CN116283251A - 一种氧化铝陶瓷及其制备方法与应用 - Google Patents

一种氧化铝陶瓷及其制备方法与应用 Download PDF

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CN116283251A
CN116283251A CN202310288229.9A CN202310288229A CN116283251A CN 116283251 A CN116283251 A CN 116283251A CN 202310288229 A CN202310288229 A CN 202310288229A CN 116283251 A CN116283251 A CN 116283251A
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alumina ceramic
alumina
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rare earth
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CN116283251B (zh
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邱基华
陈烁烁
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Guangdong Advanced Ceramic Material Technology Co ltd
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Abstract

本发明公开了一种氧化铝陶瓷及其制备方法与应用，涉及陶瓷材料技术领域。本发明所述氧化铝陶瓷包含如下重量份的制备原料：氧化铝粉体96～99份、SiO20.25～1.2份、SrF20.13～0.45份、LiF 0.52～1.8份、稀土氧化物0.1～0.55份；所述氧化铝粉体为η‑Al2O3。本发明通过选用SiO2、SrF2、LiF作为助烧剂，选用稀土氧化物作为晶粒抑制剂，从根本上解决了氧化铝陶瓷烧结温度高且容易异常生长的问题。

Description

一种氧化铝陶瓷及其制备方法与应用
技术领域
本发明涉及陶瓷材料技术领域，尤其涉及一种氧化铝陶瓷及其制备方法与应用。
背景技术
氧化铝陶瓷具有机械强度高、硬度高、高温绝缘性能好、耐腐蚀等特性，广泛应用于机械、电子及化学工程等领域。然而，对于单相氧化铝陶瓷，熔点高达2050℃，材料以离子键或共价键的方式结合，质点扩散系数小，烧结温度超过1750℃，且需要的烧结时间长，生产效率低，成本高。此外，在高温烧结的过程中容易出现生长各向异性和异常晶粒，导致结构不均匀，甚至出现内部存在残余孔隙，降低了晶粒间的结合强度，导致材料性能大幅度下降。因此，以简单可靠、低成本的方式制备高密度的氧化铝陶瓷仍然是一个巨大的挑战。
目前主要有三种方法用于降低氧化铝陶瓷的烧结温度：(1)调控粒径：通过减小氧化铝粉末的粒度，如使用纳米级陶瓷粉末来减小晶粒的起始尺寸，使最终的烧结产物保持微晶特性，并且基于其高比表面等独特纳米级效应，显著提高了陶瓷基板的烧结活性。(2)采用其他先进烧结技术：如热等静压烧结、放电等离子烧结、脉冲电流烧结或微波烧结，可以在更短的时间内增加烧结驱动力并实现致密化。(3)加入烧结助剂：烧结助剂可以通过与氧化铝形成固溶体，增加晶格畸变，提高扩散速率，从而降低氧化铝陶瓷的烧结温度，常见的有MnO2、TiO2、Fe2O3等，它们具有与氧化铝相似的晶格常数，可以与氧化铝形成不同类型的固溶体。此外，添加剂本身或添加剂与氧化铝基体之间在高温下可以形成液相，通过溶解-沉淀机制促进烧结，即当烧结温度达到添加剂熔点或共溶温度时，开始出现液相，促进了烧结体中质点的迁移、扩散，改善了氧化铝陶瓷烧结性能。
但是，使用纳米级氧化铝粉价格昂贵，生产成本较高；特殊工艺所需条件复杂且生产效率低，存在无法大批量生产、成本高等问题；常见的烧结助剂使得烧结温度降至1500～1700℃，仍存在较大的提升空间，且如TiO2等烧结助剂的添加促进了具有大纵横比的各向异性晶粒的形成，显著影响氧化铝陶瓷的微观结构，并导致陶瓷本身具有各向异性，使用方式限制较大。
发明内容
本发明的目的在于克服上述现有技术的不足之处而提供一种氧化铝陶瓷及其制备方法与应用，所述氧化铝陶瓷的烧结温度低，具有良好的力学性能，电阻率低，导热率高。
为实现上述目的，本发明所采取的技术方案为：
一种氧化铝陶瓷，所述氧化铝陶瓷包含如下重量份的制备原料：氧化铝粉体96～99份、SiO2 0.25～1.2份、SrF2 0.13～0.45份、LiF 0.52～1.8份、稀土氧化物0.1～0.55份；所述氧化铝粉体为η-Al2O3。
选用η-Al2O3作为氧化铝粉体，在煅烧时发生两次晶型转变释放的能量有利于降低氧化铝陶瓷的烧结温度。SiO2可以在氧化铝陶瓷烧结过程中形成低熔点的玻璃相，通过液相烧结机理促进致密化过程；但是，过量的SiO2会形成大量的玻璃相，会促进晶粒的异常生长，选用SiO2、SrF2、LiF作为助烧剂，三者复配不仅可以提高烧结致密度，还可以避免传统TiO2等助烧剂在烧结过程中容易使氧化铝陶瓷具有取向的问题，使晶粒趋于生长为等轴晶，可以应用于更广的领域中；选用稀土氧化物作为晶粒抑制剂，可以抑制晶粒异常长大，保证所述氧化铝陶瓷具有较高的密度、强度，以及导热性。
优选地，所述SrF2和LiF的质量比为(1～1.2):(4～4.2)，当两者的配比满足上述限定时可以制备出SrF2-4LiF二元共晶氟化物，大幅度降低烧结温度。
优选地，所述SiO2和稀土氧化物的质量比为1：(0.1～1.5)。实验发现，两者的质量比过高，对晶粒生长的抑制效果会减少，晶粒尺寸增大，成瓷强度较低，过低则会导致无法与SrF2、LiF生成低熔点的玻璃相，对降低烧结温度的作用不大。
进一步优选地，所述SiO2和稀土氧化物的质量比为1：(0.2～0.6)。当二者的配比满足上述限定时，制备得到的氧化铝陶瓷具有较高的密度、强度以及导热性。
优选地，所述稀土氧化物为La2O3、Sm2O3、CeO2、Gd2O3、Dy2O3中至少一种。稀土氧化物具有较高的化学活性，是良好的表面活性物质，加入上述物质可以改变氧化铝的润湿性，还会在晶粒交界处产生第二相，对晶界产生钉扎作用，降低晶界迁移速率，从而降低晶粒尺寸，晶粒内的孔隙得以沿晶界扩散而逸出，从而提高氧化铝陶瓷的相对密度及强度。
优选地，所述氧化铝粉体为亚微米级粉体。本发明通过对氧化铝陶瓷的组分进行筛选，使得采用价格低廉的亚微米级氧化铝粉体也可以制备出具有良好的综合性能的氧化铝陶瓷，生产成本更低。
与此同时，本发明还公开了一种所述氧化铝陶瓷的制备方法，所述制备方法包括如下步骤：
(1)按配比称取所述制备原料，得到混合物；
(2)将所述混合物与溶剂混合，球磨、干燥，得到混合均匀的粉体；
(3)将所述粉体与分散剂、粘结剂、增塑剂、溶剂混合，球磨，得到浆料；
(4)将所述浆料流延成型，得到生坯片；
(5)将所述生坯片进行排胶与烧结，得到所述氧化铝陶瓷。
优选地，所述分散剂为聚乙二醇、聚丙烯酰胺中的至少一种；所述粘结剂为有机丙烯酸类共聚物；所述增塑剂为邻苯二甲酸辛酯、聚乙二醇、二丁基邻苯二甲酸酯中的至少一种；所述溶剂为无水乙醇、丙酮、三氯乙烯中的至少一种。
优选地，所述排胶的条件为：以2～4℃/min的速率升温至350～400℃，保温2～4h；所述烧结的条件为：待排胶结束后，以5～7℃/min的速率升温至1350～1450℃，保温10～15h，得到所述氧化铝陶瓷。
此外，本发明还公开了所述氧化铝陶瓷在电子电器领域中的应用，如陶瓷基板、手机背板等。
相比于现有技术，本发明的有益效果为：
本发明通过选用η-Al2O3为陶瓷主体材料，解决了现有技术中使用纳米级氧化铝粉体价格高以及其他晶型氧化铝粉体烧结活性低的问题；在煅烧时发生两次晶型转变释放的能量有利于降低氧化铝陶瓷的烧结温度。此外，本发明选用SiO2、SrF2、LiF作为助烧剂，有助于等轴晶的形成，可获得各向同性的氧化铝晶相，扩大所述氧化铝陶瓷的应用范围。
具体实施方式
为更好地说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
实施例1～15
本发明所述氧化铝陶瓷的实施例，实施例1～15的部分制备原料如表1所示，制备方法如下：
(1)按配比称取所述制备原料，得到混合物；
(2)将所述混合物与溶剂混合，加入球磨机中进行混合，球磨混合时间为8h，干燥后得到混合均匀的粉体；所述混合物与所述溶剂的质量比为3:10；
(3)将所述粉体与分散剂聚乙二醇、粘结剂丙烯酸酯、增塑剂邻苯二甲酸辛酯、溶剂混合，在球磨罐中进行匀浆处理，球磨分散25h，得到浆料；所述溶剂为无水乙醇、丙酮、三氯乙烯质量比为3:1:1的混合物，所述粉体与分散剂、粘结剂、增塑剂、溶剂的质量比为10:0.3:0.8:0.2:3；
(4)将所述浆料流延成型，得到生坯片；
(5)将所述生坯片进行排胶与烧结，得到所述氧化铝陶瓷；排胶条件为：以3℃/min的速率升温至375℃，保温3h进行排胶，然后以6℃/min的速率升温至1400℃，保温10h，得到所述氧化铝陶瓷。
对比例1～5
对比例1～5为氧化铝陶瓷，对比例1～5的组分如表1所示，制备方法与实施例1相同。
对比例6
对比例6为氧化铝陶瓷，其与实施例1的区别仅在于，以NaF替代LiF。
表1(重量份)
Figure BDA0004140430820000041
Figure BDA0004140430820000051
对实施例和对比例进行性能测试，性能测试指标如表2所示，测试结果如表3所示。
表2
Figure BDA0004140430820000052
Figure BDA0004140430820000061
表3
Figure BDA0004140430820000062
由上述测试结果可知，实施例1～15所述氧化铝陶瓷的晶粒尺寸均小于2μm，气孔率低于1.5％，具有较高的密度(≥3.7g/cm3)以及良好的抗弯强度(≥450MPa)，体积电阻率≥1014Ω·cm(25℃)，并且导热率≥21W/(m·K)(25℃)，具有良好的综合性能，适合应用于电子电器领域中，如制备陶瓷基板等。
对比例1使用的氧化铝粉末的晶型与本发明不同，其气孔率、密度、强度、体积电阻率以及热导率均无法达到本领域的基本要求。对比例2所述氧化铝陶瓷在制备过程中未添加SiO2，其气孔率较高，综合性能较差。对比例3中未使用稀土氧化物，制备出的晶粒尺寸较大，所述氧化铝陶瓷的强度较低，无法达到本领域的一般要求。对比例4～5中分别未添加SrF2和LiF，制备出的氧化铝陶瓷的密度、气孔率、强度、体积电阻率和导热率都极差。对比例6中以NaF替代LiF，制备的氧化铝陶瓷的性能也无法达到本领域的一般要求。
此外，对比实施例1、实施例5～10的配方及测试结果可以发现，实施例1、实施例7～9的综合性能相对较差，该结果表明，SiO2和稀土氧化物的质量比为1：(0.1～1.5)时，制备的氧化铝陶瓷虽然都能满足电子电器领域陶瓷材料的基本要求，但当两者的配比为1：(0.2～0.6)时，制备的材料具有更优的综合性能，应用范围更广。
另外，由实施例11～14的测试结果可以发现，使用亚微米级的η-Al2O3也可以降低烧结温度(＜1500℃)，制备出兼具良好的致密度和强度的氧化铝陶瓷，成本较低。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，但并不脱离本发明技术方案的实质和范围。

Claims (10)

1.一种氧化铝陶瓷，其特征在于，包含如下重量份的制备原料：氧化铝粉体96～99份、SiO2 0.25～1.2份、SrF2 0.13～0.45份、LiF 0.52～1.8份、稀土氧化物0.1～0.55份；所述氧化铝粉体为η-Al2O3。
2.如权利要求1所述氧化铝陶瓷，其特征在于，所述SrF2和LiF的质量比为(1～1.2):(4～4.2)。
3.如权利要求1所述氧化铝陶瓷，其特征在于，所述SiO2和稀土氧化物的质量比为1：(0.1～1.5)。
4.如权利要求3所述氧化铝陶瓷，其特征在于，所述SiO2和稀土氧化物的质量比为1：(0.2～0.6)。
5.如权利要求1所述氧化铝陶瓷，其特征在于，所述稀土氧化物为La2O3、Sm2O3、CeO2、Gd2O3、Dy2O3中至少一种。
6.如权利要求1所述氧化铝陶瓷，其特征在于，所述氧化铝粉体为亚微米级粉体。
7.一种如权利要求1～6任一项所述氧化铝陶瓷的制备方法，其特征在于，包括如下步骤：
(1)按配比称取所述制备原料，得到混合物；
(2)将所述混合物与溶剂混合，球磨、干燥，得到混合均匀的粉体；
(3)将所述粉体与分散剂、粘结剂、增塑剂、溶剂混合，球磨，得到浆料；
(4)将所述浆料流延成型，得到生坯片；
(5)将所述生坯片进行排胶与烧结，得到所述氧化铝陶瓷。
8.如权利要求7所述制备方法，其特征在于，所述分散剂为聚乙二醇、聚丙烯酰胺中的至少一种；所述粘结剂为有机丙烯酸类共聚物；所述增塑剂为邻苯二甲酸辛酯、聚乙二醇、二丁基邻苯二甲酸酯中的至少一种；所述溶剂为无水乙醇、丙酮、三氯乙烯中的至少一种。
9.如权利要求7所述制备方法，其特征在于，所述排胶的条件为：以2～4℃/min的速率升温至350～400℃，保温2～4h；所述烧结的条件为：待排胶结束后，以5～7℃/min的速率升温至1350～1450℃，保温10～15h，得到所述氧化铝陶瓷。
10.一种如权利要求1～6任一项所述氧化铝陶瓷在电子电器领域中的应用。
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