CN116789459B - 一种陶瓷刚玉磨料及其制备方法和应用 - Google Patents
一种陶瓷刚玉磨料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种陶瓷刚玉磨料及其制备方法和应用，属于陶瓷磨料技术领域，本发明是以工业级拟薄水铝石为原料，通过加入胶溶剂HNO3形成拟薄水铝石胶粒双电子层结构，制备拟薄水铝石溶胶，经过溶胶‑凝胶、破碎、分级、烧结等工艺过程制备成品磨料。在溶胶制备以及烧结过程中分别引入特定的改良成分，促进溶胶‑凝胶以及产品性能的提升，同时提高了生产效率，具有较大的市场价值。
Description
技术领域
本发明属于陶瓷磨料技术领域，具体涉及一种陶瓷刚玉磨料及其制备方法和应用。
背景技术
陶瓷磨料是研磨机械使用的一种研磨介质，研磨机械空转的研磨效果较差，因此需要通过这些介质来达到研磨的效果，而陶瓷类型的磨料就是目前研磨机械当中使用频率比较高的一类材料，其具有加工效果好、可使用时间长、损耗小、耐腐蚀性能好的等优点。
陶瓷刚玉磨料多由溶胶凝胶工艺合成并烧结而成，即首先反应生成稳定的溶胶体系，然后转变为凝胶，蒸发去除液体介质，将凝胶干燥，干燥胶前驱体焙烧去除有机成分和结合水，最后得到所需制品。
随着陶瓷刚玉磨料的广泛应用，对其性能提出了更高的要求。现有陶瓷刚玉磨料的制备具有多种难点，如显微结构的控制、烧结条件的优化等。研究者致力于从多个方面出发探究磨料的性能，如引入添加剂、降低烧结温度、控制形貌等。
发明内容
为了提高陶瓷刚玉磨料的性能，本发明的目的一在于提供一种陶瓷刚玉磨料的制备方法，目的二在于提供采用上述制备方法制备的陶瓷刚玉磨料，目的三在于提供上述陶瓷刚玉磨料在制备研磨材料中的应用。本发明通过在溶胶制备以及烧结过程中分别引入特定的改良成分，促进溶胶-凝胶以及产品性能的提升，同时提高了生产效率，具有较大的市场价值。
为了实现上述目的，本发明采用的具体方案为：
第一方面，一种陶瓷刚玉磨料的制备方法，包括以下步骤：
步骤一、取拟薄水铝石为原料，按照质量体积比为1：4的比例加入纯净水，抽真空，在真空分散剂中进行高速分散，得浆料；向所述浆料中加入稀硝酸，使pH值为3.5-4.5，然后加入无机晶须，分散均匀，再继续加入稀硝酸，使pH值为2.0，真空条件下继续高速分散形成溶胶；所述无机晶须的加入量为所述浆料质量的0.07-0.12%；
步骤二、将步骤一所得溶胶注入平面模具，刮平溶胶层，通过所述平面模具上设置的等厚凸起，得到对应厚度的溶胶层，然后通过干燥，即得干凝胶薄片；
步骤三、将步骤二所得干凝胶薄片进行破碎，筛分，得凝胶粒；
步骤四、将步骤三所得凝胶粒在850℃进行煅烧，保温30min；然后置于改性液中进行浸渍处理；所述改性液中包含质量百分比分别为1.5%-1.8%硝酸镁、0.3%-0.5%硝酸钴、0.8%-0.9%硝酸钕、1.5%-1.8%硝酸钙和0.5%-0.7%硝酸锌；
步骤五、将经步骤四改性后的凝胶粒再次于850℃进行煅烧，保温30min，去除挥发成分；然后在高温回转炉中进行烧成，1400℃保温15min；烧成后的产品经过分级、精筛即为成品。
作为对上述制备方法的进一步优化，步骤一中，所述无机晶须为硫酸钙晶须、碳酸钙晶须和钛酸钾晶须中的任意一种。更进一步地，所述无机晶须为碳酸钙晶须。
作为对上述制备方法的进一步优化，步骤一中，所述稀硝酸的浓度为22%。
作为对上述制备方法的进一步优化，步骤四中，所述改性液中，硝酸镁、硝酸钴、硝酸钕、硝酸钙和硝酸锌的质量百分比分别为1.5%、0.4%、0.8%、1.6%和0.6%，其余为水。
作为对上述制备方法的进一步优化，步骤四中，所述浸渍处理的时间为15-25min。
第二方面，采用上述制备方法制备的陶瓷刚玉磨料。
第三方面，上述陶瓷刚玉磨料在制备研磨材料中的应用。
有益效果：
1、本发明以拟薄水铝石为原料，通过溶胶凝胶法制备陶瓷磨料，拟薄水铝石具有较好的胶溶触变性，其是一种无定型的不规则矿物，粒度分布不均一，比表面积大，易发生团聚；而针状晶须的原子排列高度有序且直径非常小，在剪切力作用下能快速取向，分布在溶胶粒子表面弥补空间缺陷，实现溶胶粒子的有效分散，在降低初胶凝时间的同时还能控制粘度，这一举措有利于烘干提高生产效率，同时有利于降低缺陷发生率提高致密性。而且，无机晶须表面在酸性溶液中能形成水化层，促使溶胶在稳定状态下建立凝胶体系，具有更高的强度和稳定性。
2、本发明在初步煅烧后，采用改性液进行着色改性，随后在850度、保温30min条件下进行二次煅烧去除挥发成分，最后在1400度、保温15min条件下烧成。其中，改性液的成分种类和含量是十分关键的，通过复合协同作用，能够促进烧结体的致密化，加快质点在晶界间的迁移速率，对产品的微观结构和力学性能均起到十分积极的作用，可显著提高磨削性能。
具体实施方式
本发明是以工业级拟薄水铝石为原料，通过加入胶溶剂HNO3形成拟薄水铝石胶粒双电子层结构，制备拟薄水铝石溶胶，经过溶胶-凝胶、破碎、分级、烧结等工艺过程。
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。
所述硫酸钙晶须和碳酸钙晶须均购自河北方骥新材料科技有限公司，货号分别为3339和9999；所述钛酸钾晶须购自济南子安化工有限公司，货号为1219。
其他若未特别提及，所用材料或试剂均为常规市售材料或试剂，所用操作手段均为常规技术手段。
实施例1
一种陶瓷刚玉磨料的制备方法，其制备工艺如下：
1、取1000g拟薄水铝石为原料，加入4000g纯净水，在真空分散机中，先抽真空，然后高速分散3min，持续抽真空，加入浓度22%的稀硝酸，使pH值为3.5-4.5，加入5g碳酸钙晶须，继续高速分散3min，再继续加入稀硝酸，使pH值为2.0，真空条件下继续高速分散形成溶胶，停高速分散，停真空泵，最后放气，倒出产物溶胶。
2、将溶胶转入储存容器，下部设有出料口，可通过计量泵定量排出溶胶。
3、生产模具为固定平面或者回转圆盘平面，将溶胶注入平面模具，模具上设置有精确高度的等厚凸起，然后用刮板刮平溶胶层。通过不同厚度的薄板条，可以得到1-5mm不同厚度的溶胶层。
4、干燥所得溶胶层及模具，即可干凝胶薄片。
5、破碎所得干凝胶片，筛分成需要的尺寸。
6、在推板窑中煅烧破碎后的凝胶片850度，保温30分钟。
7、煅烧后的凝胶片为多孔结构，可以进行着色改性处理。改性液中，硝酸镁、硝酸钴、硝酸钕、硝酸钙和硝酸锌的质量百分比分别为1.5%、0.4%、0.8%、1.6%和0.6%，其余为水。经所述煅烧后的凝胶片浸渍在改性液中15min。
8、改性后的凝胶片再次煅烧850度，保温30分钟，去除挥发成分。
9、得到的凝胶片在高温回转炉中进行烧成，1400度，保温15min。
10、烧成后的产品经过分级，精筛即为成品，所述成品即为陶瓷刚玉磨料。
实施例2
本实施例与实施例1基本相同，不同之处在于：采用硫酸钙晶须替代碳酸钙晶须。
实施例3
本实施例与实施例1基本相同，不同之处在于：采用钛酸钾晶须替代碳酸钙晶须。
实施例4
本实施例与实施例1基本相同，不同之处在于：所述改性液中，硝酸镁、硝酸钴、硝酸钕、硝酸钙和硝酸锌的质量百分比分别为1.8%、0.5%、0.8%、1.8%和0.7%，其余为水。经所述煅烧后的凝胶片浸渍在改性液中18min。
实施例5
本实施例与实施例1基本相同，不同之处在于：所述改性液中，硝酸镁、硝酸钴、硝酸钕、硝酸钙和硝酸锌的质量百分比分别为1.5%、0.3%、0.9%、1.5%和0.5%，其余为水。经所述煅烧后的凝胶片浸渍在改性液中20min。
对照例1
本对照例与实施例1基本相同，不同之处在于：未加碳酸钙晶须。
对照例2
本对照例与实施例1基本相同，不同之处在于：加入5g碳酸钙粉末。
对照例3
本对照例与实施例1基本相同，不同之处在于：改性液中，不含有硝酸钙。
对照例4
本对照例与实施例1基本相同，不同之处在于：改性液中，不含有硝酸钙和硝酸锌。
对实施例1-5和对照例1-4中制备的磨料进行性能测定。
采用ECH XL30型扫描电镜观察所述陶瓷刚玉磨料的表面形貌，其均为片状，实施例1-5的致密化程度比对照例1-4均高，气孔量更少。
分选粒度为60目的陶瓷刚玉磨料试样，利用金刚石静压强度测定仪（ZMC-Ⅱ）测定其单颗粒强度。取40粒分别测试其破碎载荷，记录抗压强度值，求算平均值。
利用MHV2000型显微硬度测试仪测试陶瓷刚玉磨料试样的显微硬度，测试结果以同一试样不同位置的5个硬度值的平均值为准。结果如下表1所示。
表1 磨料的性能对比表。
| 组别 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对照例1 | 对照例2 | 对照例3 | 对照例4 |
| 抗压强度/N | 45.67 | 43.46 | 36.42 | 37.19 | 41.21 | 28.87 | 27.34 | 23.89 | 26.54 |
| 硬度/kg/mm2 | 2152 | 2209 | 2078 | 1998 | 2013 | 1898 | 1723 | 1903 | 1888 |
试验例
采用溶胶凝胶法制备陶瓷刚玉磨料，在溶胶形成过程中，以碳酸钙晶须的加入量为变量，分别取0%、0.05%、0.07%、0.10%、0.12%和0.15%的碳酸钙晶须加入到浆料中，其他步骤按照实施例1进行，形成溶胶停止分散后，静置5min，对初胶凝时间和粘度值进行分析测定，结果如下表2所示。
表2 不同碳酸钙晶须加入量对溶胶-凝胶性能的影响。
| 质量百分比（%） | 0% | 0.05% | 0.07% | 0.10% | 0.12% | 0.15% |
| 加入量（g） | 0 | 2.5 | 3.5 | 5 | 6 | 7.5 |
| 初胶凝时间（min） | 18 | 17 | 14 | 10 | 10 | - |
| 粘度值（mpa.s） | 13.4 | 12.9 | 9.8 | 9.2 | 7.8 | 0.5 |
采用溶胶凝胶法要经过成核、生长、团聚等过程，若晶核生长速率过快，晶核形成以后，溶液会在晶核上不断沉淀导致晶粒不断长大，会造成粒子的尺寸过大；若晶核生长速率过慢，则不利于溶胶体系的生成。向由拟薄水铝石和水形成的浆料中加入特定的晶须材料，有利于溶液的快速分散，体系更均匀稳定。由上表1可知，当不加无机晶须或加入量为0.05%时，初胶凝时间和粘度值变化不大。而加入量在0.07%-0.12%时，体系中胶核数较多，胶粒间更容易形成网络结构从而使初胶凝时间下降，同时晶须在分散剪切力作用下使粘度下降。当加入量为0.15%时，难以形成网络结构，即使形成网络结构，体系也不稳定，有时还有少量沉淀生成。
需要说明的是，以上所述的实施方案应理解为说明性的，而非限制本发明的保护范围，本发明的保护范围以权利要求书为准。对于本领域技术人员而言，在不背离本发明实质和范围的前提下，对本发明作出的一些非本质的改进和调整仍属于本发明的保护范围。
Claims (7)
1.一种陶瓷刚玉磨料的制备方法，其特征在于：包括以下步骤：
步骤一、取拟薄水铝石为原料，按照质量体积比为1：4的比例加入纯净水，抽真空，在真空分散剂中进行高速分散，得浆料；向所述浆料中加入稀硝酸，使pH值为3.5-4.5，然后加入无机晶须，分散均匀，再继续加入稀硝酸，使pH值为2.0，真空条件下继续高速分散形成溶胶；所述无机晶须为硫酸钙晶须、碳酸钙晶须和钛酸钾晶须中的任意一种；所述无机晶须的加入量为所述浆料质量的0.07-0.12%；
步骤二、将步骤一所得溶胶注入平面模具，刮平溶胶层，通过所述平面模具上设置的等厚凸起，得到对应厚度的溶胶层，然后通过干燥，即得干凝胶薄片；
步骤三、将步骤二所得干凝胶薄片进行破碎，筛分，得凝胶粒；
步骤四、将步骤三所得凝胶粒在850℃进行煅烧，保温30min；然后进行着色改性处理；所述着色改性处理是将经初步煅烧的凝胶粒置于改性液中进行浸渍处理；所述改性液中包含质量百分比分别为1.5%-1.8%硝酸镁、0.3%-0.5%硝酸钴、0.8%-0.9%硝酸钕、1.5%-1.8%硝酸钙和0.5%-0.7%硝酸锌；所述浸渍处理的时间为15-25min；
步骤五、将经步骤四改性后的凝胶粒再次于850℃进行煅烧，保温30min，去除挥发成分；然后在高温回转炉中进行烧成，1400℃保温15min；烧成后的产品经过分级、精筛即为成品。
2.根据权利要求1所述的制备方法，其特征在于：所述无机晶须为碳酸钙晶须。
3.根据权利要求1所述的制备方法，其特征在于：所述无机晶须的加入量为所述浆料质量的0. 10%。
4.根据权利要求1所述的制备方法，其特征在于：步骤一中，所述稀硝酸的浓度为22%。
5.根据权利要求1所述的制备方法，其特征在于：所述改性液中，硝酸镁、硝酸钴、硝酸钕、硝酸钙和硝酸锌的质量百分比分别为1.5%、0.4%、0.8%、1.6%和0.6%，其余为水。
6.采用权利要求1-5任意一种所述的制备方法制备的陶瓷刚玉磨料。
7.根据权利要求6所述的陶瓷刚玉磨料在制备研磨材料中的应用。
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