CN101896440A - 具有掺杂的硅铝氧氮陶瓷基质的难熔产品 - Google Patents
具有掺杂的硅铝氧氮陶瓷基质的难熔产品 Download PDFInfo
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Abstract
一种包括由基质粘结的难熔粒料的烧结难熔产品,所述产品包括含有硅铝氧氮陶瓷相的结晶含氮部分,所述硅铝氧氮陶瓷相由式SixAlyOuNv表示,其中:x大于或等于0,且小于或等于1;y大于0,且小于或等于1;u大于或等于0,且小于或等于1;v大于0,且小于或等于1;基于所述结晶含氮部分的重量百分数,所述产品具有大于0.2%的磷含量。特别地适用于烘箱或熔炉或热交换器的衬套。
Description
技术领域
本发明涉及一种特别为块状形式的烧结难熔产品,以及涉及一种能够生产所述产品的颗粒混合物。本发明还涉及所述产品和块状物在冶金炉衬套生产中的用途,所述衬套特别为高炉的炉膛或鼓风口的衬套、或用于焙烧例如电解铝用阳极的熔炉衬套、或生活垃圾焚烧炉的衬套、或热交换器的难熔衬套。
背景技术
在这类应用中使用的难熔混凝土通常由粒料和基于碱土金属氧化物、特别是基于铝酸钙的水硬性粘合剂构成。该粘合剂通常称作“水泥”。然而,在称作“可铸”产品的这些产品中,碱土金属氧化物的存在对难熔性不利,并增加了载荷变形。此外,这类氧化物在还原介质中发生反应。
特别地,当构成高炉炉膛衬套时,碳质块的用途也是已知的。这类块状物通常通过使用树脂或沥青粘合剂成型膏状物,然后在大于1200℃的温度下焙烧得到。然后煅烧所述产品,并热解有机粘合剂。然而,碳质块对氧化和熔融铁腐蚀具有较低的耐受性,其具有随石墨形式的碳的比例升高而增加的耐侵蚀性。
此外,包括采用硅铝氧氮陶瓷(SiAlON)型粘结基质粘结的难熔粒料的组合难熔产品是已知的。硅铝氧氮陶瓷基难熔产品特别地由专利US 4533646、US 3991166或US 4243621中知晓。具有添加了磷的Si3N4型粘结基质的产品也是已知的,例如由US 3468992或CN 01803716中知晓。
所述产品表现出生产成本与性能之间非常理想的协调。其通常通过用于与环境中的氮气反应和用于构成所述硅铝氧氮陶瓷基质的粗产品在氮气中进行反应性烧结而得到。
然而,该技术不能用于在工业生产条件下生产较大的块状物。得到的块状物具有较高的残余金属核心含量,典型地高于2%。例如由于其可溶于熔融铁中或极易与碱性钾型产品反应,因此其还可能具有吸湿性和/或非难熔性结晶相,和/或可能不适于预期的应用。所述块状物还可能具有不利于氧化的相和不均匀的孔隙率或不可接受的性质内部梯度,特别是颜色和/或外观的梯度。所述内部梯度事实上在使用中会在块状物中产生大量热梯度,从而产生特别地在块状物中引起裂纹的机械应力和过早磨损。如此,所述块状物通常不能用于冶金高炉,特别是生产铸铁的高炉。
因此,需要能够至少部分地克服一个或多个上述问题的难熔产品。
发明内容
本发明的一个目的在于满足该需要。
本发明提出了一种包括由基质粘结的难熔粒料的烧结难熔产品,所述产品包括含有由式SixAlyOuNv表示的硅铝氧氮陶瓷相的结晶含氮部分,其中
·x大于或等于0、0.01、0.1或0.2,且小于或等于1;
·y大于0、0.01、0.05或0.14,且小于或等于1;
·u大于或等于0、0.01、0.05或0.14,且小于或等于1;
·v大于0、0.01、0.1或0.3,且小于或等于1;
基于所述结晶含氮部分的重量百分数,所述产品具有大于0.2%的磷含量。
通常,在式SixAlyOuNv中,x、y、u和v为质量指数。
所述硅铝氧氮陶瓷相的定义特别地排除Si3N4。然而,Si3N4可存在于该产品中,特别是存在于粒料中。
如在说明书下文中变得更显而易见的,该磷含量特别地且出乎预料地能够产生较高的机械强度,特别是冷弯强度和抗破碎性、抗氧化性和抗磨损性。
所述烧结产品可以是混凝土,但也可以是灰泥。特别地,补足所述结晶含氮部分的基质部分可包括或甚至由水硬性粘合剂、树脂或这些组分的混合物构成,其中所述树脂特别地为热固性树脂。
在各种实施方案中,所述烧结产品还可以具有下表所示的一个或多个任选的特性:
·基于结晶含氮部分的重量百分数,所述产品包括大于0.3%,优选大于0.4%的磷。优选地,基于结晶含氮部分的重量百分数,所述基质包括小于2.5%,或小于2%,或甚至小于1.5%,或甚至小于1%的磷;
·基于所述产品的重量百分数,所述产品包括小于0.4%,优选小于0.3%,或小于0.2%,或甚至小于0.1%的硼;
·结晶含氮部分的重量的至少90%,或甚至95%,或甚至99%,或甚至100%形成所述基质部分;
·结晶含氮部分占基质质量的至少50%,或至少80%,或甚至至少90%,或甚至至少95%,或甚至基本上100%,补足100%的其余部分由例如残余金属和氧化物,特别是氧化铝构成;
·所述产品包括式Si6-zAlzOzN8-z表示的相,其中0<z<4.2,称作“β’硅铝氧氮陶瓷”相,所述相可部分或全部处于基质中;
·z大于1,或甚至大于3和/或小于4,或甚至小于3.5;
·所述β’硅铝氧氮陶瓷相占结晶含氮部分质量的大于60%,或大于70%,或甚至大于75%;
·所述结晶含氮部分包括式SixAlyOuNv表示的AlN15R相,其中0.12≤x≤0.33,0.78≤y≤0.99,0.33≤u≤0.55,0.78≤v≤1;
·AlN15R相占结晶含氮部分质量的大于18%,或甚至大于20%;
·基于所述基质的重量百分数,结晶含氮部分重量的大于80%由所述β’硅铝氧氮陶瓷相和所述AlN15R相(若适宜)构成;
·所述β’硅铝氧氮陶瓷相和任意AlN15R相一起占结晶含氮部分质量的大于80%,或甚至大于90%,或甚至大于95%,或大于99%,或甚至基本上100%,补足100%的其余部分由磷(P),可行的其它含氮相,任选的微量氧化铝或甚至二氧化硅和杂质构成,其中所述其它含氮相特别地为BN、TiN、Si3N4、ZrN、Si2ON2、式Si2-xAlxOx+1N2-x表示的O’硅铝氧氮陶瓷(其中x>0)或X硅铝氧氮陶瓷(见US 5521129);
·所述基质占产品质量的至少5%,至少10%,至少13%,或甚至至少15%,和/或产品质量的小于60%,小于40%,小于30%,或甚至小于25%。根据定义,其余部分由粒料构成;
·所述基质通过反应性烧结得到;
·所述磷含量仅基于基质中存在的结晶含氮部分计算,即,等于100倍的产品中磷的重量/基质中存在的结晶含氮部分的质量;
·由于所述产品由如下构成:
·由粒度大于选自200μm、100μm、50μm和20μm的阈值粒度D阈值的一组微粒的质量构成的第一部分;以及
·粘结第一部分的微粒的第二部分(从而第一和第二部分的总质量等于产品质量);
从而所述磷含量仅基于第二部分中存在的结晶含氮部分测量;
·第二部分占产品质量的至少5%,至少10%,至少13%,或至少15%和/或产品质量的小于60%,小于40%,小于30%,或小于25%;
·D阈值根据预期应用确定,例如等于200μm以生产本发明的块状物,或等于100μm或50μm或20μm以生产纤薄产品;
·第二部分可包括粒度小于阈值粒度D阈值的微粒;
·基于产品的重量百分数,残余金属含量,特别是硅含量小于1.8%,或甚至1.5%,或甚至小于1%;
·AlN15R/(AlN15R+β’SiAlON)的重量比大于0.18,或甚至大于0.2;
·在一个实施方案中,基于产品的重量百分数,所述产品具有小于2%,优选小于1.5%和/或大于0.2%,或甚至大于0.4%的碱土金属氧化物总含量,特别是CaO和/或MgO含量;
·基于产品的重量百分数,所述产品具有小于1%的碱金属氧化物总含量,特别是Na2O和K2O含量;
·基于产品的重量百分数,所述产品具有大于0.4%的碱金属氧化物总含量;
·在一个实施方案中,所述粒料既不含氮也不含磷;
·大于70%,或甚至大于80%,或甚至大于90%,或甚至基本上100%重量的所述粒料由选自氧化铝、莫来石、莫来石前体、氧化铬、氧化锆、锆石、氮化物、氮化硅Si3N4、碳化物、无定形碳或至少部分为结晶形式的碳以及所述物质的混合物的材料的微粒构成,和/或由上述微粒的混合物构成,其中,所述氧化铝特别地为刚玉、白色或黑色氧化铝、或管状氧化铝,所述碳化物特别地为碳化硅SiC;
·所述粒料包括碳化硅SiC微粒,或甚至其由该类微粒构成。在一个实施方案中,基于产品的重量百分数,本发明的产品包括大于5%的SiC;
·特别地,当生产较大块状物时,至少50%,或甚至至少60%或至少70%重量的所述粒料中微粒具有大于0.2mm的粒度,和/或至少15%,或甚至至少20%,或甚至至少25%的微粒具有大于2mm,或甚至大于3mm或大于5mm的粒度,和/或至少90%,或甚至至少95%重量的所述粒料中微粒具有小于20mm,或甚至小于15mm,或甚至小于10mm或小于5mm的粒度;
·特别地,当生产较大块状物时,所述粒料中微粒的中值粒度大于3mm,或甚至4mm和/或小于15mm、10mm、6mm;
·特别地,当生产纤薄产品时,所述粒料中微粒的中值粒度大于5μm,或甚至10μm、30μm或50μm,和/或小于3mm、2mm、1mm、500μm或甚至100μm;
·基于产品的重量百分数,所述产品中氮含量大于3.1%,大于3.5%或甚至4%或更大;
·基于产品的重量百分数,所述产品中β’硅铝氧氮陶瓷含量大于12%,大于14%,或甚至15%或更大;
·所述产品由选自已处理或未处理的混凝土和已处理或未处理的灰泥材料形成;
·所述产品不包括羧酸单体,也不包括N-叔丁基丙烯酰胺。
本发明还提供一种干燥或湿润的颗粒混合物,其以适于通过在氮气中反应性烧结,或如果氮以足够量存在于颗粒混合物中,则在非氧化气氛中烧结来形成本发明的烧结产品的基质的比例和形式包括磷源、硅源、铝源和氧源、或甚至氮源。
优选地,所述颗粒混合物的组成调节为使得在与难熔粒料混合并烧结后得到根据本发明的难熔产品。换言之,所述颗粒混合物包括除所述粒料以外,烧结所需的全部组分和添加剂。
在一个实施方案中,本发明的颗粒混合物还包括所述难熔粒料。于是其构成了可原位浇铸以生产衬套的根据本发明的未烧结产品。该未烧结和未处理的产品还可以是可组装并随后原位烧结的块状物形式。在以下本发明的生产方法中描述并浇铸入模具中的初始装料构成根据本发明的未烧结产品的一个例子。
根据本发明的各种实施方案,所述颗粒混合物还可包括一个或多个以下任选的特性:
·所述颗粒混合物包括选自磷酸盐特别是氢磷酸盐、聚磷酸盐和尤其是铝磷酸盐或碱金属聚磷酸盐如六偏磷酸钠、有机磷化合物、有机磷聚合物以及以上化合物的混合物的含磷化合物;
·基于颗粒混合物的干物质的重量百分数,所述颗粒混合物包括大于1%,大于5%,或甚至大于8%,和/或小于15%,或甚至小于10%的二氧化硅,所述二氧化硅优选为微粉和/或胶体形式,例如煅制二氧化硅;
·基于颗粒混合物的干物质的重量百分数,所述颗粒混合物包括大于0.5%和/或小于5%,或甚至小于2%的金属硅,该金属硅的中值粒度优选小于200μm,或甚至小于60μm;
·基于颗粒混合物的干物质的重量百分数,所述颗粒混合物包括大于1%,或甚至大于2%,或甚至大于5%,和/或小于15%,或甚至小于10%的金属铝,该金属铝的中值粒度优选小于200μm,或甚至小于60μm;
·基于颗粒混合物的干物质的重量百分数,所述颗粒混合物包括大于0.5%,大于1%,和/或小于10%,小于8%,或甚至小于5%的煅烧氧化铝,中值粒度优选小于10μm,或甚至小于5μm;
·优选地,所述硅源为粉末二氧化硅和/或所述铝源为粉末铝和/或铝合金;
·所述颗粒混合物中包含的磷与金属铝的重量比R优选大于5×10-5和/或小于5×10-2。
根据本发明的颗粒混合物可以准备好使用的方式供给,例如包装在袋或大包中,或当其湿润时,包装在例如圆桶中。
在一个实施方案中,本发明提供一种烧结难熔块状物,其至少部分,优选全部由根据本发明的烧结难熔产品构成。
在一个实施方案中,本发明提供一种难熔块状物:
·其由以下部分构成:
·由粒度大于200μm阈值粒度D阈值的一组微粒的质量构成的第一部分;以及
·粘结第一部分的微粒的第二部分,所述第二部分例如占块状物质量的至少5%,至少10%,至少13%,或至少15%和/或块状物质量的小于60%,或甚至小于40%,或小于30%,或小于25%;
·具有至少一个至少为120mm的总体尺寸,即,厚度或长度或宽度;以及
·其中至少一部分如核心或甚至全部由以下烧结产品形成:
·包括含有硅铝氧氮陶瓷相的结晶含氮部分,所述硅铝氧氮陶瓷相由式SixAlyOuNv表示,其中
·x大于或等于0、0.01、0.1或0.2,且小于或等于1;
·y大于0、0.01、0.05或0.14,且小于或等于1;
·u大于或等于0、0.01、0.05或0.14,且小于或等于1;
·v大于0、0.01、0.1或0.3,且小于或等于1;
·基于所述结晶含氮部分的重量百分数,具有大于0.2%的磷含量。
该产品可具有一个或多个上述列表中提及的任选的产品特性。
所述第一部分和第二部分可特别地对应于粒料和基质。
在一个实施方案中,本发明提供一种难熔块状物:
·其由以下部分构成:
·由粒度大于200μm阈值粒度D阈值的一组微粒的质量构成的第一部分;以及
·粘结第一部分的微粒的第二部分,所述第二部分例如占块状物质量的至少5%,至少10%,或至少13%,或甚至至少15%和/或块状物质量的小于60%,或甚至小于40%,或小于30%,或小于25%;
·具有至少一个至少为120mm的总体尺寸,即,厚度或长度或宽度;以及
·其中至少一部分如核心或甚至全部由以下烧结产品形成:
·包括含有硅铝氧氮陶瓷相的结晶含氮部分,所述硅铝氧氮陶瓷相由式SixAlyOuNv表示,其中
○x大于或等于0、0.01、0.1或0.2,且小于或等于1;
○y大于0、0.01、0.05或0.14,且小于或等于1;
○u大于或等于0、0.01、0.05或0.14,且小于或等于1;
○v大于0、0.01、0.1或0.3,且小于或等于1;
·基于产品的重量百分数,所述烧结产品包括小于1.8%,或甚至小于1.5%,或甚至小于1%的残余金属含量,所述残余金属特别地为硅。
基于所述结晶含氮部分的重量百分数,该产品可具有大于0.2%的磷含量。其还可具有上述列表中提及的一个或多个任选的产品特性。
所述第一部分和第二部分可特别地对应于粒料和基质。
无论采用何种实施方案,所述块状物还可具有一个或多个以下任选的特性:
·所述块状物具有大于50kg,大于150kg,大于300kg或甚至大于900kg和/或小于2(公)吨的质量。特别地,其可具有约1吨的质量;
·所述块状物具有至少一个至少为120mm,优选至少150mm,或甚至200mm,或甚至300mm,或甚至400mm,或甚至600mm或甚至800mm,或甚至1000mm的尺寸(厚度、长度或宽度);
·所述块状物的厚度、长度和宽度至少为120mm,或甚至150mm,或甚至300mm,或甚至400mm,600mm或甚至800mm,或甚至1000mm;
·所述块状物的至少一个总体尺寸,特别是总体横向尺寸,和特别是总体横向长度和/或宽度,大于150mm,300mm,600mm或甚至900mm(该特性是“U”形块状物的特有效用);
·所述块状物具有通常为凸形如平行六面体形的外表面或具有凹陷的常规形状的外表面。换言之,所述块状物的外表面包括修改其常规形状的凹陷。例如,所述块状物可具有“U”、“+”或“X”形横截面;
·所述块状物可在局部具有一个或多个孔,其可任选地为通孔,例如为蜂窝或管状孔、直线或其它形式,例如用以促进任何流体(液体或气体)的通过或增加热交换表面;
·所述块状物的“核心”,即中央部分,由根据本发明的产品形成;
·除“外壳”以外,即除由表面扩展小于1000μm厚度,优选小于500μm厚度的外围部分以外,全部块状物由根据本发明的烧结产品形成。
本发明还提供一种薄烧结产品,其至少一部分,优选全部由根据本发明的烧结难熔产品构成。
根据本发明的薄烧结产品可特别地具有小于100mm,50mm,或甚至25mm的厚度“e”。其可特别地为薄片形(图6)。
本发明还提供一种由初始装料生产烧结难熔产品的方法,其中所述烧结难熔产品尤其是烧结难熔块状物,所述初始装料确定为使得所述产品为根据本发明的产品。该初始装料可特别地具有一个或多个上述本发明的颗粒混合物的任选特性。
在一个实施方式中,所述方法包括以下步骤:
a)制备包括难熔粒料、硅铝氧氮陶瓷前体和液态或固态含磷化合物的初始装料;
b)将所述初始装料浇铸入模具中;
c)在模具中通过压紧模塑初始装料,以形成粗产品;
d)将所述粗产品从模具中取出;
e)干燥所述粗产品,优选直至残余湿气含量在0-0.5%范围内;
f)在非氧化性气氛中(若氮由初始装料供给),或者在还原性氮气氛中,优选在1300℃-1600℃温度下焙烧所述粗产品,以得到块状物。
根据本发明,所述初始装料确定为使得在步骤f)末期,所述块状物为根据本发明的块状物,或使得所述初始装料为根据本发明的颗粒混合物。
最后,本发明提供根据本发明的难熔产品,或根据本发明的方法生产或可生产的难熔块状物,用于构成全部或部分熔炉衬套,特别是冶金炉衬套的用途。特别地,该衬套可以是用于高炉的衬套。特别地,其可构成高炉的炉膛和/或鼓风口和/或炉腹的至少一部分。所述衬套还可以是焙烧例如电解铝用阳极的熔炉衬套。
本发明还提供根据本发明的难熔产品或采用根据本发明的方法生产或可生产的难熔块状物用于构成全部或部分热交换器或生活垃圾焚烧炉衬套的用途。
本发明还提供一种选自熔炉和热交换器的装置,其特征在于包括至少部分由本发明的烧结难熔产品形成或由所述产品构成的衬套。
特别地,所述熔炉可以是焚烧炉、冶金炉或阳极焙烧炉,其中所述冶金炉特别地为高炉。所述热交换器可特别地为用于生活垃圾焚烧炉的热交换器。
本发明还提供根据本发明的纤薄产品用于构成焙烧陶瓷产品的载体的用途。
除非另外说明,否则全部涉及烧结产品或其他产品的组成的百分数,或涉及初始装料的百分数均为重量百分数。
定义
术语“未处理的产品”用来表示不具有固有刚性的潮湿或干燥产品,例如适于浇铸入模具中的粉末或潮湿初始装料。
相反,术语“已处理的产品”用来表示结构材料,即当使用时,保持其形状的材料,如从模具中取出的粗产品或烧结产品。
术语“未烧结的产品”在这里用来表示烧结时适于生产根据本发明的烧结产品的已处理或未处理的产品。
术语“预制品”用来表示烧结时适于生产根据本发明的烧结产品的未烧结的已处理的产品。
术语“未处理的混凝土”用来表示一种干燥或潮湿颗粒混合物,其包括至少一种能够固化以构成具有微结构的干燥固体材料的水硬性固化剂,其中所述微结构由具有微粒的粒料构成,所述微粒通过基质结合成整体。未处理的混凝土可通过浇铸(伴随有振动操作或其他方式)或通过投射使用。
术语“未处理的灰泥”用来表示不包括水硬性固化剂的干燥或潮湿颗粒混合物,其能够固化以构成具有微结构的固体干燥材料,称作“已处理的灰泥”,其中所述微结构由具有微粒的粒料构成,所述微粒通过基质结合成整体。未处理的灰泥能够通过捣打和/或压缩(伴随有振动操作或其他方式)使用。该定义特别地包括通常称作“干燥振动水泥”和“捣打混合物”的灰泥。
所述混凝土或已处理的灰泥可具有任意形状。例如当其由衬套的固化产生时,所述混凝土或已处理的灰泥可特别地具有块状或层状。通常,所述混凝土或已处理的灰泥通过固化已经经历活化阶段的颗粒混合物得到,其中所述活化阶段例如为用水润湿。
术语“烧结”用来表示热处理,由此所述产品形成由具有微粒的粒料构成的微结构,其中所述微粒通过基质结合成整体。根据本发明的烧结产品包括通过优选在1300℃-1600℃温度下烧结得到的硅铝氧氮陶瓷基质,其中如果氮由初始装料的至少一种组分供给,则烧结在非氧化性气氛中实施,或烧结在氮气氛中实施,可在氮气中反应性烧结的这类方法是技术人员公知的。
术语“在氮气中烧结”是指在包含大于90%,优选大于95%,更优选基本上100%氮气的气体环境中烧结,所述百分数为体积百分数。
术语“残余硅”用来表示以金属形式存在于烧结产品中的硅。
在根据本发明的烧结产品中,术语“粒料”用来表示通过基质粘结的难熔微粒集合,其在烧结期间基本保持其在初始装料中具有的形状和化学性质。特别地,与基质或“基质前体”的原始颗粒相比,粒料的微粒在烧结期间不完全熔合。
作为扩展,术语“粒料”还用来表示大量如其在原始装料中的那些微粒。在根据本发明的产品中的粒料的性质不受限制,从而粒料的特征在于其在烧结期间的结构稳定性和化学稳定性。如此,根据其颗粒的粒度,例如可将粉末如氧化铝看作粒料或基质前体。
在本发明的一个实施方案中,粒料由不同于基质组分的物质形成。
在本发明的另一个实施方案中,粒料由与基质中某些组分相同的物质形成。例如,所述粒料可结合结晶含氮相。于是,在不清楚生产方法的情况下,很难区分基质和粒料。基于此原因,在本发明的某些实施方案中,为评估基质的量,产品的总质量不涉及粒度高于阈值粒度的微粒。
术语“基质”是指在所述微粒间具有连续结构的结晶相或其它相,其在烧结期间由初始装料的组分以及所述初始装料的气体环境的可能组分得到。基质基本上包围粒料的微粒,即将其覆盖。
通过反应性烧结得到的基质具有特殊性质。具体地说,在反应性烧结期间,金属被氮化。产生的典型地1%-20%的体积增加可有利地堵塞基质的孔,和/或弥补由微粒烧结引起的收缩。由此,反应性烧结能够限制基质破裂,从而提高产品的机械强度。如此,反应性烧结产品具有明显小于在类似温度条件下烧结的其它产品的开放和/或闭合的孔隙率。在焙烧时,反应性烧结产品基本不表现出收缩。
术语“杂质”是指不可避免的组分,其必然随原料引入或由所述组分的反应生成。杂质不是必要组分,但可以容忍。
术语“微粉形式的二氧化硅”是指部分地具有在0.01μm-4μm范围内的中值粒度的无定形颗粒的二氧化硅粉末。胶体二氧化硅具有更小的中值粒度,通常约为数纳米。
术语“热固性树脂”是指适于通过热处理(热、辐射)或物理-化学处理(催化、焙烧)转变成不熔不溶材料的聚合物。如此,当初始固化时,热固性树脂具有其固定的形状;这是不可逆的。特别地,热固性树脂包括基于硅酮或环氧衍生物的酚醛树脂。这类树脂可用于本发明中。
在已处理的材料中,术语颗粒或微粒的“粒度”是指其最大尺寸和最小尺寸的平均值,所述尺寸在所述材料的截面上测量。
在未处理的材料中,术语颗粒或微粒的“粒度”是指在所述颗粒或微粒的图像上测量的其最大尺寸。一组中的微粒或颗粒粒度通常采用倾注于自粘性毡上的该组图像实施测定。
一组颗粒或微粒的“中值粒度”通常表示为D50,是指将该组微粒或颗粒分成质量相等的第一群体和第二群体,且所述第一群体和第二群体分别仅包含粒度大于或小于中值粒度的微粒。
术语“压紧”用来表示特别地通过压缩、挤出、浇铸、振动、捏合或结合了这些不同技术的技术来成型的任意方法。
术语“氧化锆”用来表示锆氧化物ZrO2。
术语“氧化铝”用来表示铝氧化物Al2O3。
术语“二氧化硅”用来表示硅氧化物SiO2。
“总体”尺寸是在块状物的外表面的相互距离最远的两点间沿预定方向测量的距离。所述总体尺寸是在评估“U”形块状物或具有开放和/或闭合中空部分的块状物,特别是用于焙烧电解铝用阳极的炉壁的块状物的尺寸中的特殊应用。“横向”总体尺寸对应于在横向平面,即块状物的横截面上测量的尺寸。总体横向长度和宽度是例如用于测量相互平行且朝向“U”形外部(即,其不朝向“U”形的连接部)的两个“U”形分支侧面间距离的适宜横向尺寸。如此,横向总体尺寸可大于“U”形分支的厚度或其高度。
术语“纤薄产品”用来表示厚度在3mm-120mm范围内的产品。
附图说明
通过以下详细描述和对附图的观察,本发明的其它特征和优点变得更加清晰;图1-5以立体图示出根据本发明的块状物的各种形状,以及图6以立体图示出根据本发明的纤薄产品的例子。
具体实施方式
为生产根据本发明的烧结难熔产品,可遵循上述步骤。
在步骤a)中,常规混合颗粒物质,以得到均匀混合物。
原料的性质和用量确定为使得在步骤f)末期得到的难熔产品块状物为根据本发明的难熔产品块状物。
确定初始装料的组分比例的方法是技术人员公知的。例如,技术人员知晓存在于初始装料中的碳化硅会在烧结产品中出现。技术人员还知晓如何确定会转化成基质组分的那些组分。
某些氧化物可由通常用于生产所述产品的添加剂供给,所述添加剂例如为烧结剂、分散剂如碱金属聚磷酸盐或甲基丙烯酸盐衍生物。因此,初始装料的组成可特别地根据存在的添加剂的用量和性质,以及所用原料的纯度变化。
优选地,初始装料确定为使得氧化铝、二氧化硅和粒料如碳化硅占烧结产品的干燥无机物质量的至少80%,优选至少85%。
所述粒料可由基于难熔氧化物或非氧化难熔材料的微粒构成,或者由基于碳,特别是无烟煤或石墨的微粒构成,或者由基于碳化物如碳化硅的微粒构成。特别地,所述粒料可由其组成包括铝(Al)和/或硅(Si)元素的微粒构成。
优选地,大于70%或甚至大于80%或甚至大于90%或甚至基本上100%重量的粒料由氧化铝,和/或莫来石或莫来石前体,和/或氧化铬,和/或氧化锆,和/或锆石,和/或氮化物,和/或碳化物的微粒构成,其中所述氧化铝特别地为刚玉、白色或黑色氧化铝、或管状氧化铝,所述氮化物尤其是氮化硅Si3N4,所述碳化物尤其是碳化硅SiC。其还可由前述组分的混合物构成的微粒形成。最后,其可由上述微粒的混合物形成。
在一个实施方案中,特别地,当期望高导热率例如以生产用于电解铝用阳极生产的熔炉壁或生活垃圾焚烧炉或热交换器的衬套时,所述粒料包括碳化硅SiC微粒,或甚至可由该类微粒构成。此时,基于产品的重量百分数,所述产品可包括大于5%的SiC。
于是,本发明的产品可具有优于目前使用的基于粘土或氧化铝的难熔产品的导热率。
所述磷可以液体形式或固体形式或粉末形式供给。特别地,其可以磷酸盐形式尤其是氢磷酸盐形式供给,或者以聚磷酸盐形式特别是铝磷酸盐或碱金属聚磷酸盐如六偏磷酸钠形式供给。有机磷化合物或有机磷聚合物同样也是适宜的。
优选地,用于基质的元素硅由二氧化硅供给,特别地用以生产至少50kg,或甚至至少150kg和/或具有至少120mm尺寸和/或大于120mm的总体尺寸的块状物,其中所述二氧化硅特别地为微粉二氧化硅形式(例如煅制二氧化硅或微粉化的二氧化硅形式)或胶体二氧化硅形式。
特别地,基质中的硅可至少部分地作为硅金属粉末供给。
用于构成基质的铝源可包括含金属铝的粉末。有利地,使用金属铝意味着烧结后,得到完全包围粒料的微粒的稳定基质。优选使用同时供给元素磷和部分元素铝的铝磷酸盐粉末。
优选地,用于基质的铝源还包括氧化铝粉末,特别是煅烧的氧化铝。
还可使用含硅和铝元素的混合合金。
优选地,按照相对于干燥初始装料的质量的重量百分数,初始装料包括0.1%-2%范围内,优选小于0.5%的分散剂。所述分散剂可例如选自碱金属聚磷酸盐和甲基丙烯酸盐衍生物。可使用任何已知的分散剂,其可以完全为离子性或立体的,例如聚甲基丙烯酸钠型,或其组合。添加分散剂意味着可更好地分散粒度小于150微米的微粒,从而提高基质的机械强度。
若适宜,必须考虑含磷酸盐分散剂的添加,以确定待添加至初始装料中的剩余磷量。
还可将粘合剂添加至初始装料中。粘合剂的作用是能够保持颗粒混合物的形状,直至将其焙烧。粘合剂的选择取决于所期望的形状。为保证处理后产品变硬以及提供具有良好机械强度的烧结产品,基于石灰的水硬性水泥型粘合剂是有利的。按照相对于干燥初始装料的无机物质量的重量百分数,初始装料中碱土金属氧化物,特别是CaO的总量可大于0.2%。
然而,优选地,特别是对于较大块状物,基于相对于干燥初始装料的无机物质量的重量百分数,初始装料中碱土金属氧化物的总量小于2%,优选小于1.5%,或甚至小于1%。这些氧化物实际上对难熔性和载荷变形不利。此外,这些氧化物不利于氮化。
将干燥初始装料充分干混,以得到构成根据本发明的未处理的产品的均匀混合物,其可以此形式包装和运输。
接着,将水常规添加至所述初始装料中。在一个实施方式中,按照相对于干燥初始装料的无机物质量的重量百分数,添加至少2%,优选至少2.5%和/或小于10%,或小于8%,或小于5%的水。将水逐渐添加至运转的混合器中,直至得到充分均匀的潮湿混合物。
继续进行初始装料的混合,直至得到充分均匀的潮湿混合物。
在步骤b)中,将潮湿混合物浇铸至塑造成用于生产具有例如1.0×0.8×0.25m3的期望尺寸的块状物的模具中。在一个实施方式中,所述块状物的至少一个尺寸或甚至块状物的全部尺寸大于0.15m,0.25m或0.4m。
较大块状物的使用可有利地降低装配的难熔砖中接缝的数量。从而限制通过接缝的腐蚀作用。采用较大块状物还会使其本身能够实现难熔衬套的快速安装。
在接下来的步骤c)中,模具内物质的压紧例如可经历振动步骤。采用所述混合物填充模具可通过采用例如在土木工程中使用的那些常规针状振捣器来改进。根据块状物的尺寸,在潮湿混合物中所述针的振动优选进行3-20分钟。
在压紧步骤末期,优选用防水油布覆盖模具,以减少表面干燥。
为促进硬化,当压紧完成时,优选将模具立即在优选大于40℃且优选小于60℃的温度下放置在烘箱中,根据块状物的尺寸,通常放置数小时至24小时时间。
然后将粗产品从模具中取出(步骤d)),并放置干燥(步骤e))。干燥可在适度高的温度下进行。优选地,其优选在空气或可控湿度气氛中在110℃-200℃范围内的温度下进行。取决于粗产品的形式,其通常持续10小时至一周,优选直至粗产品的残余湿气含量小于0.5%。
所述从模具中取出的粗产品为根据本发明的预制块状物,其有利地具有足以能被操作、运输和装配的机械强度。
然后焙烧干燥的粗产品(步骤f))。焙烧时间取决于材料以及块状物的尺寸和形状,例如由冷却至冷却约3至15天。根据本发明,焙烧优选在氮气中进行。如果氮由原料供给,则在中性气氛如氩气中焙烧也是可行的。
焙烧循环优选在接近1巴的氮气压和优选在1300℃-1600℃的温度下进行,但更高的压力也是适宜的。
焙烧期间,氮气与粗产品中某些组分,特别是与煅烧的氧化铝和微粉形式的二氧化硅以及与金属粉末反应(“反应性烧结”),以形成基质,从而粘结所述粒料的微粒。
焙烧期间在粗产品中固定氮导致粗产品重量增加。重量增加成为预定焙烧方法的焙烧量指标。在焙烧阶段末期,得到根据本发明的烧结块状物。在一个变型中,即使实践证明存在困难,仍可将本发明的产品不经烧结而放在其使用位置上,其中烧结在原位实施。
在烧结末期,得到根据本发明的烧结块状物,其具有降低的开孔孔隙率和显著的冷碎强度以及冷弯强度。更准确地说,所述产品具有50MPa或更高,或甚至大于100MPa的冷碎强度。
不希望受到一种理论解释的限制,本发明人通过高度均匀的氮化解释该显著性能,所述高度均匀的氮化意味着可得到较大的AlN15R相含量和不含裂纹的材料。
氮化均匀性通过低残余金属含量,特别是硅含量来说明。基于产品的重量百分数,即使在块状物的核心处,该含量事实上也低于1.8%,1.5%或甚至低于1%。
此外,典型地,基于重量百分数,作为公知的[4(AlN)](SiO2)型相的AlN15R相占基质的结晶含氮相的大于18%,或甚至大于20%。
本发明的产品可特别地用于生产形状不受限制的块状物。这些块状物10可特别地包括凸起的外表面13;其可以是例如平行六面体形(例如图1),或其可包括具有修改其常规形状的凹陷的外表面13。从而,块状物10可具有气体的凹槽14或通槽16(图4)。作为例子,块状物10例如可以是分别如图2、3、4和5所示的“X”、“U”、圆柱或“+”形。
无论其为何种一般形状,所述块状物均可在局部具有凸起、孔15或蜂窝;其可以是开放或闭合的。其外表面13可以是平滑的(图1、3-5),或特别地为增加热交换表面可具有褶皱17(图2)。
如图6所示,本发明的产品还可用于生产纤薄产品20。
在图1-6中,块状物和纤薄产品的厚度、长度和宽度分别由标号“e”、“L”和“l”表示。在图2-5中,总长度由标号“L’”表示。
实施例
以下实施例基于说明的目的提供,而不以任何方式限制本发明。
在实施例中,根据上述方法的步骤a)-f)生产各种块状物。
对于表1的实施例,通过干混各种以粉末形式添加的组分来制成初始装料。然后将水逐渐添加至运转中的混合器中,以得到具有适于浇铸入模具的稠度的混合物。所述模具适于生产具有300mm×300mm×250mm尺寸的块状物。在将初始装料浇铸入模具中后,采用土木工程型针状振捣器实施振动步骤1-5分钟。
然后采用防水油布覆盖模具,以限制表面干燥,此后立即将其放置在温度约40℃-60℃的烘箱中约10小时,以促进产品硬化。然后将块状物从模具中取出并在空气中在110℃下干燥,直至残余湿气含量低于0.5%。最后,将干燥的块状物在氮气中在1500℃下焙烧至少10小时。
使用以下物质:
·Alcan销售的电熔融棕色刚玉混合物,其中包括20重量%粒度为7mm-15mm的微粒,60重量%粒度为0.2mm-7mm的微粒,和20重量%粒度低于0.2mm的微粒;
·基本上具有以下粒度分布的碳化硅(SiC)粉末,基于重量百分数:
·2mm-5mm:25%
·0.2mm-2mm:50%
·0mm-0.2mm:25%;
·Elkem销售的983U型煅制二氧化硅;
·Alcan销售的具有约4微米中值粒度的AC 44B4型煅烧的氧化铝粉末;
·Rhodia销售的粉末形式的HMPNa(六偏磷酸钠);
·FFB32,其为Budenheim销售的商业酸式磷酸铝;
·E452,其为Brenntag供给的聚磷酸钙型食品添加剂;
·Alcoa销售的基于铝酸钙CA 270的水泥。
开孔孔隙率和表观密度根据国际标准ISO 5017测量。
冷碎强度测量根据法国标准NFB 40322,在由块状物的核心切取的直径为50mm、高为50mm的圆柱形样品上实施。
结晶相通过X射线衍射测量。
产品中的氮(N)含量采用LECO型分析仪(LECO TC 436DR;LECO CS300)测量。其值以重量百分数表示。
磷含量通常采用X射线荧光确定。
下表1汇总了实施的试验和得到的结果。
表1
ND:不可检测
-:未检测到裂纹
表1表明,无论以何种形式引入磷,本发明的产品均具有显著的冷碎强度,测得的强度比对比例A产品测得的强度高约4倍。
此外,本发明的实施例具有明显高于对比例的氮含量和β’硅铝氧氮陶瓷含量。
本发明的实施例在核心处还具有不可检测的残余硅含量,而以重量百分数计,AlN15R相占基质中AlN15R相和β’硅铝氧氮陶瓷相之和的大于18%,或甚至大于20%和甚至大于25%。
本发明的产品与在相同条件下得到的除磷含量外具有相同组成的产品(其磷含量小于0.2%)相比,可具有高出20%或甚至高出30%重量的氮含量,磷含量之差由硅和/或铝弥补。因此,氮化品质是显著的。
最后,与对比例相比,本发明的实施例均未显示出裂纹。
因此,本发明的产品完全适用于预期应用。实施例1构成了本发明的优选实施方案。
显然,本发明不限于以非限制性说明方式提供的所述实施方案。
特别地,本发明的产品可用于除高炉以外的应用,例如作为金属熔炉的衬套。
Claims (55)
1.一种包括由基质粘结的难熔粒料的烧结难熔产品,其中,所述基质由反应性烧结得到,所述产品包括含有由式SixAlyOuNv表示的硅铝氧氮陶瓷相的结晶含氮部分,其中
·x大于或等于0,且小于或等于1;
·y大于0,且小于或等于1;
·u大于或等于0,且小于或等于1;
·v大于0,且小于或等于1;
基于所述结晶含氮部分的重量百分数,所述产品具有大于0.2%的磷含量。
2.如前一权利要求所述的产品,基于所述结晶含氮部分的重量百分数,具有大于0.3%的磷含量。
3.如前一权利要求所述的产品,基于所述结晶含氮部分的重量百分数,具有大于0.4%的磷含量。
4.如任一前述权利要求所述的产品,基于所述结晶含氮部分的重量百分数,具有小于2.5%的磷含量。
5.如前一权利要求所述的产品,基于所述结晶含氮部分的重量百分数,具有小于1%的磷含量。
6.如任一前述权利要求所述的产品,其中,所述结晶含氮部分占所述基质质量的至少50%。
7.如前一权利要求所述的产品,其中,所述结晶含氮部分占所述基质质量的至少95%。
8.如任一前述权利要求所述的产品,包括由式Si6-zAlzOzN8-z表示的相或“β’硅铝氧氮陶瓷”相,其中,0<z<4.2。
9.如前一权利要求所述的产品,其中,z>1。
10.如前一权利要求所述的产品,其中,z>3。
11.如权利要求8-10中任一项所述的产品,其中,z<4。
12.如前一权利要求所述的产品,其中,z<3.5。
13.如权利要求8-12中任一项所述的产品,其中,所述β’硅铝氧氮陶瓷相占所述结晶含氮部分质量的大于60%。
14.如前一权利要求所述的产品,其中,所述β’硅铝氧氮陶瓷相占所述结晶含氮部分质量的大于75%。
15.如任一前述权利要求所述的产品,包括AlN15R相。
16.如前一权利要求所述的产品,其中,所述AlN15R相占所述结晶含氮部分质量的大于18%。
17.如前一权利要求所述的产品,其中,所述AlN15R相占所述结晶含氮部分质量的大于20%。
18.如权利要求8-17中任一项所述的产品,其中,基于所述基质的重量百分数,大于80重量%的所述结晶含氮部分由所述β’硅铝氧氮陶瓷相构成,并且若适宜,由所述β’硅铝氧氮陶瓷相和AlN15R相构成。
19.如权利要求8-18中任一项所述的产品,其中,所述β’硅铝氧氮陶瓷相和任意AlN15R相一起占所述结晶含氮部分质量的大于90%。
20.如任一前述权利要求所述的产品,其中,所述基质占所述产品质量的至少5%。
21.如前一权利要求所述的产品,其中,所述基质占所述产品质量的至少15%。
22.如任一前述权利要求所述的产品,其中,所述基质占所述产品质量的小于60%。
23.如前一权利要求所述的产品,其中,所述基质占所述产品质量的小于25%。
24.如任一前述权利要求所述的产品,由以下部分构成:
·由粒度大于选自200μm、100μm、50μm和20μm的阈值粒度D阈值的一组微粒的质量构成的第一部分;以及
·粘结所述第一部分的微粒的第二部分;
所述磷含量仅基于所述第二部分中存在的所述结晶含氮部分测量。
25.如前一权利要求所述的产品,其中,所述第二部分占所述产品质量的至少5%。
26.如前一权利要求所述的产品,其中,所述第二部分占所述产品质量的至少15%。
27.如任一前述权利要求所述的产品,其中,所述第二部分占所述产品质量的小于60%。
28.如前一权利要求所述的产品,其中,所述第二部分占所述产品质量的小于25%。
29.如权利要求24-28中任一项所述的产品,其中,D阈值等于200μm。
30.如任一前述权利要求所述的产品,其中,全部所述结晶含氮部分形成所述基质。
31.如任一前述权利要求所述的产品,其中,基于所述产品的重量百分数,残余硅含量小于1.8%。
32.如前一权利要求所述的产品,其中,基于所述产品的重量百分数,所述残余硅含量小于1%。
33.如任一前述权利要求所述的产品,基于所述产品的重量百分数,碱土金属氧化物总含量小于2%。
34.如任一前述权利要求所述的产品,基于所述产品的重量百分数,碱土金属氧化物总含量大于0.2%。
35.如任一前述权利要求所述的产品,基于所述产品的重量百分数,碱金属氧化物总含量小于1%。
36.如任一前述权利要求所述的产品,基于所述产品的重量百分数,碱金属氧化物总含量大于0.4%。
37.如任一前述权利要求所述的产品,其中,超过70重量%的粒料由选自氧化铝、莫来石、莫来石前体、氧化铬、氧化锆、锆石、氮化物、碳化物、无定形或至少部分结晶的碳及所述物质的混合物的材料形成的微粒构成,和/或由所述微粒的混合物构成。
38.如任一前述权利要求所述的产品,其中
·至少50%的粒料微粒具有大于0.2mm的粒度;以及
·至少15%的微粒具有大于2mm的粒度;以及
·至少90重量%的粒料微粒具有小于20mm的粒度。
39.如任一前述权利要求所述的产品,其中,x≥0.01和/或y>0.01和/或u≥0.01和/或v>0.01。
40.如任一前述权利要求所述的产品,其中,x≥0.1和/或y>0.05和/或u≥0.05和/或v>0.1。
41.如任一前述权利要求所述的产品,其中,x≥0.2和/或y>0.14和/或u≥0.14和/或v>0.3。
42.如任一前述权利要求所述的产品,其中,x≥0.1和y>0.05和u≥0.05和v>0.1。
43.一种由第一部分和第二部分构成的难熔块状物,所述第一部分由粒度大于200μm的一组微粒的质量构成,所述第二部分粘结所述第一部分的微粒,所述块状物具有至少一个至少为120mm的总体尺寸并包括至少一个由烧结部分形成的部分,所述烧结部分包括含有由式SixAlyOuNv表示的硅铝氧氮陶瓷相的结晶含氮部分,其中:
·x大于或等于0,且小于或等于1;
·y大于0,且小于或等于1;
·u大于或等于0,且小于或等于1;
·v大于0,且小于或等于1;
基于所述产品的重量百分数,所述烧结产品包括小于1.8%的残余硅含量。
44.如前一权利要求所述的块状物,其中,基于所述产品的重量百分数,所述残余硅含量小于1%。
45.如前两项权利要求之一所述的块状物,其中,所述烧结产品为如权利要求1-39中任一项所述的产品。
46.如权利要求43-45中任一项所述的块状物,其具有大于50kg的质量。
47.如权利要求43-46中任一项所述的块状物,其具有大于300kg的质量。
48.如权利要求43-47中任一项所述的块状物,其至少具有大于120mm的长度或宽度或厚度。
49.如权利要求43-48中任一项所述的块状物,其中,所述厚度、长度和宽度至少为150mm。
50.一种颗粒混合物,其以适于通过在氮气中反应性烧结,或在氮以足够量存在于所述颗粒混合物中的情况下则在非氧化性气氛中烧结来形成如权利要求1-42中任一项所述的烧结难熔产品的基质的比例和形式包括磷源、硅源、铝源和氧源,或甚至氮源。
51.如前一权利要求所述的颗粒混合物,包括选自氢磷酸盐、铝磷酸盐和碱金属聚磷酸盐、有机磷化合物和有机磷聚合物以及以上化合物的混合物的含磷化合物。
52.如前两项权利要求之一所述的颗粒混合物,包括:
·大于1%且小于15%的二氧化硅;和/或
·大于0.5%且小于5%的金属硅,所述金属硅的中值粒度小于200μm;和/或
·大于2%且小于15%的金属铝,所述金属铝的中值粒度小于200μm;和/或
·大于0.5%且小于10%的煅烧的氧化铝,所述煅烧的氧化铝的中值粒度小于10μm;
所述百分数为基于所述颗粒混合物的干物质的重量百分数。
53.如前三项权利要求中任一项所述的颗粒混合物,其中,磷与金属铝的重量比大于5×10-5且小于5×10-2。
54.一种选自熔炉和热交换器的装置,其包括至少部分由如权利要求1-42中任一项所述的烧结难熔产品形成或由所述产品构成的衬套。
55.一种生产难熔块状物的方法,包括如下步骤:
a)制备包括难熔粒料、硅铝氧氮陶瓷前体和含磷液体或固体化合物的初始装料;
b)将所述初始装料浇铸入模具中;
c)在所述模具中通过压紧模塑所述初始装料以形成粗产品;
d)从所述模具中取出所述粗产品;
e)干燥所述粗产品;
f)在还原性氮气氛中,或在氮由所述初始装料供给的情况下则在非氧化性气氛中,在1300℃-1600℃温度下焙烧所述粗产品以得到块状物;
所述初始装料确定为使得在步骤f)末期,所述块状物为权利要求43-49中任一项所述的块状物,或如此构成根据权利要求50-53中任一项的颗粒混合物。
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FR0759747A FR2924711B1 (fr) | 2007-12-11 | 2007-12-11 | Produit refractaire a matrice de sialon dope |
FR0759747 | 2007-12-11 | ||
PCT/FR2008/052272 WO2009083678A2 (fr) | 2007-12-11 | 2008-12-11 | PRODUIT REFRACTAIRE A MATRICE DE SiAlON DOPE |
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EP (1) | EP2222616B1 (zh) |
CN (1) | CN101896440B (zh) |
BR (1) | BRPI0821583B1 (zh) |
FR (1) | FR2924711B1 (zh) |
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Cited By (2)
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CN104120454A (zh) * | 2014-07-01 | 2014-10-29 | 湖南创元铝业有限公司 | 预焙阳极抗氧化性陶瓷基涂层及其涂覆方法 |
CN105593192A (zh) * | 2013-09-30 | 2016-05-18 | 圣戈班研究中心与欧洲研究院 | 具有SiAlON基体的耐火产品 |
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FR2953512B1 (fr) * | 2009-12-09 | 2017-03-31 | Saint Gobain Centre De Rech Et D'etudes Europeen | Produit refractaire a matrice de siaion dope bore |
CN102134164B (zh) * | 2010-01-21 | 2013-04-17 | 宜兴市国强炉业有限公司 | 高温耐磨修补涂料及其制备方法 |
CN102093078B (zh) * | 2010-12-13 | 2013-01-09 | 华东理工大学 | 轻质节能仿天然石材的陶瓷装饰材料及其制造方法 |
CN103964794B (zh) * | 2014-04-25 | 2015-06-17 | 焦作安泰新型耐磨材料有限公司 | 纳米增强耐磨防腐陶瓷料及其制备方法和使用方法 |
CN111138205B (zh) * | 2020-02-18 | 2022-04-12 | 中钢洛耐科技股份有限公司 | 一种抗侵蚀赛隆刚玉制品的制备方法 |
CN115536397B (zh) * | 2022-10-30 | 2023-06-16 | 中钢集团洛阳耐火材料研究院有限公司 | 一种用于埋碳气氛的自修复碳化硅耐火材料 |
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DE1646700B1 (de) * | 1965-04-22 | 1970-12-17 | Montedison Spa | Verfahren zur Herstellung von Formkoerpern aus Siliziumnitrid oder dessen Gemischen mit Siliziumcarbid |
US3991166A (en) * | 1972-01-11 | 1976-11-09 | Joseph Lucas (Industries) Limited | Ceramic materials |
DE2805292C2 (de) * | 1977-09-28 | 1982-03-11 | Toshiba Ceramics Co., Ltd., Tokyo | Verfahren zur Herstellung eines Sinterkörpers |
US4533646A (en) * | 1982-06-03 | 1985-08-06 | Dresser Industries, Inc. | Nitride bonded oxide refractories |
JP3164917B2 (ja) * | 1992-10-14 | 2001-05-14 | 株式会社いすゞセラミックス研究所 | 低摩擦セラミックス |
US5380782A (en) * | 1993-10-04 | 1995-01-10 | Rohm And Haas Company | Polymeric dispersants for ceramic materials |
CN1189417C (zh) * | 2000-09-06 | 2005-02-16 | 冶金工业部洛阳耐火材料研究院 | 高炉出铁沟用免烘烤型捣打料 |
CN1166583C (zh) * | 2001-10-23 | 2004-09-15 | 洛阳市洛华粉体工程特种耐火材料厂 | 进口闪速炉、奥斯曼特冶金炉用耐火浇注料 |
CN1261388C (zh) * | 2003-05-09 | 2006-06-28 | 宜兴天霸非金属材料有限公司 | 抗氧化碳化硅浇注料 |
CN1528708A (zh) * | 2003-10-16 | 2004-09-15 | 上海交通大学 | 陶瓷材料及利用陶瓷材料制作旋转喷头的工艺 |
CN100348538C (zh) * | 2003-12-22 | 2007-11-14 | 北京天坛股份有限公司 | 一种耐火浇注料的制备方法 |
JP4581120B2 (ja) * | 2004-04-26 | 2010-11-17 | 独立行政法人物質・材料研究機構 | 酸窒化物粉末およびその製造方法 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105593192A (zh) * | 2013-09-30 | 2016-05-18 | 圣戈班研究中心与欧洲研究院 | 具有SiAlON基体的耐火产品 |
CN105593192B (zh) * | 2013-09-30 | 2018-04-24 | 圣戈班研究中心与欧洲研究院 | 具有SiAlON基体的耐火产品 |
CN104120454A (zh) * | 2014-07-01 | 2014-10-29 | 湖南创元铝业有限公司 | 预焙阳极抗氧化性陶瓷基涂层及其涂覆方法 |
CN104120454B (zh) * | 2014-07-01 | 2016-08-17 | 湖南创元铝业有限公司 | 预焙阳极抗氧化性陶瓷基涂层及其涂覆方法 |
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HUE040367T2 (hu) | 2019-03-28 |
EP2222616B1 (fr) | 2018-09-12 |
FR2924711A1 (fr) | 2009-06-12 |
FR2924711B1 (fr) | 2010-11-19 |
BRPI0821583B1 (pt) | 2019-06-04 |
BRPI0821583A2 (pt) | 2015-06-16 |
WO2009083678A2 (fr) | 2009-07-09 |
WO2009083678A3 (fr) | 2009-10-08 |
EP2222616A2 (fr) | 2010-09-01 |
CN101896440B (zh) | 2013-03-13 |
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