 승온속도로 0~1500℃까지 승온하고, 아르곤(Ar) 가스분위기에서 4℃/min의 승온속도로 1500~2100℃까지 승온하여 2~3시간 유지하여 SiC디스크를 형성하였다. Introducing the granules into a mold to form a formed body; The molded article obtained in the above-described molding step was heated to a degreasing maximum temperature of 800 DEG C at a rate of 1 DEG C / min in a vacuum state, maintained for 1.5 to 2 hours to remove the added organic matter, The temperature was raised to 0 to 1500 ° C at a heating rate of 0 ° C / min, the temperature was raised to 1500 to 2100 ° C at a rate of 4 ° C / min in an argon (Ar) gas atmosphere, and the temperature was maintained for 2 to 3 hours to form a SiC disk.

상기 소결공정에서 소성된 SiC디스크를 래핑기에서 회전수 60rpm, 1~5분 동안 래핑가공하고, 상기 래핑가공이 완료된 SiC디스크를 폴리싱 장비에 투입하여 다이아몬드 연마입자의 크기가 1~5㎛를 포함하는 슬러리를 분무하여 폴리싱 가공하여 자기윤활성 SiC세라믹디스크를 제조하였다.The sintered SiC disk is lapped in a lapping machine at a rotation speed of 60 rpm for 1 to 5 minutes and the SiC disk having been subjected to the lapping process is charged into a polishing machine to form a diamond abrasive particle having a size of 1 to 5 탆 Was sprayed and polished to produce a self-lubricating SiC ceramic disk.

상기와 같이 제조된 자기윤활성 SiC세라믹디스크를 사용하여 SiC세라믹카트리지를 제조하여 준비한 다음, 성능시험을 실시하였다. A SiC ceramic cartridge was prepared using the self-lubricating SiC ceramic disk prepared as described above, and then the performance test was performed.

가. 내수압성능 시험end. Water pressure performance test

<시험방법><Test Method>

내수압성능 시험 장치에 SiC세라믹카트리지를 장착한 한 개 레버식 온냉수 혼합꼭지를 설치한다. Install one lever type hot and cold water mixing faucet equipped with SiC ceramic cartridge in the water pressure performance testing device.

SiC세라믹카트리지를 장착한 한 개 레버식 온냉수 혼합꼭지의 레버를 완전히 닫은 상태에서 내압부에수압 5MPa를 1분간 지속하여 가한다. When the levers of a lever-type hot / cold water mixing cock equipped with a SiC ceramic cartridge are fully closed, apply a pressure of 5 MPa for 1 minute to the pressure-proof part.

시험완료 후 육안으로 변형, 파손 및 누수가 있는지 확인한다. After completion of the test, visually check for deformation, breakage and leakage.

<시험결과><Test Results>

총 10회 실시하여 보았으며, 그 결과 내수압이 4.9MPa 이상을 나타내었다. As a result, the water pressure was over 4.9MPa.

나. 내구성능 시험I. Endurance performance test

하기 첨부된 사진과 같은 내구성능시험기를 준비하여 SiC세라믹카트리지의 내구성능을 시험하여 보았다. A durability tester such as the one shown below was prepared to test the durability of the SiC ceramic cartridge.

<그림 1: 내구성능시험기><Figure 1: Endurance performance tester>

Figure 112016022962002-pat00004
Figure 112016022962002-pat00004

<시험방법><Test Method>

SiC세라믹 카트리지를 장착한 한 개 레버식 온냉수 혼합꼭지를 내구성능 시험기에 장착한다. One lever type hot and cold water mixing faucet equipped with SiC ceramic cartridge is attached to the endurance performance tester.

수압은 지수 상태에서 0.196 MPa 이상으로 한다. The water pressure should be at least 0.196 MPa in the exponential state.

사용수의 온도는 상온(5 ℃ ∼ 35 ℃)으로 한다. The temperature of the water used should be room temperature (5 ℃ ~ 35 ℃).

개폐의 동작을 1회로 하며, 개폐 조작은 1시간에 1200회 이상으로 실시한다. The opening and closing operation is performed once, and the opening and closing operation is performed at least 1,200 times per hour.

회전 각도는 120°±30°로 한다.  The rotation angle is 120 ° ± 30 °.

50만 회의 레버 개폐 조작을 실시한다. 500,000 levers are opened and closed.

시험 종료 후 다음의 성능을 만족하는지 시험한다. After completion of the test, test whether the following performance is satisfied.

a) 조작 성능 a) Operational performance

수동으로 개폐 또는 전환조작을 실시하여 조작상태가 원활하고 확실한지 확인한다. Perform manual opening / closing or switching operation to check that the operation status is smooth and reliable.

b) 내압 성능 b) Withstand pressure performance

조작성능 시험완료 후 레버를 완전히 닫은 상태에서 내압부에 수압 1.72MPa을 1분간 지속하여 가한다. Operational performance After completion of the test, apply 1.72 MPa of water pressure to the pressure-proof part for 1 minute with the lever fully closed.

<시험결과><Test Results>

도 11에 도시된 바와 같이, 내구성능은 50만 사이클 시험에서 누수 및 조작성능에 이상이 없음을 확인하였다.As shown in Fig. 11, the endurance performance was confirmed to be no abnormality in leakage and operation performance in the test of 500,000 cycles.

다. 토크성능 시험All. Torque performance test

<시험방법><Test Method>

SiC세라믹 카트리지를 장착한 한 개 레버식 온냉수 혼합꼭지의 레버에 토크게이지를 연결한다. Connect a torque gauge to the lever of a lever-type hot / cold water mixing faucet with a SiC ceramic cartridge.

토크게이지를 시계방향으로 회전시켜 최대 토크(N·m)를 측정한다. Turn the torque gauge clockwise to measure the maximum torque (N · m).

<시험결과><Test Results>

토크성능은 50만 사이클 시험 후 측정결과 0.3kgf·㎝(0.0294N·m) 이하였다. The torque performance was 0.3 kgf · cm (0.0294 N · m) or less after the test of 500,000 cycles.

이상의 성능시험 결과, 본 발명에 따라 제공되는 조성물 및 그 제조방법에 따라 제조된 자기윤활성 SiC세라믹디스크를 적용하여 제조된 SiC세라믹카트리지는 내압성능(kgf/㎠) 50(kgf/㎠)이상, 내구성능(cycle) 50만(cycle) 이상, 토크성능(kgfcm) 0.3(kgfcm) 이하의 매우 우수한 성능을 가진 SiC세라믹카트리지를 제공할 수 있는 것을 알 수 있었다. As a result of the above performance tests, the SiC ceramic cartridge manufactured by applying the self-lubricating SiC ceramic disk manufactured according to the present invention and the method of manufacturing the same according to the present invention has an internal pressure capability (kgf / cm2) of 50 (kgf / It was found that SiC ceramic cartridge having excellent performance of less than 0.3 (kgfcm) in torque performance (kgfcm) can be provided over a cycle of 50,000 cycles or more.

Claims (4)

삭제delete 삭제delete 평균입도크기 0.3~2㎛의 SiC 75~95중량부; 평균입도크기 0.1~50㎛의 카본파우더 5~20중량부; 탄화붕소(B4C) 0.5~1.5중량부; 카본블랙 1.0~5.0중량부; 트리에탄올아민(TEA) 0.1~1.0중량부; 폴리비닐알콜(PVA) 0.5~4.0중량부; 폴리에틸렌글리콜(PEG) 0.5~4.0중량부를 포함하도록 볼밀링장치에 투입하고, 회전수 15~20rpm 조건으로 20~24시간 볼밀링하여 혼합하는 상압소결용 SiC세라믹 슬러리를 준비하는 혼합공정;
상기 혼합공정의 슬러리를 분무건조기에 투입하여 과립화하는 과립공정;
상기 과립공정에서 얻어지 과립을 금형에 투입하여 성형하는 성형공정;
상기 성형공정에서 얻어진 성형체를 진공상태에서 첨가된 유기물을 제거하기 위한 탈지공정;
상기 탈지공정이 완료된 후, 그 성형체를 진공분위기에서 10℃/min의 승온속도로 0~1500℃까지 승온하고, 아르곤(Ar) 가스분위기에서 4℃/min의 승온속도로 1500~2100℃까지 승온하여 2~3시간 유지하여 소결하여 SiC디스크를 형성하는 소결공정; 및
상기 소결공정에서 소성된 SiC디스크를 래핑기에서 래핑가공하고, 상기 래핑가공이 완료된 SiC디스크를 폴리싱장비에 투입하여 폴리싱가공하는 가공공정을 포함하여 이루어지는 것을 특징으로 하는 자기윤활성 SiC 세라믹디스크 제조방법.
75 to 95 parts by weight of SiC having an average particle size of 0.3 to 2 탆; 5 to 20 parts by weight of carbon powder having an average particle size of 0.1 to 50 탆; 0.5 to 1.5 parts by weight of boron carbide (B 4 C); 1.0 to 5.0 parts by weight of carbon black; 0.1-1.0 parts by weight of triethanolamine (TEA); 0.5 to 4.0 parts by weight of polyvinyl alcohol (PVA); 0.5 to 4.0 parts by weight of polyethylene glycol (PEG) is put into a ball milling apparatus and ball milling is performed for 20 to 24 hours at a rotation speed of 15 to 20 rpm to prepare a SiC ceramic slurry for pressure-sintering;
A granulation step of granulating the slurry of the mixing step into a spray dryer;
A molding step of molding the granules obtained in the granulation process into a mold;
A degreasing step of removing the organic material added in the vacuum state of the formed body obtained in the forming step;
After the degreasing step is completed, the formed body is heated in a vacuum atmosphere at a temperature raising rate of 10 DEG C / min to a temperature of 0 to 1500 DEG C and heated to a temperature of 1500 to 2100 DEG C at a temperature raising rate of 4 DEG C / min in an argon A sintering step of sintering the raw material for 2 to 3 hours to form a SiC disk; And
And a processing step of lapping the sintered SiC disk in the sintering process and lapping the SiC disk having been subjected to the lapping process into a polishing machine to polish the sintered silicon carbide disk.
제3항에 있어서,
상기 가공공정의 래핑기에서 래핑은 회전수 5~100rpm으로 1~5분 동안 래핑가공하고, 상기 폴리싱가공은 폴리싱장비에서 다이야몬드 연마입자의 크기가 1~5㎛를 포함하는 슬러리를 분무하여 폴리싱 가공하는 것을 특징으로 하는 자기윤활성 SiC 세라믹디스크 제조방법.
The method of claim 3,
The lapping in the lapping machine of the above-described processing is performed by lapping at a rotation speed of 5 to 100 rpm for 1 to 5 minutes, and the polishing processing is performed by spraying a slurry containing diamine abrasive grains of 1 to 5 탆 in a polishing machine, Wherein the step of forming the magnetic layer comprises:
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