CN113754435A - 一种Y2O3-MgO红外透明陶瓷的制备方法 - Google Patents
一种Y2O3-MgO红外透明陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种Y2O3‑MgO红外透明陶瓷的制备方法，属于透明陶瓷材料技术领域；包括以下步骤：按比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；将纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；将排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结得到复相陶瓷坯体；将复相陶瓷坯体串联在电路中，施加电场强度进行闪烧，冷却后得到高致密度的Y2O3‑MgO陶瓷。本发明通过在石墨模具中进行热压烧结，在复相陶瓷坯体中引入大量氧空位，从而使闪烧可以在较低的温度场和电场的环境下发生，最终在达到高致密度的同时抑制晶粒尺寸的长大，有助于机械性能的提升和透过率的稳定，可用作红外窗口材料。
Description
技术领域
本发明涉及一种红外光学窗口材料的制备方法，具体涉及一种Y2O3-MgO红外透明陶瓷的制备方法，属于透明陶瓷材料技术领域。
背景技术
红外光学窗口材料是指在红外成像与制导技术中用于制造窗口、整流罩等的一类材料。这些材料具备良好的红外透明性、较宽的透射波段和一定的机械强度。近年来，红外制导飞行器向着更快的攻击速度和更高的打击精度方向发展，对红外窗口材料提出了更高的性能要求，如更高的机械性能和更低的发射率。
在常见的红外窗口材料中，Y2O3陶瓷的热稳定性和化学稳定性很高，但其力学性能较低。引入MgO作为第二相，可抑制Y2O3相的晶粒生长，从而获得比单相Y2O3陶瓷更好的力学性能、抗热冲击性、同时兼具良好的光学透过性的Y2O3-MgO纳米复相陶瓷。
为获得具有更高机械性能的高透过率红外窗口材料，研究者们提出了多种Y2O3-MgO陶瓷烧结技术。例如公开号为CN109369183A的发明专利公开了“一种红外透明陶瓷及其制备方法”，这种红外透明陶瓷是由Y2O3纳米粉末、MgO纳米粉末和Gd2O3纳米粉末组成的纳米复合粉末烧制而成的，其中Gd2O3纳米粉末占纳米复合粉末总摩尔量的百分数为0.1～18％，可采用真空烧结、热压烧结、放电等离子烧结或真空热压烧结等烧结工艺，烧结时间为0.1～15h，烧结温度为1100～1850℃。该发明通过Gd2O3的加入抑制晶界的扩散速度，降低晶粒长大速率，降低陶瓷材料的晶粒尺寸，达到细化晶粒的目的，使得透明陶瓷材料的机械性能得到进一步提高。
公开号为CN110922169A的发明专利公开了“一种Y2O3-MgO纳米复相红外透明陶瓷的制备方法”，这种红外透明陶瓷的制备方法是采用Y2O3-MgO纳米复相粉体制成素坯，通过在马弗炉中进行两步烧结的工艺获得陶瓷坯体，烧结温度为1300～1600℃，保温时间为0.5～100h；然后再辅助以热等静压烧结，烧结温度为1200～1500℃，保温时间为0.5～5h，最终制得红外透明的Y2O3-MgO纳米复相陶瓷。
上述两个专利关于Y2O3-MgO纳米复相陶瓷材料及制备工艺，均存在需要添加助剂、烧结设备昂贵、烧结工艺复杂繁琐、烧结温度高、保温时间长的问题，从而造成Y2O3-MgO复相陶瓷中晶粒尺寸长大，最终影响其机械性能。因此改进烧结工艺，缩短烧结时间，阻止晶粒长大，从而获得高透过率和优异机械性能的高致密度Y2O3-MgO纳米复相陶瓷仍是一个有待攻克的难题。
发明内容
本发明的目的是：针对现有Y2O3-MgO纳米复相陶瓷烧结技术中存在的烧结工艺复杂，烧结温度高，保温时间长、需要烧结助剂的问题，提供一种Y2O3-MgO红外透明陶瓷的制备方法，通过在石墨模具中进行热压烧结，在复相陶瓷坯体中引入大量氧空位，从而使得闪烧可以在较低的温度场和电场的环境下发生，从而在几分钟甚至数十秒钟的时间内完成烧结过程，最终在达到高致密度的同时抑制晶粒尺寸的长大，有助于机械性能的提升和透过率的稳定。
为实现上述目的，本发明采用了以下技术方案：一种Y2O3-MgO红外透明陶瓷的制备方法，包括以下步骤：
S1：按比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为900～1200℃，压力为20～40MPa，时间为10～30min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1150～1350℃条件下，施加600～1000V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为20～100mA/mm2，并保持10s～5min，结束后在炉内冷却，得到高致密度的Y2O3-MgO陶瓷。
所述步骤S1中，Y2O3与MgO纳米粉体的体积比为1：1。
所述步骤S4中，电路中的电流为直流或交流。
所述步骤S4中，冷却方法采用炉内控制降温冷却，冷却速率为2～10℃/min。
所述步骤S4中，冷却方法也可采用随炉冷却。
本发明的有益效果是：
1)本发明方法通过在石墨模具中进行热压烧结，在复相陶瓷坯体中引入大量氧空位，从而使得闪烧可以在较低的温度场和电场的环境下发生，从而在几分钟甚至数十秒钟的时间内完成烧结过程，最终在达到高致密度的同时抑制晶粒尺寸的长大，获得小晶粒尺寸的高致密度Y2O3-MgO纳米复相陶瓷。
2)本发明方法与现有烧结Y2O3-MgO陶瓷的技术相比，烧结设备简单，烧结最高温度降低了300～550℃，烧结时间不超过5min，大大降低了烧结成本；并且烧结时间短、烧结温度低可以避免晶粒尺寸的长大，从而获得致密度高、晶粒尺寸小的Y2O3-MgO纳米复相陶瓷，有助于机械性能的提升和透过率的稳定。
附图说明
图1为本发明实施例1中制备的Y2O3-MgO纳米复相陶瓷断口的扫描电子显微镜照片；
图2为本发明实施例的参数对照表。
具体实施方式
下面结合附图和具体实施例对本发明作进一步的解释说明。
如图1-2所示，本发明实施例中实施闪烧所采用的外接电源型号为EA PowerControl，显微组织照片扫描设备采用型号为JSM-7001F的SEM扫描电子显微镜。
实施例1：一种Y2O3-MgO红外透明陶瓷的制备方法，包括以下步骤：
S1：按体积比为1：1的比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为1100℃，压力为30MPa，时间为20min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1250℃条件下，施加900V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为60mA/mm2，并保持1min，结束后在炉内冷却，冷却速率为10℃/min，得到高致密度的Y2O3-MgO陶瓷，相对密度为98.8％。
如图1所示，为本发明实施例1中制备的Y2O3-MgO纳米复相陶瓷断口的扫描电子显微镜照片，可以看出复合材料中两相分布均匀，没有显著的晶粒长大现象，晶粒尺寸均小于1微米；复合材料的没有明显的裂纹、空洞等缺陷，说明该Y2O3-MgO复相陶瓷具有较高的致密度。
实施例2：一种Y2O3-MgO红外透明陶瓷的制备方法，包括以下步骤：
S1：按体积比为1：1的比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为1200℃，压力为30MPa，时间为10min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1150℃条件下，施加1000V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为20mA/mm2，并保持5min，结束后在炉内冷却，冷却速率为5℃/min，得到高致密度的Y2O3-MgO陶瓷，相对密度为97.6％。
实施例3：一种Y2O3-MgO红外透明陶瓷的制备方法，包括以下步骤：
S1：按体积比为1：1的比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为900℃，压力为40MPa，时间为30min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1350℃条件下，施加600V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为80mA/mm2，并保持2min，结束后在炉内随炉冷却，得到高致密度的Y2O3-MgO陶瓷，相对密度为98.2％。
实施例4：一种Y2O3-MgO红外透明陶瓷的制备方法，包括以下步骤：
S1：按体积比为1：1的比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为1200℃，压力为20MPa，时间为20min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1280℃条件下，施加900V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为100mA/mm2，并保持10s，结束后在炉内冷却，冷却速率为2℃/min，得到高致密度的Y2O3-MgO陶瓷，相对密度为96.4％。
如图2所示，从上述实施例可以看出，本方法可以在1150～1350℃的温度范围完成烧结，比现有烧结技术的最高烧结温度降低了300～550℃，并且可以在5min内完成烧结，具有烧结温度低、烧结时间短的特点；并且这种快速烧结技术获得的Y2O3-MgO复相陶瓷的相对密度均高于96％，晶粒尺寸没有显著长大，有助于机械性能的提升，可用作红外窗口材料。
本发明方法通过在石墨模具中进行热压烧结，在复相陶瓷坯体中引入大量氧空位，从而使得闪烧可以在较低的温度场和电场的环境下发生，从而在几分钟甚至数十秒钟的时间内完成烧结过程，最终在达到高致密度的同时抑制晶粒尺寸的长大，获得小晶粒尺寸的高致密度Y2O3-MgO纳米复相陶瓷。
以上所述，仅用以说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其他修改或者等同替换，只要不脱离本发明技术方案的精神和范围，均应涵盖在本发明的权利要求范围当中。
Claims (5)
1.一种Y2O3-MgO红外透明陶瓷的制备方法，其特征在于：包括以下步骤：
S1：按比例称量Y2O3和MgO纳米粉体，分别进行球磨、干燥和过筛，混合均匀后获得纳米复合粉末；
S2：将S1中获得的纳米复合粉末放入马弗炉中进行预烧排胶处理，去除粉体中的有机物；
S3：将S2中排胶处理后的纳米复合粉末放入石墨模具中，进行热压烧结，烧结温度为900～1200℃，压力为20～40MPa，时间为10～30min，得到复相陶瓷坯体；
S4：将S3中得到的复相陶瓷坯体用铂丝串联在外接电源的正负极两端，在炉温为1150～1350℃条件下，施加600～1000V/cm的电场强度，待复相陶瓷坯体发生闪烧现象后，控制电流密度为20～100mA/mm2，并保持10s～5min，结束后在炉内冷却，得到高致密度的Y2O3-MgO陶瓷。
2.根据权利要求1所述的一种Y2O3-MgO红外透明陶瓷的制备方法，其特征在于：所述步骤S1中，Y2O3与MgO纳米粉体的体积比为1：1。
3.根据权利要求1所述的一种Y2O3-MgO红外透明陶瓷的制备方法，其特征在于：所述步骤S4中，电路中的电流为直流或交流。
4.根据权利要求1所述的一种Y2O3-MgO红外透明陶瓷的制备方法，其特征在于：所述步骤S4中，冷却方法采用炉内控制降温冷却，冷却速率为2～10℃/min。
5.根据权利要求4所述的一种Y2O3-MgO红外透明陶瓷的制备方法，其特征在于：所述步骤S4中，冷却方法采用随炉冷却。
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