KR20010098317A - Preparation of Inorganic Adhesive for High Temperature Usage - Google Patents
Preparation of Inorganic Adhesive for High Temperature Usage Download PDFInfo
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- KR20010098317A KR20010098317A KR1020000023822A KR20000023822A KR20010098317A KR 20010098317 A KR20010098317 A KR 20010098317A KR 1020000023822 A KR1020000023822 A KR 1020000023822A KR 20000023822 A KR20000023822 A KR 20000023822A KR 20010098317 A KR20010098317 A KR 20010098317A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
본 발명은 해당 부위에 적용하고 약 1시간동안 150∼200℃의 온도 범위에서 경화시켜서 접착시킨 후, 1200℃ 이상의 고온에서도 우수한 접착성을 가지며 물 존재하에서도 pH 등의 액성에 변화를 주지 않으며, 전기 부도체인 무기계 접착제를 제조하는 방법에 대한 것이다.The present invention is applied to the site and cured in a temperature range of 150 ~ 200 ℃ for about 1 hour, and then bonded, and excellent adhesion even at high temperature of 1200 ℃ or more does not change the liquidity such as pH even in the presence of water, The present invention relates to a method for producing an inorganic non-conductive adhesive.
일반적으로 고온용, 무기계 접착제는 내열성 특수도료, 내화 벽돌 제조용, 전기로 내부용 특수 페인트, 유리용 접착제, 각 종 건축재료의 접합용, 산소 센서의 접합제, 각종 반도체 소자의 접착제 등으로 이용되며 일반적으로 1200℃ 이상에서도 접착력이 유지되는 물성을 가져야 한다. 또한 고온 열처리용 전기로 등이 설치되어 있지 않은 일반 산업계에서 용이하게 접착을 실시할 수 있도록 경화 시간은 1시간내외로 짧고, 경화온도는 일반 오븐의 건조 온도인 150℃ 정도로 비교적 낮아야 한다. 따라서 본 발명을 통하여 산화규소, 알루미늄, 석고, 벤토나이트, 지당, 질산 나트륨, 수산화나트륨 및 물을 섞어서 바인더 용액을 제조한 후 150℃에서 20시간동안 숙성 열처리하고 이 용액에 활성 알루미나, 에탄올, 타닌산, 글리세린, 로진, 폴리이마이트 및 소량의 점증제를 가하여 무기계 접착제를 제조하는 방법이 개발되었다. 개발한 무기계 접착제를 tile(58x58x4㎣)에 대하여 33x58㎣의 면적에 도포하여 150℃에서 열처리하고 KS(M 3734, 접착제의 인장 전단 접착 강도 시험 방법)규격 기준에 따라 인장강도 관련 실험을 실시하였으며 tile에 대하여(면적 : 33x58㎟) 추의 질량이 5Kg 이상으로 가해지는 경우에도 접착력이 유지되어 우수한접착력을 보인다. 유리시편 위에 본 고온용 무기 접착제를 코팅하고서 700℃에서 2시간 열처리한 후 상온(20℃)에서 800℃까지 전류와 전위차를 독립적으로 측정하는 표준 사탐침 직류법 (standard four probe d.c. technique)을 적용하여 전기전도도를 측정한 결과 부도체의 영역의 전도도 값(α< 10-8cm-1Ω-1)을 보였다.Generally, high temperature and inorganic adhesives are used as heat-resistant special paints, fire bricks, special paints for electric furnace interiors, glass adhesives, bonding of various building materials, bonding of oxygen sensors, adhesives of various semiconductor devices, etc. In general, it should have physical properties to maintain the adhesion even at 1200 ℃ or more. In addition, the curing time should be less than about 1 hour, and the curing temperature should be relatively low, such as 150 ℃, which is the drying temperature of a general oven, so that it can be easily bonded in a general industry without high temperature heat treatment electric furnace. Therefore, through the present invention, a binder solution is prepared by mixing silicon oxide, aluminum, gypsum, bentonite, fat sugar, sodium nitrate, sodium hydroxide and water, followed by aging and heat treatment at 150 ° C. for 20 hours, and activated alumina, ethanol, tannic acid, A method has been developed for preparing inorganic adhesives by adding glycerin, rosin, polyimite and small amounts of thickener. The developed inorganic adhesive was applied to the tile (58x58x4㎣) on the area of 33x58㎣ and heat treated at 150 ℃, and the tensile strength test was conducted according to KS (M 3734, tensile shear bond strength test method). The adhesive strength is maintained even when the mass of the weight is applied at 5kg or more, showing excellent adhesion. After coating this high temperature inorganic adhesive on glass specimen, heat treatment at 700 ℃ for 2 hours, and using standard four probe dc technique to measure current and potential difference independently from room temperature (20 ℃) to 800 ℃. As a result of measuring the electrical conductivity, the conductivity value (α <10 -8 cm -1 Ω -1 ) of the region of the insulator was shown.
Description
접착 대상 물체에 도포한 후, 약 1시간동안 150∼200℃의 온도 범위에서 경화시킨 후, 1200℃ 이상의 고온에서도 우수한 접착성을 가지며 물 존재하에서도 pH 등의 액성에 변화를 주지 않으며, 전기 부도체인 무기계 접착제를 제조한다.After coating on the object to be bonded, it is cured at a temperature range of 150 to 200 ° C. for about 1 hour, and then has excellent adhesion even at a high temperature of 1200 ° C. or higher, and does not change the liquidity such as pH even in the presence of water. To prepare a phosphorous inorganic adhesive.
본 발명은 산화규소, 알루미늄, 석고, 벤토나이트, 지당, 질산 나트륨, 수산화나트륨 및 물을 섞어서 바인더 용액을 제조한 후 150℃에서 20시간동안 숙성 열처리하고 이 용액에 활성 알루미나, 에탄올, 타닌산, 글리세린, 로진, 폴리이마이트 및 소량의 점증제를 가하여 무기계 접착제를 제조하는 방법에 대한 것이다.In the present invention, a binder solution is prepared by mixing silicon oxide, aluminum, gypsum, bentonite, fat sugar, sodium nitrate, sodium hydroxide and water, followed by aging and heat treatment at 150 ° C. for 20 hours, and activated alumina, ethanol, tannic acid, glycerin, Rosin, polyimite and a small amount of thickener are added to produce an inorganic adhesive.
일반적으로 무기계 접착제는 유기계 및 무기계 내화 도료, 반도체 관련 기기의 접착제, 내화 벽돌 제조용, 전기로 내부용 특수 페인트, 내열성 특수도료, 유리용 접착제, 특수벽돌의 접착제, 각 종 건축재료의 접합용, 각종 충진제, 산소 센서의 접합제, 각종 반도체 소자의 접착제 등으로 이용되며 일반적으로 1200℃ 이상에서도 접착력이 유지되는 물성을 가져야 한다. 또한 고온 열처리용 전기로 등이 설치되어 있지 않은 일반 업체에서 용이하게 접착을 실시할 수 있도록 경화 시간은 1시간내외로 짧고, 경화온도는 일반 오븐의 건조 온도인 150℃ 정도로 비교적 낮아야 한다. 현재 국내에서 관련 외제품이 시판되고 있으나 30000원/100g으로 너무 비싸서 범용으로 사용되기에는 상당히 문제가 있다.In general, inorganic adhesives include organic and inorganic refractory paints, adhesives for semiconductor-related equipment, manufacture of refractory bricks, special paints for electric furnace interiors, heat-resistant special paints, glass adhesives, special brick adhesives, and bonding of various building materials. It is used as a filler, an adhesive for oxygen sensors, adhesives for various semiconductor devices, etc., and generally has physical properties that maintain adhesive strength even at 1200 ° C or higher. In addition, the curing time should be short within about 1 hour, and the curing temperature should be relatively low, such as 150 ℃, the drying temperature of a general oven, so that a general company that is not equipped with a high temperature heat treatment electric furnace is easily installed. Currently, the related foreign products are commercially available in Korea, but it is too expensive to be used for general purposes because it is too expensive at 30,000 won / 100g.
해당 부위에 적용한 후, 고온에서 경화시키지 않고 약 1시간동안 150∼200℃의 온도 범위에서 경화시켜서 접착시킨 후, 1200℃ 이상의 고온에서도 우수한 접착성을 유지하고 전기부도성을 갖는 무기계 접착제를 개발한다.After applying to the site, it is cured at 150 ~ 200 ℃ for 1 hour without being cured at high temperature and then adhered to it.Then, it develops inorganic adhesive which maintains good adhesion even at high temperature of 1200 ℃ or higher and has electrical conductivity. .
산화규소 72.1(±5.0)g, 알루미늄 15.0(±3.0)g, 석고 2.0(±0.5)g, 벤토나이트 1.0(±0.1)g, 지당 2.2(±0.1)g 및 질산 나트륨 6.0g(±0.5)의 질량비로 섞어서 이 혼합물을 120분간 분말분쇄기에서 연마하여 500매쉬 정도의 입도를 가진 분말로 분쇄한 후 4시간 동안 1100(±200)℃로 전기로에서 하소시킨다. 이 혼합물을 공기중에서 3시간 방치하여 냉각하고서 수산화나트륨 48.0(±10.0)g과 300(±150)mL의 물을 섞어서 혼합기를 이용하여 8시간 교반시킨 후 가압솥에서 150℃, 2기압의 조건에서 5시간동안 쪄서 바인더 용액을 제조한다. 이 용액을 삼각 플라스크에 넣고 물을 100(±30)mL, 가한 후 150℃에서 20시간동안 숙성 열처리한다. 이 용액에 활성 알루미나 61.2(±5.0, 300매쉬)g, 에탄올 5.0(±2.0)mL, 타닌산 0.2(±0.05)g, 글리세린 1.5(±0.5)g, 로진 1.0(±0.1)g, 폴리이마이트 1.0(±0.3)g 및 소량의 점증제를 가하여 무기계 접착제를 제조한다.72.1 (± 5.0) g of silicon oxide, 15.0 (± 3.0) g of aluminum, 2.0 (± 0.5) g of gypsum, 1.0 (± 0.1) g of bentonite, 2.2 (± 0.1) g per branch, and 6.0g (± 0.5) of sodium nitrate Mix by mass ratio and grind the mixture in a powder grinder for 120 minutes, pulverize into a powder with a particle size of 500 mesh, and calcinate in an electric furnace at 1100 (± 200) ° C for 4 hours. The mixture was left to stand in air for 3 hours, cooled, and 48.0 (± 10.0) g of sodium hydroxide and 300 (± 150) mL of water were mixed and stirred for 8 hours using a mixer. At 150 ° C and 2 atmospheres in a pressure cooker The binder solution is prepared by steaming for 5 hours. The solution is placed in an Erlenmeyer flask, and 100 (± 30) mL of water is added thereto, followed by aging heat treatment at 150 ° C. for 20 hours. 61.2 (± 5.0, 300 mesh) g of active alumina, 5.0 (± 2.0) mL of ethanol, 0.2 (± 0.05) g of tannic acid, 1.5 (± 0.5) g of glycerin, 1.0 (± 0.1) g of rosin 1.0, polyimite 1.0 (± 0.3) g and a small amount of thickener are added to prepare an inorganic adhesive.
개발한 무기계 접착제를 tile(58x58x4㎣, Glazed mosaic tile)에 대하여 33x58㎟의 면적에 도포하여 150℃에서 열처리하고 인장강도 관련 실험(KS(M 3734, 접착제의 인장 전단 접착강도 시험 방법)규격 기준)을 실시하였으며 tile에 대하여(면적 : 33x58㎟) 추의 질량이 5Kg 이상으로 가해지는 경우에도 접착력이 유지되어 우수한 물성을 보였다. 유리 시편을 이용하여 접착실험을 한 후, 이 시편을 순수한 물에 담가두고서 pH를 변화를 검사하였으며 1일 간격으로 2달 동안 검사한 pH 값은 중성값(pH=6.9∼7.2)의 범위에서 전혀 벗어나지 않았다.The developed inorganic adhesive was applied to the tile (58x58x4㎣, Glazed mosaic tile) on the area of 33x58mm2, heat treated at 150 ℃ and tensile strength test (based on KS (M 3734, tensile shear bond strength test method of adhesive) standard) The adhesive strength was maintained even when the weight of the weight was more than 5Kg with respect to the tile (area: 33x58㎡). After the adhesion test using glass specimens, the specimens were immersed in pure water and their pH was examined for changes of pH. The pH values examined for two months at daily intervals were not within the range of neutral values (pH = 6.9 to 7.2). Did not escape.
또한 전자업계에서 반도체 관련 세라믹스의 접착제로 사용하는 경우 발생할지 모르는 전기전도성을 검사하기 위하여 유리시편 위에 본 고온용 무기 접착제를 코팅하고서 700℃에서 2시간 열처리한 후 상온(20℃)에서 800℃까지 전류와 전위차를 독립적으로 측정하는 표준사탐침 직류법 (standard four probe d.c. technique)을 적용하여 전기전도도를 측정하였고 부도체의 영역의 전도도 값(σ< 10-8cm-1 Ω -1)을 보여서 전도성의 우려는 없는 것으로 나타났다. 이 때 전도도 측정기기는 KEITHLEY SMU(Source Measure Unit) 236을 사용하였으며 온도 측정을 위해 KEITHLEY Digital Multimeter를 사용하여 측정하였다.In addition, in order to test the electrical conductivity that may occur when used as an adhesive for semiconductor-related ceramics in the electronics industry, the high temperature inorganic adhesive is coated on glass specimens, and then heat-treated at 700 ° C. for 2 hours and then at room temperature (20 ° C.) to 800 ° C. Conductivity was measured by applying standard four probe dc technique to measure current and potential difference independently. Conductivity was shown by showing the conductivity value (σ <10 -8 cm -1 Ω -1 ) of the insulator region. There was no concern. In this case, KEITHLEY SMU (Source Measure Unit) 236 was used as the conductivity measuring device and KEITHLEY Digital Multimeter was used for temperature measurement.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20040004806A (en) * | 2002-07-05 | 2004-01-16 | 김혜숙 | Manufacture method of improvement brick |
KR100713191B1 (en) * | 2006-03-15 | 2007-05-02 | 주식회사 에이엠티코리아 | Adhesives for non-flammability inorganic paint and preparing method thereof |
KR100742230B1 (en) * | 2005-11-18 | 2007-07-24 | 최병환 | Manufacturing method of caly bricks using a charcoal powder and clay powder |
US7605541B2 (en) | 2003-11-25 | 2009-10-20 | Nec Corporation | External-electrode discharge lamp with no light leakage from external electrode portion |
-
2000
- 2000-04-29 KR KR1020000023822A patent/KR20010098317A/en not_active Application Discontinuation
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20040004806A (en) * | 2002-07-05 | 2004-01-16 | 김혜숙 | Manufacture method of improvement brick |
US7605541B2 (en) | 2003-11-25 | 2009-10-20 | Nec Corporation | External-electrode discharge lamp with no light leakage from external electrode portion |
US7997949B2 (en) | 2003-11-25 | 2011-08-16 | Nec Corporation | External-electrode discharge lamp with no light leakage from external electrode portion |
KR100742230B1 (en) * | 2005-11-18 | 2007-07-24 | 최병환 | Manufacturing method of caly bricks using a charcoal powder and clay powder |
KR100713191B1 (en) * | 2006-03-15 | 2007-05-02 | 주식회사 에이엠티코리아 | Adhesives for non-flammability inorganic paint and preparing method thereof |
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