CN109053160A - 一种高抗折强度氧化铍陶瓷的制备方法 - Google Patents
一种高抗折强度氧化铍陶瓷的制备方法 Download PDFInfo
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- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 title claims abstract description 25
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000011224 oxide ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 43
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000919 ceramic Substances 0.000 claims abstract description 20
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000010433 feldspar Substances 0.000 claims abstract description 18
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 235000012222 talc Nutrition 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 13
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 235000019241 carbon black Nutrition 0.000 claims abstract description 10
- 239000006229 carbon black Substances 0.000 claims abstract description 10
- 239000000454 talc Substances 0.000 claims abstract description 10
- 229910052623 talc Inorganic materials 0.000 claims abstract description 10
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 7
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 5
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 235000010215 titanium dioxide Nutrition 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 description 12
- 238000007254 oxidation reaction Methods 0.000 description 12
- 239000002019 doping agent Substances 0.000 description 9
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- -1 A12O3 Chemical compound 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种高抗折强度氧化铍陶瓷的制备方法，包括以下步骤：（1）以99BeO为原料，添加0.3‑0.5wt%氧化镁和0.5‑1%的烧结助剂，添加去离子水，球磨20‑24h，烘干；（2）将烘干后的原料添加10‑20%的粘结剂，高压成型，得陶瓷坯料；（3）对成型后的陶瓷坯料在空气中烧结进行烧结，得高抗折强度氧化铍陶瓷；所述的烧结助剂，按照重量份计，包括30‑40份生滑石、50‑60份长石、1份氧化铈、3‑5份白炭黑、1‑3份钛白粉。本发明通过添加烧结助剂，烧结助剂采用生滑石、长石、氧化铈、白炭黑和钛白粉，并且其进行除杂和烧结处理，使得得到的烧结助剂具有优良的性能，能够有效的降低氧化铍陶瓷的烧结温度，提高热导率和机械性能。
Description
技术领域
本发明涉及一种高抗折强度氧化铍陶瓷的制备方法，属于无机陶瓷材料领域。
背景技术
BeO陶瓷由于具有高导热、高熔点、高强度、高绝缘性、高的化学性和热稳定性、低介电常数、低介质损耗及良好的工艺适应性等特点，广泛应用于微电子器件、功率模块大功率电阻基板、电力电子管壳等产品中，在电子信息装备中也多有应用。但氧化被陶瓷晶粒尺寸的不均匀和致密度较难提高，影响到BeO陶瓷材料的热学性能和力学性能，致使它的使用寿命和更广泛的应用受到制约。氧化被陶瓷的热导率、介电常数、介质损耗等关键参数的优劣与氧化被陶瓷的纯度、密度紧密相关。一般而言，纯度越高，氧化被陶瓷的性能越好，但是高纯的氧化被陶瓷很难烧结，烧结温度非常高，一般要在其配方中添加少量的掺杂剂来降低其烧成温度，改善其烧结性能。目前被用作掺杂剂以降低氧化被陶瓷的烧结温度的材料主要有氧化铝、氧化镁和二氧化硅等。但多数含有掺杂剂的氧化镀陶瓷材料都是采用一元或二元的掺杂剂，即只含氧化铝、氧化镁和二氧化硅中的一种或两种掺杂剂，这种一元或二元的掺杂剂掺杂的氧化被陶瓷材料的烧结温度高、陶瓷材料热导率也不理想，室温热导率通常在240W/m·k以下。授权公告号CN101182189B，发明名称：多元掺杂的高性能氧化被陶瓷材料及制备方法，多元掺杂的高性能氧化被陶瓷材料，除氧化镀外，还包括0.2-6％质量的多元掺杂剂；所述多元掺杂剂由MgO、A12O3、SiO2、CaO.ZnO和稀土氧化物组成，通过溶胶一凝胶法制备多元掺杂剂，然后与高纯氧化镀原料混合、成型、高温烧结后得到本发明的多元掺杂的高性能氧化被陶瓷材料。该发明提供的多元掺杂的高性能氧化镀陶瓷材料具有较低的烧结温度、更高的密度、热导率和机械性能；其微观结构具有致密、晶粒均匀、气孔少的特点。其制备方法工艺简单、生产成本较低，且具有良好的重复性，适合于工业化生产。该发明存在制备方法复杂，导致其成本高。
发明内容
本发明提供了一种高抗折强度氧化铍陶瓷的制备方法，解决了现有氧化铍陶瓷制备方法复杂、制备的陶瓷强度和热导率不是很好等问题。
为解决上述技术问题，本发明采用的技术方案为：
一种高抗折强度氧化铍陶瓷的制备方法，包括以下步骤：
(1)以99BeO为原料，添加0.3-0.5wt％氧化镁和0.5-1％的烧结助剂，添加去离子水，球磨20-24h，烘干；
(2)将烘干后的原料添加10-20％的粘结剂，高压成型，得陶瓷坯料；
(3)对成型后的陶瓷坯料在空气中烧结进行烧结，得高抗折强度氧化铍陶瓷；所述的烧结助剂，按照重量份计，包括30-40份生滑石、50-60份长石、1份氧化铈、3-5份白炭黑、1-3份钛白粉。
进一步，本发明的一种优选方案：所述的高压成型的压力为20-30MPa。
进一步，本发明的一种优选方案：所述的粘结剂为羧甲基纤维素。
进一步，本发明的一种优选方案：所述的烧结具体为：以1℃/min的速率缓慢升温至230℃，保温2小时，然后以2℃/min，升温至500℃，保温2小时，5℃/min升至1650℃保温4小时烧结，然后随炉冷却。
进一步，本发明的一种优选方案：所述的烧结助剂的制备方法，(1)将生滑石、长石分别800℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的生滑石、长石、氧化铈、白炭黑和钛白粉混合均匀，然后4℃/min升至1500℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
本发明的有益效果：
本发明通过添加烧结助剂，烧结助剂采用生滑石、长石、氧化铈、白炭黑和钛白粉，并且其进行除杂和烧结处理，使得得到的烧结助剂具有优良的性能，能够有效的降低氧化铍陶瓷的烧结温度，提高热导率和机械性能。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种高抗折强度氧化铍陶瓷的制备方法，包括以下步骤：
(1)以99BeO为原料，添加0.3wt％氧化镁和0.8％的烧结助剂，添加去离子水，球磨20h，烘干；
(2)将烘干后的原料添加10％的粘结剂，高压成型，高压成型的压力为20MPa，得陶瓷坯料，所述的粘结剂为羧甲基纤维素；
(3)对成型后的陶瓷坯料在空气中烧结进行烧结，以1℃/min的速率缓慢升温至230℃，保温2小时，然后以2℃/min，升温至500℃，保温2小时，5℃/min升至1650℃保温4小时烧结，然后随炉冷却，得高抗折强度氧化铍陶瓷；
所述的烧结助剂，按照重量份计，包括30份生滑石、60份长石、1份氧化铈、5份白炭黑、1份钛白粉。
烧结助剂的制备方法，(1)将生滑石、长石分别800℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的生滑石、长石、氧化铈、白炭黑和钛白粉混合均匀，然后4℃/min升至1500℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
实施例2
一种高抗折强度氧化铍陶瓷的制备方法，包括以下步骤：
(1)以99BeO为原料，添加0.4wt％氧化镁和1％的烧结助剂，添加去离子水，球磨22h，烘干；
(2)将烘干后的原料添加15％的粘结剂，高压成型，高压成型的压力为25MPa，得陶瓷坯料，所述的粘结剂为羧甲基纤维素；
(3)对成型后的陶瓷坯料在空气中烧结进行烧结，以1℃/min的速率缓慢升温至230℃，保温2小时，然后以2℃/min，升温至500℃，保温2小时，5℃/min升至1650℃保温4小时烧结，然后随炉冷却，得高抗折强度氧化铍陶瓷；
所述的烧结助剂，按照重量份计，包括35份生滑石、55份长石、1份氧化铈、4份白炭黑、2份钛白粉。
烧结助剂的制备方法，(1)将生滑石、长石分别800℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的生滑石、长石、氧化铈、白炭黑和钛白粉混合均匀，然后4℃/min升至1500℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
实施例3
一种高抗折强度氧化铍陶瓷的制备方法，包括以下步骤：
(1)以99BeO为原料，添加0.5wt％氧化镁和0.5％的烧结助剂，添加去离子水，球磨24h，烘干；
(2)将烘干后的原料添加20％的粘结剂，高压成型，高压成型的压力为30MPa，得陶瓷坯料，所述的粘结剂为羧甲基纤维素；
(3)对成型后的陶瓷坯料在空气中烧结进行烧结，以1℃/min的速率缓慢升温至230℃，保温2小时，然后以2℃/min，升温至500℃，保温2小时，5℃/min升至1650℃保温4小时烧结，然后随炉冷却，得高抗折强度氧化铍陶瓷；
所述的烧结助剂，按照重量份计，包括40份生滑石、50份长石、1份氧化铈、3份白炭黑、3份钛白粉。
烧结助剂的制备方法，(1)将生滑石、长石分别800℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的生滑石、长石、氧化铈、白炭黑和钛白粉混合均匀，然后4℃/min升至1500℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
性能测试
测定实施例1-3所制备的氧化铍陶瓷性能，具体见下表。
| 密度(g/cm<sup>3</sup>) | 热导率(25℃W/m·k) | 抗弯强度(Mpa) | |
| 实施例1 | 2.98 | 312 | 256 |
| 实施例2 | 3.03 | 308 | 254 |
| 实施例3 | 2.99 | 310 | 255 |
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种高抗折强度氧化铍陶瓷的制备方法，其特征在于，包括以下步骤：
（1）以99BeO为原料，添加0.3-0.5wt%氧化镁和0.5-1%的烧结助剂，添加去离子水，球磨20-24h，烘干；
（2）将烘干后的原料添加10-20%的粘结剂，高压成型，得陶瓷坯料；
（3）对成型后的陶瓷坯料在空气中烧结进行烧结，得高抗折强度氧化铍陶瓷；所述的烧结助剂，按照重量份计，包括30-40份生滑石、50-60份长石、1份氧化铈、3-5份白炭黑、1-3份钛白粉。
2.根据权利要求1所述的一种高抗折强度氧化铍陶瓷的制备方法，其特征在于：所述的高压成型的压力为20-30MPa。
3.根据权利要求1所述的一种高抗折强度氧化铍陶瓷的制备方法，其特征在于：所述的粘结剂为羧甲基纤维素。
4.根据权利要求1所述的一种高抗折强度氧化铍陶瓷的制备方法，其特征在于：所述的烧结具体为：以1℃/min 的速率缓慢升温至230℃，保温2小时，然后以2℃/min，升温至500℃，保温2小时， 5℃ /min升至 1650℃保温4小时烧结，然后随炉冷却。
5.根据权利要求1所述的一种高抗折强度氧化铍陶瓷的制备方法，其特征在于：所述的烧结助剂的制备方法，（1）将生滑石、长石分别800℃焙烧2h后，按照液固比为 3∶1加入浓度为 40%硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；（2）将处理后的生滑石、长石、氧化铈、白炭黑和钛白粉混合均匀，然后4℃ /min升至 1500℃保温3小时烧结，然后随炉冷却；（4）将得到的烧结物粉碎，球磨，即得烧结助剂。
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| CN101219899A (zh) * | 2008-01-10 | 2008-07-16 | 电子科技大学 | 一种高导热、高抗折强度氧化铍陶瓷材料的制备方法 |
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| CN101219899A (zh) * | 2008-01-10 | 2008-07-16 | 电子科技大学 | 一种高导热、高抗折强度氧化铍陶瓷材料的制备方法 |
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