CN112125674A - 一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷及其制备方法 - Google Patents
一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷及其制备方法 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
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- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 description 1
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- MPCKOQMIBZHVGJ-UHFFFAOYSA-N benzene-1,3-dicarboxylic acid;ethane-1,2-diol Chemical compound OCCO.OC(=O)C1=CC=CC(C(O)=O)=C1 MPCKOQMIBZHVGJ-UHFFFAOYSA-N 0.000 description 1
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 1
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- 229940075529 glyceryl stearate Drugs 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
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- 238000001000 micrograph Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
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- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910021341 titanium silicide Inorganic materials 0.000 description 1
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Abstract
一种高强抗热震抗氧化SiC/O’‑Sialon复相陶瓷及其制备方法,制备所述复相陶瓷的原料及各原料所占质量百分数为:SiC粉40%、α‑Si3N4粉30%、石英粉10%、α‑Al2O3粉5~10%、Y2O3粉3~5%、Sm2O3粉2~4%、ZrO2粉1~10%,原料中加入粘结剂,所述粘结剂的质量为原料的5~10%。本发明制备的陶瓷材料的抗高温性能、抗氧化性能优良,抗热震性好,有效延长吸热系统的使用寿命。
Description
技术领域
本发明涉及新能源材料技术领域,尤其涉及一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷及其制备方法。
背景技术
太阳能作为最理想的可再生能源,开发和利用太阳能的太阳能热发电技术是最具潜力的绿色发电方式,然而,太阳能的昼夜间断性和天气变化导致的不连续性也限制了太阳能热发电技术的应用。塔式太阳能热发电系统由于聚光比高、热力循环温度高、热损耗小、系统简单且效率高的特点得到世界各国的重视,是目前各国都在大力研究的先进的大规模太阳能热发电技术,作为塔式太阳能热发电核心的空气吸热器,其中的高温吸热体材料担负着接收太阳聚光能量,以及吸热换热的重要作用,影响着整个热发电系统的稳定性及效率的高低。
但是,由于塔式吸热器聚光能流密度不均匀性和不稳定性形成的吸热体局部热斑造成材料热应力破坏、空气流动稳定性差以及耐久性不高等问题,对于吸热材料的抗热震抗氧化性能有较高的要求。
目前对吸热材料的研究主要集中在机械性能、热性能和高温稳定性方面。如中国发明专利《铁尾矿基黑色太阳能吸热陶瓷及其制备方法》(CN110128105A)公开了一种以铁尾矿、四氧化三铁、氧化铝、二氧化硅、钾长石、钠长石为原料制备的太阳能吸热陶瓷材料,抗压强度95MPa,30次抗热震后表面无裂纹(室温~500℃),但是没有测试高温抗氧化性能。中国发明专利《一种太阳能热发电用吸热材料》(CN106188758A)公开了一种以间苯二甲酸乙二醇酯、硬脂酸甘油酯、聚乙烯和2-丙烯酰胺基-2-甲基丙磺酸、己酸、苯丁醇等为原料制备的太阳能发电用吸热材料,冲击强度达到了63.89MPa以上,热导率达到了102.12W/m-1·K-1,但是软化温度仅为370.8℃,耐高温性能有待提高。中国发明专利《一种应用于太阳能热发电系统的低成本太阳能陶瓷材料》(CN107162623A)公开了一种以硅化钛、氧化锂、氧化铌、氧化铝、氧化钠、氧化硼、氟化钡和氮化硼为原料制备的太阳能吸热陶瓷材料,具有抗热震能力强,高比表面和高热导率等特点,但其抗压强度仅有0.33MPa,其强度有待提高。因而迫切的需要开发具有抗高温氧化性好、抗热震性好、高强度的新型吸热体材料。
发明内容
为解决上述问题,本发明提出高强抗热震抗氧化SiC/O’-Sialon复相陶瓷及其制备方法,具体技术方案为:
一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷,制备所述复相陶瓷的原料及各原料所占质量百分数为:SiC粉40%、α-Si3N4粉30%、石英粉10%、α-Al2O3粉5~10%、Y2O3粉3~5%、Sm2O3粉2~4%、ZrO2粉1~10%,原料中加入粘结剂,所述粘结剂的质量为原料的5~10%。
进一步地,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1。
进一步地,所述粘结剂为聚乙烯醇水溶液,溶液中聚乙烯醇含量为5wt%。
一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷的制备方法,包括以下步骤:
(1)原料混合:按各原料的配比称取原料,并进行球磨混合1~3h,得到混合料;
(2)造粒和陈腐:加入粘结剂,采用喷雾造粒法进行造粒,然后在容器中密闭陈腐24~36h,得到坯料;其中,粘结剂的加入量为混合料质量的5~10%;
(3)制备坯体:用液压机将坯料压制成型,样品长×宽×高的尺寸为36mm×6.5mm×6.5mm,质量为3g/根,压力为50kN,得到生坯,将生坯置于干燥箱中在95~100℃下干燥10~24h;
(4)烧成:将干燥好的生坯采用分层埋粉烧结工艺,烧成温度1440~1600℃,在烧成温度下保温2~3h,随炉自然冷却后得到SiC/O’-Sialon复相陶瓷材料。
进一步地,步骤(1)中所述SiC粉粗细的粒径分别为240目和700目,其他原料的粒径为200~250目。
进一步地,步骤(4)中采用的埋粉为石墨粉和Si3N4粉,其埋粉工艺为:在匣钵内先铺石墨粉,然后铺Si3N4粉,将生坯埋于Si3N4粉中,最上面再铺一层石墨粉。
进一步地,步骤(4)中的烧结工艺为:1000℃以下升温速率为5℃/min,每隔100℃保温30min,其中300、400、500、600℃保温60min;1000℃及以上升温速率为3℃/min,每隔100℃保温60min,最高烧结温度点1440~1600℃保温3h。
有益效果:
(1)本发明中Sm2O3作为添加剂,可有效促进SiC/O’-Sialon复相陶瓷材料的致密化,降低SiC/O’-Sialon复相陶瓷材料的烧结温度,提高样品的抗高温性能。
(2)本发明提供的太阳能热发电吸热SiC/O’-Sialon复相陶瓷材料具有以下特征:该太阳能热发电吸热SiC/O’-Sialon复相陶瓷材料的抗折强度为100MPa~120MPa,强度高,经1000℃氧化100h后氧化增重率小于11mg·cm-2,抗氧化性能优良。
(3)本发明中制得的陶瓷材料抗热震性能优异,30次热震(1100℃~室温,风冷)循环后无开裂,其抗折强度不低于100MPa,从而可有效延长吸热系统的使用寿命。
附图说明
图1为本发明实施例1中制得的陶瓷材料抗热震30次循环后的扫描电镜图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,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作出创造性劳动的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。
需要说明的是,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。
下面结合附图和具体实施例对本发明做进一步描述:
一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷,制备所述复相陶瓷的原料及各原料所占质量百分数为:SiC粉40%、α-Si3N4粉30%、石英粉10%、α-Al2O3粉5~10%、Y2O3粉3~5%、Sm2O3粉2~4%、ZrO2粉1~10%,原料中加入粘结剂,所述粘结剂的质量为原料的5~10%。
优选地,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1;所述粘结剂为聚乙烯醇水溶液,溶液中聚乙烯醇含量为5wt%。
实施例1:
一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷的制备方法,包括以下步骤:
(1)原料混合:称取40wt%SiC粉、30wt%α-Si3N4粉、10wt%石英粉、5%α-Al2O3粉、3%Y2O3粉、2wt%Sm2O3粉和10wt%ZrO2粉,进行球磨混合1h,得到混合料;其中,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1,所述SiC粉粗细的粒径分别为240目和700目,其他原料的粒径为200目;
(2)造粒和陈腐:加入粘结剂,采用喷雾造粒法进行造粒,然后在容器中密闭陈腐24h,得到坯料;其中,粘结剂为含量为5wt%的聚乙烯醇水溶液,其加入量为混合料质量的5%;
(3)制备坯体:用液压机将坯料压制成型,样品长×宽×高的尺寸为36mm×6.5mm×6.5mm,质量为3g/根,压力为50kN,得到生坯,将生坯置于干燥箱中在95℃下干燥10h;
(4)烧成:将干燥好的生坯采用分层埋粉烧结工艺,烧成温度1440℃,在烧成温度下保温2h,随炉自然冷却后得到SiC/O’-Sialon复相陶瓷材料;其中,采用的埋粉为石墨粉和Si3N4粉,其埋粉工艺为:在匣钵内先铺石墨粉,然后铺Si3N4粉,将生坯埋于Si3N4粉中,最上面再铺一层石墨粉;烧结工艺为:1000℃以下升温速率为5℃/min,每隔100℃保温30min,其中300,400,500,600℃保温60min;1000℃及以上升温速率为3℃/min,每隔100℃保温60min,最高烧结温度点1440℃保温2h。
由附图1可看出,本发明提供的由不同粒径的SiC颗粒和其它原料反应生成的O’-Sialon紧密结合,而不同粒径的SiC颗粒与O’-Sialon结合界面并无较为明显的气孔,这使得材料最终的机械性能、抗热震和抗氧化性能较好。具体的,检测表明,本实施例中提供的陶瓷材料吸水率达6.52%,体积密度达2.40g·cm-3,抗折强度达132.39MPa,经1000℃氧化100h后氧化增重率为8.47mg·cm-2。
检测表明,本实施例中提供的陶瓷材料经30次热震循环实验在(1100℃~室温)后无开裂,其抗折强度为120.90MPa,可满足新一代太阳能热发电技术对吸热材料的性能要求。
实施例2:
(1)原料混合:称取40wt%SiC粉、30wt%α-Si3N4粉、10wt%石英粉、7%α-Al2O3粉、4%Y2O3粉、3wt%Sm2O3粉和6wt%ZrO2粉,进行球磨混合3h,得到混合料;其中,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1,所述SiC粉粗细的粒径分别为240目和700目,其他原料的粒径为250目;
(2)造粒和陈腐:加入粘结剂,采用喷雾造粒法进行造粒,然后在容器中密闭陈腐36h,得到坯料;其中,粘结剂为含量为5wt%的聚乙烯醇水溶液,其加入量为混合料质量的5%;
(3)制备坯体:用液压机将坯料压制成型,样品长×宽×高的尺寸为36mm×6.5mm×6.5mm,质量为3g/根,压力为50kN,得到生坯,将生坯置于干燥箱中在100℃下干燥24h;
(4)烧成:将干燥好的生坯采用分层埋粉烧结工艺,烧成温度1600℃,在烧成温度下保温3h,随炉自然冷却后得到SiC/O’-Sialon复相陶瓷材料;其中,采用的埋粉为石墨粉和Si3N4粉,其埋粉工艺为:在匣钵内先铺石墨粉,然后铺Si3N4粉,将生坯埋于Si3N4粉中,最上面再铺一层石墨粉;烧结工艺为:1000℃以下升温速率为5℃/min,每隔100℃保温30min,其中300,400,500,600℃保温60min;1000℃及以上升温速率为3℃/min,每隔100℃保温60min,最高烧结温度点1600℃保温3h。
检测表明,本实施例中提供的陶瓷材料吸水率达8.92%,体积密度达2.30g·cm-3,抗折强度达108.80MPa,经1000℃氧化100h后氧化增重率为10.56mg·cm-2。本实施例中提供的陶瓷材料经30次热震循环实验在(1100℃~室温)后无开裂,其抗折强度为100.61MPa,可满足新一代太阳能热发电技术对吸热材料的性能要求。
实施例3:
(1)原料混合:称取40wt%SiC粉、30wt%α-Si3N4粉、10wt%石英粉、10%α-Al2O3粉、5%Y2O3粉、4wt%Sm2O3粉和1wt%ZrO2粉,进行球磨混合2h,得到混合料;其中,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1,所述SiC粉粗细的粒径分别为240目和700目,其他原料的粒径为230目;
(2)造粒和陈腐:加入粘结剂,采用喷雾造粒法进行造粒,然后在容器中密闭陈腐30h,得到坯料;其中,粘结剂为含量为5wt%的聚乙烯醇水溶液,其加入量为混合料质量的5%;
(3)制备坯体:用液压机将坯料压制成型,样品长×宽×高的尺寸为36mm×6.5mm×6.5mm,质量为3g/根,压力为50kN,得到生坯,将生坯置于干燥箱中在97℃下干燥17h;
(4)烧成:将干燥好的生坯采用分层埋粉烧结工艺,烧成温度1520℃,在烧成温度下保温2.5h,随炉自然冷却后得到SiC/O’-Sialon复相陶瓷材料;其中,采用的埋粉为石墨粉和Si3N4粉,其埋粉工艺为:在匣钵内先铺石墨粉,然后铺Si3N4粉,将生坯埋于Si3N4粉中,最上面再铺一层石墨粉;烧结工艺为:1000℃以下升温速率为5℃/min,每隔100℃保温30min,其中300,400,500,600℃保温60min;1000℃及以上升温速率为3℃/min,每隔100℃保温60min,最高烧结温度点1600℃保温2h。
检测表明,本实施例中提供的陶瓷材料吸水率达7.53%,体积密度达2.34g·cm-3,抗折强度达115.60MPa,经1000℃氧化100h后氧化增重率为9.36mg·cm-2。检测表明,本实施例中提供的陶瓷材料经30次热震循环实验在(1100℃~室温)后无开裂,其抗折强度为106.12MPa,可满足新一代太阳能热发电技术对吸热材料的性能要求。
综上,本发明制备的陶瓷材料吸水率达6.52~8.92%,体积密度达2.30~2.40g·cm-3,抗折强度达108.80~132.39MPa,经1000℃氧化100h后氧化增重率为8.47~10.56mg·cm-2;经30次热震循环实验在(1100℃~室温)后无开裂,其抗折强度为100.61~120.90MPa,可满足新一代太阳能热发电技术对吸热材料的性能要求。
以上所述仅为本发明较佳的实施例,并非因此限制本发明的实施方式及保护范围,对于本领域技术人员而言,应当能够意识到凡运用本发明说明书及图示内容所作出的等同替换和显而易见的变化所得到的方案,均应当包含在本发明的保护范围内。
Claims (7)
1.一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷,其特征在于,制备所述复相陶瓷的原料及各原料所占质量百分数为:SiC粉40%、α-Si3N4粉30%、石英粉10%、α-Al2O3粉5~10%、Y2O3粉3~5%、Sm2O3粉2~4%、ZrO2粉1~10%,原料中加入粘结剂,所述粘结剂的质量为原料的5~10%。
2.根据权利要求1所述的一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷,其特征在于,所述SiC粉为级配的SiC粉,其粗细的质量比为4:1。
3.根据权利要求1所述的一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷,其特征在于,所述粘结剂为聚乙烯醇水溶液,溶液中聚乙烯醇含量为5wt%。
4.权利要求1~3任一项所述的一种高强抗热震抗氧化SiC/O’-Sialon复相陶瓷的制备方法,其特征在于,包括以下步骤:
(1)原料混合:按各原料的配比称取原料,并进行球磨混合1~3h,得到混合料;
(2)造粒和陈腐:加入粘结剂,采用喷雾造粒法进行造粒,然后在容器中密闭陈腐24~36h,得到坯料;其中,粘结剂的加入量为混合料质量的5~10%;
(3)制备坯体:用液压机将坯料压制成型,样品长×宽×高的尺寸为36mm×6.5mm×6.5mm,质量为3g/根,压力为50kN,得到生坯,将生坯置于干燥箱中在95~100℃下干燥10~24h;
(4)烧成:将干燥好的生坯采用分层埋粉烧结工艺,烧成温度1440~1600℃,在烧成温度下保温2~3h,随炉自然冷却后得到SiC/O’-Sialon复相陶瓷材料。
5.根据权利要求4所述制备方法,其特征在于,步骤(1)中所述SiC粉粗细的粒径分别为240目和700目,其他原料的粒径为200~250目。
6.根据权利要求5所述制备方法,其特征在于,步骤(4)中采用的埋粉为石墨粉和Si3N4粉,其埋粉工艺为:在匣钵内先铺石墨粉,然后铺Si3N4粉,将生坯埋于Si3N4粉中,最上面再铺一层石墨粉。
7.根据权利要求6所述制备方法,其特征在于,步骤(4)中的烧结工艺为:1000℃以下升温速率为5℃/min,每隔100℃保温30min,其中300、400、500、600℃保温60min;1000℃及以上升温速率为3℃/min,每隔100℃保温60min,最高烧结温度点1440~1600℃保温3h。
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