KR0173404B1 - Coating method - Google Patents
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- KR0173404B1 KR0173404B1 KR1019960026786A KR19960026786A KR0173404B1 KR 0173404 B1 KR0173404 B1 KR 0173404B1 KR 1019960026786 A KR1019960026786 A KR 1019960026786A KR 19960026786 A KR19960026786 A KR 19960026786A KR 0173404 B1 KR0173404 B1 KR 0173404B1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4535—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied as a solution, emulsion, dispersion or suspension
- C04B41/4537—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied as a solution, emulsion, dispersion or suspension by the sol-gel process
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/515—Other specific metals
- C04B41/5155—Aluminium
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- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
본 발명은 ISG(interlayer sol-gel)법에 의하여 금속에 세라믹을 합성, 코팅함에 있어 밀착강도를 높이기 위한 세라믹 합성과 필요한 조성 및 제조방법에 관한 것으로, 세라믹 기판과 금속도금층에 SiO2-Al2O3-MgO를 주성분으로 하는 세라믹 박막을 제조 코팅하여 코팅박막층에 미세한 크랙(Crack)과 기공(Void)을 형성시킴으로써 기공의 발달에 의해 요철과 같은 anchoring effect를 세라믹 표면에 부여하여 세라믹 소재의 금속화 과정시 기판과 전착층간의 밀착강도를 개선한 것이다.The present invention relates to ceramic synthesis and necessary composition and manufacturing method for increasing the adhesion strength in the synthesis and coating of ceramics on metal by ISG (interlayer sol-gel) method, SiO 2 -Al 2 on the ceramic substrate and metal plating layer Manufacture and coating a ceramic thin film containing O 3 -MgO as a main component to form fine cracks and voids in the coating thin film layer to impart anchoring effects such as irregularities to the ceramic surface by the development of pores In this process, the adhesion strength between the substrate and the electrodeposition layer was improved.
Description
통상적으로 세라믹 소재를 금속화(metalization)하는 방법에는 paste법, 진공중착법, 무전해도금법등이 사용되고 있으나, 상기 방법은 그 단점이 많이 지적되고 있는바, 예를 들면, 무전해 도금방법은 조작이 간단하고 비교적 생산비가 저렴하며, 재현성이 뛰어나다는 장점은 있으나, 도금층과 세라믹 기판층과의 밀착강도가 저하되는 단점이 있으며, 이를 개선하고자 귀금속 paste를 열적 융착하여 밀착강도를 높이는 방법이 있으나, 귀금속 paste의 경우 가격의 변동폭이 크고, 안정적인 공급, 복잡한 형상의 금속화 등에 문제점이 있었다.In general, a method of metallizing a ceramic material is used by a paste method, a vacuum deposition method, an electroless plating method, etc. However, the method has many disadvantages. For example, the electroless plating method is operated. This simple, relatively low production cost, and excellent reproducibility, but has the disadvantage that the adhesion strength between the plating layer and the ceramic substrate layer is reduced, there is a method to improve the adhesion strength by thermal fusion of the precious metal paste, In the case of the precious metal paste, the price fluctuated largely, and there were problems such as stable supply and metallization of complex shapes.
따라서, 최근에는 무전해 도금을 기판에 직접 행하여 생산성과 경제성을 개선하려는 연구가 진행되고 있다. 그러나 무전해 도금방법은 앞에서 이미 설명한 바와 같이 만족할만한 높은 밀착강도를 얻기가 어렵기 때문에 이를 해결하기 위하여 세라믹 기판 표면에 요철이 부여하고, 이와 같은 물리적인 앵커(anchor) 효과에 의하여 밀착강도를 향상시키는 방법이 많이 연구되고 있는 것이다.Therefore, in recent years, research is being conducted to improve productivity and economy by performing electroless plating directly on a substrate. However, in the electroless plating method, as described above, it is difficult to obtain a satisfactory high adhesion strength. Therefore, irregularities are applied to the surface of the ceramic substrate to solve this problem, and the adhesion strength is improved by the physical anchor effect. How to make is being studied a lot.
한편 ISG(interlayer sol-gel)방법을 간략하게 설명하면, 이는 금속알콕사이드와 물과의 가스분해 반응시 생기는 수화물을 이용하여 여러 형태의 특성에 맞는 성질을 부여할 수가 있는바, 이와 같은 ISG방법의 장점은,On the other hand, ISG (interlayer sol-gel) method briefly described, it can be given the properties suitable for various types of characteristics by using the hydrate generated during the gas decomposition reaction of the metal alkoxide and water. Advantage
① 저온합성이 가능함으로서 세라믹에 대한 저온고밀도 소결이 가능하고,① Low temperature synthesis enables low temperature high density sintering of ceramics,
② 다성분계 다결정 세라믹의 균질한 합성이 가능하며,② The homogeneous synthesis of multicomponent polycrystalline ceramics is possible,
③ 다양한 조성의 산화물 박막이 용이하게 합성될 수 있고.③ The oxide thin films of various compositions can be easily synthesized.
④ 산화물 박막층이 두께 조절이 용이하여 생산효율이 높은 장점을 가지고 있다.④ The oxide thin film layer has the advantage of high production efficiency because of easy thickness control.
따라서, 이러한 균일성, 고순도 및 저온합성 등의 장점으로 인해 세라믹 박막, 고융점 초미립 분말제조, 산화물 합성분야 등에 응용이 많이 되고 있다.Therefore, due to the advantages such as uniformity, high purity and low temperature synthesis, many applications have been made in ceramic thin films, high melting point ultrafine powder production, oxide synthesis, and the like.
본 발명에서도 이와 같은 ISG방법에 의하여 세라믹기판과 금속도금층에 세라믹박막을 제조 코팅하여 코팅박막층에 미세한 크랙(Crack)과 기공(Void)을 형성시킴으로서 기공의 발달에 의해 요철과 같은 anchoring effect를 세라믹 표면에 부여하여 세라믹 소재의 금속화 과정시 기판과 전착층간의 밀착강도를 개선한 것이다.In the present invention, by producing and coating a ceramic thin film on the ceramic substrate and the metal plating layer by the ISG method as described above, fine cracks and voids are formed in the coating thin film layer, and thus the anchoring effect such as irregularities is developed by the development of pores. In this case, the adhesion strength between the substrate and the electrodeposition layer was improved during the metallization process of the ceramic material.
본 발명의 목적물인 세라믹 기판과 금속도금층간에 형성되는 합성코팅층은 성분이 단순화된 3원계 즉, SiO2-Al2O3-MgO로 구성되어 있으며, 이와 같은 주성분을 얻기 위해서는 Si(OC2H5)4(실리콘 알콕사이드), Al(NO3)3·9H2O(질산알미늄) C4H6MgO4·4H2O(마그네슘염)을 사용하며, 균일한 졸로서 형성시키기 위한 용제로는 C2H5OH(에틸알콜)를 사용한다.The synthetic coating layer formed between the ceramic substrate and the metal plating layer, which is the object of the present invention, is composed of a simplified ternary system, that is, SiO 2 -Al 2 O 3 -MgO, and in order to obtain such a main component, Si (OC 2 H 5 ) 4 (silicon alkoxide), Al (NO 3 ) 3 .9H 2 O (aluminum nitrate) C 4 H 6 MgO 4 .4H 2 O (magnesium salt) is used as a solvent to form as a uniform sol C 2 H 5 OH (ethyl alcohol) is used.
한편, 이와 같은 주성분으로 코팅층을 합성함에 있어 적당한 mole%는 Si(OC2H5)4은 1∼2mole, Al(NO3)3·9H2O은 0.3∼1mole, C4H6MgO4·4H2O는 0.2∼0.5mole의 범위에서 조성변화를 하게 되며, 기공(Void)을 형성시키기 위해서 800∼1200℃에서 1∼4시간 소성하면 기공이 형성된 표면 개질층을 얻을 수 있다.On the other hand, in synthesizing the coating layer with such a main component, the appropriate mole% is Si (OC 2 H 5 ) 4 as 1 to 2 mole, Al (NO 3 ) 3 · 9H 2 O as 0.3 to 1 mole, C 4 H 6 MgO 4 · 4H 2 O undergoes a composition change in the range of 0.2 to 0.5 mole, and the surface modified layer having pores can be obtained by firing at 800 to 1200 ° C. for 1 to 4 hours to form voids.
이때 미세한 기공(Void)을 무수히 형성시킴과 동시에 고른 분포도를 갖도록 하기 위한 최적의 mole%는 Si(OC2H5)42mole : Al(NO3)3·9H2O 1mole : C4H6MgO4·4H2O 0.5mole 정도이며, 용제인 C2H5OH는 15∼31mole 정도인 바, 이와 같은 mole%로 합성된 투명한 졸로 세라믹기판을 코팅한 후, 열처리를 하면 코팅하지 않고 직접 도금하는 종래 방법에 비하여 10배의 높은 밀착강도를 얻을 수 있다.The myriad forms fine pores (Void) Sikkim and at the same time optimum mole% to have a uniform distribution of the Si (OC 2 H 5) 4 2mole: Al (NO 3) 3 · 9H 2 O 1mole: C 4 H 6 MgO 4 · 4H 2 O is 0.5mole and the solvent C 2 H 5 OH is about 15 ~ 31mole.The ceramic substrate is coated with a transparent sol synthesized in such mole%, and then plated directly without heat treatment when coated. Compared with the conventional method, a ten times higher adhesion strength can be obtained.
이와 같은 본 발명을 실예를 들어 간략하게 다시 한번 설명하면 다음과 같다.The present invention is briefly described once again by way of example as follows.
세라믹 기판 두께가 6.5mm의 96% 알루미나 기판을 10㎠ 넓이로 레이저 커팅하고, 이를 초음파 세척 및 H3PO4(인산)로 1차 에칭을 한 통상적인 세라믹 기판을 준비한 후, 이 세라믹 기판을 Si(OC2H5)42mole : Al(NO3)3·9H2O 1mole : C4H6MgO4·4H2O 0.5mole : C2H5OH(에틸알콜 용제) 15∼31mole 비율로 ISG방법으로 합성한 투명졸에 코팅하여 24시간 상온에서 건조하고, 건조한 시편을 각 조성에 따 800∼1200℃에서 1∼4시간 본소성을 하여 열처리를 행하면 본 발명이 목적으로 하는 아주 높은 밀착강도를 얻을 수 있게 되는 것인 바, 이는 X선 회절분석을 하여 석출상을 확인하고, 주사 전자 현미경을 사용하여 미세조직을 관찰하여 보면 도금층과 세라믹 기판층간에 충분한 anchoring effect가 나타날 수 있도록 미세한 기공이 고르게 분포되어 있는 것을 확인할 수가 있게 되는 것이다.After cutting a 96% alumina substrate having a thickness of 6.5 mm into a 10 cm 2 laser substrate, and preparing a conventional ceramic substrate subjected to ultrasonic cleaning and primary etching with H 3 PO 4 (phosphate), the ceramic substrate was prepared by Si. (OC 2 H 5 ) 4 2mole: Al (NO 3 ) 3 9H 2 O 1mole: C 4 H 6 MgO 4 4H 2 O 0.5mole: C 2 H 5 OH (ethyl alcohol solvent) ISG at 15 to 31 mole ratio It is coated on the transparent sol synthesized by the method and dried at room temperature for 24 hours, and the dried specimen is subjected to heat treatment for 1 to 4 hours at 800 to 1200 ° C. according to each composition to give very high adhesion strength for the purpose of the present invention. X-ray diffraction analysis confirms the precipitated phase, and microscopic observation using a scanning electron microscope shows fine pores evenly so that sufficient anchoring effect can be seen between the plating layer and the ceramic substrate layer. You can see that it is distributed Will.
이상과 같은 본 발명은 세라믹 기판을 금속화하는 방법에 있어서 세라믹 기판에 ISG법으로 투명하게 합성된 졸을 코팅하여 기판과 도금층간에 interlayer를 도포한 시료가 코팅층에 형성되는 기공에 의해 anchoring effect를 충분히 발휘함으로서 코팅하지 아니하고 직접 도금한 종래의 시료보다 10배의 높은 밀착강도(밀착강도값 1000gf)를 얻을 수 있도록 한 것으로서 그 응용범위도 압전소자, 건축재료, 부식방지재료, 파인세라믹 등의 금속화 등에 적용이 가능하며 금속화 재로로서 Cu, Cr, Ni, Au, Co 등을 이용할 수도 있으므로 널리 응용될 수 있는 유용한 발명인 것이다.In the present invention as described above, in the method of metallizing the ceramic substrate, the sol, which is transparently synthesized by the ISG method, is coated on the ceramic substrate to sufficiently anchoring effect by pores in which a sample formed by applying an interlayer between the substrate and the plating layer is formed on the coating layer. It can be used to obtain 10 times higher adhesion strength (adhesive strength value of 1000 gf) than conventional samples coated without direct coating. The scope of application is also metallization of piezoelectric elements, building materials, corrosion prevention materials, and fine ceramics. It can be applied to and the like, and may be used as a metallization material, such as Cu, Cr, Ni, Au, Co is a useful invention that can be widely applied.
본 발명은 ISG(interlayer sol-gel)법에 의하여 금속에 세라믹을 합성, 코팅함에 있어 밀차강도를 높이기 위한 세라믹 합성과 필요한 조성 및 제조방법에 관한 것으로, 세라믹 기판과 금속도금층에 SiO2(산화규소)-Al2O3(산화알루미늄)-MgO(산화마그네슘)를 주성분으로 하는 세라믹 박막을 제조 코팅하여 코팅박막층에 미세한 크랙(Crack)과 기공(Void)을 형성시킴으로서 기공의 발달에 의해 요철과 같은 anchoring effect를 세라믹 표면에 부여하여 세라믹 소재의 금속화 과정시 기판과 전착층간의 밀착강도를 개선한 것이다.The present invention relates to a ceramic composite with the required composition and method for increasing the milcha intensity I as composite, coating the ceramic in the metal by the ISG (interlayer sol-gel) process, SiO 2 (silicon oxide on the ceramic substrate and the metal plating layer Manufacture and coating ceramic thin films mainly composed of) -Al 2 O 3 (aluminum oxide) -MgO (magnesium oxide) to form fine cracks and voids in the coating thin film layer. The anchoring effect is applied to the ceramic surface to improve the adhesion strength between the substrate and the electrodeposition layer during the metallization of the ceramic material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019960026786A KR0173404B1 (en) | 1996-07-03 | 1996-07-03 | Coating method |
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| KR1019960026786A KR0173404B1 (en) | 1996-07-03 | 1996-07-03 | Coating method |
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| KR980008355A KR980008355A (en) | 1998-04-30 |
| KR0173404B1 true KR0173404B1 (en) | 1999-02-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100364851B1 (en) * | 1999-10-26 | 2002-12-26 | 유창남 | Coating composition for protecting thin layer of precious metal and method of preparing coating layer using the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100364851B1 (en) * | 1999-10-26 | 2002-12-26 | 유창남 | Coating composition for protecting thin layer of precious metal and method of preparing coating layer using the same |
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| KR980008355A (en) | 1998-04-30 |
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