CN116813326A - 一种基于Isobam凝胶体系制备透明陶瓷的方法 - Google Patents
一种基于Isobam凝胶体系制备透明陶瓷的方法 Download PDFInfo
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Abstract
本发明公开了一种基于Isobam凝胶体系制备透明陶瓷的方法，在透明陶瓷制备过程中，采用硅烷偶联剂促进透明陶瓷材料在Isobam凝胶体系中的凝胶化及凝胶均匀性，所述透明陶瓷材料具有六方、立方或等轴晶体结构，制备得到的透明陶瓷均匀致密、无缺陷，透过率高达理论透过率的95.7‑97.9％，强度提升为31.8‑35.6MPa。该方法采用硅烷偶联剂促进原料粉体在Isobam凝胶体系中凝胶化，工艺简单，可操作性强，提高了凝胶效率，提高陶瓷光学性能，制备出的透明陶瓷透过率大幅度提高，素坯均匀性和强度的提升。
Description
技术领域
本发明属于透明陶瓷成型和制造工艺技术领域，具体涉及一种基于Isobam凝胶体系制备透明陶瓷的方法。
背景技术
凝胶注模成型是在20世纪90年代初，由美国橡树岭国家实验室的Omatete和Ja22ey发明的，它将传统的注浆成型与高分子化学结合，是一种净尺寸陶瓷成型技术。陶瓷粉体在静电斥力或空间位阻作用下均匀分散在含有有机分子的溶剂中，形成具有流动性良好，黏度较低的陶瓷浆料，浆料填充模具后，浆料内有机分子通过交联或聚合反应形成由分子链构成的高分子三维网络结构。
与其他陶瓷成型技术相比，凝胶注模成型具有工艺简单，设备成本低及成型素坯均匀的优点。与注浆成型相比，凝胶注模成型制备素坯强度高，与塑性成型相比，有机物含量少，广泛用于大尺寸及复杂形状陶瓷的成型。
现有专利CN 107721424 A公开了一种凝胶注模成型制备YAG透明陶瓷的方法，采用Isobam作为分散剂和凝胶剂，同时采用Ziegler-Natta催化剂体系、过硫酸铵-四甲基乙二胺催化体系和2，2-偶氮[2-(2-咪唑啉-2-基)丙烷]盐酸盐催化体系，制备出透过率较高的YAG透明陶瓷。专利CN 108516818 B采用Isobam作为分散剂和凝胶剂，在预混液中加入树脂交联剂和分散剂，并增加了陶瓷浆料的固含量，提高了真空烧结制备的YAG透明陶瓷透过率。文献1(Pa2 G,Le Z B,Qy B,et al.Ceramics I2ter2atio2al,2020,46(2):2365-2372)在固含量45vol％的条件下，生坯具有约29MPa的弯曲强度，但由于有机物未排除完全，陶瓷光学透过率质量还能进一步提升。
以上方法由于凝胶体系中所固有的性质导致凝胶时间较长，浆料在凝胶过程中容易沉降，凝胶均匀性差，素坯强度不高，影响制备陶瓷的效率和在透明陶瓷领域中的实际应用。
发明内容
针对上述存在的技术不足，本发明的目的是提供一种基于Isobam凝胶体系制备透明陶瓷的方法，采用硅烷偶联剂促进原料粉体在Isobam凝胶体系中凝胶化，工艺简单，可操作性强，提高了凝胶效率，提高陶瓷光学性能，制备出的透明陶瓷透过率大幅度提高，素坯均匀性和强度的提升。
本发明提出的一种基于Isobam凝胶体系制备透明陶瓷的方法，以硅烷偶联剂所带的基团与Isobam中的官能团反应，从而可以使硅烷偶联剂与Isobam高分子相连。当其中可水解的活性基团水解时，产生Si-OH，与粉体表面OH形成氢键，产生缩合脱水反应，形成共价键结合。由此通过硅烷偶联剂可将粉体原料与Isobam产生很好的界面结合，使得两者紧密的连接到一起，从而加快了凝胶速度。同时硅烷偶联剂改善了与Isobam的交联性，增强素坯均匀性和强度，提高产品附加值。
本发明采用的具体技术方案如下：
一种基于Isobam凝胶体系制备透明陶瓷的方法，在透明陶瓷制备过程中，采用硅烷偶联剂促进透明陶瓷材料在Isobam凝胶体系中的凝胶化及凝胶均匀性，所述透明陶瓷材料具有六方、立方或等轴晶体结构，制备得到的透明陶瓷均匀致密、无缺陷，透过率高达理论透过率的95.7-97.9％，强度提升为31.8-35.6MPa。
进一步地，具体包括以下步骤：
S1：按照透明陶瓷材料分子式的化学计量比称量原料粉体，进行除杂预处理，并在原料粉体中加入烧结助剂，获得陶瓷粉体；
S2：将硅烷偶联剂、消泡剂、凝胶剂Isobam和去离子水配置成预混液，将步骤S1所制备的陶瓷粉体加入预混液中，配置成固含量为60-75wt.％的凝胶注模浆料；
S3：将步骤S2得到的凝胶注模浆料真空除去气泡，注入模具成型，在室温条件下凝胶固化2-4h后得到湿素坯并从模具中脱出；
S4：将步骤S3脱模后的湿素坯干燥处理，得到陶瓷素坯；将干燥后的陶瓷素坯排胶；
S5：将排胶后的陶瓷素坯真空烧结并退火，抛光后得到透明陶瓷。
进一步地，步骤S1中，所述的透明陶瓷材料选自YAG、MgAl2O4、Al2O3中的一种或多种，所述原料粉体在马弗炉中进行煅烧除杂。
进一步地，步骤S1中，所述的烧结助剂为MgO、SiO2、CaO中的一种或多种，添加量为原料粉体总重量的0.4-0.6wt.％。
进一步地，步骤S2中，所述硅烷偶联剂选自氨基硅烷偶联剂、氨丙基三甲氧基硅烷偶联剂、氧丙基三甲氧基硅烷偶联剂中的一种或多种，添加量为陶瓷粉体总重量的0.6-0.9wt.％。
进一步地，步骤S2中，所述的消泡剂选自低级醇类或有机极性化合物，添加量为陶瓷粉体总重量的0.4-0.6wt.％。
进一步地，步骤S2中，所述的凝胶剂Isobam选自Isobam04、Isobam104、Isobam600中的一种或几种，添加量为陶瓷粉体总重量的15-25wt.％。
进一步地，步骤S4中，干燥处理工艺为：60-80℃的烘箱中干燥10-15h。
进一步地，步骤S4中，排胶制度工艺为：室温下以0.5-2℃2mi2的速率升温至400-500℃，保温4-8h，再以0.5-2℃2mi2升温到800-900℃，并保温4-8h。
进一步地，步骤S5中，真空烧结工艺为：首先在室温按8-10℃2mi2升温到200℃，保温20-30mi2，其次按10-20℃2mi2升温到800℃并保温20-30mi2，再次按6-10℃2mi2升温到1200℃并保温1-2h，然后按1-5℃2mi2升温到1780℃并保温8-16h，最后以5-10℃2mi2降温到室温，整个烧结过程中真空度保持在1×10-2-1×10-5Pa；
取出烧结后的陶瓷再退火，退火工艺为：从室温开始按5-7℃2mi2升温速率升温到200℃，按10-12℃2mi2升温速率升温到1200℃，1200℃按4-6℃2mi2升温速率升温到1450℃并保温6h，然后从1450℃以10-12℃2mi2降温速率降到室温。
本发明的有益效果在于：
1、为促进Isobam凝胶体系的凝胶化，将硅烷偶联剂引入凝胶体系，缩短了凝胶时间，降低到2-4h，提高了凝胶效率，经真空烧结制备出的透明陶瓷透过率大幅度提高，透过率高达理论透过率的95.7-97.9％，接近理论透过率；
2、为有效改善Isobam凝胶体系中本身存在的坯体强度不高的问题，硅烷偶联剂在缩短凝胶时间的同时，从化学反应和物理键合的层面将Isobam与原料粉体间产生界面结合，有效的提高了素坯均匀性和强度，最终脱模干燥排胶后制成的陶瓷密度大，强度好，强度可提升至31.8-35.6MPa；
3、本申请的制备方法工艺简单，设备简单，可操作性强，并解决了Isobam的凝胶、强度、透光率问题，大幅度提高了最终制备的透明陶瓷的光学质量，有利于工业化生产发展。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为实施例1真空烧结后双面抛光的陶瓷样品实物图。
图2为实施例1制备陶瓷素坯的SEM微观结构图。
图3为实施例1烧结后的陶瓷表面与断面的SEM微观结构图。
图4为实施例1测得YAG透明陶瓷样品在10642m波长处的透过率图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种基于Isobam凝胶体系制备透明陶瓷的方法，它包括以下步骤：
(1)按照YAG分子式的化学计量比称量原料粉体125g并进行除杂预处理，在原料粉体中添加0.625g烧结助剂MgO，获得陶瓷粉体；
(2)将0.879g的硅烷偶联剂KH570、0.628g消泡剂正丁醇、25.125g凝胶剂Isobam104和去离子水56.617mL配置成预混液，将步骤(1)陶瓷粉体加入预混液中，配置成固含量为68wt.％的凝胶注模浆料；
(3)将凝胶注模浆料真空除去气泡，注入模具成型，在室温条件下凝胶固化3h后得到湿素坯并从模具中脱出；
(4)将脱模后的湿素坯放入70℃的烘箱中干燥15h，得到陶瓷素坯，如图2所示，其强度为35.6MPa，与文献1对比可知，其强度达到传统凝胶体系素坯强度123％。将干燥后的陶瓷素坯排胶，胶制度为：室温下以1℃2mi2的速率升温至450℃，保温6h，再以0.5℃2mi2升温到850℃，并保温6h；
(5)将排胶后的陶瓷素坯置于真空气氛中烧结，于室温下首先按8℃2mi2升温到200℃，保温20mi2，其次按10℃2mi2升温到800℃，保温20mi2，再次按6℃2mi2升温到1200℃，保温1h，然后按1℃2mi2升温到烧结温度1780℃并保温8h，最后以5℃2mi2降温到室温。取出烧结后的陶瓷再退火从室温开始按5℃2mi2升温速率升温到200℃，200℃按10℃2mi2升温速率升温到1200℃，1200℃按4℃2mi2升温速率升温到1450℃并保温6h，然后从1450℃以10℃2mi2降温速率降到室温如图3所示；抛光后得到YAG透明陶瓷，其双面抛光至3mm，如图1所示；在10642m波长处透过率为80.4％，达到理论透过率84％的95.7％。具体如图4所示。
图1为真空烧结后双面抛光的陶瓷样品实物图。
图2为制备素坯的SEM微观结构图，可以看到成型素坯的结构均匀。
图3为烧结后的陶瓷表面与断面的SEM，陶瓷致密无气孔。
图4为测得YAG透明陶瓷样品在10642m波长处的透过率图。
该实施例1通过硅烷偶联剂可将原料粉体与Isobam产生很好的界面结合，使得两者紧密的连接到一起，从而加快了凝胶速度，凝胶固化仅需3h；并且本申请的方法从化学反应和物理键合的层面将Isobam与原料粉体间产生界面结合，硅烷偶联剂所带的基团与Isobam中的官能团反应，从而可以使硅烷偶联剂与Isobam高分子相连，当其中可水解的活性基团水解时，产生Si-OH，与原料粉体表面-OH形成氢键，产生缩合脱水反应，形成共价键结合，由此硅烷偶联剂改善了原料粉体与Isobam的交联性，增强素坯均匀性和强度，其强度达35.6MPa，在10642m波长处透过率为80.4％，提高产品附加值。
实施例2
一种基于Isobam凝胶体系制备透明陶瓷的方法，它包括以下步骤：
(1)按照MgAl2O4分子式的化学计量比称量原料粉体125g并进行除杂预处理，在原料粉体中添加0.5g烧结助剂SiO2，获得陶瓷粉体；
(2)将0.753g的硅烷偶联剂KH560、0.628g消泡剂正丁醇、18.825g凝胶剂Isobam04和去离子水58.617mL配置成预混液，将陶瓷粉体加入预混液中，配置成固含量为60％的凝胶注模浆料；
(3)将凝胶注模浆料真空除去气泡，注入模具成型，在室温条件下凝胶固化2h后得到湿素坯并从模具中脱出；
(4)将脱模后的湿坯放入60℃的烘箱中干燥10h，得到陶瓷素坯，其强度为32.4MPa，与文献1对比可知，其强度达到传统凝胶体系素坯强度112％。将干燥后的素坯排胶，排胶制度为：室温下以0.5℃2mi2的速率升温至400℃，保温4h，再以2℃2mi2升温到800℃，并保温4h；
(5)将排胶后的素坯置于真空气氛中烧结，于室温下首先按9℃2mi2升温到200℃，保温25mi2，其次按15℃2mi2升温到800℃，保温25mi2，再次按8℃2mi2升温到1200℃，保温1h，然后按3℃2mi2升温到烧结温度1780℃并保温12h，最后以7℃2mi2降温到室温。取出烧结后的陶瓷再退火从室温开始按6℃2mi2升温速率升温到200℃，200℃按11℃2mi2升温速率升温到1200℃，1200℃按5℃2mi2升温速率升温到1450℃并保温6h，然后从1450℃以11℃2mi2降温速率降到室温抛光后得到透明陶瓷，其双面抛光至3mm，在10642m波长处透过率为82.3％，达到理论透过率84％的97.9％。
实施例3
一种基于Isobam凝胶体系制备透明陶瓷的方法，它包括以下步骤：
(1)按照Al2O3分子式的化学计量比称量粉体125g并进行除杂预处理，在陶瓷粉体中添加0.625g烧结助剂CaO，获得陶瓷粉体；
(2)将1.130g的硅烷偶联剂KH540、0.628g消泡剂正丁醇、31.406g凝胶剂Isobam600和去离子水62.418mL配置成预混液，将陶瓷粉体加入预混液中，配置成固含量为75％的凝胶注模浆料；
(3)将凝胶注模浆料真空除去气泡，注入模具成型，在室温条件下凝胶固化4h后得到湿素坯并从模具中脱出；
(4)将脱模后的湿坯放入80℃的烘箱中干燥15h，得到陶瓷素坯，其强度为31.8MPa，与文献1对比可知，其强度达到传统凝胶体系素坯强度110％。将干燥后的素坯排胶，排胶制度为：室温下以2℃2mi2的速率升温至500℃，保温8h，再以2℃2mi2升温到900℃，并保温8h；
(5)将排胶后的素坯置于真空气氛中烧结并退火，于室温下首先按10℃2mi2升温到200℃，保温30mi2，其次按20℃2mi2升温到800℃，保温30mi2，再次按10℃2mi2升温到1200℃，保温2h，然后按5℃2mi2升温到烧结温度1780℃并保温16h，最后以10℃2mi2降温到室温。取出烧结后的陶瓷再退火从室温开始按7℃2mi2升温速率升温到200℃，200℃按12℃2mi2升温速率升温到1200℃，1200℃按6℃2mi2升温速率升温到1450℃并保温6h，然后从1450℃以12℃2mi2降温速率降到室温抛光后得到透明陶瓷，其双面抛光至3mm，在10642m波长处透过率为81.6％，达到理论透过率84％的97.1％。
显然，本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样，倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内，则本发明也意图包含这些改动和变型在内。
Claims (10)
1.一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，在透明陶瓷制备过程中，采用硅烷偶联剂促进透明陶瓷材料在Isobam凝胶体系中的凝胶化及凝胶均匀性，所述透明陶瓷材料具有六方、立方或等轴晶体结构，制备得到的透明陶瓷均匀致密、无缺陷，透过率高达理论透过率的95.7-97.9％，强度提升为31.8-35.6MPa。
2.根据权利要求1所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，包括以下步骤：
S1：按照透明陶瓷材料分子式的化学计量比称量原料粉体，进行除杂预处理，并在原料粉体中加入烧结助剂，获得陶瓷粉体；
S2：将硅烷偶联剂、消泡剂、凝胶剂Isobam和去离子水配置成预混液，将步骤S1制备的陶瓷粉体加入预混液中，配置成固含量为60-75wt.％的凝胶注模浆料；
S3：将步骤S2得到的凝胶注模浆料真空除去气泡，注入模具成型，在室温条件下凝胶固化2-4h后得到湿素坯并从模具中脱出；
S4：将步骤S3脱模后的湿素坯干燥处理，得到陶瓷素坯；将干燥后的陶瓷素坯排胶；
S5：将排胶后的陶瓷素坯真空烧结并退火，抛光后得到透明陶瓷。
3.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S1中，所述的透明陶瓷材料选自YAG、MgAl2O4、Al2O3中的一种或多种，所述原料粉体在马弗炉中进行煅烧除杂。
4.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S1中，所述的烧结助剂选自MgO、SiO2、CaO中的一种或多种，添加量为原料粉体总重量的0.4-0.6wt.％。
5.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法的，其特征在于，步骤S2中，所述的硅烷偶联剂选自氨基硅烷偶联剂、氨丙基三甲氧基硅烷偶联剂、氧丙基三甲氧基硅烷偶联剂中的一种或多种，添加量为陶瓷粉体总重量的0.6-0.9wt.％。
6.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S2中，所述的消泡剂采用低级醇类或有机极性化合物，添加量为陶瓷粉体总重量的0.4-0.6wt.％。
7.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S2中，所述的凝胶剂Isobam选自Isobam04、Isobam104、Isobam600中的一种或几种，添加量为陶瓷粉体总重量的15-25wt.％。
8.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S4中，干燥处理工艺为：60-80℃的烘箱中干燥10-15h。
9.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S4中，排胶制度工艺为：室温下以0.5-2℃2mi2的速率升温至400-500℃，保温4-8h，再以0.5-2℃2mi2升温到800-900℃，并保温4-8h。
10.根据权利要求2所述的一种基于Isobam凝胶体系制备透明陶瓷的方法，其特征在于，步骤S5中，真空烧结工艺为：首先在室温按8-10℃2mi2升温到200℃，保温20-30mi2，其次按10-20℃2mi2升温到800℃并保温20-30mi2，再次按6-10℃2mi2升温到1200℃并保温1-2h，然后按1-5℃2mi2升温到1780℃并保温8-16h，最后以5-10℃2mi2降温到室温，整个烧结过程中真空度保持在1×10-2-1×10-5Pa；
取出烧结后的陶瓷再退火，退火工艺为：从室温开始按5-7℃2mi2升温速率升温到200℃，接着按10-12℃2mi2升温速率升温到1200℃，再按4-6℃2mi2升温速率升温到1450℃并保温6h，然后从1450℃以10-12℃2mi2降温速率降到室温。
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