CN116217220A - 一种致密六铝酸钙陶瓷的制备方法 - Google Patents
一种致密六铝酸钙陶瓷的制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 92
- 238000000498 ball milling Methods 0.000 claims abstract description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 abstract description 5
- 239000010959 steel Substances 0.000 abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000000280 densification Methods 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 235000010216 calcium carbonate Nutrition 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
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- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
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- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
本发明公开了一种致密六铝酸钙陶瓷的制备方法,包括以下步骤:取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,所述Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1:0.07~0.2:0.07~0.28;将原料以氧化铝球为球磨介质,在乙醇溶液中球磨12~24h得到球磨浆料;将球磨浆料在90~100℃下干燥12~24h得到混合粉末;将干燥后的混合粉末经80~100目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品。本发明中通过使用Ba2+取代Ca2+和Ti4+取代Al3+的Ba和Ti共掺杂的方法,提高了CA6的致密度,可在钢铁、石化等行业应用。
Description
技术领域
本发明涉及六铝酸钙陶瓷制备领域,尤其涉及一种致密六铝酸钙陶瓷的制备方法。
背景技术
六铝酸钙(CaAl12O19,CA6)是CaO-Al2O3体系中最富铝的中间化合物,其由镜面[CaAlO3]-分隔的层状尖晶石块[Al11O16]+组成,呈六边形结构。CA6具有良好的抗渣蚀性、抗热震性和抗蠕变性,是一种很有前途的耐火材料。而松散的结构会导致强度低,抗熔渣能力差,从而影响CA6在钢铁、石化等需要高密度行业的应用。由于抑制了离子的层间扩散,CA6化合物的细长形貌使其难以通过固相反应致密化。如,1600oC烧结的CA6的开气孔率相当高(> 20%),导致其强度和抗熔渣性能下降。因此,如何在1650oC以下温度获得高容重的CA6对其在钢铁、石化等领域的应用具有重要意义。
CA6的结构决定了其各向异性晶体生长,晶核较好地沿基面生长,形成具有薄片或片状特征的CA6晶粒。但是,薄片结构抑制了其密度的提高,在1600oC~1650 oC制备的CA6的密度通常仅为1.9-2.5 g/cm3(CA6的理论密度是3.79 g/cm3)。目前,大多报道的CA6是薄片结构的,其厚度在100到500纳米,密度较低。Li等以轻质碳酸钙和活性氧化铝为原料,在1650℃、200MPa条件下制备出密度为2.5 g/cm3、孔隙率为35%的CA6,其远达不到于某些特殊应用的要求。Iglesia和Nagaoka等人分别采用火花等离子烧结和热压法制备了具有等轴晶形貌的致密CA6陶瓷,其在沿c轴方向的缺陷可以提高CA6的致密化,然而,上述方法制备的CA6开气孔率(18.5%)仍然很高。近年来,在1650℃以下合成的CA6大部分在1.8~2.3 g/cm3的范围内,甚至在1700℃下合成的CA6也不能达到3.0 g/cm3的密度。
CA6致密化和改变晶化最基本的方法是在c轴或尖晶石块之间产生更多的缺陷,增加沿c轴的扩散速率。Ca2+和Al3+在CA6中的有效扩散系数之比为8:3,对Ca2+或Al3+的取代对CA6陶瓷致密化具有促进作用。因此,从结构调整方面考虑,离子取代是一种提高CA6致密度的较好方法。然而,现有技术难获得可在不高于1600oC烧结温度下制备致密CA6陶瓷的方法。
发明内容
本发明的目的是提供一种致密六铝酸钙陶瓷的制备方法。
本发明的创新点在于本发明中通过使用Ba2+取代Ca2+和Ti4+取代Al3+的Ba和Ti共掺杂的方法,提高了CA6的致密度,可在钢铁、石化等行业应用。
为实现上述发明目的,本发明的技术方案是:
一种致密六铝酸钙陶瓷的制备方法,其特征在于,包括以下步骤:
(1)取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,所述Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1:0.07~0.2:0.07~0.28;
(2)将原料以氧化铝球为球磨介质,在乙醇溶液中球磨12~24h得到球磨浆料;
(3)将球磨浆料在90~100℃下干燥12~24h得到混合粉末;
(4)将干燥后的混合粉末经80~100目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品。
进一步地,所述Al2O3粉末粉末纯度为≥99.5%,CaCO3粉末纯度为≥99%,BaO粉末纯度为≥99.5%,TiO2粉末纯度为≥99%。
进一步地,所述步骤(2)中球磨时原料:球磨介质:乙醇溶液的质量比为1:1~2.5:2~4。
进一步地,所述步骤(4)中高温炉中煅烧温度为1500~1600℃,时间为2~4h。
进一步地,所述氧化铝球的直径为4~8mm。
进一步地,所述步骤(2)中球磨时球磨速度为200~250r/min。
进一步地,所述乙醇溶液的浓度为50~70%。
本发明的有益效果是 :
1、本发明中通过使用Ba2+取代Ca2+和Ti4+取代Al3+的Ba和Ti共掺杂的方法,由于Ba2 +和Ti4+的协同效应,提高了CA6的致密度,可在钢铁、石化等行业应用。
2、本发明中的制备方法只需将粉料混合均匀,成型,干燥后烧结,烧结温度低,成本低廉和工艺简单。
3、本发明中用Ba2+取代Ca2+,增加了CA6的短轴方向长度。用Ti4+取代Al3+,会在CA6的镜像面形成Al空位。当更多的Al空位在镜像面产生时,镜像面和尖晶石块之间的空位浓度会变化很大,从而促进CA6致密。
附图说明
图1为实施例1中制备的共掺杂后CA6的XRD图;
图2为实施例1中制备的未掺杂BaO粉末、TiO2粉末的(a)和共掺杂后CA6的(b)SEM对比图;
图3为实施例2中制备的未掺杂BaO粉末、TiO2粉末的(a)和共掺杂后CA6的(b)SEM对比图;
图4为实施例3中制备的未掺杂BaO粉末、TiO2粉末的(a)和共掺杂后CA6的(b)SEM对比图。
具体实施方式
下面将结合附图对本发明实施例中的技术方案进行清楚、完整地描述。
实施例1:一种致密六铝酸钙陶瓷的制备方法,包括以下步骤:取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,Al2O3粉末粉末纯度为99.5%,CaCO3粉末纯度为99%,BaO粉末纯度为99.5%,TiO2粉末纯度为99%;Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1:0.07:0.07;将原料以氧化铝球为球磨介质,在乙醇溶液中球磨12h得到球磨浆料,氧化铝球的直径为4mm,乙醇溶液的浓度为50%,将球磨浆料在90℃下干燥16h得到混合粉末,球磨时原料:球磨介质:乙醇溶液的质量比为1:1:2;球磨时球磨速度为200r/min。将干燥后的混合粉末经80目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品;高温炉中煅烧温度为1500℃,时间为2h。
如图1所示,其只有CA6相,表明Ba和Ti共掺杂制备的样品是纯CA6相。对比未掺杂和掺杂后的CA6样品,其SEM结果如图2,可见经过共掺杂后,CA6的致密度大大提高。未掺杂CA6的开气孔率高达24%,而共掺杂后CA6的开气孔率仅为7.5%。
实施例2:一种致密六铝酸钙陶瓷的制备方法,包括以下步骤:取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,Al2O3粉末粉末纯度为99.6%,CaCO3粉末纯度为99.2%,BaO粉末纯度为99.6%,TiO2粉末纯度为99.2%;Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1:0.1:0.14;将原料以氧化铝球为球磨介质,在乙醇溶液中球磨18h得到球磨浆料,氧化铝球的直径为6mm,乙醇溶液的浓度为60%,将球磨浆料在95℃下干燥14h得到混合粉末,球磨时原料:球磨介质:乙醇溶液的质量比为1:2:3;球磨时球磨速度为220r/min。将干燥后的混合粉末经90目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品;高温炉中煅烧温度为1550℃,时间为3h。
对本实施例制备的致密CA6六铝酸钙陶瓷进行分析,对比未掺杂和掺杂后的CA6样品,其SEM结果如图3,经过共掺杂后,CA6的致密度大大提高。未掺杂CA6的开气孔率高达21%,而共掺杂后CA6的开气孔率仅为6.2%。
实施例3:一种致密六铝酸钙陶瓷的制备方法,包括以下步骤:取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,Al2O3粉末粉末纯度为99.7%,CaCO3粉末纯度为99.5%,BaO粉末纯度为99.8%,TiO2粉末纯度为99.6%;Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1: 0.2: 0.28;将原料以氧化铝球为球磨介质,在乙醇溶液中球磨12~24h得到球磨浆料,氧化铝球的直径为8mm,乙醇溶液的浓度为70%,将球磨浆料在100℃下干燥12h得到混合粉末,球磨时原料:球磨介质:乙醇溶液的质量比为1: 2.5: 4;球磨时球磨速度为250r/min。将干燥后的混合粉末经100目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品;高温炉中煅烧温度为1600℃,时间为4h。
对本实施例制备的致密CA6六铝酸钙陶瓷进行分析,对比未掺杂和掺杂后的CA6样品,其SEM结果如图4,经过共掺杂后,CA6的致密度大大提高。未掺杂CA6的开气孔率高达18%,而共掺杂后CA6的开气孔率仅为5.5%。
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。
Claims (7)
1.一种致密六铝酸钙陶瓷的制备方法,其特征在于,包括以下步骤:
取Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末为原料,所述Al2O3粉末、CaCO3粉末、BaO粉末、TiO2粉末的质量比为6.12:1:0.07~0.2:0.07~0.28;
将原料以氧化铝球为球磨介质,在乙醇溶液中球磨12~24h得到球磨浆料;
将球磨浆料在90~100℃下干燥12~24h得到混合粉末;
将干燥后的混合粉末经80~100目筛得到过筛粉末,将过筛粉末干压成型,然后在高温炉中煅烧,煅烧后随炉冷却至室温后取出,制得成品。
2.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述Al2O3粉末粉末纯度为≥99.5%,CaCO3粉末纯度为≥99%,BaO粉末纯度为≥99.5%,TiO2粉末纯度为≥99%。
3.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述步骤(2)中球磨时原料:球磨介质:乙醇溶液的质量比为1:1~2.5:2~4。
4.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述步骤(4)中高温炉中煅烧温度为1500~1600℃,时间为2~4h。
5.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述氧化铝球的直径为4~8mm。
6.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述步骤(2)中球磨时球磨速度为200~250r/min。
7.根据权利要求1所述的致密六铝酸钙陶瓷的制备方法,其特征在于,所述乙醇溶液的浓度为50~70%。
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