CN1415579A - Method for preparing heat elimination base plate made from alumina ceramics - Google Patents
Method for preparing heat elimination base plate made from alumina ceramics Download PDFInfo
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- CN1415579A CN1415579A CN 02137603 CN02137603A CN1415579A CN 1415579 A CN1415579 A CN 1415579A CN 02137603 CN02137603 CN 02137603 CN 02137603 A CN02137603 A CN 02137603A CN 1415579 A CN1415579 A CN 1415579A
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Abstract
An alumina ceramic substrate for heat radiator is prepared from alumina powder and relative auxiliaries through mixing, pulverizing, baking, coarse grinding, fine grinding, punching and calcining. Its advantages are high quality and low cost.
Description
Technical field
The invention belongs to technical field of ceramic material, be specifically related to a kind of preparation method of heat elimination base plate made from alumina ceramics.
Background technology
Alumina ceramic substrate is because it has high physical strength, good performance of heat dissipation etc., and be widely used in every field, as machinery, instrument, chemical industry, biology, space flight and aviation etc., the preparation process of alumina-ceramic has very big influence to the performance quality of pottery.At present, the preparation method of ceramic substrate mainly contains following several: repeatedly roll embrane method, once roll embrane method, hot die-casting method, casting method etc.Roll repeatedly wherein that membrane process craft is ripe, investment is less, adaptability is strong, and still, technological fluctuation is bigger, and product surface is more coarse, and porcelain is more loose.The hot die-casting method facility investment is big, the production cost height, and adaptability is relatively poor, and yield rate is lower.Other method also has its weak point.
Summary of the invention
The object of the present invention is to provide a kind of stable process conditions, reliable product quality, and the preparation method of less investment, alumina ceramic substrate that cost is low.
The preparation method of the alumina ceramic substrate that the present invention proposes is repeatedly rolling the improvement of embrane method, and it is with aluminum oxide (Al
2O
3) powder is basic material, adds relevant auxiliary materials, forms mixed powder, concrete technical process is as follows:
1, pulverize: adopt ball milled, mixed powder is pressed material: ball: water=(1.5-1.8): (1.8-2.2): 1 weight proportion, place in the airtight rotatingcylindrical drum, ball milling 48-56 hour, make the mixed powder breakage of particles become tiny powder;
2, oven dry: through the powder oven dry of ball mill pulverizing, 80-100 purpose screen cloth sieves;
3, kibble: mixed powder and binding agent are become with solvent granule, place between two roller mills and mix, make powder, binding agent and solvent thorough mixing even, follow blowing and preheat, make solvent evaporates, form thicker base sheet;
4, the smart stone roller: the base sheet is placed on the roller mill again, and continuous several draws thin, up to the desired thickness size.The thickness of general film is 0.72 ± 0.02mm;
5, punching: according to the actual product requirement, utilize mould, punching out goes out the product profit of different size, erases punching out base sheet surface and pitchers all around;
6, burn till: heat up from room temperature, until 950-960 ℃,, be incubated 1-2 hour, then cooling to firing temperature (1600-1750 ℃).Wherein, being warming up to about 300 ℃, is body drying, gets rid of mechanically mixing water and planar water; In the time of 300-900 ℃, mainly be to get rid of water of constitution, the decomposition of alkaline-earth metal salt, the oxidation of organism, inorganics etc.; Hot stage 950-960 ℃ to firing temperature, and above-mentioned oxidation, decomposition reaction continue, and form liquid phase, and the solid phase dissolving forms new crystalline phase and crystalline phase and grows up.At this moment, the void content of base reduces rapidly, and sharply shrinks, and intensity, hardness increase.Base substrate is bleached by yellowish (or red) deashing, gloss occurs, and translucent sense is arranged; By the different requirements of product, select the type of cooling.
To the above-mentioned ceramics that burns till, more as requested through grinding machine processing, go-on-go, packing then.
In the inventive method, the weight proportion of mixed powder is as follows:
Aluminum oxide (Al
2O
3): 85-90%,
Silicon-dioxide (SiO
2): 1.5-2.5%,
Talcum powder: 3-5%,
Clay: 6-8%,
Total amount satisfies 100%.
In the inventive method, the component weight proportion that binding agent and solvent are suitable when kibbling is as follows:
Polydiene alcohol: 14-17%,
Ethylene glycol: 1.2-1.5%,
Glycerine: 8-12%,
Water: 65-75%,
Alcohol: 4.5-5.5,
Total amount satisfies 100%.
And powder and binding agent consumption (weight) proportioning are as follows:
Virgin material: 45.5-49%
Reclaimed materials: 38-41%,
Binding agent: 10-16%,
Total amount satisfies 100%.
In the inventive method,, in mixed powder, also can add trace element: Cadmium oxide, tantalum oxide, niobium oxides etc. in order to improve the physicals of pottery.Studies show that, add these compositions and help activating the crystalline phase material, and can further reduce sintering temperature.
The inventive method process stabilizing, reliable in quality, the product suitability is wide, and facility investment is few, product cost is low.
Embodiment
The invention is further illustrated by the following examples.
1, ball milling adopts wet milling process, mixed powder is placed in the airtight rotatingcylindrical drum in the ratio of material, ball, water=1.7: 2: 1, roll along axle horizontal then, rotating speed is controlled at 60-65 rev/min, make ceramic particle at fricting movement between abrading-ball and the abrading-ball or between abrading-ball and the wall of container, and be broken into smaller particles.Ball milling 48---56 hour.
2, with the oven dry of the powder behind the ball milling,, make the alumina-ceramic powder, get procedure ready and use after 80 purpose screen clothes.
3, kibble, with alumina powder and binding agent (as polyvinyl alcohol) and water, becoming granule to place between two roller mills according to certain mixed mixes, make thorough mixing such as powder tackiness agent and solvent even, be accompanied by the blowing and preheat, solvent is progressively volatilized, form one deck thick film base sheet.Because the mode of operation of roll is only rolled blank at thickness direction, lack enough pressure at width.Thereby colloid molecule and powder all had certain directivity, make the physical strength of base substrate and density all have anisotropy.Make the base sheet easily from longitudinal tear, transverse contraction is bigger during sintering, thus in the rolling process, must constantly the base sheet be swung to, otherwise anisotropy can not be reduced to minimum.
4, the smart stone roller: place on the roller mill through the no pit of check, decorative pattern, bubble, cut, after bright and clean again after the little cold of base sheet the base sheet kibbled, draw thin up to desired size through continuous several roads, gauge control is in the scope of 0.72MM ± 0.02MM, to roll good base sheet keeps under the certain humidity environment, prevent dry embrittlement, be beneficial to next step procedure and use.
5, punching: the specification kind different according to the production requirement punching out, size guarantees by the film tool, examination towards the first inspection of product qualified after punching out in batches, with the raw cook of going out manually erase base sheet surface and around pitchers, and weed out damaged, pit, salient point sheet, reclaim and use.With the qualified green sheet in back of plastering, neatly put well, be equipped with binder removal and use.
6, burn till: be by pyroprocessing, make base substrate that a series of physicochemical change take place, form the mineral composition and the microstructure of expection, thereby reach fixed profile and obtain the operation of desired performance.Sintering process is divided into five-stage: body drying, goods, intensification, insulation (being incubated under top temperature) sintering, cooling.The eliminating of machinery mixing water and planar water during body drying.Under body drying temperature (300 ℃), the plastic material of base substrate medium clay soil matter the more, exsiccant carries out further difficulty (draw up easily, defectives such as distortion consequently cause waste product).At the decomposition crystal conversion of the 300-900 ℃ of oxidation of getting rid of water of constitution, organism, carbon and inorganics etc., carbonate, sulfide etc. etc.1600-1750 ℃ of 950 ℃-firing temperature of hot stage, the continuation of above-mentioned oxidation, decomposition reaction forms liquid phase, and the solid phase dissolving forms new crystalline phase and crystalline phase and grows up.The characteristics of this moment are that the void content of base reduces rapidly, and sharply shrink, and intensity, hardness increase, and base substrate is bleached by yellowish (or red) deashing, and base substrate reveals gloss and translucent sense of tool and higher mechanical strength.The different types of cooling is adopted in then base substrate cooling as required, to reach the purpose of producing product.
7, grinding machine: product branch after multiple putting down that sintering is gone out detects product up to standard, the requirement of product before next procedure one mill of being allowed for access.With the ceramics of pressing after burning, quantity is contained on the surface grinding machine table top in accordance with regulations, fills up 2 useless ceramics at buting iron and between by the mill ceramics, and clamps with buting iron.With the corase grind finishing wheel ceramics is carried out ground finish, reach size, the tolerance-0.05mm requirement of regulation.The corase grind depth of cut≤0.02mm, the correct grinding depth of cut≤0.01mm changes the sheet depth of cut≤0.05mm.Carry out self check physical dimension, damaged rate after size is ground to, check the position: worktable left, center, right, front, centre, each a slice of back, and fill in mill back inspection process list.Take off and ground ceramics and carry out flushing with clean water, pickling, flushing with clean water oven dry, calcine acid discharge again.
8, product be will calcine after the acid discharge and no salient point, closed pore, color spot, blackening, pit, damaged, unfilled corner, cut, ripple and the good packing of product shipping of smooth finish detected through branch.
In the present embodiment, the component of compound prescription is as follows: Al
2O
3: 87%, SiO
2: 2%, talcum powder: 4%, clay: 7%.Add micro-Cadmium oxide in addition.
The proportioning of binding agent is in kibbling:
| Polyvinyl alcohol | Ethylene glycol | Glycerine | Water | Alcohol |
| 15％ | 1.5％ | 9％ | 70％ | 4.5％ |
The proportioning of powder and binding agent is:
| Virgin material | Reclaimed materials | Glue |
| ????48％ | ????40％ | ????12％ |
The aluminum oxide pottery heat radiation ceramic chip that makes through above-mentioned technology reaches following index:
The dynamo-electric physical index of table 1 alumina ceramic substrate:
| Project | Index | |
| State | Fine and closely woven | |
| Color | White is with little ash | |
| Alumina content | ????≥ | ????97％ |
| Volume density | ????g/cm 3 | ????3.80 |
| Water-intake rate | ????％ | ????0.00 |
| The anti-intensity of producing | ????MPa≥ | ????294 |
| Thermal expansivity | ????mm/℃ | ????6.8～7.8*10 -6 |
| Thermal conductivity | ????W/M.K≥ | ????20 |
| Volume specific resistance | ????Ω.cm | ????10 14 |
| Relative permittivity | ????(IMZ.25℃) | ????9.5～10.2 |
| Dielectric loss angle tangent | ????(IMZ.25℃) | ????4 *10 -4 |
| Surface roughness Ra | ?????MM | ????0.3～0.5 |
Claims (4)
1, a kind of preparation method of alumina ceramic substrate is a basic raw material with the alumina powder, adds relevant auxiliary materials, forms mixed powder, it is characterized in that technical process is as follows:
(1) pulverize: adopt ball milled, mixed powder is pressed material: ball: water=(1.5-1.8): (1.8-2.2): 1 weight proportion, place in the airtight rotatingcylindrical drum, ball milling 48-56 hour, make the mixed powder breakage of particles become tiny powder;
(2) oven dry: through the powder oven dry of ball mill pulverizing, 80-100 purpose screen cloth sieves;
(3) kibble: mixed powder and binding agent are become with solvent granule, place between two roller mills and mix, make powder, binding agent and solvent thorough mixing even, follow blowing and preheat, make solvent evaporates, form thicker base sheet;
(4) the smart stone roller: the base sheet is placed on the roller mill, and continuous several draws thin, is 0.72 ± 0.02mm up to thickness;
(5) punching: according to the actual product requirement, utilize mould, punching out goes out the kind of different size, erases punching out base sheet surface and pitchers all around;
(6) burn till: heat up from room temperature, until 950-960 ℃,, be incubated 1-2 hour, then cooling to firing temperature.
2, preparation method according to claim 1 is characterized in that the weight proportion of mixed powder is as follows:
Aluminum oxide: 85-90%,
Silicon-dioxide: 1.5-2.5%,
Talcum powder: 3-5%,
Clay: 6-8%,
Total amount satisfies 100%.
3, preparation method according to claim 1 and 2, when it is characterized in that kibbling, the component weight proportion of binding agent is as follows:
Polydiene alcohol: 14-17%,
Ethylene glycol: 1.2-1.5%,
Glycerine: 8-12%,
Water: 65-75%,
Alcohol: 4.5-5.5,
Total amount satisfies 100%.
4, preparation method according to claim 3 is characterized in that the weight proportion of powder and binding agent is as follows:
Virgin material: 45.5-49%
Reclaimed materials: 38-41%,
Binding agent: 10-16%,
Total amount satisfies 100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137603 CN1197821C (en) | 2002-10-24 | 2002-10-24 | Method for preparing heat elimination base plate made from alumina ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137603 CN1197821C (en) | 2002-10-24 | 2002-10-24 | Method for preparing heat elimination base plate made from alumina ceramics |
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|---|---|
| CN1415579A true CN1415579A (en) | 2003-05-07 |
| CN1197821C CN1197821C (en) | 2005-04-20 |
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|---|---|---|---|
| CN 02137603 Expired - Fee Related CN1197821C (en) | 2002-10-24 | 2002-10-24 | Method for preparing heat elimination base plate made from alumina ceramics |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012055206A1 (en) * | 2010-10-26 | 2012-05-03 | Yu Jianping | Alumina/graphite composite ceramic material and led light source utilizing the material as substrate |
| WO2013097324A1 (en) * | 2011-12-31 | 2013-07-04 | 中国电子科技集团公司第十三研究所 | Refined white ceramic material and method for preparing same |
| CN104148645A (en) * | 2014-08-15 | 2014-11-19 | 苏州天泽新能源科技有限公司 | Composite ceramic heat-radiating material and preparation method thereof |
| CN108947504A (en) * | 2018-08-29 | 2018-12-07 | 厦门朝瓷科技有限公司 | Submicrometer structure ultrathin alumina ceramic substrate and preparation method |
| CN109049289A (en) * | 2018-08-29 | 2018-12-21 | 厦门朝瓷科技有限公司 | A kind of preparation method of submicrometer structure ultrathin alumina ceramic green |
| CN109160809A (en) * | 2018-08-29 | 2019-01-08 | 厦门朝瓷科技有限公司 | A kind of submicrometer structure ultrathin alumina ceramic substrate and preparation method |
| CN112047728A (en) * | 2020-09-28 | 2020-12-08 | 成都万士达瓷业有限公司 | Manufacturing method of Al2O3 ceramic substrate |
| CN112062548A (en) * | 2020-09-28 | 2020-12-11 | 成都万士达瓷业有限公司 | Production method of Al2O3 ceramic green body |
| CN112079630A (en) * | 2020-09-28 | 2020-12-15 | 成都万士达瓷业有限公司 | Sintering process of Al2O3 ceramic substrate |
| CN116023861A (en) * | 2022-12-12 | 2023-04-28 | 广东粤港澳大湾区黄埔材料研究院 | Nano granular alumina for polishing and preparation method and application thereof |
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| CN107759204A (en) * | 2017-07-06 | 2018-03-06 | 华东理工大学 | A kind of uvioresistant irradiation low-dielectric loss Al2O3Ceramics and its manufacture method |
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2002
- 2002-10-24 CN CN 02137603 patent/CN1197821C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012055206A1 (en) * | 2010-10-26 | 2012-05-03 | Yu Jianping | Alumina/graphite composite ceramic material and led light source utilizing the material as substrate |
| WO2013097324A1 (en) * | 2011-12-31 | 2013-07-04 | 中国电子科技集团公司第十三研究所 | Refined white ceramic material and method for preparing same |
| US9242901B2 (en) | 2011-12-31 | 2016-01-26 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Refined white ceramic material and method for preparing same |
| CN104148645A (en) * | 2014-08-15 | 2014-11-19 | 苏州天泽新能源科技有限公司 | Composite ceramic heat-radiating material and preparation method thereof |
| CN108947504A (en) * | 2018-08-29 | 2018-12-07 | 厦门朝瓷科技有限公司 | Submicrometer structure ultrathin alumina ceramic substrate and preparation method |
| CN109049289A (en) * | 2018-08-29 | 2018-12-21 | 厦门朝瓷科技有限公司 | A kind of preparation method of submicrometer structure ultrathin alumina ceramic green |
| CN109160809A (en) * | 2018-08-29 | 2019-01-08 | 厦门朝瓷科技有限公司 | A kind of submicrometer structure ultrathin alumina ceramic substrate and preparation method |
| CN112047728A (en) * | 2020-09-28 | 2020-12-08 | 成都万士达瓷业有限公司 | Manufacturing method of Al2O3 ceramic substrate |
| CN112062548A (en) * | 2020-09-28 | 2020-12-11 | 成都万士达瓷业有限公司 | Production method of Al2O3 ceramic green body |
| CN112079630A (en) * | 2020-09-28 | 2020-12-15 | 成都万士达瓷业有限公司 | Sintering process of Al2O3 ceramic substrate |
| CN116023861A (en) * | 2022-12-12 | 2023-04-28 | 广东粤港澳大湾区黄埔材料研究院 | Nano granular alumina for polishing and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1197821C (en) | 2005-04-20 |
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