CN105622071A - 一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用 - Google Patents

一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用 Download PDF

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CN105622071A
CN105622071A CN201510975607.6A CN201510975607A CN105622071A CN 105622071 A CN105622071 A CN 105622071A CN 201510975607 A CN201510975607 A CN 201510975607A CN 105622071 A CN105622071 A CN 105622071A
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张立
焦秀玲
陈代荣
张建
韩颖
刘洋
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Abstract

本发明涉及一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用，该α-A12O3陶瓷颗粒，由磁铅石片晶和氧化铝晶体组成，并且磁铅石片晶穿插于氧化铝晶体中。具体制备方法为：1)将低成本的工业级拟薄水铝石分散成浆液，然后加入酸及添加剂水溶液，搅拌均匀；2)将浆液在180～240℃下水热处理24～72h得凝胶；3)将凝胶干燥，粉碎、筛分成不同粒度的半成品；4)将半成品在真空状态下缓慢升温到1500～1600℃，在目标温度下保温2～4h，即得。本发明的含有片状微晶的α-A12O3陶瓷颗粒韧性好，一次晶体形貌可控性好，有优异的磨削性能，陶瓷颗粒硬度值大于20GPa，球磨韧性大于76％。

Description

一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用
技术领域
本发明涉及一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用，属于无机非金属材料领域。
背景技术
氧化铝陶瓷是以α-A12O3为主晶相的陶瓷材料，具有机械强度高、硬度大、熔点高、电阻率高、绝缘性好、热膨胀系数小且耐磨性、耐腐蚀性能好等优点，广泛应用于机械、电子、电力、化工、医学、建筑以及其它的高科技领域(参见：新材料产业2006,12,17)，但是氧化铝陶瓷有弱点，即断裂韧性低。氧化铝微晶陶瓷的晶粒、晶界都是纳米数量级，晶界数量大，因此氧化铝微晶陶瓷不仅具有氧化铝陶瓷的一系列优点，而且具有强度高、韧性好和超塑性等优异性能。因此制备硬度高、韧性好的氧化铝微晶陶瓷受到广泛关注(参见：NanoLett.2007,7,3196)。某些稀土氧化物与二价金属阳离子同氧化铝会在烧结过程中反应生成六方稀土铝酸盐，用化学式表示是LnMAl11O19，式中：Ln是一种镧系稀土离子，如La3+、Nd3+、Ce3+、Pr3+、Sm3+、Gd3+、Eu3+；M是一种两价金属阳离子，如Mg2+、Mn2+、Zn2+、Ni2+、Co2+，这类六方稀土铝酸盐具有磁铅石型结构。磁铅石型六铝酸盐结构和β-Al2O3很相近，都属于空间群P63/mmc，是由互成镜像的氧化铝尖晶石结构单元和M离子形成的镜面层交替堆积而成的层状结构，允许各种取代，如La1-xSrxMgAl11-xTixO19(参见：J.Am.Ceram.Soc.2013,96,1063)。两者的区别主要在镜面层上：磁铅石型结构中的镜面层由一个M、一个Al和三个O组成，而β-Al2O3型结构中的镜面层仅由一个M和一个O组成。磁铅石型六铝酸盐显微结构通常呈片晶状，一般长约0.5～3μm，厚约0.05～0.1μm，片状形貌为六铝酸盐的特征微观结构的宏观反映。经研究发现，这种片晶的引入，使得氧化铝微晶陶瓷颗粒表现出一系列的优异性能，而这种片晶可改善陶瓷颗粒的韧性，纳米片可增强陶瓷纳米颗粒中的晶间结构，使得陶瓷颗粒具有优异的性能。这是因为片状纳米结构可增强晶间结构而引起穿晶断裂，使主要的断裂方式不会延伸到晶界，而进入到基体晶粒。在基体晶粒中，片状纳米结构可使断裂方式偏转，使断裂途径延伸且更加曲折，并且阻碍其它地方的断裂，导致消耗更大的断裂能；因而能增强陶瓷颗粒的强度和韧性(参见：J.Ceram.Soc.Jpn.1990,25,17)。
中国专利文件CN1772695A(申请号：200510112725.0)公开了一种微晶氧化铝陶瓷颗粒的制备方法，其特征在于其制备过程是采用超细氢氧化铝为起始原料，制备出的α-氧化铝，再与氢氧化铝和拟薄水铝石混合研磨，配制成悬浮液，制备成凝胶体干燥、破碎后，在1250～1650℃的温度下烧结，破碎、筛分，制得微晶氧化铝陶瓷颗粒。采用该方法制备的氧化铝陶瓷颗粒相对于白刚玉、棕刚玉等传统氧化铝基磨粒而言，具有硬度高，韧性好，耐磨性好等优点，一次结晶颗粒粒径为200nm～2μm，由这种磨料所制备的磨具的耐用性大大提高。
但是，上述微晶氧化铝陶瓷颗粒的制备方法中主要原材料为超细氢氧化铝和拟薄水铝石两种，其中超细氢氧化铝制备成本较高，需经过特殊的研磨工艺才能得到；此外，还需要首先制备α-氧化铝，这样在整个工艺过程中就存在两个煅烧步骤，而且还需要两次长时间的研磨，工艺步骤繁琐冗长。所制备的微晶氧化铝陶瓷颗粒尺寸可控性差，形貌为类多面体状。
目前，磁铅石型六铝酸盐多采用固相法合成，烧成温度一般在1600℃，也有一些用微浮液方法合成前驱体在1400℃可以烧成，但是制备方法本身存在局限性，很难实现工业化生产。
发明内容
针对现有技术的不足，本发明提供一种含有片状微晶的α-A12O3陶瓷颗粒及其制备方法和应用。以低成本的工业级拟薄水铝石作原料，采用水热法制备出半成品，然后在较低温度下烧成了一种α-A12O3微晶陶瓷颗粒，这种α-A12O3微晶陶瓷颗粒具有独特的片状结构，含有片状微晶；陶瓷颗粒微观结构致密，硬度值>18GPa，球磨韧性>70％。
本发明的技术方案如下：
一种含有片状微晶的α-A12O3陶瓷颗粒，由磁铅石片晶和氧化铝晶体组成，并且磁铅石片晶穿插于氧化铝晶体中。
根据本发明，优选的，所述的磁铅石片晶的化学组成为LnMeAl11O19，其中：Ln为镧系元素；Me为Mg、Mn、Fe、Co。
根据本发明，优选的，所述的含有片状微晶的α-A12O3陶瓷颗粒中，磁铅石片晶占氧化铝晶体的5～20％，进一步优选8～12％，质量百分比。磁铅石片晶的含量通过调整添加剂的量进行控制。在上述范围内α-A12O3陶瓷颗粒性能最佳。
根据本发明，优选的，所述的磁铅石片晶的厚度为100～200nm，长度为1～2μm。
根据本发明，上述含有片状微晶的α-A12O3陶瓷颗粒的制备方法，包括以下步骤：
(1)将拟薄水铝石分散于水中，制得均匀的拟薄水铝石悬浮液；然后在拟薄水铝石悬浮液中加入添加剂水溶液和酸液，混合分散均匀，得浆液；
所述添加剂为稀土金属氧化物、过渡金属氧化物、碱土金属氧化物、稀土金属硝酸盐、过渡金属硝酸盐、碱土金属硝酸盐中的两种以上混合；
(2)将步骤(1)得到的浆液在180～240℃下水热反应24～72h，得到凝胶；
(3)将步骤(2)得到的凝胶干燥、粉碎后，筛分，取120目筛以上的颗粒；在真空状态下升温到1500～1600℃，保温2～4h，即得含有片状微晶的α-A12O3陶瓷颗粒。
根据本发明的制备方法，优选的，步骤(1)拟薄水铝石悬浮液中，拟薄水铝石占悬浮液总质量的10～25％。
根据本发明的制备方法，优选的，步骤(1)中所述的稀土金属为镧系元素，进一步优选La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm或/和Yb，最优选La或/和Nd；
优选的，所述的过渡金属为Mn、Fe或/和Co，进一步优选Mn或/和Co；
优选的，所述的碱土金属为镁。
根据本发明的制备方法，优选的，步骤(1)中所述的酸液为硝酸、盐酸或醋酸；进一步优选硝酸。
根据本发明的制备方法，优选的，步骤(1)中添加剂的加入量控制在最终产物中磁铅石型六铝酸盐占氧化铝晶体的5～20％，进一步优选8～12％，质量百分比；酸液的加入量为拟薄水铝石的1～6％，质量百分比。
根据本发明的制备方法，优选的，步骤(2)中水热反应的温度为200～220℃。
根据本发明的制备方法，优选的，步骤(3)中在真空状态下升温到1500～1600℃的升温速率为1～5℃/min；
优选的，真空状态下的真空度为-0.05～-0.09MPa。
根据本发明，所述的含有片状微晶的α-A12O3陶瓷颗粒作为磨料在研磨材料中的应用。
根据本发明，所述的含有片状微晶的α-A12O3陶瓷颗粒在研磨材料方面有较好的应用效果，尤其作为磨料应用于固结及涂附磨具领域时，展现了优异的磨削性能，主要体现在磨削精度高，磨削阻力小，可以实现大进给磨削。
本发明的有益效果：
1、本发明的含有片状微晶的α-A12O3陶瓷颗粒韧性更好，一次晶体形貌可控性好，具有优异的磨削性能，对难磨削的材料具有更好的磨削效果，且磨削进给量可以大大提高。
2、本发明采用水热法与溶胶凝胶相结合的方法，制备前驱体，磁铅石型六铝酸盐是在煅烧过程中与α-A12O3同进形成的，煅烧温度较低，工业化前景较好。
3、本发明所采用的原材料单一，且为常规工业品，成本较低，而且工艺过程中不需要长时间的研磨，制备方法简单易控。
附图说明
图1为本发明实施例1所得的含有片状微晶的α-A12O3陶瓷颗粒的表面结构扫描电镜图。
图2为本发明实施例1所得的含有片状微晶的α-A12O3陶瓷颗粒的断面结构扫描电镜图。
具体实施方式
下面通过具体实施例并结合附图对本发明作进一步说明，但不限于此。
实施例中所用原料均为常规原料，市购产品。
本发明以简单稳定的工艺制得了一种含有片状微晶的α-A12O3陶瓷颗粒，表面是磁铅石片晶穿插于氧化铝晶体中，附图1；断面致密无孔，附图2。
实施例1、含有片状微晶的α-A12O3陶瓷颗粒的制备
(1)将200.0g拟薄水铝石滤饼加入2.0kg去离子水中，搅拌分散成拟薄水铝石悬浮液；将8.0g六水合硝酸镧、5.0g六水合硝酸镁、0.1g六水合硝酸钴和10.0g硝酸(65wt％)加入200.0g去离子水中制得溶液；将得到的水溶液加到拟薄水铝石悬浮液中，混合分散均匀，得浆液；
(2)将步骤(1)得到的浆液在200℃下水热反应36h，得到凝胶；
(3)将步骤(2)得到的凝胶在80℃的烘箱中干燥得到干凝胶颗粒，用万能粉碎机粉碎，过筛，得120目以上的颗粒，在真空状态下(-0.05MPa)以2.0℃/min的速度缓慢升温到1500℃，在目标温度下保温3h，即得含有片状微晶的α-A12O3陶瓷颗粒。
对本实施例制得的含有片状微晶的α-A12O3陶瓷颗粒进行电镜扫描，如图1、2所示；由图1可知，所得α-A12O3陶瓷颗粒表面是磁铅石片晶穿插于氧化铝晶体中，磁铅石片晶的厚度为100～200nm，长度为1～2μm。磁铅石片晶的化学组成为LaMg1-xCoxAl11O19(0.01≤x≤0.02)。由图2可知，所得含有片状微晶的α-A12O3陶瓷颗粒断面致密无孔，硬度为20GPa，球磨韧性为79％。
实施例2、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(3)将凝胶在80℃干燥得到干凝胶颗粒，用万能粉碎机粉碎，过筛得120目以上的颗粒，在真空状态下以2.0℃/min的速度缓慢升温到1600℃，在目标温度下保温3h，即可得到含有片状微晶的α-A12O3陶瓷颗粒。
所得的α-A12O3微晶陶瓷颗粒的硬度为19.5GPa，球磨韧性为75％。
实施例3、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(3)将凝胶在80℃干燥得到干凝胶颗粒，用万能粉碎机粉碎，过筛得120目以上的颗粒，在真空状态下以2.0℃/min的速度缓慢升温到1450℃，在目标温度下保温3h，即可得到含有片状微晶的α-A12O3陶瓷颗粒。
所得的α-A12O3微晶陶瓷颗粒的硬度为18.5GPa，球磨韧性为78％。
实施例4、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(1)中的添加剂为12.0g六水合硝酸镧、6.0g六水合硝酸镁、0.5g六水合硝酸钴，酸为5.0g硝酸(65wt％)，加入200.0g去离子水溶解得水溶液。
所得的α-A12O3微晶陶瓷颗粒的硬度为21GPa，球磨韧性为77％。
实施例5、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例4所述，所不同的是将步骤(2)将凝胶在80℃干燥得到干凝胶颗粒，用万能粉碎机粉碎，过筛得120目以上的颗粒，在真空状态下以5.0℃/min的速度缓慢升温到1500℃，在目标温度下保温3h，即可得到含有片状微晶的α-A12O3陶瓷颗粒。
所得的α-A12O3陶瓷颗粒的硬度为20.5GPa，球磨韧性为71％。
实施例6、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例4所述，所不同的是步骤(2)将凝胶在80℃干燥得到干凝胶颗粒，用万能粉碎机粉碎，过筛得120目以上的颗粒，在真空状态下以5.0℃/min的速度缓慢升温到1600℃，在目标温度下保温3h，即可得到含有片状微晶的α-A12O3陶瓷颗粒。
所得的α-A12O3陶瓷颗粒的硬度为22GPa，球磨韧性为76％。
实施例7、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(1)将200.0g拟薄水铝石滤饼加入2.0kg去离子水中，搅拌分散成拟薄水铝石悬浮液；将8.0g六水合硝酸钕、5.0g六水合硝酸镁和10.0g硝酸(65wt％)加入200.0g去离子水中制得溶液；将得到的水溶液加到拟薄水铝石悬浮液中，混合分散均匀，得浆液；
所得的α-A12O3陶瓷颗粒的硬度为20.5GPa，球磨韧性为78.5％。
实施例8、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(1)将200.0g拟薄水铝石滤饼加入2.0kg去离子水中，搅拌分散成拟薄水铝石悬浮液；将4.0g六水合硝酸钕、4.0g六水合硝酸镧、5.0g六水合硝酸镁和10.0g硝酸(65wt％)加入200.0g去离子水中制得溶液；将得到的水溶液加到拟薄水铝石悬浮液中，混合分散均匀，得浆液；
所得的α-A12O3陶瓷颗粒的硬度为20GPa，球磨韧性为80％。
实施例9、含有片状微晶的α-A12O3陶瓷颗粒的制备
如实施例1所述，所不同的是步骤(1)将200.0g拟薄水铝石滤饼加入2.0kg去离子水中，搅拌分散成拟薄水铝石悬浮液；将8.0g六水合硝酸镧、5.0g六水合硝酸钴和10.0g硝酸(65wt％)加入200.0g去离子水中制得溶液；将得到的水溶液加到拟薄水铝石悬浮液中，混合分散均匀，得浆液；
所得的α-A12O3陶瓷颗粒的硬度为18.5GPa，球磨韧性为72％。

Claims (10)

1.一种含有片状微晶的α-A12O3陶瓷颗粒，其特征在于，该陶瓷颗粒由磁铅石片晶和氧化铝晶体组成，并且磁铅石片晶穿插于氧化铝晶体中。
2.根据权利要求1所述的含有片状微晶的α-A12O3陶瓷颗粒，其特征在于，所述的磁铅石片晶的化学组成为LnMeAl11O19，其中：Ln为镧系元素；Me为Mg、Mn、Fe、Co。
3.根据权利要求1所述的含有片状微晶的α-A12O3陶瓷颗粒，其特征在于，所述的含有片状微晶的α-A12O3陶瓷颗粒中，磁铅石片晶占氧化铝晶体的5～20％，优选8～12％，质量百分比。
4.根据权利要求1所述的含有片状微晶的α-A12O3陶瓷颗粒，其特征在于，所述的磁铅石片晶的厚度为100～200nm，长度为1～2μm。
5.一种权利要求1-4任一项所述的含有片状微晶的α-A12O3陶瓷颗粒的制备方法，包括以下步骤：
(1)将拟薄水铝石分散于水中，制得均匀的拟薄水铝石悬浮液；然后在拟薄水铝石悬浮液中加入添加剂水溶液和酸液，混合分散均匀，得浆液；
所述添加剂为稀土金属氧化物、过渡金属氧化物、碱土金属氧化物、稀土金属硝酸盐、过渡金属硝酸盐、碱土金属硝酸盐中的两种以上混合；
(2)将步骤(1)得到的浆液在180～240℃下水热反应24～72h，得到凝胶；
(3)将步骤(2)得到的凝胶干燥、粉碎后，筛分，取120目筛以上的颗粒；在真空状态下升温到1500～1600℃，保温2～4h，即得含有片状微晶的α-A12O3陶瓷颗粒。
6.根据权利要求5所述的制备方法，其特征在于，步骤(1)拟薄水铝石悬浮液中，拟薄水铝石占悬浮液总质量的10～25％。
7.根据权利要求5所述的制备方法，其特征在于，步骤(1)中所述的稀土金属为镧系元素，优选La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm或/和Yb，
所述的过渡金属为Mn、Fe或/和Co，
所述的碱土金属为镁。
8.根据权利要求5所述的制备方法，其特征在于，步骤(1)中所述的酸液为硝酸、盐酸或醋酸。
9.根据权利要求5所述的制备方法，其特征在于，步骤(1)中添加剂的加入量控制在最终产物中磁铅石型六铝酸盐占氧化铝晶体的5～20％，质量百分比；酸液的加入量为拟薄水铝石的1～6％，质量百分比。
10.权利要求1-4任一项所述的含有片状微晶的α-A12O3陶瓷颗粒作为磨料在研磨材料中的应用。
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