CN105859263A - 一种高性能96氧化铝陶瓷及其制备方法 - Google Patents
一种高性能96氧化铝陶瓷及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000011224 oxide ceramic Substances 0.000 title abstract 6
- 229910052574 oxide ceramic Inorganic materials 0.000 title abstract 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 151
- 239000000919 ceramic Substances 0.000 claims description 48
- 238000005245 sintering Methods 0.000 claims description 26
- 239000011812 mixed powder Substances 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
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- 238000003825 pressing Methods 0.000 claims description 6
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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Abstract
本发明涉及电子材料技术领域，具体为一种高性能96氧化铝陶瓷及其制备方法。本发明通过向α‑Al2O3中添加适量的SiO2、MgO和CaO，可显著提高所制备的96氧化铝陶瓷的绝缘性能、介电强度、力学性能及导热性。通过控制制备工艺可制备性能稳定的96氧化铝陶瓷，所制备的96氧化铝陶瓷在室温及25％湿度环境中的体积电阻率可高达7×1014Ω·cm，在室温及70％湿度环境中其体积电阻率仍可保持在1012的数量级以上，当温度为600℃时其体积电阻率还能达到108数量级以上；室温条件下96氧化铝陶瓷的介电强度高达30kV/mm，抗弯强度高达约400MPa，维氏硬度高达14GPa。
Description
技术领域
本发明涉及电子材料技术领域，尤其涉及一种高性能96氧化铝陶瓷及其制备方法。
背景技术
电子技术的快速发展促使电路元件用绝缘承载材料的高速发展。电子设备向薄、轻、小和数字化发展，使得研制新型电子材料迫在眉睫。电子元件的高密度化、高功率化及高集成度对其配套电子材料的综合性能提出更高的要求。近年来，制备低成本、高性能、无毒电子绝缘材料成为电子材料领域研究的热点。
众所周知，氧化铝陶瓷具有高强度、耐高温、耐腐蚀、耐磨损、抗氧化及良好的化学稳定性和电绝缘性能，且成本低廉、制备工艺成熟，已被广泛应用在电子电气、航空航天、石油化工等领域。然而，一般工业用氧化铝陶瓷大多采用成本低、生产量大的拜耳法制备而成，烧结活性较差，导致其烧结温度高、耗能大、制备成本较高。为降低其烧结温度，通常会向氧化铝粉体中引入一定量的烧结助剂(如CaO，SiO2等)来促进其烧结。目前氧化铝陶瓷在电子元器件材料领域已占有一席之地，但是市场上应用最为广泛的是低铝陶瓷。低铝陶瓷的电绝缘性能一般且受环境影响较大，很难满足在高温高湿环境中使用的要求。另外低铝陶瓷的机械性能较差，在对机械性能要求较高的领域也无法应用，因此高铝陶瓷电子元器件材料应运而生。目前高铝陶瓷电子材料中均含有钠离子(Na+)，而Na+半径小，且是一价离子，其与硅氧四面体网体的连接力弱，高温下与玻璃相共熔，使无规网络出现非桥接氧(即断头)，结构疏松，激活能低，在热运动下极易迁移，所以含钠高铝陶瓷材料的电阻率较低、介电损耗大。
发明内容
本发明针对现有氧化铝陶瓷的机电性能较差的问题，提供一种具有优异绝缘性能、介电强度、力学性能及导热性的高性能96氧化铝陶瓷，以及该种高性能96氧化铝陶瓷的制备方法。
为实现上述目的，本发明采用以下技术方案。
一种高性能96氧化铝陶瓷，由以下质量百分比的各组分制备而成：96％的α-Al2O3，0.1-1.5％的MgO，0.01-0.5％的CaO，余量为SiO2。
优选的，所述高性能96氧化铝陶瓷由以下质量百分比的各组分制备而成：96％的α-Al2O3，2.75％的SiO2，1.0％的MgO，0.25％的CaO。
以上所述高性能96氧化铝陶瓷的制备方法，包括以下步骤：
S1制混合粉体：按各组分配比分别称取α-Al2O3、SiO2、MgO和CaO，然后将各组分混合在一起并分散均匀，得到混合粉体。
优选的，将α-Al2O3、SiO2、MgO和CaO置于无水乙醇中并超声分散至混合物的粘稠度增大到该混合物无法流动，得到分散体；然后干燥分散体，得到混合粉体。
更优选的，干燥分散体得到混合粉体后，还包括以下步骤：研磨混合粉体并使混合粉体过100目筛。
S2成型：将混合粉体模压成坯体。
优选的，以干压与冷等静压相结合的方式在10-500MPa下将混合粉体模压成坯体。
S3烧结：将坯体置于烧结炉中烧结，制得氧化铝陶瓷。
优选的，在空气中以无压烧结的方式烧结坯体，烧结温度为1500-1600℃，保温时间为1-4h。
更优选的，将坯体置于烧结炉中，以20℃/min的升温速度将坯体由室温加热至1200℃，然后再以10℃/min的升温速度将坯体继续加热至1500-1600℃，接着使坯体在1500-1600℃下保温1-4h。
与现有技术相比，本发明的有益效果是：本发明通过向α-Al2O3中添加适量的SiO2、MgO和CaO，可显著提高所制备的96氧化铝陶瓷的绝缘性能、介电强度、力学性能及导热性。通过控制工艺可制备性能稳定的96氧化铝陶瓷，所制备的96氧化铝陶瓷在室温及25％湿度环境中的体积电阻率可高达7×1014Ω·cm，在室温及70％湿度环境中其体积电阻率仍可保持在1012的数量级以上，当温度为600℃时其体积电阻率还能达到108数量级以上；室温条件下96氧化铝陶瓷的介电强度高达30kV/mm，抗弯强度高达约400MPa，维氏硬度高达14GPa。
尤其是采用无水乙醇作为分散剂使混合物在超声下分散，超声过程中无水乙醇不断挥发使混合物悬浮液逐渐变粘稠，超声至混合物不能流动，至此可将各组分分散均匀，为96氧化铝陶瓷提供有保障的混合粉体。将烧结温度控制在1500-1600℃的范围内可保障96氧化铝陶瓷的致密度，若烧结温度低于1500℃会导致96氧化铝陶瓷的致密度达不到要求，而当烧结温度大于1600℃时因材料中的晶体生长过大，导致96氧化铝陶瓷各方面的性能均有所下降。
附图说明
图1为实施例4制备高性能96氧化铝陶瓷的工艺流程图；
图2为实施例4制备高性能96氧化铝陶瓷的烧结曲线图；
图3为实施例4制备的高性能96氧化铝陶瓷的体积电阻率在室温下(25℃)随环境湿度变化的曲线图；
图4为实施例4制备的高性能96氧化铝陶瓷的体积电阻率随温度变化的曲线图。
具体实施方式
为了更充分的理解本发明的技术内容，下面结合具体实施例对本发明的技术方案作进一步介绍和说明。
实施例1-23
实施例1-23提供一种高性能96氧化铝陶瓷以及该种96氧化铝陶瓷的制备方法。具体制备步骤如下(实施例4的工艺流程如图1所示)：
(1)配料
按各组分的质量百分比分别称取一定量的α-Al2O3、SiO2、MgO和CaO，各物质的具体质量百分比如下表1所示。
(2)制混合粉体
将α-Al2O3、SiO2、MgO、CaO和无水乙醇分散剂加入到大功率超声分散仪中进行超声分散，在超声分散的过程中无水乙醇缓慢被挥发掉，混合悬浮液的粘稠度逐渐增大，直至混合物无法流动时停止超声，得到分散体。然后对分散体依次进行干燥处理和研磨处理，所得粉体过100目筛，得到混合粉体。
(3)成型
首先将混合粉体倒入50mm×50mm×8mm的方形钢模中进行干压成型，压力为10MPa，保压时间为60s，获得方形的坯体；坯体再经冷等静压成型，压力为200MPa，时间300s。
(4)烧结
将坯体置于烧结炉中，并在空气中以无压烧结的方式烧结坯体。烧结的控温方式如下：以20℃/min的升温速度(一阶升温速度)将坯体由室温加热至1200℃(一阶温度)，然后再以10℃/min的升温速度(二阶升温速度)将坯体继续加热至1600℃(保温温度)，接着使坯体在1600℃下保温1h(保温时间)，制得96氧化铝陶瓷。实施例4制备高性能96氧化铝陶瓷的烧结曲线如图2所示。实施例1-23制备的96氧化铝陶瓷分别记为TC1-TC23。
表1 实施例1-23中各组分的质量百分比
实施例24-37
实施例24-37提供一种高性能96氧化铝陶瓷以及该种96氧化铝陶瓷的制备方法。实施例24-37中α-Al2O3、SiO2、MgO和CaO的质量百分比及制混合粉体步骤、成型步骤、烧结方式均与实施例4的一致，不同之处在于烧结步骤中的控温方式，具体的烧结控温方式如下表2所示。实施例24-37制备的96氧化铝陶瓷分别记为TC24-TC37。
表2 实施例24-37中具体的烧结控温方式
分别测试实施例1-37制备的96氧化铝陶瓷TC1-TC37在室温/环境湿度25％、室温/环境湿度70％、600℃(完全干燥)下的体积电阻率，室温下TC1-TC37的介电强度、抗弯强度、维氏硬度，以及TC1-TC37的热膨胀系数和热导率。具体测试结果如下表3所示。
表3 实施例1-37制备的96氧化铝陶瓷TC1-TC37的各性能参数
实施例4制备的高性能96氧化铝陶瓷的体积电阻率随环境湿度变化的曲线如图3所示；图4为实施例4制备的高性能96氧化铝陶瓷的体积电阻率随温度变化的曲线如图4所示。从上述实施例的制备步骤、图3和图4以及表3中96氧化铝陶瓷的性能数据可知，通过向α-Al2O3中添加适量的SiO2、MgO和CaO以及控制制备工艺的各参数，可显著提高所制备的96氧化铝陶瓷的绝缘性能、介电强度、力学性能及导热性。
采用无水乙醇作为分散剂使混合物在超声下分散，超声过程中无水乙醇不断挥发使混合物悬浮液逐渐变粘稠，超声至混合物不能流动，至此可将各组分分散均匀，为96氧化铝陶瓷提供有保障的混合粉体。
将烧结温度控制在1500-1600℃的范围内可保障96氧化铝陶瓷的致密度，若烧结温度低于1500℃会导致96氧化铝陶瓷的致密度达不到要求，而当烧结温度大于1600℃时因材料中的晶体生长过大，导致96氧化铝陶瓷各方面的性能均有所下降。
以上所述仅以实施例来进一步说明本发明的技术内容，以便于读者更容易理解，但不代表本发明的实施方式仅限于此，任何依本发明所做的技术延伸或再创造，均受本发明的保护。
Claims (8)
1.一种高性能96氧化铝陶瓷，其特征在于，由以下质量百分比的各组分制备而成：96％的α-Al2O3，0.1-1.5％的MgO，0.01-0.5％的CaO，余量为SiO2。
2.根据权利要求1所述一种高性能96氧化铝陶瓷，其特征在于，由以下质量百分比的各组分制备而成：96％的α-Al2O3，2.75％的SiO2，1％的MgO，0.25％的CaO。
3.一种如权利要求1所述高性能96氧化铝陶瓷的制备方法，其特征在于，包括以下步骤：
S1制混合粉体：按各组分配比分别称取α-Al2O3、SiO2、MgO和CaO，然后将各组分混合在一起并分散均匀，得到混合粉体；
S2成型：将混合粉体模压成坯体；
S3烧结：将坯体置于烧结炉中烧结，制得氧化铝陶瓷。
4.根据权利要求3所述一种高性能96氧化铝陶瓷的制备方法，其特征在于，步骤S1中，将α-Al2O3、SiO2、MgO和CaO置于无水乙醇中并超声分散至混合物的粘稠度增大到该混合物无法流动，得到分散体；然后干燥分散体，得到混合粉体。
5.根据权利要求4所述一种高性能96氧化铝陶瓷的制备方法，其特征在于，步骤S1中，干燥分散体得到混合粉体后，还包括以下步骤：研磨混合粉体并使混合粉体过100目筛。
6.根据权利要求3所述一种高性能96氧化铝陶瓷的制备方法，其特征在于，步骤S2中，以干压与冷等静压相结合的方式在10-500MPa下将混合粉体模压成坯体。
7.根据权利要求3所述一种高性能96氧化铝陶瓷的制备方法，其特征在于，步骤S3中，在空气中以无压烧结的方式烧结坯体，烧结温度为1500-1600℃，保温时间为1-4h。
8.根据权利要求7所述一种高性能96氧化铝陶瓷的制备方法，其特征在于，步骤S3中，将坯体置于烧结炉中，以20℃/min的升温速度将坯体由室温加热至1200℃，然后再以10℃/min的升温速度将坯体继续加热至1500-1600℃，接着坯体在1500-1600℃下保温1-4h。
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