CN110922175A - 一种高性能多晶硅铸锭用熔融石英坩埚的制备方法 - Google Patents

一种高性能多晶硅铸锭用熔融石英坩埚的制备方法 Download PDF

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CN110922175A
CN110922175A CN201911209071.1A CN201911209071A CN110922175A CN 110922175 A CN110922175 A CN 110922175A CN 201911209071 A CN201911209071 A CN 201911209071A CN 110922175 A CN110922175 A CN 110922175A
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fused quartz
polycrystalline silicon
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曹伟
黄蓉帅
钟德京
习小青
张学日
赵子豪
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SINOMA JIANGSU SOLAR ENERGY NEW MATERIALS CO Ltd
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Abstract

一种高性能多晶硅铸锭用熔融石英坩埚的制备方法，使用了一定比例的整形砂作为骨料，降低了料浆水分和浆砂比，调整了骨料配方里粗、中端的占比，实现了体密的明显提升，也提升了抗折强度，同时减少了析晶比例和增加了坩埚的高温蠕变性。本发明技术方案实现了体密2%~8%的提升，抗折强度提升4%~15%，在铸锭端的具体表现包括缩短铸锭时间2~7小时/炉，极大地提升了生产效率。以此同时，坩埚的抗热震稳定性和高温低蠕变性得到保障，坩埚的安全性得到明显提升。

Description

一种高性能多晶硅铸锭用熔融石英坩埚的制备方法
技术领域
本发明涉及一种石英坩埚的生产制造技术，特别是一种高性能多晶硅铸锭用熔融石英坩埚的制备方法。
背景技术
为适应铸锭厂家越来越大的过冷度和高安全性需求，坩埚需提高抗热震性和高温蠕变强度；另外，单多晶硅铸锭厂家越来越关注生产效率，坩埚的导热性逐渐成为一项关键指标，在铸锭工艺允许的范围内坩埚的导热性有保障可缩短铸锭时间。
现有技术中《一种高致密度石英坩埚的制备方法》申请号为：201810397839.1的中国专利申请，它公开了一种高致密度石英坩埚的制备方法，包括如下步骤：1)浸渍：将养护后排净内部水分的石英坩埚生坯置于硅溶胶中于常温常压下浸渍，控制每只坩埚的二氧化硅浸渍量不超过坩埚重量的1％；2)烘干、烧制：将浸渍后的石英坩埚坯体取出后烘干，后置于1160～1170℃的环境下烧制12～18小时，即得。采用硅溶胶浸渍的方法所得的石英坩埚体密不高，高温蠕变性性差。
《一种注凝成型熔融石英坩埚的制造方法》申请号：201710161949.3的中国专利申请，它分开了一种注凝成型熔融石英坩埚的制造方法，包括以下步骤：步骤S1、将熔融石英砂、水、丙烯酰胺和交联剂混合并充分搅拌，得到料浆；步骤S2、在不锈钢模具的内表面上涂覆粒度在30微米以内的熔融石英砂，再向所述不锈钢模具内浇注所述浆料；步骤S3、将浇注后的不锈钢模具置于烘箱中进行保温固化，并脱模得到坩埚坯体；步骤S4、对所得坩埚坯体依次进行干燥和烧成，得到注凝成型熔融石英坩埚。所涂覆熔融石英砂会烧结形成更加致密的一层熔融石英砂陶瓷层，从而提高了坩埚外表面的致密度和强度，但在养护过程因收缩会导致出现缺陷和裂纹。
发明内容
本发明要解决的技术问题是针对现有技术的不足，提出了一种高性能多晶硅铸锭用熔融石英坩埚的制备方法。生产的坩埚具有高体密、高导热性、高抗热震强度和高温低蠕变性。
本发明要解决的技术问题是通过以下技术方案来实现的，一种高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特点是：
1）制备细浆，将粗颗粒熔融石英砂、熔融石英玻璃料两种原料按照配比1：0.2~1混合，加水研磨成细浆，细浆的中位粒径在7~10μm之间；最终细浆的水分的质量百分比控制在10%~15%之间；
2）细浆和骨料混匀搅拌，按照1：0.9~1.2的比例取细浆与熔融石英砂颗粒骨料搅拌混合，
所述的熔融石英砂颗粒骨料是指在粒度15~200目的熔融石英砂中掺入有质量百分比为20%~70%的整形砂颗粒，
添加的整形砂颗粒级配为15目~30目：30目~50目：50目~80目=0.3~0.5：0.3~0.5：0.1~0.3；
在混合过程中分别加入占混合砂浆总重0.2％~1%的单体、占混合砂浆总重0.002%~0.01%的交联剂、占混合砂浆总重0.005%~0.03%的乳酸；混合砂浆最终水分控制在6.0%~6.8%；
3）抽真空搅拌消除气泡，在上述混合砂浆中加入水溶性偶氮类引发剂，添加比例为混合砂浆总重的0.03%~0.08%，抽真空负压状态下搅拌消除混合砂浆中的气泡，保持砂浆在10℃~18℃之间；
4）将不锈钢材质的模具整个腔体内表面均匀地涂覆一层油性脱模剂，内、外模组合好即完成进行密封，只留注浆口和出气孔，涂覆好脱模剂后干燥10~30min成膜后上注浆平台进行注浆操作，注浆过程采用微正压0.1~0.3MPa；
5）完成注浆后密闭注浆口和出气孔，将模具整体浸入60℃~80℃的温水中水浴加热10min~60min，使腔体内的砂浆固化成型，形成生坯；
6）将成型的生坯从模具中解出，下一步养护干燥，65℃以上温度保温10h~20h烘干生坯内的水分；
7）烘干后的坩埚生坯进隧道窑烧制，经过1160℃~1175℃的高温，时长260min~300min的烧结，坩埚由生坯烧至成品；
8）成品坩埚抽检体密和抗折强度，达标后产品流入后加工工序，至此坩埚的制备完成。
本发明要解决的技术问题还可以通过以下技术方案来进一步实现，添加的单体为氯乙烯、已内酰胺或丙烯酰胺中一种或任意几种的组合。
本发明要解决的技术问题还可以通过以下技术方案来进一步实现，交联剂为有机过氧化物。
本发明要解决的技术问题还可以通过以下技术方案来进一步实现，水溶性偶氮类引发剂为V-50引发剂、VA-044引发剂或V-501引发剂中的任意一种。
本发明要解决的技术问题还可以通过以下技术方案来进一步实现，体密标准为1.93~2.07g/cm3，抗折强度标准为23MPa~28MPa。
本发明与现有技术相比，
本发明在稳定现有制浆工艺及过程的前提下，生产出了高体密、高导热性、高安全性、高抗热震强度、高温低蠕变性的坩埚；料浆骨料中的熔融石英砂颗粒整形处理，提高颗粒的堆积密度；通过添加整形颗粒，在保证料浆粘度可实现顺利注浆的基础上，形成低水份、低浆砂比的料浆，具有较好的流动性和较小触变性；一种良好的骨料颗粒级配配比，增加堆密的同时，保证粗、中端有较高的占比；保证坩埚的烧结程度和均一性。
优点在于：通过颗粒整形，在保证注浆可行性的基础上实现了低水份、低浆砂比料浆，进而降低了坩埚在养护过程因收缩导致的缺陷和裂纹；另外，由于固相含量的增加及更紧密的填充堆积，减少了坩埚高温状态下的蠕变性，同时提高了坩埚的抗热震稳定性，骨料配方里粗、中端较高的占比减缓了坩埚在铸锭端长时间高温下的析晶反应等。
使用了一定比例的整形砂作为骨料，降低了料浆水分和浆砂比，调整了骨料配方里粗、中端的占比，实现了体密的明显提升，也提升了抗折强度，同时减少了析晶比例和增加了坩埚的高温蠕变性。
附图说明
图1为β 方石英→α方石英的晶相转变过程（a→f）图；
图2为30目骨料颗粒整形前后处理后放大（×50）效果图。
具体实施方式
以下进一步描述本发明的具体技术方案，以便于本领域的技术人员进一步地理解本发明，而不构成对其权利的限制。
一种高性能多晶硅铸锭用熔融石英坩埚的制备方法，
1）制备细浆，细浆是指中位粒径在7~10μm之间的熔融石英浆。将粗颗粒熔融石英砂（颗粒大小2~15mm）、熔融石英玻璃料（形状不规则，大小20~200mm）两种原料按照配比1：（0.2~1）加水研磨，使用1~10t容量的大型球磨机研磨成细浆，研磨所用球石材料不仅限于氧化铝、氧化锆，球石粒径为50mm~150mm之间，最终细浆的水分在10%~15%之间；
2）细浆和骨料混匀搅拌，过程中加入单体、交联剂、乳酸。按照比例（1：0.9~1.2）取细浆与已掺入20%~70%整形砂（15目~80目）的熔融石英砂颗粒搅拌混合，该整形砂已边角圆滑处理，获得办法不仅限于湿磨、干磨、化学抛光法，所得整形砂的球度范围0.5~0.9，混合砂浆最终水分6.0%~6.8%；
原生的颗粒骨料为直接物理撞击破碎所得，棱角分明且形状不规则，粒度15~200目，本发明中涉及整形砂颗粒的边角圆滑处理，获得办法不仅限于湿磨、干磨、化学抛光法，所得整形砂的球度范围0.5~0.9，通过添加该颗粒可提升一定的坩埚体密；
所述的熔融石英砂颗粒骨料是指在粒度15~200目的原生的熔融石英砂中掺入有质量百分比为20%~70%的整形砂颗粒，
添加的整形砂颗粒级配为15目~30目：30目~50目：50目~80目=0.3~0.5：0.3~0.5：0.1~0.3；
添加的单体不仅限于氯乙烯、已内酰胺、丙烯酰胺，添加比例为混合砂浆总重的0.2％~1%，添加单体可使混合砂浆内部发生聚合反应或缩聚反应；添加的交联剂为有机过氧化物，不仅限于过氧化二异丙苯(DCP）、过氧化氢二异丙苯、二叔丁基过氧化物(DTBP），交联剂又称作架桥剂，在聚合物分子链之间形成桥键，变为三维结构的不溶性物质，添加比例为混合砂浆总重的0.002%~0.01%；乳酸，添加比例为混合砂浆总重的0.005%~0.03%，作用是降低料浆的粘度，改善浆砂流动性；
3）抽真空搅拌消除气泡。混合砂浆中加入水溶性偶氮类引发剂，添加比例为混合砂浆总重的0.03%~0.08%，用于不饱和聚酯的交联固化和高分子交联反应，不仅限于V-50引发剂、VA-044引发剂、V-501引发剂，抽真空负压状态下搅拌消除混合砂浆中的气泡，真空度范围(-0.08MPa)~（-0.1MPa），保持砂浆在循环水冷却下温度在10℃~18℃之间；混合料浆粘度范围7000mPa.s~12000mPa.s。
4）同时，将不锈钢材质的模具整个腔体内表面均匀地涂覆一层油性脱模剂（厚度＜100μm），作用是防止混合砂浆与模具腔体内部黏连，阻碍脱模。模具分为内模和外模，内、外模组合好即完成进行密封，只留注浆口和出气孔。涂覆好脱模剂后干燥10~30min成膜后上注浆平台进行注浆操作，注浆过程采用微正压0.1~0.3MPa；
5）完成注浆后密闭注浆口和出气孔，将模具整体浸入温水（60℃~80℃）中水浴加热10min~60min，使腔体内的砂浆固化成型，形成生坯；
6）将成型的生坯从模具中解出，下一步养护干燥，65℃以上温度保温10h~20h烘干生坯内的水分；
7）烘干后的坩埚生坯进隧道窑烧制，经过1160℃~1175℃的高温，时长260min~300min的烧结，坩埚由生坯烧至成品；
8）成品坩埚抽检体密和抗折强度，体密标准1.93~2.07g/cm3，抗折强度标准23MPa~28MPa，达标后产品流入后加工工序，至此坩埚的制备完成。
坩埚在铸锭过程中，熔融石英逐渐转变为方石英，方石英的析出自石英颗粒的界面处逐渐向内部进行，在铸锭过程结束后，小颗粒熔融石英基本转变为方石英，而较大的颗粒则外侧转变为晶体，内部保留熔融石英的状态，如图1（a→f）所示。整形后的石英颗粒减少了反应界面，进而减少了析晶比例，也间接增强了坩埚抗热震性。
实验证明：骨料中的大石英颗粒边角变圆滑，实现了整形效果。边角圆滑能一定程度上的提升料浆的流动性，在此基础上，再进一步实现降低水分和低浆砂比，这对提升坩埚体密、抗折强度和均一性均有正向作用。在进行骨料颗粒整形后，30目骨料颗粒边角明显圆滑。根据实验验证，通过颗粒整形，骨料颗粒的堆积密度可提升15%~20%，坩埚成品的体密提升2%~8%。

Claims (5)

1.一种高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特征在于：
1）制备细浆，将粗颗粒熔融石英砂、熔融石英玻璃料两种原料按照配比1：0.2~1混合，加水研磨成细浆，细浆的中位粒径在7~10μm之间；最终细浆的水分的质量百分比控制在10%~15%之间；
2）细浆和骨料混匀搅拌，按照1：0.9~1.2的比例取细浆与熔融石英砂颗粒骨料搅拌混合，
所述的熔融石英砂颗粒骨料是指在粒度15~200目的熔融石英砂中掺入有质量百分比为20%~70%的整形砂颗粒，
添加的整形砂颗粒级配为15目~30目：30目~50目：50目~80目=0.3~0.5：0.3~0.5：0.1~0.3；
在混合过程中分别加入占混合砂浆总重0.2％~1%的单体、占混合砂浆总重0.002%~0.01%的交联剂、占混合砂浆总重0.005%~0.03%的乳酸；混合砂浆最终水分控制在6.0%~6.8%；
3）抽真空搅拌消除气泡，在上述混合砂浆中加入水溶性偶氮类引发剂，添加比例为混合砂浆总重的0.03%~0.08%，抽真空负压状态下搅拌消除混合砂浆中的气泡，保持砂浆在10℃~18℃之间；
4）将不锈钢材质的模具整个腔体内表面均匀地涂覆一层油性脱模剂，内、外模组合好即完成进行密封，只留注浆口和出气孔，涂覆好脱模剂后干燥10~30min成膜后上注浆平台进行注浆操作，注浆过程采用微正压0.1~0.3MPa；
5）完成注浆后密闭注浆口和出气孔，将模具整体浸入60℃~80℃的温水中水浴加热10min~60min，使腔体内的砂浆固化成型，形成生坯；
6）将成型的生坯从模具中解出，下一步养护干燥，65℃以上温度保温10h~20h烘干生坯内的水分；
7）烘干后的坩埚生坯进隧道窑烧制，经过1160℃~1175℃的高温，时长260min~300min的烧结，坩埚由生坯烧至成品；
8）成品坩埚抽检体密和抗折强度，达标后产品流入后加工工序，至此坩埚的制备完成。
2.根据权利要求1所述的高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特征在于：添加的单体为氯乙烯、已内酰胺或丙烯酰胺中一种或任意几种的组合。
3.根据权利要求1所述的高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特征在于：交联剂为有机过氧化物。
4.根据权利要求1所述的高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特征在于：水溶性偶氮类引发剂为V-50引发剂、VA-044引发剂或V-501引发剂中的任意一种。
5.根据权利要求1所述的高性能多晶硅铸锭用熔融石英坩埚的制备方法，其特征在于：体密标准为1.93~2.07g/cm3，抗折强度标准为23MPa~28MPa。
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