CN104311077B - 一种Si3N4/SiCw复相结合SiC耐火材料及其制备方法 - Google Patents

一种Si3N4/SiCw复相结合SiC耐火材料及其制备方法 Download PDF

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CN104311077B
CN104311077B CN201410540517.XA CN201410540517A CN104311077B CN 104311077 B CN104311077 B CN 104311077B CN 201410540517 A CN201410540517 A CN 201410540517A CN 104311077 B CN104311077 B CN 104311077B
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李楠
陈俊峰
鄢文
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种Si3N4/SiCW复相结合SiC耐火材料及其制备方法。其技术方案是:以50~75wt%的碳化硅、18~36wt%的单质硅和2~15wt%的碳为原料,外加所述原料3~7wt%的改性结合剂,搅拌均匀,机压成型,成型后的坯体在220℃条件下干燥8~48小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得Si3N4/SiCW复相结合SiC耐火材料。所述烧成的温度制度是:先升温至890~920℃,保温1~3小时;再升温至1180~1350℃,保温4~10小时;然后升温至在1380~1500℃,保温4~10小时。本发明制备工艺简单、物相组成可控和形貌可控;其制品具有优异的抗热震性,解决了现有Si3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。

Description

—种S i 3N4/S iC„复相结合S i c耐火材料及其制备方法
技术领域
[0001] 本发明属于Si3N4结合SiC材料技术领域。具体涉及一种Si #4/31(^复相结合SiC耐火材料及其制备方法。
背景技术
[0002] Si3N4结合SiC材料一般采用反应烧结工艺制备,在烧成过程中,材料边缘先与N 2发生氮化反应,随着反应进行,材料边缘致密化逐渐增加,会阻止氮气向材料内部渗透,致使材料中心氮化反应难以完全,最终使得材料中心部分因难以形成氮化硅增强相导致材料性能下降。一般此类材料的氮化深度很难超过45mm,尽管加入添加剂提高氮化深度,但一方面添加剂会引入杂质,影响材料高温性能,另一方面氮化深度的提高很有限,依然难以解决材料中心难以氮化的问题。
[0003] 为了解决Si3N4结合SiC材料中心难以氮化的问题,“一种超厚氮化硅结合碳化硅制品”(CN201320575873.6)专利技术在大块材料生坯上沿同一方向制造了分布均匀的贯通孔,让氮气能渗透到材料内部使氮化反应完全,但由于贯通孔的存在,一方面限制了砖形,另一方面会在材料内部造成应力集中,影响材料的力学性能。
发明内容
[0004] 本发明旨在克服现有技术缺陷,目的是提供一种制备工艺简单、物相组成可控和形貌可控的相结合SiC耐火材料的制备方法;用该方法制备的Si #4/31(^复相结合SiC耐火材料具有优异的抗热震性,能解决现有Si3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。
[0005] 为实现上述目的,本发明采用的技术方案是:以50~75wt%的碳化硅、18~36wt%的单质娃和2~15wt%的碳为原料,外加所述原料3~7wt%的改性结合剂,搅拌均勾,机压成型,成型后的坯体在220°C条件下干燥8~48小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/31(^复相结合SiC耐火材料。
[0006] 所述烧成的温度制度是:先升温至890~920 °C,保温1~3小时;再升温至1180~1350°C,保温4~10小时;然后升温至在1380~1500°C,保温4~10小时。
[0007] 所述改性结合剂的制备方法是:先将45~60wt%酸醛树脂和40~55wt%单质娃为混合料混合,再外加所述混合料12~25wt%的无水乙醇,然后在55~65°C的水浴锅中搅拌1~3小时,即得改性结合剂。
[0008] 所述碳为鳞片石墨、碳黑和酚醛树脂中的两种或三种的混合物;其中:鳞片石墨的c含量大于97wt%,粒径小于88 μ m ;碳黑的C含量大于99wt%,粒径小于60nm ;酚醛树脂的残碳率大于35wt%。
[0009] 所述单质娃的Si含量大于98wt%,粒径小于40 μ m。
[0010] 所述机压成型的压强为120MPa~250MPa。
[0011] 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:
[0012] 本发明通过控制原料组成和烧成制度,控制Si3N4的含量、SiC的成核及SiC晶须形貌和含量,制备工艺简单;所制备的31#4/31(^复相结合SiC耐火材料的所有部位均得到以Si3N4为主要结合相和以SiC晶须为增韧相,解决了现有Si 3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。
[0013] 本发明制备的Si3N4/SiC#相结合SiC耐火材料经检测:显气孔率为11~18% ;体积密度为2.60-2.80g/cm3;耐压强度为172~220MPa ;1100°C -20°C水冷循环5次后的抗折强度保持率为42~55%。该材料适用于高炉和干熄焦炉。
[0014] 因此,本发明的制备工艺简单、物相组成可控和形貌可控;所制备的相结合SiC耐火材料具有优异的抗热震性,解决了现有Si3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。
具体实施方式
[0015] 下面结合具体实施方式对本发明作进一步的描述,并非对其保护范围的限制。
[0016] 为避免重复,先将本具体实施方式中的原料和改性结合剂统一描述如下,实施例中不再赘述:
[0017] 所述鳞片石墨的C含量大于97wt%,粒径小于88 μm ;所述碳黑的C含量大于99wt%,粒径小于60nm ;所述酸醛树脂的残碳率大于35wt%。
[0018] 所述单质娃的Si含量大于98wt%,粒径小于40 μ m。
[0019] 所述改性结合剂的制备方法是:先将45~60wt%酸醛树脂和40~55wt%单质娃为混合料混合,再外加所述混合料12~25wt%的无水乙醇,然后在55~65°C的水浴锅中搅拌1~3小时,即得改性结合剂。
[0020] 实施例1
[0021] 一种相结合SiC耐火材料及其制备方法。以65~71wt%的碳化硅、20~25wt%的单质娃和5~10wt%的碳为原料,外加所述原料5~7wt%的改性结合剂,搅拌均匀,在压强为120~160MPa条件下机压成型,成型后的坯体在220°C条件下干燥8~16小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/51(^复相结合SiC耐火材料。
[0022] 本实施例所述碳为鳞片石墨和酚醛树脂的混合物。
[0023] 本实施例所述烧成的温度制度是:先升温至890~900°C,保温2~3小时;再升温至1180~1220°C,保温8~10小时;然后升温至在1380~1420°C,保温8~10小时。
[0024] 本实施例制备的Si3N4/SiC^相结合SiC耐火材料经检测:显气孔率为15~18% ;体积密度为2.60-2.68g/cm3;耐压强度为172~198MPa ;1100°C -20°C水冷循环5次后的抗折强度保持率为42~46%。
[0025] 实施例2
[0026] 一种相结合SiC耐火材料及其制备方法。以71~75wt%的碳化硅、18~23wt%的单质娃和2~7wt%的碳为原料,外加所述原料3~5wt%的改性结合剂,搅拌均勾,在压强为150~190MPa的条件下机压成型,成型后的坯体在220°C条件下干燥16~24小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/51(^复相结合SiC耐火材料。
[0027] 本实施例所述碳为碳黑和酚醛树脂的混合物。
[0028] 本实施例所述烧成的温度制度是:先升温至890~900°C,保温2~3小时;再升温至1220~1270°C,保温6~9小时;然后升温至在1420~1460°C,保温6~9小时。
[0029] 本实施例制备的3丨#4/3丨(;复相结合SiC耐火材料经检测:显气孔率为11~14% ;体积密度为2.72-2.80g/cm3;耐压强度为180~200MPa ;1100°C -20°C水冷循环5次后的抗折强度保持率为44~48%。
[0030] 实施例3
[0031] 一种Si3N4/SiCwM相结合SiC耐火材料及其制备方法。以58~65wt%的碳化硅、24~30wt%的单质娃和7~12wt%的碳为原料,外加所述原料4~6wt%的改性结合剂,搅拌均匀,在压强为180~210 MPa的条件下机压成型,成型后的坯体在220°C条件下干燥24~32小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/51(^复相结合SiC耐火材料。
[0032] 本实施例所述碳为鳞片石墨和碳黑的混合物。
[0033] 本实施例所述烧成的温度制度是:先升温至900~910°C,保温1~2小时;再升温至1270~1310°C,保温5~8小时;然后升温至在1450~1480°C,保温5~8小时。
[0034] 本实施例制备的Si3N4/SiC^相结合SiC耐火材料经检测:显气孔率为14~16% ;体积密度为2.68-2.76g/cm3;耐压强度为185~210MPa ;1100°C -20°C水冷循环5次后的抗折强度保持率为46~50%。
[0035] 实施例4
[0036] 一种相结合SiC耐火材料及其制备方法。以50~58wt%的碳化硅、28~36wt%的单质娃和8~15wt%的碳为原料,外加所述原料3~5wt%的改性结合剂,搅拌均匀,在压强为在210~250 MPa的条件下机压成型,成型后的坯体在220°C条件下干燥32~48小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/51(^复相结合SiC耐火材料。
[0037] 本实施例所述碳为鳞片石墨、碳黑和酚醛树脂的混合物。
[0038] 本实施例所述烧成的温度制度是:先升温至910~920°C,保温1~2小时,再升温至1310~1350°C,保温4~6小时,然后升温至在1460~1500°C,保温4~6小时。
[0039] 本实施例制备的3丨#4/3丨(;复相结合SiC耐火材料经检测:显气孔率为12~15% ;体积密度为2.70-2.78g/cm3;耐压强度为190~220MPa ;1100°C -20°C水冷循环5次后的抗折强度保持率为50~55%。
[0040] 本具体实施方式与现有技术相比具有如下积极效果:
[0041] 本具体实施方式通过控制原料组成和烧成制度,控制Si3N4的含量、SiC的成核及SiC晶须形貌和含量,制备工艺简单;所制备的31#4/31(^复相结合SiC耐火材料的所有部位均得到以Si3N4为主要结合相和以SiC晶须为增韧相,解决了现有Si 3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。
[0042] 本具体实施方式制备的31#4/31(^复相结合SiC耐火材料经检测:显气孔率为11-18% ;体积密度为2.60-2.80g/cm3;耐压强度为172~220MPa ;1100°C _20°C水冷循环5次后的抗折强度保持率为42~55%。该材料适用于高炉和干熄焦炉。
[0043] 因此,本具体实施方式的制备工艺简单、物相组成可控和形貌可控;所制备的相结合SiC耐火材料具有优异的抗热震性,解决了现有Si 3N4结合SiC材料因中心部位氮化不完全导致性能下降的问题。

Claims (5)

1.一种Si #4/31(^复相结合SiC耐火材料的制备方法,其特征在于以50~75wt%的碳化娃、18~36wt%的单质娃和2~15wt%的碳为原料,外加所述原料3~7wt%的改性结合剂,搅拌均匀,机压成型,成型后的坯体在220°C条件下干燥8~48小时;干燥后的坯体在氮气气氛中烧成,随炉自然冷却至室温,即得31#4/31(^复相结合SiC耐火材料; 所述烧成的温度制度是:先升温至890~920°C,保温1~3小时,再升温至1180~1350°C,保温4~10小时,然后升温至在1380~1500°C,保温4~10小时; 所述改性结合剂的制备方法是:先将45~60wt%酸醛树脂和40~55wt%单质娃为混合料混合,再外加所述混合料12~25wt%的无水乙醇,然后在55~65°C的水浴锅中搅拌1~3小时,即得改性结合剂; 所述碳为鳞片石墨、碳黑和酚醛树脂中的两种或三种的混合物;其中:鳞片石墨的C含量大于97wt%,碳黑的C含量大于99wt%,酚醛树脂的残碳率大于35wt%。
2.根据权利要求1所述的Si #4/31(^复相结合SiC耐火材料的制备方法,其特征在于所述鳞片石墨的粒径小于88 μm ;所述碳黑的粒径小于60nm。
3.根据权利要求1所述的Si #4/31(^复相结合SiC耐火材料的制备方法,其特征在于所述单质娃的Si含量大于98wt%,粒径小于40 μπι。
4.根据权利要求1所述的Si #4/3;[(^复相结合SiC耐火材料的制备方法,其特征在于所述机压成型的压强为120MPa~250MPa。
5.—种Si #4/31(^复相结合SiC耐火材料,其特征在于所述的Si #4/31(^复相结合SiC耐火材料是根据权利要求1~4项中任一项所述3:[;^4/3;[(^复相结合SiC耐火材料的制备方法所制备的Si3N4/SiCwM相结合SiC耐火材料。
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CN102838360A (zh) * 2012-09-12 2012-12-26 首钢总公司 一种复合耐火材料及其制备方法
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