CN105424444A - 一种耐火材料抗渣试样及其制备方法 - Google Patents
一种耐火材料抗渣试样及其制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 31
- 229910052742 iron Inorganic materials 0.000 abstract description 15
- 238000002474 experimental method Methods 0.000 abstract description 2
- 235000013339 cereals Nutrition 0.000 description 53
- 239000010431 corundum Substances 0.000 description 51
- 229910052593 corundum Inorganic materials 0.000 description 51
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 35
- 239000003595 mist Substances 0.000 description 29
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 15
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Abstract
本发明属于耐火材料领域,主要涉及一种耐火材料抗渣试样及其制备方法。提出的一种耐火材料抗渣试样为下端面封闭的圆筒状坩埚;圆筒状坩埚具有上下设置的反应区(1)和盛铁区(2);反应区(1)与盛铁区(2)的接合面与圆筒状坩埚上端面之间的距离为圆筒状坩埚内腔深度的1/2~3/4;反应区(1)至少由两块不同材质的弧形块一体成型;圆筒状坩埚的内径为100mm~200mm;圆筒状坩埚的侧壁厚为10mm~30m,底厚为20mm~50mm;圆筒状坩埚的内腔深度为内径的1.2~2倍。本发明避免了试验中渣从材料间接缝的渗漏,成功解决了多组不同材质耐火材料样品同炉、同时、同渣条件下抗渣性可进行对比的技术问题。
Description
技术领域
本发明属于耐火材料领域,主要涉及一种耐火材料抗渣试样及其制备方法。
背景技术
耐火材料是高温领域的关键材料;绝大部分耐火材料在高温下与熔体直接接触,熔渣对耐火材料的损毁程度将直接影响耐火材料的使用性能。在实际使用中,熔渣与耐火材料的相互作用十分复杂,主要表现为熔渣对耐火材料的化学侵蚀、渗透和冲刷。而熔渣的成分、粘度、与耐火材料相对运动的速率等,以及环境的温度、压强、气氛等都对耐火材料的抗渣性产生影响。
在实际生产和工业应用中,以及耐火材料的科学研究中,耐火材料的抗渣性被作为评价耐火材料的一项重要性能被广泛使用;但由于影响耐火材料的抗渣性因素太多,各种热工设备使用的耐火材料所处的工况各不相同,目前的耐火材料抗渣性试验方法对许多特定应用环境所使用的耐火材料评价结果与实际使用结果存在较大出入。而各种实验方法对抗渣试样及其制备方法也提出了不同的要求。
美国材料与试验协会提出了耐火材料的回转抗渣试验方法标准(ASTMC874-11aStandardTestMethodforRotarySlagTestingofRefractoryMaterials),它是将6组耐火材料制品切成一定尺寸和形状的试样,通过耐火泥浆粘接组成一个具有六棱柱空腔的结构,将其砌筑在一个圆筒形炉壳内,以六棱柱空腔为炉膛,六棱柱的顶部和底部分别为进渣/进气口和出渣/出气口;试验时将炉膛卧倒呈水平,炉膛以六棱柱轴线为轴进行转动,以可燃气体和氧气的混合气体为加热源对炉膛中心加热,试验过程中间歇性加渣和出渣;通过测定试验前后耐火材料试样厚度的变化评价耐火材料的抗渣性;该方法以标型砖为原始测试样品,通过后期切削成一定的规则形状,然后通过耐火泥浆涂抹粘接的方式实现了多个样品的拼接组合;其抗渣试样的优点在于可以保留市售产品的组织结构和原砖面,最大限度地保证了被测试样品的“原汁原味”;然而,由于样品之间是靠耐火泥浆粘接,而非天然一体,导致抗渣过程中两个样品间的接缝常常成为薄弱部位,造成熔渣从砖缝处渗漏而被迫终止试验;而且,这种抗渣试样的厚度一般为64mm~65mm,若采用中频感应等间接加热方式时,由于砖太厚电磁场的穿透性受到一定限制。
我国现行国家标准GB/T8931—2007耐火材料抗渣性试验方法中出提出和美国ASTM标准相似的回转渣蚀法外,还提出了一种耐火材料研究中普遍采用的抗渣性试验方法——静态坩埚法,它是将耐火材料样品制成坩埚状,给坩埚内装上试验渣后置于炉膛内,让高温下熔渣与坩埚发生反应,以熔渣对坩埚试样剖面的侵蚀量和渗透量来评价耐火材料抗渣性的优劣;该方法所用抗渣试样的制备通常是从大块样品上切削钻磨来制取,或者以模具压制散装料成型坯体或振动浇注坯体后烧制而成;该试验方法强调试样个体之间的独立和试验条件的一致,其试样一般由一种材质构成,无法实现多材质的相互拼接组合。
发明内容
为解决上述技术问题,本发明的目的是提出一种耐火材料抗渣试样及其制备方法。
一种耐火材料抗渣试样,所述的耐火材料抗渣试样为下端面封闭的圆筒状坩埚;所述的圆筒状坩埚具有上下设置的反应区和盛铁区;所述反应区与盛铁区的接合面与圆筒状坩埚上端面之间的距离为圆筒状坩埚内腔深度的1/2~3/4;所述的反应区至少由两块不同材质的弧形块一体成型;所述圆筒状坩埚的内径为100mm~200mm;所述圆筒状坩埚的侧壁厚为10mm~30mm;所述圆筒形坩埚的底厚为20mm~50mm;所述圆筒状坩埚的内腔深度为内径的1.2~2倍。
所述盛铁区的材质为刚玉、刚玉-尖晶石、莫来石、刚玉-莫来石中的一种。
制备上述一种耐火材料抗渣试样的制备方法,其具体步骤如下:
1)耐火材料抗渣试样材料的准备:将制作耐火材料抗渣试样的反应区的多种材料、盛铁区的材料分别造粒成型,得到反应区多种材料的造粒料以及盛铁区材料的造粒料;
2)然后根据所制备耐火材料抗渣试样的大小选择合适的圆筒状坩埚模具,并准备与圆筒状坩埚模具的侧壁厚度相同的塑料条或硬纸条若干个;
3)根据反应区所选用材质的数量选取相同数量的塑料条或硬纸条;然后将塑料条或硬纸条的放入圆筒状坩埚模具内,并使多个所述的塑料条或硬纸条在圆筒状坩埚模具内均匀分布;在每两个相邻塑料条或硬纸条所构成的区域内放置所对应的反应区材料造粒料,当反应区材料造粒料布料的高度到达反应区所需的高度后;抽出之前用于阻隔物料的塑料条或硬纸条,再将盛铁区材质的造粒料布料到模具空腔的剩余空间内,采用冷等静压成形工艺或振动加压捣打成形工艺成形坯体;坯体干燥后经1500℃~1800℃高温烧成,经检测无裂纹、无变形后即得耐火材料抗渣试样。
本发明提出的一种耐火材料抗渣试样及其制备方法,耐火材料抗渣试样的反应区由多种材质一体成型,可以在相同条件下同时对多种材质进行抗渣性对比;避免了试验中渣从材料间接缝的渗漏,成功解决了多组不同材质耐火材料样品同炉、同时、同渣条件下抗渣性可进行对比的技术问题,抗渣试样的制备方法简单易行;耐火材料抗渣试样采用圆筒状坩埚,在对耐火材料抗渣试样可以较好的保证了对比样试验条件和环境的一致性,提高了对比结果的说服性;耐火材料抗渣试样盛铁区的设置是为了利用中频感应产生的涡流加热熔化铁水,而以这些熔化的铁水为热源通过热的传导和辐射来加热试验渣和耐火材料坩埚试样,当铁和渣都熔化后由于铁的密度高,渣的密度低,会使坩埚内形成铁水在下、渣液在上的熔池,在电磁场的作用下,铁水形成涡流带动渣液翻滚流动;铁水和渣液之间的平面俗称“铁线”,在此试验中由于渣液和铁水的波动,“铁线”并非静止的;为防止“铁线”降低时熔渣对盛铁区耐火材料的侵蚀,需要将具有抗渣性的耐火材料布置在理论铁线位置以下,而本发明中设计的理论铁线位置位于坩埚深度的中部,因而要求盛铁区和反应区耐火材料的界线位于距坩埚上沿内腔深度的1/2~3/4。
附图说明
图1为本发明中抗渣试样的材质分布示意图。
图中,1、反应区,2、盛铁区。
具体实施方式
结合附图和具体实施例对本发明加以说明:
实施例1,如图1所示,一种耐火材料抗渣试样,所述的耐火材料抗渣试样为下端面封闭的圆筒状坩埚;所述的圆筒状坩埚具有上下设置的反应区1和盛铁区2;所述反应区1与盛铁区2的接合面与圆筒状坩埚上端面之间的距离为圆筒状坩埚内腔深度的2/3;所述的反应区1至少由两块不同材质的弧形块一体成型;该实施例中,所述的反应区1由四块不同材质的弧形块一体成型;所述圆筒状坩埚的内径为100mm~200mm;所述圆筒状坩埚的侧壁厚为10mm~30mm;所述圆筒形坩埚的底厚为20mm~50mm;所述圆筒状坩埚的内腔深度为内径的1.2~2倍;该实施例中,所述的圆筒状坩埚由刚玉(Al2O3≥99%)、刚玉-莫来石(Al2O3=95%、SiO2=5%)、莫来石(Al2O3=72%、SiO2=28%)、刚玉-尖晶石(Al2O3=95%、MgO=5%)4种材质的样品拼接组合而成,圆筒状坩埚的内径为150mm,侧壁厚20mm,底厚35mm,内腔深度192mm;盛铁区2的材质为刚玉-莫来石(Al2O3=95%、SiO2=5%),反应区1以坩埚底朝下口朝上俯视逆时针材质依次为刚玉(Al2O3≥99%)、刚玉-莫来石(Al2O3=95%、SiO2=5%)、莫来石(Al2O3=72%、SiO2=28%)、刚玉-尖晶石(Al2O3=95%、MgO=5%),4种材质将圆周等分;盛铁区和反应区的分界线位于坩埚圆周上距坩埚上沿128mm处;坩埚采用冷等静压一体成形,坯体是一个无接缝整体,经1650℃保温5h电炉内烧成,烧成后的坩埚无裂纹、尺寸规整、无变形。
制备上述一种耐火材料抗渣试样的制备方法,其具体步骤如下:
1)耐火材料抗渣试样材料的准备:将制作耐火材料抗渣试样的反应区的多种材料、盛铁区的材料分别造粒成型,得到反应区多种材料的造粒料以及盛铁区材料的造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、D50=5μm的烧结氧化铝微粉20份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉15份、D50=5μm的烧结氧化铝微粉20份、D50=1μm的硅微粉5份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉-莫来石造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔莫来石颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的烧结莫来石细粉20份、D50=5μm的烧结氧化铝微粉15份、D50=1μm的硅微粉5份、纸浆废液4份采用高速混炼机混合均匀,形成莫来石造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、颗粒粒度小于0.074mm大于等于0.043mm的烧结镁砂5份、D50=5μm的烧结氧化铝微粉15份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉-尖晶石造粒料;各原料组分的份数以质量计;
2)然后根据所制备耐火材料抗渣试样的大小选择合适的圆筒状坩埚模具,并准备与圆筒状坩埚模具的侧壁厚度相同的塑料条或硬纸条4个;
3)根据反应区所选用材质的数量选取相同数量的塑料条或硬纸条;然后将塑料条或硬纸条的放入圆筒状坩埚模具内,并使4个所述的塑料条或硬纸条在圆筒状坩埚模具内均匀分布;在每两个相邻塑料条或硬纸条所构成的区域内放置所对应的反应区材料造粒料,当反应区材料造粒料布料的高度到达反应区所需的高度后;抽出之前用于阻隔物料的塑料条或硬纸条,再将盛铁区材质的造粒料布料到模具空腔的剩余空间内,采用冷等静压成形工艺成形坯体;坯体干燥后经1650℃保温5h电炉内烧成,经检测无裂纹、无变形后即得抗渣试样。
若反应区中有高温下易氧化的材质,坯体在高温烧成时应采用惰性气氛或埋炭气氛;防止试样在烧成时性能被破坏,影响后期的抗渣试验。
实施例2
实施例2的主体结构同实施例1,该实施例中,所述的圆筒状坩埚是由刚玉(Al2O3≥99%)、高铬(Cr2O3=90%、Al2O3=10%)、铬刚玉(Cr2O3=10%、Al2O3=90%)、刚玉-尖晶石(Al2O3=95%、MgO=5%)4种材质的样品拼接组合而成的坩埚,坩埚有底无盖呈圆筒状,试样坩埚内径为200mm,侧壁厚30mm,底厚50mm,内腔深度400mm;盛铁区的材质为刚玉-尖晶石(Al2O3=95%、MgO=5%),反应区以坩埚底朝下口朝上俯视逆时针材质依次为刚玉(Al2O3≥99%)、高铬(Cr2O3=90%、Al2O3=10%)、铬刚玉(Cr2O3=10%、Al2O3=90%),3种材质将圆周等分;盛铁区和反应区的分界线位于坩埚圆周上距坩埚上沿200mm处;坩埚采用冷等静压一体成形,坯体是一个无接缝整体,经1800℃保温10h燃气窑内烧成,烧成后的坩埚无裂纹、尺寸规整、无变形。
该坩埚的制备方法如下:
首先,将用于坩埚制作的4种选定材质的材料分别进行造粒成形。以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、D50=5μm的烧结氧化铝微粉20份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔氧化铬颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔氧化铬细粉15份、D50=5μm的烧结氧化铝微粉10份、D50=5μm的氧化铬绿微粉15份、磷酸二氢铝水溶液4份采用高速混炼机混合均匀,形成高铬造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的板状刚玉细粉20份、D50=5μm的烧结氧化铝微粉10份、D50=5μm的氧化铬绿微粉10份、纸浆废液4份采用高速混炼机混合均匀,形成莫来石造粒料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、颗粒粒度小于0.074mm大于等于0.043mm的烧结镁砂5份、D50=5μm的烧结氧化铝微粉15份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉-尖晶石造粒料。
然后,采用冷等静压成形工艺成形耐火材料抗渣试样坩埚坯体。采用坩埚底朝上、口朝下的加料方式,用与坩埚侧壁模具空腔厚度相当宽度的塑料条将坩埚侧壁模具空腔分割成所需数量的单元空间,反应区的刚玉、高铬、铬刚玉3种造粒料分别加入到不同单元空间内,布料至设定的高度后抽出之前用于阻隔物料的塑料条,再将盛铁区刚玉-尖晶石造粒料布料到模具空腔剩余空间,在冷等静压机中一定压力下成形坯体。
最后,坯体干燥后经1800℃保温10h燃气窑内烧成,经检测无裂纹、无变形后即得抗渣试样。
实施例3:
实施例2的主体结构同实施例1,该实施例中,所述的圆筒形坩埚由刚玉(Al2O3≈99%)、刚玉-尖晶石-ZrO2(Al2O3=87%、MgO=8%、ZrO2=4%)、Al2O3-ZrO2(Al2O3=94%、ZrO2=5%)3种材质的样品拼接组合而成的坩埚,坩埚有底无盖呈圆筒状,试样坩埚内径为100mm,侧壁厚10mm,底厚25mm,内腔深度120mm;盛铁区材质为刚玉(Al2O3≈99%),反应区材质分别为刚玉-尖晶石-ZrO2(Al2O3=90%、MgO=5%、ZrO2=4%)、Al2O3-ZrO2(Al2O3=94%、ZrO2=5%),2种材质将圆周等分;盛铁区和反应区的分界线位于坩埚圆周上距坩埚上沿90mm处;坩埚采用振动加压捣打一体成形,坯体是一个无接缝整体,经1500℃保温5h电炉内烧成,烧成后的坩埚无裂纹、尺寸规整、无变形。
该坩埚的制备方法如下:
首先,将用于坩埚制作的3种选定材质的材料分别进行混料。以颗粒粒度小于2mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、D50=5μm的烧结氧化铝微粉20份、纸浆废液5份采用碾轮式混砂机混合均匀,形成刚玉泥料;以颗粒粒度小于2mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔尖晶石细粉(Al2O3≈78%)15份、颗粒粒度小于0.074mm大于等于0.043mm的烧结镁砂5份、D50=5μm的烧结氧化铝微粉16份、D50=5μm的单斜氧化锆微粉4份、酚醛树脂溶液5份采用高速混炼机混合均匀,形成刚玉-尖晶石-ZrO2泥料;以颗粒粒度小于2mm大于等于0.1mm的板状刚玉颗粒50份、颗粒粒度小于0.1mm大于等于0.043mm的板状刚玉细粉25份、D50=5μm的烧结氧化铝微粉15份、D50=1μm的特种氧化铝粉5份、D50=5μm的单斜氧化锆微粉5份、纸浆废液5份采用碾轮式混砂机中混合均匀,形成Al2O3-ZrO2泥料。
然后,采用振动加压捣打成形工艺成形耐火材料抗渣试样坩埚坯体;采用坩埚底朝上、口朝下的加料方式,用与坩埚侧壁模具空腔厚度相当宽度的硬纸条将坩埚侧壁模具空腔分割成所需数量的单元空间,反应区的2种材质的泥料分别加入到不同单元空间内,布料至设定的高度后抽出之前用于阻隔物料的硬纸条,用捣打棒将所布物料捣打振实后,再用锐器将捣打面刮毛,再将盛铁区刚玉泥料布料到模具空腔剩余空间,盖上上模头,在振动加压成形机上完成坯体的制作。
最后,坯体干燥后经1500℃保温5h电炉内烧成,经检测无裂纹、无变形后即得抗渣试样。
实施例4:
实施例4的主体结构同实施例1,该实施例中,所述的圆筒形坩埚是由刚玉(Al2O3≥99%)、刚玉-莫来石(Al2O3=95%、SiO2=5%)、莫来石(Al2O3=72%、SiO2=28%)、刚玉-尖晶石(Al2O3=95%、MgO=5%)4种材质的样品拼接组合而成的坩埚,坩埚有底无盖呈圆筒状,试样坩埚内径为150mm,侧壁厚20mm,底厚35mm,内腔深度192mm;坩埚底和侧壁下端(命名为盛铁区)材质为莫来石(Al2O3=72%、SiO2=28%),坩埚侧壁上端(命名为反应区)以坩埚底朝下口朝上俯视逆时针材质依次为刚玉(Al2O3≥99%)、刚玉-莫来石(Al2O3=95%、SiO2=5%)、莫来石(Al2O3=72%、SiO2=28%)、刚玉-尖晶石(Al2O3=95%、MgO=5%),4种材质将圆周等分;盛铁区和反应区的分界线位于坩埚圆周上距坩埚上沿128mm处;坩埚采用振动加压捣打一体成形,坯体是一个无接缝整体,经1650℃保温5h电炉内烧成,烧成后的坩埚无裂纹、尺寸规整、无变形。
该坩埚的制备方法如下:
首先,将用于坩埚制作的4种选定材质的材料分别进行混料。以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、D50=5μm的烧结氧化铝微粉20份、纸浆废液5份采用碾轮式混砂机混合均匀,形成刚玉泥料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉15份、D50=5μm的烧结氧化铝微粉20份、D50=1μm的硅微粉5份、纸浆废液5份采用碾轮式混砂机混合均匀,形成刚玉-莫来石泥料;以颗粒粒度小于3mm大于等于0.1mm的电熔莫来石颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的烧结莫来石细粉20份、D50=5μm的烧结氧化铝微粉15份、D50=1μm的硅微粉5份、纸浆废液5份采用碾轮式混砂机混合均匀,形成莫来石泥料;以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、颗粒粒度小于0.074mm大于等于0.043mm的烧结镁砂5份、D50=5μm的烧结氧化铝微粉15份、纸浆废液5份采用碾轮式混砂机混合均匀,形成刚玉-尖晶石泥料。
然后,采用振动加压捣打成形工艺成形耐火材料抗渣试样坩埚坯体。采用坩埚底朝上、口朝下的加料方式,用与坩埚侧壁模具空腔厚度相当宽度的硬纸条将坩埚侧壁模具空腔分割成所需数量的单元空间,反应区的4种材质的泥料分别加入到不同单元空间内,布料至设定的高度后抽出之前用于阻隔物料的硬纸条,用捣打棒将所布物料捣打振实后,再用锐器将捣打面刮毛,再将盛铁区的莫来石泥料布料到模具空腔剩余空间,盖上上模头,在振动加压成形机上完成坯体的制作。
最后,坯体干燥后经1650℃保温5h电炉内烧成,经检测无裂纹、无变形后即得抗渣试样。
实施例5:
实施例5的主体结构同实施例1,该实施例中,所述的圆筒形坩埚是由刚玉(Al2O3≥99%)、高铬(Cr2O3=90%、Al2O3=10%)、铬刚玉1(Cr2O3=10%、Al2O3=90%)、刚玉-尖晶石(Al2O3=95%、MgO=5%)、铬刚玉2(Cr2O3=50%、Al2O3=50%)、Sialon结合刚玉(Al2O3=83%、Si=8%、N=5%)、刚玉-碳化硅(Al2O3=85%、SiC=14%)7种材质的样品拼接组合而成的坩埚,坩埚有底无盖呈圆筒状,试样坩埚内径为150mm,侧壁厚25mm,底厚40mm,内腔深度280mm;坩埚底和侧壁下端(命名为盛铁区)材质为刚玉(Al2O3≥99%),坩埚侧壁上端(命名为反应区)以坩埚底朝下口朝上俯视逆时针材质依次为高铬、铬刚玉(Cr2O3=10%)、刚玉-尖晶石、铬刚玉(Cr2O3=50%)、Sialon结合刚玉、刚玉-碳化硅,6种材质将圆周等分;盛铁区和反应区的分界线位于坩埚圆周上距坩埚上沿200mm处;坩埚采用冷等静压一体成形,坯体是一个无接缝整体,经气氛保护电炉内1580℃保温5h持续通入高纯N2气烧成,烧成后的坩埚无裂纹、尺寸规整、无变形。
该坩埚的制备方法如下:
首先,将用于坩埚制作的7种选定材质的材料分别进行造粒成形。1)以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、D50=5μm的烧结氧化铝微粉20份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉造粒料;2)以颗粒粒度小于3mm大于等于0.1mm的电熔氧化铬颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔氧化铬细粉15份、D50=5μm的烧结氧化铝微粉10份、D50=5μm的氧化铬绿微粉15份、磷酸二氢铝水溶液4份采用高速混炼机混合均匀,形成高铬造粒料;3)以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉15份、D50=5μm的烧结氧化铝微粉15份、D50=5μm的氧化铬绿微粉10份、磷酸二氢铝水溶液4份采用高速混炼机混合均匀,形成铬刚玉(Cr2O3=10%)造粒料;4)以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔白刚玉细粉20份、颗粒粒度小于0.074mm大于等于0.043mm的烧结镁砂5份、D50=5μm的烧结氧化铝微粉15份、纸浆废液4份采用高速混炼机混合均匀,形成刚玉-尖晶石造粒料;5)以颗粒粒度小于3mm大于等于0.1mm的电熔铬刚玉颗粒(Cr2O3=30%)60份、颗粒粒度小于0.1mm大于等于0.043mm的电熔氧化铬细粉15份、D50=5μm的烧结氧化铝微粉8份、D50=5μm的氧化铬绿微粉17份、磷酸二氢铝水溶液4份采用高速混炼机混合均匀,形成铬刚玉(Cr2O3=50%)造粒料;6)以颗粒粒度小于3mm大于等于0.1mm的电熔棕刚玉颗粒50份、颗粒粒度小于0.1mm大于等于0.043mm的电熔棕刚玉细粉10份、颗粒粒度小于等于0.074mm的板状刚玉细粉8份、颗粒粒度小于等于0.074mm的金属铝粉3份、颗粒粒度小于等于0.043mm的单质硅粉9份、D50=5μm的烧结氧化铝微粉20份、液体酚醛树脂5份采用高速混炼机混合均匀,形成莫来石造粒料;7)以颗粒粒度小于3mm大于等于0.1mm的电熔白刚玉颗粒60份、颗粒粒度小于0.1mm大于等于0.043mm的板状刚玉细粉10份、颗粒粒度小于0.1mm大于等于0.043mm的碳化硅细粉(SiC≈95%)15份、D50=5μm的烧结氧化铝微粉15份、液体酚醛树脂5份采用高速混炼机混合均匀,形成刚玉-碳化硅造粒料。
然后,采用冷等静压成形工艺成形耐火材料抗渣试样坩埚坯体。采用坩埚底朝上、口朝下的加料方式,用与坩埚侧壁模具空腔厚度相当宽度的塑料条将坩埚侧壁模具空腔分割成所需数量的单元空间,反应区的高铬、铬刚玉(Cr2O3=10%)、刚玉-尖晶石、铬刚玉(Cr2O3=50%)、Sialon结合刚玉、刚玉-碳化硅6种造粒料分别加入到不同单元空间内,布料至设定的高度后抽出之前用于阻隔物料的塑料条,再将盛铁区刚玉造粒料布料到模具空腔剩余空间,在冷等静压机中一定压力下成形坯体。
最后,坯体干燥后经气氛保护电炉内1580℃保温5h持续通入高纯N2气烧成,经检测无裂纹、无变形后即得抗渣试样。
Claims (2)
1.一种耐火材料抗渣试样,其特征在于:所述的耐火材料抗渣试样为下端面封闭的圆筒状坩埚;所述的圆筒状坩埚具有上下设置的反应区(1)和盛铁区(2);所述反应区(1)与盛铁区(2)的接合面与圆筒状坩埚上端面之间的距离为圆筒状坩埚内腔深度的1/2~3/4;所述的反应区(1)至少由两块不同材质的弧形块一体成型;所述圆筒状坩埚的内径为100mm~200mm;所述圆筒状坩埚的侧壁厚为10mm~30mm;所述圆筒形坩埚的底厚为20mm~50mm;所述圆筒状坩埚的内腔深度为内径的1.2~2倍。
2.制备上述一种耐火材料抗渣试样的制备方法,其特征在于,制备方法的具体步骤如下:
1)耐火材料抗渣试样材料的准备:将制作耐火材料抗渣试样的反应区的多种材料、盛铁区的材料分别造粒成型,得到反应区多种材料的造粒料以及盛铁区材料的造粒料;
2)然后根据所制备耐火材料抗渣试样的大小选择合适的圆筒状坩埚模具,并准备与圆筒状坩埚模具的侧壁厚度相同的塑料条或硬纸条若干个;
3)根据反应区所选用材质的数量选取相同数量的塑料条或硬纸条;然后将塑料条或硬纸条的放入圆筒状坩埚模具内,并使多个所述的塑料条或硬纸条在圆筒状坩埚模具内均匀分布;在每两个相邻塑料条或硬纸条所构成的区域内放置所对应的反应区材料造粒料,当反应区材料造粒料布料的高度到达反应区所需的高度后;抽出之前用于阻隔物料的塑料条或硬纸条,再将盛铁区材质的造粒料布料到模具空腔的剩余空间内,采用冷等静压成形工艺或振动加压捣打成形工艺成形坯体;坯体干燥后经1500℃~1800℃高温烧成,经检测无裂纹、无变形后即得耐火材料抗渣试样。
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