CN116639958A - 一种氧化铝粉体及其制备方法和应用 - Google Patents
一种氧化铝粉体及其制备方法和应用 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000000843 powder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003381 stabilizer Substances 0.000 claims abstract description 30
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 28
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 18
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 235000019270 ammonium chloride Nutrition 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 8
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 8
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- -1 polysiloxane Polymers 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 239000013078 crystal Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 13
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000007789 gas Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种氧化铝粉体及其制备方法和应用。本发明的氧化铝粉体的制备方法包括以下步骤：1)将γ‑氧化铝、矿化剂、稳定剂和分散剂混合进行湿法球磨，得到浆料；2)将浆料进行干燥，得到前驱体；3)将前驱体进行烧结，得到块状氧化铝；4)将块状氧化铝进行湿法球磨，再进行干燥，即得氧化铝粉体。本发明的氧化铝粉体具有纯度高、活性高、晶型转化率高、球形度高等优点，可以用于制备性能优异的氧化铝陶瓷，且其制备流程简单，易于进行大规模工业化生产。
Description
技术领域
本发明涉及陶瓷材料技术领域，具体涉及一种氧化铝粉体及其制备方法和应用。
背景技术
氧化铝陶瓷材料在纳米电子、陶瓷增韧、光电器件、太阳能电池、气体传感器、光催化等领域应用广泛，而随着科学技术的高速发展，人们对氧化铝陶瓷材料的性能要求和质量要求也越来越高，现有的氧化铝陶瓷材料已经难以完全满足日益增长的实际应用要求。
氧化铝粉体的质量对于氧化铝陶瓷的最终性能会起到决定性作用，要想制备得到高性能的氧化铝陶瓷就必须先制备出高活性的氧化铝粉体。目前，氧化铝粉体的制备方法主要包括以下两种：1)通过将三水铝石或工业氢氧化铝加热脱水来制备氧化铝粉体；2)通过中和铝盐或利用醇铝分解获得铝胶、拟薄水铝石或一水软铝石，再进行活化来制备氧化铝粉体。然而，这两种制备方法不仅存在工艺流程繁琐、产率低、生产成本高等问题，而且制备得到的氧化铝粉体的化学纯度不高，活性很难提升，难以实现氧化铝陶瓷性能的进一步提升。
因此，开发一种制备流程简单、易于大规模生产的方法，并制备出高活性、高纯度的氧化铝粉体具有十分重要的意义。
发明内容
本发明的目的在于提供一种氧化铝粉体及其制备方法和应用。
本发明所采取的技术方案是：
一种氧化铝粉体的制备方法包括以下步骤：
1)将γ-氧化铝、矿化剂、稳定剂和分散剂混合进行湿法球磨，得到浆料；
2)将浆料进行干燥，得到前驱体；
3)将前驱体进行烧结，得到块状氧化铝；
4)将块状氧化铝进行湿法球磨，再进行干燥，即得氧化铝粉体。
优选的，步骤1)所述γ-氧化铝、矿化剂、稳定剂、分散剂的质量比为1:0.005～0.013:0.0005～0.0010:0.0008～0.0018。若矿化剂的用量小于上述范围，则不能很好地实现促进晶型转换、降低烧结温度的效果，若矿化剂的用量太大，则后期又难以除干净，会导致氧化铝粉体的纯度下降；若稳定剂的用量小于上述范围，则稳定效果不佳，若稳定剂的用量过大，则又会产生杂相。
优选的，步骤1)所述矿化剂由氟化镁、氟化铵和氯化铵按照质量比1:0.20～0.33:0.15～0.50复配而成。采用上述组成及比例的矿化剂能够更好地实现促进氧化铝晶型转换、降低烧结温度、降低钠含量的效果，矿化剂中的氟离子取代氧离子进入刚玉晶格可以破坏晶型结构制造点缺陷，而铵根离子释放出氮气，可以提供氧空位；若矿化剂不按照上述组成和比例添加(例如：只加一种或两种，或某一种加的太少)，会导致晶型转化不完全；若氟化镁加入过多，会导致杂质含量高；若氟化铵或者氯化铵加入过多，会产生过多气体，造成氧化铝粉体的孔隙率高、致密性差。
优选的，步骤1)所述稳定剂为氧化钇、氧化铬、氧化镁中的至少一种。
进一步优选的，步骤1)所述稳定剂由氧化钇、氧化铬和氧化镁按照质量比1:0.6～2.0:0.2～1.1复配而成。
优选的，步骤1)所述分散剂为聚羧酸型分散剂、EVA蜡、聚硅氧烷、丙烯酸类聚合物中的至少一种。
进一步优选的，步骤1)所述分散剂由聚羧酸型分散剂D-134和EVA蜡Licowax PE890按照质量比0.4～0.9:1复配而成。
优选的，步骤3)所述烧结的具体操作为：先以2℃/min～10℃/min的升温速率从室温(25℃±5℃)升温至600℃～1400℃，保温2h～4h，再以3℃/min～15℃/min的降温速率降至室温。
优选的，步骤3)所述烧结在还原性气氛中进行。
优选的，所述还原性气氛为氮气-氢气混合气氛。
一种氧化铝粉体，其由上述制备方法制成。
优选的，所述氧化铝粉体的纯度≥99.99％，Na含量<100ppm，F含量<50ppm，氧空位含量为8％～10％。氧空位的存在能够提高晶格活性，但氧空位的含量过高时会导致缺陷过高，活性太高容易吸附杂质元素，从而会增加后续处理工序的难度。
一种氧化铝陶瓷，其由上述氧化铝粉体制成。
本发明的原理：本发明利用矿化剂促进氧化铝的晶型转换，并降低烧结温度以及降低钠含量，利用稳定剂稳定氧化铝的微观结构和促进烧结，利用分散剂使γ-氧化铝形成悬浮液，进而矿化剂和稳定剂可以均匀分布，将γ-氧化铝、矿化剂、稳定剂和分散剂混合进行湿法球磨和干燥后进行烧结，能够使γ-氧化铝发生晶型转换，且可以产生一定的氧空位，最终形成具有高活性、高纯度的氧化铝粉体。
本发明的有益效果是：本发明的氧化铝粉体具有纯度高、活性高、晶型转化率高、球形度高等优点，可以用于制备性能优异的氧化铝陶瓷，且其制备流程简单，易于进行大规模工业化生产。
具体实施方式
下面结合具体实施例对本发明作进一步的解释和说明。
实施例1：
一种氧化铝粉体，其制备方法包括以下步骤：
1)将γ-氧化铝、矿化剂、稳定剂和分散剂按照质量比1:0.01:0.0005:0.001加入球磨罐，矿化剂由氟化镁、氟化铵和氯化铵按照质量比1:0.2:0.15复配而成，稳定剂由氧化钇、氧化铬和氧化镁按照质量比1:0.6:0.2复配而成，分散剂由聚羧酸型分散剂D-134和EVA蜡Licowax PE 890按照质量比0.8:1复配而成，再加入水后进行球磨，得到浆料；
2)将浆料进行加热搅拌干燥，加热的温度为90℃，搅拌的速率为300r/min，搅拌的时间为2h，得到前驱体；
3)将前驱体置于管式炉中，充入氮气-氢气混合气，气流流量为50m3/h，再以10℃/min的升温速率从室温升温至600℃，保温2h，再以10℃/min的降温速率降至室温，得到块状氧化铝；
4)将块状氧化铝进行湿法球磨，再进行干燥，即得氧化铝粉体。
实施例2～4：
与实施例1的区别仅在于γ-氧化铝、矿化剂、稳定剂和分散剂的配比不同，具体如下：
实施例2：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.005:0.0005:0.0008；
实施例3：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.008:0.00075:0.0014；
实施例4：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.013:0.001:0.0018。
实施例5～9：
与实施例1的区别仅在于矿化剂的成分比例不同，具体如下：
实施例5：氟化镁、氟化铵和氯化铵的质量比为1:0.22:0.22；
实施例6：氟化镁、氟化铵和氯化铵的质量比为1:0.24:0.30；
实施例7：氟化镁、氟化铵和氯化铵的质量比为1:0.27:0.35；
实施例8：氟化镁、氟化铵和氯化铵的质量比为1:0.30:0.42；
实施例9：氟化镁、氟化铵和氯化铵的质量比为1:0.33:0.50。
实施例10～12：
与实施例1的区别仅在于稳定剂的成分比例不同，具体如下：
实施例10：氧化钇、氧化铬和氧化镁的质量比为1:0.9:0.4；
实施例11：氧化钇、氧化铬和氧化镁的质量比为1:1.4:0.8；
实施例12：氧化钇、氧化铬和氧化镁的质量比为1:2.0:1.1。
实施例13～15：
与实施例1的区别仅在于烧结工艺不同，具体如下：
实施例13：以2℃/min的升温速率从室温升温至800℃，保温4h，再以3℃/min的降温速率降至室温；
实施例14：以4℃/min的升温速率从室温升温至1200℃，保温2h，再以6℃/min的降温速率降至室温；
实施例15：以8℃/min的升温速率从室温升温至1400℃，保温3h，再以15℃/min的降温速率降至室温。
对比例1～6：
与实施例1的区别仅在于γ-氧化铝、矿化剂、稳定剂和分散剂的配比不同，具体如下：
对比例1：γ-氧化铝、稳定剂和分散剂的质量比为1:0.0005:0.001；
对比例2：γ-氧化铝、矿化剂和分散剂的质量比为1:0.01:0.001；
对比例3：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.001:0.0005:0.001；
对比例4：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.02:0.0005:0.001；
对比例5：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.01:0.0001:0.001；
对比例6：γ-氧化铝、矿化剂、稳定剂和分散剂的质量比为1:0.01:0.002:0.001。
对比例7～13：
与实施例1的区别仅在于矿化剂的成分及比例不同，具体如下：
对比例7：只加氟化镁；
对比例8：氟化镁和氟化铵的质量比为1:0.27；
对比例9：氟化铵和氯化铵的质量比为0.2:0.15；
对比例10：氟化镁、氟化铵和氯化铵的质量比为1:0.1:0.07；
对比例11：氟化镁、氟化铵和氯化铵的质量比为1:0.66:1；
对比例12：氟化镁、氟化铵和氯化铵的质量比为1:0.2:0.8；
对比例13：氟化镁、氟化铵和氯化铵的质量比为1:0.2:0.01。
性能测试：
实施例1～15和对比例1～13的氧化铝粉体的性能测试数据如下表所示：
表1实施例1～15和对比例1～13的氧化铝粉体的性能测试数据
注：
氧空位含量：测试XPS，其中O1s谱图中的533.66peak位置峰值为C＝O和氧空位的含量，C1s谱图中的288.71peak位置峰值为C＝O的含量；由于O总含量等于O空位含量加上C＝O的含量，在知道O总含量及C＝O的含量的情况下，可以通过计算得到氧空位含量。
转化率：准备5g的粉体，通过XRD进行测试。
球形度：采用场发射扫描电镜拍摄粉体形貌，量出片状颗粒的长和宽，然后计算出片状颗粒的面积，即为S片(片状颗粒面积)，然后测量出整个粉体形貌图片的长和宽，S总＝L总×W总，片状占比＝S片/S总×100％；球形度以片状占比来评价。
纯度：准备5g的粉体，通过XRF和ICP进行测试。
孔隙率：拍摄FE-SEM照片，放大800倍，测量空隙的尺寸计算出孔面积S孔，测量照片的长和宽计算出总面积S总，再计算孔隙率：S孔/S总＝孔隙率。
密度：准备3g的成瓷，通过气体密度计测试。
氧化铝粉体的转化率、纯度、球形度和氧空位含量达标标准如下：转化率达标标准：>99％；纯度达标标准：>99.99％；球形度达标标准：片状占比<10％；氧空位含量达标标准：8％～10％；密度合格范围：>3.7g/cm3；孔隙率达标标准：<2.5％。
由表1可知：
1)由实施例1～15可知：当实验条件控制在本发明给出的范围时，制备的氧化铝粉体的性能在合格的范围内；
2)由对比例1、3和4可知：如果不添加矿化剂或矿化剂的添加量小于本发明给出的范围，会导致晶型转化率不合格，产品的氧空位含量、球形度等性能也不够理想，如果矿化剂的添加量大于本发明给出的范围，会导致产品纯度太低，氧空位含量、孔隙率过高等问题；
3)由对比例2、5和6可知：如果不添加稳定剂或稳定剂的添加量小于本发明给出的范围，会导致稳定效果不佳，产品的晶型转化率不理想，如果稳定剂的添加量大于本发明给出的范围，会导致产品纯度偏低；
4)由对比例7～13可知：矿化剂的组分及各组分比例应控制在本发明给出范围内，才能实现最佳效果；在不添加氟化镁或氟化镁的添加量太少时，会导致晶型转换不完全，氧化铝粉体活性不够高，同时由于产生气体过多，粉体孔隙率高，不够致密，而氟化镁的添加量太多时，会导致纯度不足，氧空位含量不足，导致活性偏低，晶型转化率不理想。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种氧化铝粉体的制备方法，其特征在于，包括以下步骤：
1)将γ-氧化铝、矿化剂、稳定剂和分散剂混合进行湿法球磨，得到浆料；
2)将浆料进行干燥，得到前驱体；
3)将前驱体进行烧结，得到块状氧化铝；
4)将块状氧化铝进行湿法球磨，再进行干燥，即得氧化铝粉体。
2.根据权利要求1所述的制备方法，其特征在于：步骤1)所述γ-氧化铝、矿化剂、稳定剂、分散剂的质量比为1:0.005～0.013:0.0005～0.0010:0.0008～0.0018。
3.根据权利要求1或2所述的制备方法，其特征在于：步骤1)所述矿化剂由氟化镁、氟化铵和氯化铵按照质量比1:0.20～0.33:0.15～0.50复配而成。
4.根据权利要求1或2所述的制备方法，其特征在于：步骤1)所述稳定剂为氧化钇、氧化铬、氧化镁中的至少一种。
5.根据权利要求4所述的制备方法，其特征在于：步骤1)所述稳定剂由氧化钇、氧化铬和氧化镁按照质量比1:0.6～2.0:0.2～1.1复配而成。
6.根据权利要求1或2所述的制备方法，其特征在于：步骤1)所述分散剂为聚羧酸型分散剂、EVA蜡、聚硅氧烷、丙烯酸类聚合物中的至少一种。
7.根据权利要求1所述的制备方法，其特征在于：步骤3)所述烧结的具体操作为：先以2℃/min～10℃/min的升温速率从室温升温至600℃～1400℃，保温2h～4h，再以3℃/min～15℃/min的降温速率降至室温。
8.根据权利要求1或7所述的制备方法，其特征在于：步骤3)所述烧结在还原性气氛中进行。
9.一种氧化铝粉体，其特征在于，由权利要求1～8中任意一项所述的制备方法制成。
10.一种氧化铝陶瓷，其特征在于，由权利要求9所述的氧化铝粉体制成。
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