CN1358690A - Method for prepairng TiB2-BN conductive composite material - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims description 12
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 239000000919 ceramic Substances 0.000 claims abstract description 22
- 238000002485 combustion reaction Methods 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 7
- 230000006698 induction Effects 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 15
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000001465 metallisation Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 8
- 229910033181 TiB2 Inorganic materials 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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Abstract
本发明涉及一种具有耐高温、耐腐蚀、抗热冲击的导电陶瓷材料,其成分由导电相TiB2(40－58wt%),非导电相BN(42－60wt%),添加剂AlN(0～10wt%)和SiC(0～5wt%)复合构成,采用感应热压烧结或通电加压烧结方法在1700℃～2000℃之间烧结而成。这种导电陶瓷复合材料的主要原料TiB2由燃烧还原合成方法制备(专利申请号:01128497.8),这种TiB2陶瓷原料具有较高的烧结活性,可大大降低烧结温度。本发明涉及的导电陶瓷复合材料可制成陶瓷坩埚,用于各种材料和部件的表面金属化,具有电阻率稳定,使用寿命长的特点。The invention relates to a conductive ceramic material with high temperature resistance, corrosion resistance and thermal shock resistance. 10wt%) and SiC (0-5wt%) composite composition, which is sintered between 1700°C and 2000°C by induction hot pressing sintering or electrification and pressure sintering. The main raw material TiB 2 of this conductive ceramic composite material is prepared by combustion reduction synthesis method (patent application number: 01128497.8). This TiB 2 ceramic raw material has high sintering activity and can greatly reduce the sintering temperature. The conductive ceramic composite material involved in the invention can be made into a ceramic crucible, which is used for surface metallization of various materials and components, and has the characteristics of stable resistivity and long service life.
Description
技术领域Technical field
本发明属于陶瓷复合材料及其制造工艺。特别是TiB2陶瓷复合材料。The invention belongs to a ceramic composite material and a manufacturing process thereof. Especially TiB2 ceramic composites.
背景技术 Background technique
TiB2陶瓷是重要的新型工程材料，具有许多重要的物理化学特性，如高熔点、高模量、耐腐蚀、高导热、高导电性等，具有广泛的应用价值。在TiB2中引入BN来调节其电阻率和抗热震性，可制成新型的导电陶瓷复合材料，这种导电陶瓷复合材料可广泛使用于各种材料表面金属化和表面改性，在包装材料、多层膜电容器及显象管金属化方面大量使用，是真空蒸镀行业的关键耗材。TiB 2 ceramics are important new engineering materials with many important physical and chemical properties, such as high melting point, high modulus, corrosion resistance, high thermal conductivity, high electrical conductivity, etc., and have a wide range of application values. Introducing BN into TiB 2 to adjust its resistivity and thermal shock resistance can make a new type of conductive ceramic composite material, which can be widely used in surface metallization and surface modification of various materials, in packaging Materials, multilayer film capacitors and kinescope metallization are widely used, and they are key consumables in the vacuum evaporation industry.
TiB2-BN复合陶瓷可采用反应烧结法来制备。它是以Ti+BN为原料，通过高温反应来形成TiB2+BN。该工艺的主要缺点在于合成相组成难控制，材料结构不均匀，因此，产品成品率低，电导率不稳定，耐金属熔蚀性差，使用寿命短。TiB 2 -BN composite ceramics can be prepared by reaction sintering method. It uses Ti+BN as raw material to form TiB 2 +BN through high temperature reaction. The main disadvantages of this process are that the composition of the synthesized phase is difficult to control and the structure of the material is not uniform. Therefore, the yield of the product is low, the conductivity is unstable, the resistance to metal corrosion is poor, and the service life is short.
发明内容Contents of Invention
本发明所要解决的技术问题是：克服现有技术的上述缺点，采用燃烧还原合成工艺制备的TiB2为主要原料，配以市售BN和添加剂AlN，SiC，在1700℃～2000℃之间感应热压烧结或通电加压烧结，可形成结构均匀的高密度TiB2-BN复合材料。这种TiB2-BN导电陶瓷复合材料具有稳定的电导率，良好的耐金属熔蚀性。The technical problem to be solved by the present invention is: to overcome the above-mentioned shortcomings of the prior art, use TiB2 prepared by the combustion reduction synthesis process as the main raw material, mix with commercially available BN and additives AlN, SiC, and induce High-density TiB 2 -BN composite materials with uniform structure can be formed by hot-pressing sintering or electrified-pressurized sintering. The TiB 2 -BN conductive ceramic composite material has stable electrical conductivity and good metal corrosion resistance.
本发明解决其技术问题所采用的技术方案是：将TiO2、B2O3、Mg粉末均匀混合并模压成型，在常温常压下置于氩气保护的自蔓延高温合成装置(国家实用新型专利：ZL93216816.7)中，点火燃烧，燃烧产物经破碎、酸洗后得到具有高烧结活性、微细的TiB2粉料(纯度大于98％，粒度小于5μm)，将其与市售BN和添加剂AlN，SiC按一定比例配合，通过感应热压烧结或通电加压烧结来获得具有高密度的TiB2-BN导电陶瓷复合材料。The technical solution adopted by the present invention to solve the technical problem is: uniformly mix TiO 2 , B 2 O 3 , and Mg powders and mold them into a self-propagating high-temperature synthesis device protected by argon at normal temperature and pressure (National Utility Model Patent: ZL93216816.7), ignite and burn, and the combustion product is crushed and pickled to obtain a high sintering activity, fine TiB 2 powder (purity greater than 98%, particle size less than 5 μm), which is combined with commercially available BN and additives AlN and SiC are mixed in a certain proportion, and the TiB 2 -BN conductive ceramic composite material with high density is obtained by induction hot pressing sintering or electrification and pressure sintering.
本发明是这样实现的：The present invention is achieved like this:
1.将TiO2、B2O3和Mg粉末均匀混合并模压成型，在常温常压下置于氩气保护的自蔓延高温合成装置(国家实用新型专利：ZL93216816.7)中，点火燃烧，得到燃烧产物。1. Uniformly mix TiO 2 , B 2 O 3 and Mg powders and mold them, place them in argon-protected self-propagating high-temperature synthesis device (national utility model patent: ZL93216816.7) at room temperature and pressure, ignite and burn, Combustion products are obtained.
其中TiO2粉末粒径应小于80μm，B2O3粉末粒径应小于120μm，Mg粉末粒径应小于200μm。Among them, the particle size of TiO 2 powder should be less than 80 μm, that of B 2 O 3 powder should be less than 120 μm, and that of Mg powder should be less than 200 μm.
自蔓延高温还原合成用的TiO2、B2O3、Mg粉末原料其配方按重量百分比为：TiO2为27-29wt％，B2O3为26-28wt％、Mg为43-47wt％。The composition of TiO 2 , B 2 O 3 , and Mg powder raw materials for self-propagating high-temperature reduction synthesis is as follows: TiO 2 is 27-29 wt%, B 2 O 3 is 26-28 wt%, and Mg is 43-47 wt%.
2.TiB2陶瓷微粉的提纯、分离可按照如下工艺来实现：燃烧产物经球磨机破碎后过筛得到粒径小于0.5mm的粉末；将粉末置于反应釜内，在浓度为0.5～2.0mol/l的盐酸或硫酸中于20～80℃温度下酸洗1～10小时，所获产物经过滤、烘干，即为高纯二硼化钛陶瓷微粉。2. The purification and separation of TiB 2 ceramic micropowder can be realized according to the following process: the combustion product is crushed by a ball mill and sieved to obtain a powder with a particle size of less than 0.5mm; Pickling in 1 hydrochloric acid or sulfuric acid at a temperature of 20-80°C for 1-10 hours, and the obtained product is filtered and dried to obtain high-purity titanium diboride ceramic powder.
采用自蔓延高温还原合成(SHRS)技术结合化学纯化后合成高纯TiB2陶瓷微粉，其成分为：Ti67-69wt％，B29-32wt％，O≤0.75wt％，N≤0.1wt％，Mg≤0.15wt％，平均粒径为5μm。High-purity TiB2 ceramic micropowder is synthesized by self-propagating high-temperature reduction synthesis (SHRS) technology combined with chemical purification, and its composition is: Ti67-69wt%, B29-32wt%, O≤0.75wt%, N≤0.1wt%, Mg≤ 0.15wt%, the average particle size is 5μm.
3.将燃烧还原合成工艺制备的TiB2微粉(纯度＞98％、粒径小于5μm)与市售BN(纯度＞97％、粒径小于1μm)和添加剂AlN(纯度＞97％、粒径小于1μm)，SiC(纯度＞97％、粒径小于1μm)充分混合，喷雾干燥后，置于感应热压或通电加压炉中，热压烧结时间为2小时，烧结温度：1700--2000℃，烧结压力：40Mpa。随炉冷却后，可获得密度大于95％的TiB2-BN复合导电材料。3. Combine TiB 2 micropowder (purity>98%, particle size less than 5 μm) prepared by combustion reduction synthesis process with commercially available BN (purity>97%, particle size less than 1 μm) and additive AlN (purity>97%, particle size less than 1μm), SiC (purity > 97%, particle size less than 1μm) are fully mixed, spray-dried, placed in induction hot pressing or electrified pressurized furnace, hot pressing sintering time is 2 hours, sintering temperature: 1700--2000 ° C , Sintering pressure: 40Mpa. After cooling in a furnace, a TiB 2 -BN composite conductive material with a density greater than 95% can be obtained.
其中TiB2微粉、BN、AlN、SiC的配方按重量百分比为：Wherein the formula of TiB micropowder , BN, AlN, SiC is by weight percentage:
TiB2：40～60wt％ BN：40～60wt％ AlN：0～10wt％ SiC：0～5wt％TiB 2 : 40-60wt% BN: 40-60wt% AlN: 0-10wt% SiC: 0-5wt%
本发明与传统工艺相比，TiB2-BN复合材料具有产品密度高，质量好，电导率稳定，耐金属熔蚀性好的优点。Compared with the traditional technology, the TiB 2 -BN composite material of the present invention has the advantages of high product density, good quality, stable electrical conductivity and good metal corrosion resistance.
本发明涉及的导电陶瓷复合材料可制成陶瓷坩埚，用于各种材料和部件的表面金属化，具有电阻率稳定，使用寿命长的特点。The conductive ceramic composite material involved in the invention can be made into a ceramic crucible, which is used for surface metallization of various materials and parts, and has the characteristics of stable resistivity and long service life.
具体实施方案Specific implementation plan
本发明所述TiB2微粉的制备方法以及具体实施例，已在申请号为01128497、发明名称为“自蔓延高温还原合成法制备高纯二硼化钛陶瓷微粉”的发明专利申请中有详细的描述，在下述实施例中所涉及的“燃烧还原合成的高纯TiB2粉末”均为用该发明方法制备的TiB2微粉。The preparation method and specific examples of the TiB2 micropowder of the present invention have been detailed in the invention patent application whose application number is 01128497 and the title of the invention is "preparation of high-purity titanium diboride ceramic micropowder by self-propagating high-temperature reduction synthesis method" Description, the "combustion reduction synthesis of high-purity TiB2 powder" involved in the following examples are all TiB2 micropowders prepared by the inventive method.
实施例1：Example 1:
首先将42g燃烧还原合成的高纯TiB2粉末(纯度＞98％、粒径小于5μm)，58g市售BN(纯度＞97％、粒径小于1μm)充分混合，经喷雾干燥后，置于高强石墨模具中，在感应热压炉中进行热压烧结，烧结工艺制度为：烧结温度：2000℃，压力：40MPa，烧结时间2小时。烧结后随炉缓慢冷却，可获得相对密度大于95％的TiB2-BN导电陶瓷复合材料。First, 42g of high-purity TiB 2 powder (purity>98%, particle size less than 5μm) synthesized by combustion reduction, and 58g of commercially available BN (purity>97%, particle size less than 1μm) were fully mixed, after spray drying, placed in high-strength In the graphite mold, hot-press sintering is carried out in an induction hot-press furnace. The sintering process system is as follows: sintering temperature: 2000°C, pressure: 40MPa, and sintering time for 2 hours. After sintering and cooling slowly with the furnace, a TiB 2 -BN conductive ceramic composite material with a relative density greater than 95% can be obtained.
实施例2：Example 2:
首先将44g燃烧还原合成的高纯TiB2粉末(纯度＞98％、粒径小于5μm)，44g市售BN(纯度＞97％、粒径小于1μm)，8gAlN(纯度＞97％、粒径小于1μm)，4g SiC(纯度＞97％、粒径小于1μm)充分混合，经喷雾干燥后，置于高强石墨模具中，在通电加压炉中进行热压烧结，烧结工艺制度为：烧结温度：1900℃，压力：40MPa，烧结时间2小时。烧结后随炉缓慢冷却，可获得相对密度大于95％的TiB2-BN导电陶瓷复合材料。First, 44g of high-purity TiB 2 powder (purity>98%, particle size less than 5μm) synthesized by combustion reduction, 44g commercially available BN (purity>97%, particle size less than 1μm), 8g AlN (purity>97%, particle size smaller than 1μm), 4g SiC (purity > 97%, particle size less than 1μm) are fully mixed, after spray drying, placed in a high-strength graphite mold, and hot-pressed and sintered in an electrified pressurized furnace. The sintering process system is: Sintering temperature: 1900°C, pressure: 40MPa, sintering time 2 hours. After sintering and cooling slowly with the furnace, a TiB 2 -BN conductive ceramic composite material with a relative density greater than 95% can be obtained.
实施例3：Example 3:
首先将60g燃烧还原合成的高纯TiB2粉末(纯度＞98％、粒径小于5μm)，35g市售BN(纯度＞97％、粒径小于1μm)，5gAlN(纯度＞97％、粒径小于1μm)充分混合，经喷雾干燥后，置于高强石墨模具中，在感应热压炉中进行热压烧结，烧结工艺制度为：烧结温度：1800℃，压力：40MPa，烧结时间2小时。烧结后随炉缓慢冷却，可获得相对密度大于95％的TiB2-BN导电陶瓷复合材料。First, 60g of high-purity TiB 2 powder (purity>98%, particle size less than 5μm) synthesized by combustion reduction, 35g commercially available BN (purity>97%, particle size less than 1μm), 5g AlN (purity>97%, particle size smaller than 1μm) mixed thoroughly, spray-dried, placed in a high-strength graphite mold, and hot-pressed and sintered in an induction hot-press furnace. After sintering and cooling slowly with the furnace, a TiB 2 -BN conductive ceramic composite material with a relative density greater than 95% can be obtained.
实施例4：Example 4:
首先将45g燃烧还原合成的高纯TiB2粉末(纯度＞98％、粒径小于5μm)，50g市售BN(纯度＞97％、粒径小于1μm)，3gAlN(纯度＞97％、粒径小于1μm)，2g SiC(纯度＞97％、粒径小于1μm)充分混合，经喷雾干燥后，置于高强石墨模具中，在通电加压炉中进行热压烧结，烧结工艺制度为：烧结温度：1700℃，压力：40MPa，烧结时间2小时。烧结后随炉缓慢冷却，可获得相对密度大于95％的TiB2-BN导电陶瓷复合材料。First, 45g of high-purity TiB 2 powder (purity>98%, particle size less than 5μm) synthesized by combustion reduction, 50g commercially available BN (purity>97%, particle size less than 1μm), 3g AlN (purity>97%, particle size smaller than 1μm), 2g SiC (purity > 97%, particle size less than 1μm) are fully mixed, spray-dried, placed in a high-strength graphite mold, and hot-pressed and sintered in an electrified pressurized furnace. The sintering process system is: Sintering temperature: 1700°C, pressure: 40MPa, sintering time 2 hours. After sintering and cooling slowly with the furnace, a TiB 2 -BN conductive ceramic composite material with a relative density greater than 95% can be obtained.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460649B (en) * | 2006-06-02 | 2010-12-08 | 株式会社丰田中央研究所 | Conductive corrosion-resistant material and manufacturing method thereof |
| US8034153B2 (en) | 2005-12-22 | 2011-10-11 | Momentive Performances Materials, Inc. | Wear resistant low friction coating composition, coated components, and method for coating thereof |
| CN102983015A (en) * | 2011-09-06 | 2013-03-20 | 施耐德电器工业公司 | Contact material containing BN/TiB2 composite phase ceramic material, application of contact material and circuit breaker containing the contact material |
| CN1922119B (en) * | 2004-02-20 | 2013-11-13 | 戴蒙得创新股份有限公司 | Sintered Composite |
| CN117187753A (en) * | 2023-10-18 | 2023-12-08 | 安徽赛福电子有限公司 | Evaporation boat for evaporating metallized polypropylene copper film and preparation method thereof |
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2001
- 2001-09-28 CN CN 01133505 patent/CN1358690A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1922119B (en) * | 2004-02-20 | 2013-11-13 | 戴蒙得创新股份有限公司 | Sintered Composite |
| US8034153B2 (en) | 2005-12-22 | 2011-10-11 | Momentive Performances Materials, Inc. | Wear resistant low friction coating composition, coated components, and method for coating thereof |
| CN101037566B (en) * | 2005-12-22 | 2012-05-30 | 莫门蒂夫性能材料股份有限公司 | Wear-resistant and low-friction coating composition, coated element, and method for preparing said coating composition |
| CN101460649B (en) * | 2006-06-02 | 2010-12-08 | 株式会社丰田中央研究所 | Conductive corrosion-resistant material and manufacturing method thereof |
| CN102983015A (en) * | 2011-09-06 | 2013-03-20 | 施耐德电器工业公司 | Contact material containing BN/TiB2 composite phase ceramic material, application of contact material and circuit breaker containing the contact material |
| CN102983015B (en) * | 2011-09-06 | 2015-09-30 | 施耐德电器工业公司 | Comprise BN/TiB 2the contact material of diphase ceramic material, the purposes of contact material and the circuit breaker containing this contact material |
| CN117187753A (en) * | 2023-10-18 | 2023-12-08 | 安徽赛福电子有限公司 | Evaporation boat for evaporating metallized polypropylene copper film and preparation method thereof |
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