CN115504653A - 一种抗热震开裂的粘土坩埚及制备工艺 - Google Patents

一种抗热震开裂的粘土坩埚及制备工艺 Download PDF

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CN115504653A
CN115504653A CN202211122990.7A CN202211122990A CN115504653A CN 115504653 A CN115504653 A CN 115504653A CN 202211122990 A CN202211122990 A CN 202211122990A CN 115504653 A CN115504653 A CN 115504653A
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crucible
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杨建明
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Anhui Qiji Technology Co.,Ltd.
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Abstract

本发明公开了一种抗热震开裂的粘土坩埚，包括坩埚锅体，一种抗热震开裂的粘土坩埚的制备工艺，包括如下步骤：S1、备料，S2、配料：将多种粉料在搅拌机进行干混，S3、成型：通过成型模具将坩埚挤压成型；S4、修整：去除坩埚表面的不平整处；S5、干燥：坩埚放进干燥设备中60‑80℃干燥2‑4天；S6、烧制；采用本发明制备工艺制得的坩埚热变性能好，对于急冷急热，不易破裂，采用自动光面技术，使接触部位高度致密，延长了坩埚的使用寿命；增加有效传热面，缩小底部剩余料，传热快容量大，耗能省；降低坩埚的高温软化变形及不均匀收缩,提高坩埚的抗玻璃液侵蚀能力，提高坩埚的耐高温、抗玻璃液侵蚀及抗热震性能。

Description

一种抗热震开裂的粘土坩埚及制备工艺
技术领域
本发明属于坩埚技术领域，更具体地说，尤其涉及一种抗热震开裂的粘土坩埚。同时，本发明还涉及一种抗热震开裂的粘土坩埚的制备工艺。
背景技术
坩埚是化学仪器的重要组成部分，它是熔化和精炼金属液体以及固液加热、反应的容器，是保证化学反应顺利进行的基础。
经检索，申请号为201711286342.4的专利公开了坩埚的制备方法及坩埚，该制备方法包括：步骤1：制备坩埚本体；步骤2：在坩埚本体的底壁和侧壁上涂覆石英砂与磷的混合浆液以形成石英砂-磷粉层；步骤3：在石英砂-磷粉层上涂覆氮化硅、硅与磷的混合浆液以形成氮化硅-硅-磷层；步骤4：烘干步骤3中的坩埚本体。石英砂-磷粉层中的磷在利用坩埚铸锭时用于吸附坩埚本体中的金属杂质以防止金属杂质向硅锭中扩散。氮化硅-硅-磷层中的磷在硅锭底壁和侧壁形成一层高磷区，这层高磷区就是一层吸杂层，该吸杂层用于将硅锭内的金属杂质吸附到硅锭的外表面，从而提高硅锭的铸锭质量。
但是上述方案制得的坩埚抗热震性能不佳，耐热冲击性能有待提升，在急冷急热的环境中较容易发生开裂甚至破裂，且上述坩埚的传热效果不佳，耗能高，因此我们需要提出一种抗热震开裂的粘土坩埚及制备工艺。
发明内容
本发明的目的是为了解决现有技术中存在的缺点，采用本发明制备工艺制得的坩埚热变性能好，耐热冲击性能强，对于急冷急热，不易破裂，采用自动光面技术，使接触部位高度致密，既提高了溶液料的纯度，延长了坩埚的使用寿命；增加有效传热面，缩小底部剩余料，传热快容量大，耗能省；降低坩埚的高温软化变形及不均匀收缩,提高坩埚的抗玻璃液侵蚀能力，提高坩埚的耐高温、抗玻璃液侵蚀及抗热震性能，而提出的一种抗热震开裂的粘土坩埚及制备工艺。
为实现上述目的，本发明提供如下技术方案：一种抗热震开裂的粘土坩埚，包括坩埚锅体，坩埚锅体的外径与坩埚锅体的高度之比为0.8：1，所述坩埚锅体包括锅体上部和锅体下部，所述锅体上部包括锅体外壁和锅体内侧壁，所述锅体下部包括锅底和锅体内底部，所述锅体外壁和锅体内侧壁之间的间距为0.8-1.5cm，即坩埚锅体的侧壁厚度为0.8-1.5cm，所述锅体内底部设置为圆弧状的内底部，所述锅底设置为平底，所述锅底和锅体外壁之间设置有圆角。
一种抗热震开裂的粘土坩埚的制备工艺，包括如下步骤：
S1、备料：按照质量份数计，取氧化铝38-50份、氧化硅51-60份、氧化铁5-7份、球黏土2-4份、熟焦1-2份、蜡石0.5-1份、蓝晶石0.2-0.5份、氧化钙0.3-0.6份、氧化钛0.8-1.5份、氧化钠0.05-0.1份、氧化钾0.1-0.5份和硼砂0.8-1.5份，存放备用；
S2、配料：将硼砂首先用热水熔化，将上述称取的其他原料研磨成粉末状，并将多种粉料在搅拌机进行干混，再将硼砂的水溶液倒进干混的混合料中进行湿混；
S3、成型：将上述湿混的半干型泥料过筛，筛除尺寸不合要求的大颗粒块状泥料，并将符合要求的泥料添加至成型模具中，然后通过成型模具将坩埚挤压成型；
S4、修整：对成型的坩埚进行精修和抹平，去除坩埚表面的不平整处；
S5、干燥：将修整好的坩埚放进干燥设备中进行干燥处理，干燥设备的干燥温度设置为60-80℃，干燥的时间为2-4天，使坩埚中的水分含量小于2％；
S6、烧制：首先在干燥后的坩埚表面进行涂釉，然后将坩埚放进窑炉中进行烧制，烧制的过程中，8h升湿至40℃，16h升湿至80℃，24h升温至100℃，32h升温至110℃，40h升温至120℃，48h升温至130C，56h升温至150℃，64h升温至180℃，72h升温至230℃，8Oh升温至290℃，88h升温至370℃，96h升温至470℃，104h升温至610℃，112h升温至860℃，120h升温至1060℃，128h升温至1160℃、保温2h，最后出窑，并在出窑的24h内在坩埚表面刷油。
优选的，按照质量份数计，取氧化铝38份、氧化硅51份、氧化铁5份、球黏土2份、熟焦1份、蜡石0.5份、蓝晶石0.25份、氧化钙0.3份、氧化钛0.8份、氧化钠0.05份、氧化钾0.1份和硼砂0.8份。
优选的，按照质量份数计，取氧化铝44份、氧化硅55份、氧化铁6份、球黏土3份、熟焦1.5份、蜡石0.8份、蓝晶石0.3份、氧化钙0.5份、氧化钛1.2份、氧化钠0.08份、氧化钾0.3份和硼砂1.2份。
优选的，按照质量份数计，取氧化铝50份、氧化硅60份、氧化铁7份、球黏土4份、熟焦2份、蜡石1份、蓝晶石0.5份、氧化钙0.6份、氧化钛1.5份、氧化钠0.1份、氧化钾0.5份和硼砂1.5份。
优选的，在S2中，称取的原料研磨的粉末颗粒的粒径10-50目，多种原料在搅拌机干混的时间为15-20min，原料湿混的时间为25-40min，且混好的泥料需经过15天的困料，泥料在成型前，需在湿碾机上滚压呈泥饼。
优选的，在S3中，过筛时，需将半干型泥料通过8-10目的筛子，成型模具中上模的压力控制在20-25MPa。
优选的，在S5中，干燥设备包括干燥室以及位于干燥室内的链式传输机，所述坩埚位于链式传输机上进行链式烘干，小坩埚的干燥时间为2天，中坩埚的干燥时间为3天，大坩埚的干燥时间为4天。
优选的，在S6中，坩埚表面涂刷的油的配比为沥青漆和汽油各占50％，油漆的比重为0.75-0.85。
本发明的技术效果和优点：本发明提供的一种抗热震开裂的粘土坩埚及制备工艺，与现有技术相比，采用本发明制备工艺制得的坩埚热变性能好，耐热冲击性能强，对于急冷急热，不易破裂，采用自动光面技术，使接触部位高度致密，既提高了溶液料的纯度，延长了坩埚的使用寿命；增加有效传热面，缩小底部剩余料，传热快容量大，耗能省；降低坩埚的高温软化变形及不均匀收缩,提高坩埚的抗玻璃液侵蚀能力，提高坩埚的耐高温、抗玻璃液侵蚀及抗热震性能。
附图说明
图1为本发明的工艺流程图；
图2为本发明坩埚锅体的结构图；
图3为本发明坩埚锅体的剖视图。
图中：1、坩埚锅体；101、锅体外壁；102、锅底；103、锅体内侧壁；104、锅体内底部；105、圆角。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。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
一种抗热震开裂的粘土坩埚，包括坩埚锅体1，坩埚锅体1的外径与坩埚锅体1的高度之比为0.8：1，坩埚锅体1包括锅体上部和锅体下部，锅体上部包括锅体外壁101和锅体内侧壁103，锅体下部包括锅底102和锅体内底部104，锅体外壁101和锅体内侧壁103之间的间距为0.8-1.5cm，即坩埚锅体1的侧壁厚度为0.8-1.5cm，锅体内底部104设置为圆弧状的内底部，锅底102设置为平底，锅底102和锅体外壁101之间设置有圆角105。
一种抗热震开裂的粘土坩埚的制备工艺，包括如下步骤：
S1、备料：按照质量份数计，取氧化铝38-50份、氧化硅51-60份、氧化铁5-7份、球黏土2-4份、熟焦1-2份、蜡石0.5-1份、蓝晶石0.2-0.5份、氧化钙0.3-0.6份、氧化钛0.8-1.5份、氧化钠0.05-0.1份、氧化钾0.1-0.5份和硼砂0.8-1.5份，存放备用；蜡石以径粒状引入；
球黏土可降低坩埚的高温软化变形及不均匀收缩,提高坩埚的抗玻璃液侵蚀能力；增加熟焦用量、减少蜡石用量、引入少量蓝晶石细粉、蜡石以小粒径颗粒引入、提高坩埚泥料的密实性与均匀性等,有益于提高坩埚的耐高温、抗玻璃液侵蚀及抗热震性能；
S2、配料：将硼砂首先用热水熔化，将上述称取的其他原料研磨成粉末状，并将多种粉料在搅拌机进行干混，再将硼砂的水溶液倒进干混的混合料中进行湿混；
S3、成型：将上述湿混的半干型泥料过筛，筛除尺寸不合要求的大颗粒块状泥料，并将符合要求的泥料添加至成型模具中，然后通过成型模具将坩埚挤压成型；
S4、修整：对成型的坩埚进行精修和抹平，去除坩埚表面的不平整处；采用自动光面技术，使接触部位高度致密，既提高了溶液料的纯度，延长了坩埚的使用寿命；
S5、干燥：将修整好的坩埚放进干燥设备中进行干燥处理，干燥设备的干燥温度设置为60-80℃，干燥的时间为2-4天，使坩埚中的水分含量小于2％；
S6、烧制：首先在干燥后的坩埚表面进行涂釉，然后将坩埚放进窑炉中进行烧制，烧制的过程中，8h升湿至40℃，16h升湿至80℃，24h升温至100℃，32h升温至110℃，40h升温至120℃，48h升温至130C，56h升温至150℃，64h升温至180℃，72h升温至230℃，8Oh升温至290℃，88h升温至370℃，96h升温至470℃，104h升温至610℃，112h升温至860℃，120h升温至1060℃，128h升温至1160℃、保温2h，最后出窑，并在出窑的24h内在坩埚表面刷油。
按照质量份数计，取氧化铝38份、氧化硅51份、氧化铁5份、球黏土2份、熟焦1份、蜡石0.5份、蓝晶石0.25份、氧化钙0.3份、氧化钛0.8份、氧化钠0.05份、氧化钾0.1份和硼砂0.8份。
在S2中，称取的原料研磨的粉末颗粒的粒径10-50目，多种原料在搅拌机干混的时间为15-20min，原料湿混的时间为25-40min，且混好的泥料需经过15天的困料，泥料在成型前，需在湿碾机上滚压呈泥饼。
在S3中，过筛时，需将半干型泥料通过8-10目的筛子，成型模具中上模的压力控制在20-25MPa。
在S5中，干燥设备包括干燥室以及位于干燥室内的链式传输机，所述坩埚位于链式传输机上进行链式烘干，小坩埚的干燥时间为2天，中坩埚的干燥时间为3天，大坩埚的干燥时间为4天。
在S6中，坩埚表面涂刷的油的配比为沥青漆和汽油各占50％，油漆的比重为0.75-0.85。
实施例2
与实施例1不同的是，
在S1中，按照质量份数计，取氧化铝44份、氧化硅55份、氧化铁6份、球黏土3份、熟焦1.5份、蜡石0.8份、蓝晶石0.3份、氧化钙0.5份、氧化钛1.2份、氧化钠0.08份、氧化钾0.3份和硼砂1.2份。
实施例3
与实施例1不同的是，
在S1中，按照质量份数计，取氧化铝50份、氧化硅60份、氧化铁7份、球黏土4份、熟焦2份、蜡石1份、蓝晶石0.5份、氧化钙0.6份、氧化钛1.5份、氧化钠0.1份、氧化钾0.5份和硼砂1.5份。
实施例1 实施例2 实施例3
氧化铝 38份 44份 50份
氧化硅 51份 55份 60份
氧化铁 5份 6份 7份
球黏土 2份 3份 4份
熟焦 1份 1.5份 2份
蜡石 0.5份 0.8份 1份
蓝晶石 0.25份 0.3份 0.5份
氧化钙 0.3份 0.5份 0.6份
氧化钛 0.8份 1.2份 1.5份
氧化钠 0.05份 0.08份 0.1份
氧化钾 0.1份 0.3份 0.5份
硼砂 0.8份 1.2份 1.5份
尤其的，在坩埚烧制完成后，还需要对坩埚进行性能测试，先将坩埚放进1100℃的熔样炉中1h，然后取出坩埚冷却，重复3-5次，再对坩埚进行各项理化性能测试；
表1：实施例1中烧制的坩埚性能测试结果
理化性能 企标 实测结果 国内指标 国外指标
耐火度/℃ >1610 1654 1630 1410
显气孔率/％ <35 34 31 32
体积密度/g*cm<sup>-3</sup> >1.6 1.69 1.68 1.77
常温耐压/kg*cm<sup>2</sup> >53 57 56 55
常温抗折强度/MPa >25 26 26 27
表2：实施例1中烧制的坩埚性能测试结果
理化性能 企标 实测结果 国内指标 国外指标
耐火度/℃ >1610 1653 1630 1410
显气孔率/％ <35 36 31 32
体积密度/g*cm<sup>-3</sup> >1.6 1.70 1.68 1.77
常温耐压/kg*cm<sup>2</sup> >53 56 56 55
常温抗折强度/MPa >25 27 26 27
表3：实施例1中烧制的坩埚性能测试结果
理化性能 企标 实测结果 国内指标 国外指标
耐火度/℃ >1610 1655 1630 1410
显气孔率/％ <35 35 31 32
体积密度/g*cm<sup>-3</sup> >1.6 1.65 1.68 1.77
常温耐压/kg*cm<sup>2</sup> >53 55 56 55
常温抗折强度/MPa >25 27 26 27
综上所述：采用本发明制备工艺制得的坩埚热变性能好，耐热冲击性能强，对于急冷急热，不易破裂，采用自动光面技术，使接触部位高度致密，既提高了溶液料的纯度，延长了坩埚的使用寿命；增加有效传热面，缩小底部剩余料，传热快容量大，耗能省；降低坩埚的高温软化变形及不均匀收缩,提高坩埚的抗玻璃液侵蚀能力，提高坩埚的耐高温、抗玻璃液侵蚀及抗热震性能。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种抗热震开裂的粘土坩埚，包括坩埚锅体(1)，坩埚锅体(1)的外径与坩埚锅体(1)的高度之比为0.8：1，其特征在于：所述坩埚锅体(1)包括锅体上部和锅体下部，所述锅体上部包括锅体外壁(101)和锅体内侧壁(103)，所述锅体下部包括锅底(102)和锅体内底部(104)，所述锅体外壁(101)和锅体内侧壁(103)之间的间距为0.8-1.5cm，即坩埚锅体(1)的侧壁厚度为0.8-1.5cm，所述锅体内底部(104)设置为圆弧状的内底部，所述锅底(102)设置为平底，所述锅底(102)和锅体外壁(101)之间设置有圆角(105)。
2.一种抗热震开裂的粘土坩埚的制备工艺，基于权利要求1所述的一种抗热震开裂的粘土坩埚，其特征在于，包括如下步骤：
S1、备料：按照质量份数计，取氧化铝38-50份、氧化硅51-60份、氧化铁5-7份、球黏土2-4份、熟焦1-2份、蜡石0.5-1份、蓝晶石0.2-0.5份、氧化钙0.3-0.6份、氧化钛0.8-1.5份、氧化钠0.05-0.1份、氧化钾0.1-0.5份和硼砂0.8-1.5份，存放备用；
S2、配料：将硼砂首先用热水熔化，将上述称取的其他原料研磨成粉末状，并将多种粉料在搅拌机进行干混，再将硼砂的水溶液倒进干混的混合料中进行湿混；
S3、成型：将上述湿混的半干型泥料过筛，筛除尺寸不合要求的大颗粒块状泥料，并将符合要求的泥料添加至成型模具中，然后通过成型模具将坩埚挤压成型；
S4、修整：对成型的坩埚进行精修和抹平，去除坩埚表面的不平整处；
S5、干燥：将修整好的坩埚放进干燥设备中进行干燥处理，干燥设备的干燥温度设置为60-80℃，干燥的时间为2-4天，使坩埚中的水分含量小于2％；
S6、烧制：首先在干燥后的坩埚表面进行涂釉，然后将坩埚放进窑炉中进行烧制，烧制的过程中，8h升湿至40℃，16h升湿至80℃，24h升温至100℃，32h升温至110℃，40h升温至120℃，48h升温至130C，56h升温至150℃，64h升温至180℃，72h升温至230℃，8Oh升温至290℃，88h升温至370℃，96h升温至470℃，104h升温至610℃，112h升温至860℃，120h升温至1060℃，128h升温至1160℃、保温2h，最后出窑，并在出窑的24h内在坩埚表面刷油。
3.根据权利要求2所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：按照质量份数计，取氧化铝38份、氧化硅51份、氧化铁5份、球黏土2份、熟焦1份、蜡石0.5份、蓝晶石0.25份、氧化钙0.3份、氧化钛0.8份、氧化钠0.05份、氧化钾0.1份和硼砂0.8份。
4.根据权利要求3所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：按照质量份数计，取氧化铝44份、氧化硅55份、氧化铁6份、球黏土3份、熟焦1.5份、蜡石0.8份、蓝晶石0.3份、氧化钙0.5份、氧化钛1.2份、氧化钠0.08份、氧化钾0.3份和硼砂1.2份。
5.一种权利要求3所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：按照质量份数计，取氧化铝50份、氧化硅60份、氧化铁7份、球黏土4份、熟焦2份、蜡石1份、蓝晶石0.5份、氧化钙0.6份、氧化钛1.5份、氧化钠0.1份、氧化钾0.5份和硼砂1.5份。
6.根据权利要求2所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：在S2中，称取的原料研磨的粉末颗粒的粒径10-50目，多种原料在搅拌机干混的时间为15-20min，原料湿混的时间为25-40min，且混好的泥料需经过15天的困料，泥料在成型前，需在湿碾机上滚压呈泥饼。
7.根据权利要求2所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：在S3中，过筛时，需将半干型泥料通过8-10目的筛子，成型模具中上模的压力控制在20-25MPa。
8.根据权利要求2所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：在S5中，干燥设备包括干燥室以及位于干燥室内的链式传输机，所述坩埚位于链式传输机上进行链式烘干，小坩埚的干燥时间为2天，中坩埚的干燥时间为3天，大坩埚的干燥时间为4天。
9.根据权利要求2所述的一种抗热震开裂的粘土坩埚的制备工艺，其特征在于：在S6中，坩埚表面涂刷的油的配比为沥青漆和汽油各占50％，油漆的比重为0.75-0.85。
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