CN112341169A - 一种原位碳化硅晶须强化轻量矾土熟料及其制备方法 - Google Patents
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 54
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000843 powder Substances 0.000 claims abstract description 55
- 239000002994 raw material Substances 0.000 claims abstract description 46
- 239000006229 carbon black Substances 0.000 claims abstract description 31
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 235000012054 meals Nutrition 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 239000002893 slag Substances 0.000 abstract description 22
- 230000035939 shock Effects 0.000 abstract description 12
- 239000011148 porous material Substances 0.000 description 20
- 230000007797 corrosion Effects 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 10
- 230000035699 permeability Effects 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000011819 refractory material Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 4
- 238000001764 infiltration Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 4
- 229910001950 potassium oxide Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 4
- 229910001948 sodium oxide Inorganic materials 0.000 description 4
- 230000008646 thermal stress Effects 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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Abstract
本发明涉及一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。其技术方案是：以80～92wt％的矾土生料微粉、5～11wt％的炭黑和3～9wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，然后在100～200MPa条件下机压成型，得到生坯；最后将所述生坯在110～200℃条件下干燥12～36小时，在1550～1750℃埋碳条件下保温3～8小时，即得原位碳化硅晶须强化轻量矾土熟料。本发明制备的原位碳化硅晶须强化轻量矾土熟料具有孔径小、强度高、抗热震性能好和抗熔渣能力强的特点。
Description
技术领域
本发明属于轻量矾土熟料技术领域。具体涉及一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。
背景技术
2016年，全球175个国家联合签署《巴黎协定》，主要目标是将本世纪全球平均气温上升幅度控制在2摄氏度以内，节约能源和提高能源利用效率已成为国际社会的共识。钢铁、水泥和石化等高温行业能源和资源消耗量大，是节能降耗的重点。研究和开发高温工业用高温轻量化耐火材料可大大降低工业炉窑能耗，对整个高温工业节能减排具有举足轻重的意义。
隔热耐火材料越靠近工作面，其隔热效果越显著。开发可直接用于工作层的低导热、高强、耐热震和抗侵蚀的耐火材料，已成为目前本领域所关注的重要课题之一，其关键在于制备孔径小、高强、耐热震和耐渣蚀的轻量耐火骨料。
矾土熟料是耐火材料消耗量最大的耐火原料之一，被广泛用于高温工业炉的耐火材料。目前国内外针对轻量矾土熟料的制备开展了一定的研究。方义能等(方义能,顾华志,冯运生,等.有机聚合物原位分解法制备微孔轻质矾土骨料[C]//耐火材料综合学术会议,全国不定形耐火材料学术会议,耐火原料学术交流会.2013)采用有机聚合物原位分解法，虽制得微孔轻质矾土骨料，但是所制备的骨料孔径较大、强度不佳、抗热震性能和抗渣性能都不理想。“一种微孔轻量矾土耐火骨料及其制备方法”(ZL 201410447797.X)专利技术，该技术以矾土生料、有机聚合物和添加剂为原料，加水后在行星球磨机湿磨，固化，干燥，高温烧成，制得微孔轻量矾土耐火骨料，但所制备的微孔轻量矾土耐火骨料孔径较大，抗熔渣侵蚀渗透能力有待提高。范昌龙等(范昌龙.轻量微孔矾土熟料的制备与性能研究[D].2015.)以矾土生料、造孔剂、氧化镁为原料，采用湿法球磨虽制得轻量微孔矾土熟料，但是孔径较大，抗热震性能和抗熔渣侵蚀渗透能力不佳。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种孔径小、强度高、抗热震性能好和抗熔渣能力强的原位碳化硅晶须强化轻量矾土熟料及其制备方法。
为实现上述任务，本发明所采用的技术方案是：以80～92wt％的矾土生料微粉、5～11wt％的炭黑和3～9wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在100～200MPa条件下机压成型，得到生坯；然后将所述生坯在110～200℃条件下干燥12～36小时，在1550～1750℃和埋碳条件下保温3～8小时，即得原位碳化硅晶须强化轻量矾土熟料。
所述矾土生料微粉的Al2O3含量≥60wt％；矾土生料微粉的粒径D50为1～10μm。
所述炭黑的C含量≥99wt％；炭黑的粒径≤100nm。
所述二氧化硅微粉的SiO2含量≥98wt％；二氧化硅微粉的粒径≤1μm。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
(1)本发明引入的二氧化硅微粉粒度较细，反应活性高，能够在高温下与矾土生料微粉中含有较多的氧化钾、氧化钠、氧化铁等杂质快速形成液相。在埋碳气氛下，这些液相中的铁和硅组分会被炭黑还原析出成为细小颗粒。一方面，析出的铁具有一定催化作用；另一方面，矾土生料微粉中的氧化钾和氧化钠液相也具有催化作用，使得析出的硅会与炭黑发生反应，原位生成碳化硅晶须。碳化硅晶须的生成能显著提升所制备的原位碳化硅晶须强化轻量矾土熟料(以下简称轻量矾土熟料)的强度、抗热震性能和抗熔渣能力。
(2)本发明中的矾土生料微粉在热处理过程中存在约10％的酌减，同时，炭黑反应也能够原位形成气孔，这些气孔孔径都较大，而原位碳化硅晶须的形成能够分割及堵塞大气孔，因此，所制备的轻量矾土熟料孔径较小。
(3)本发明生成的原位碳化硅晶须具有优异的力学性能，一方面，可以在轻量矾土熟料形成次界面，钉扎位错作用可阻碍裂纹扩展；另一方面，由于原位碳化硅晶须与基体热膨胀系数的差异，将在轻量矾土熟料内部形成残余热应力，使得裂纹发生桥联和偏转，扩展路径延长，能够进一步提升韧性和强度。在承受温度急变时，可以缓冲热应力，材料不易破坏。因此，所制备的轻量矾土熟料强度高和抗热震性能好。
(4)本发明生成的原位碳化硅晶须与熔渣的润湿性较差，可以增大二相界面间的接触角，延缓或阻碍侵蚀和渗透过程，提升矾土熟料的抗熔渣侵蚀渗透能力。
本发明所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.7～3.1g/cm3；平均孔径为200～500nm；1600℃浸泡法抗渣实验侵蚀指数为1～8％，渗透指数为7～20％。
因此，本发明制备的原位碳化硅晶须强化轻量矾土熟料具有孔径小、强度高、抗热震性能好和抗熔渣能力强的特点。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对保护范围的限制：
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。所述制备方法是：以80～92wt％的矾土生料微粉、5～11wt％的炭黑和3～9wt％的二氧化硅微粉为原料；先将所述炭黑和所述二氧化硅微粉在行星球磨机中混匀，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在100～200MPa条件下机压成型，得到生坯；然后将所述生坯在110～200℃条件下干燥12～36小时，在1550～1750℃埋碳条件下保温3～8小时，即得原位碳化硅晶须强化轻量矾土熟料。
本具体实施方式中：
所述矾土生料微粉的Al2O3含量≥60wt％；矾土生料微粉的粒径D50为1～10μm。
所述炭黑的C含量≥99wt％；炭黑的粒径≤100nm。
所述二氧化硅微粉的SiO2含量≥98wt％；二氧化硅微粉的粒径≤1μm。
实施例中不再赘述。
实施例1
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以80wt％的矾土生料微粉、11wt％的炭黑和9wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在200MPa条件下机压成型，得到生坯；然后将所述生坯在200℃条件下干燥12小时，在1550℃和埋碳条件下保温8小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.73g/cm3；平均孔径为496nm；1600℃浸泡法抗渣实验侵蚀指数为8％，渗透指数为20％。
实施例2
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以83wt％的矾土生料微粉、10wt％的炭黑和7wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在150MPa条件下机压成型，得到生坯；然后将所述生坯在160℃条件下干燥24小时，在1650℃和埋碳条件下保温5小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.81g/cm3；平均孔径为432nm；1600℃浸泡法抗渣实验侵蚀指数为7％，渗透指数为16％。
实施例3
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以84wt％的矾土生料微粉、8wt％的炭黑和8wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在170MPa条件下机压成型，得到生坯；然后将所述生坯在150℃条件下干燥24小时，在1600℃和埋碳条件下保温6小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.94g/cm3；平均孔径为324nm；1600℃浸泡法抗渣实验侵蚀指数为6％，渗透指数为12％。
实施例4
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以86wt％的矾土生料微粉、9wt％的炭黑和5wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在120MPa条件下机压成型，得到生坯；然后将所述生坯在180℃条件下干燥18小时，在1700℃和埋碳条件下保温3小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.83g/cm3；平均孔径为286nm；1600℃浸泡法抗渣实验侵蚀指数为3％，渗透指数为13％。
实施例5
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以87wt％的矾土生料微粉、7wt％的炭黑和6wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在150MPa条件下机压成型，得到生坯；然后将所述生坯在130℃条件下干燥30小时，在1650℃和埋碳条件下保温4小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为3.08g/cm3；平均孔径为347nm；1600℃浸泡法抗渣实验侵蚀指数为1％，渗透指数为9％。
实施例6
一种原位碳化硅晶须强化轻量矾土熟料及其制备方法。本实施例所述制备方法是：
以92wt％的矾土生料微粉、5wt％的炭黑和3wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在100MPa条件下机压成型，得到生坯；然后将所述生坯在110℃条件下干燥36小时，在1750℃和埋碳条件下保温3小时，即得原位碳化硅晶须强化轻量矾土熟料。
本实施例所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为3.05g/cm3；平均孔径为212nm；1600℃浸泡法抗渣实验侵蚀指数为2％，渗透指数为7％。
本具体实施方式与现有技术相比具有如下积极效果：
(1)本具体实施方式引入的二氧化硅微粉粒度较细，反应活性高，能够在高温下与矾土生料微粉中含有较多的氧化钾、氧化钠、氧化铁等杂质快速形成液相。在埋碳气氛下，这些液相中的铁和硅组分会被炭黑还原析出成为细小颗粒。一方面，析出的铁具有一定催化作用；另一方面，矾土生料微粉中的氧化钾和氧化钠液相也具有催化作用，使得析出的硅会与炭黑发生反应，原位生成碳化硅晶须。碳化硅晶须的生成能显著提升所制备的原位碳化硅晶须强化轻量矾土熟料(以下简称轻量矾土熟料)的强度、抗热震性能和抗熔渣能力。
(2)本具体实施方式中的矾土生料微粉在热处理过程中存在约10％的酌减，同时，炭黑反应也能够原位形成气孔，这些气孔孔径都较大，而原位碳化硅晶须的形成能够分割及堵塞大气孔，因此，所制备的轻量矾土熟料孔径较小。
(3)本具体实施方式生成的原位碳化硅晶须具有优异的力学性能，一方面，可以在轻量矾土熟料形成次界面，钉扎位错作用可阻碍裂纹扩展；另一方面，由于原位碳化硅晶须与基体热膨胀系数的差异，将在轻量矾土熟料内部形成残余热应力，使得裂纹发生桥联和偏转，扩展路径延长，能够进一步提升韧性和强度。在承受温度急变时，可以缓冲热应力，材料不易破坏。因此，所制备的轻量矾土熟料强度高和抗热震性能好。
(4)本具体实施方式生成的原位碳化硅晶须与熔渣的润湿性较差，可以增大二相界面间的接触角，延缓或阻碍侵蚀和渗透过程，提升矾土熟料的抗熔渣侵蚀渗透能力。
本具体实施方式所制备的原位碳化硅晶须强化轻量矾土熟料经检测：体积密度为2.7～3.1g/cm3；平均孔径为200～500nm；1600℃浸泡法抗渣实验侵蚀指数为1～8％，渗透指数为7～20％。
因此，本具体实施方式制备的原位碳化硅晶须强化轻量矾土熟料具有孔径小、强度高、抗热震性能好和抗熔渣能力强的特点。
Claims (5)
1.一种原位碳化硅晶须强化轻量矾土熟料的制备方法，其特征在于所述制备方法是：以80～92wt％的矾土生料微粉、5～11wt％的炭黑和3～9wt％的二氧化硅微粉为原料，先将所述炭黑和所述二氧化硅微粉在行星球磨机中混合，得到混合料；再将所述矾土生料微粉加入到所述混合料中，在行星球磨机中混合均匀，在100～200MPa条件下机压成型，得到生坯；然后将所述生坯在110～200℃条件下干燥12～36小时，在1550～1750℃和埋碳条件下保温3～8小时，即得原位碳化硅晶须强化轻量矾土熟料。
2.根据权利要求1所述的原位碳化硅晶须强化轻量矾土熟料的制备方法，其特征在于所述矾土生料微粉的Al2O3含量≥60wt％；矾土生料微粉的粒径D50为1～10μm。
3.根据权利要求1所述的原位碳化硅晶须强化轻量矾土熟料的制备方法，其特征在于所述炭黑的C含量≥99wt％；炭黑的粒径≤100nm。
4.根据权利要求1所述的原位碳化硅晶须强化轻量矾土熟料的制备方法，其特征在于所述二氧化硅微粉的SiO2含量≥98wt％；二氧化硅微粉的粒径≤1μm。
5.一种原位碳化硅晶须强化轻量矾土熟料，其特征在于所述的原位碳化硅晶须强化轻量矾土熟料是根据权利要求1～4项中任一项所述的原位碳化硅晶须强化轻量矾土熟料的制备方法所制备的原位碳化硅晶须强化轻量矾土熟料。
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