CN113860881A - 相转化法制备纤维独石结构氮化硅陶瓷材料 - Google Patents
相转化法制备纤维独石结构氮化硅陶瓷材料 Download PDFInfo
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 35
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Abstract
本发明属于高温陶瓷材料技术领域,具体涉及相转化法制备纤维独石结构氮化硅陶瓷材料,本发明以Si3N4陶瓷为胞体材料,稀土硅酸盐(RE2SiO5、RE2Si2O7,RE=稀土元素)为新型胞界面材料,开发一种简单、有效的相转化方法,成功制备得到仿竹木结构的Si3N4纤维独石陶瓷材料,克服了现有氮化硅基陶瓷材料断裂韧性低的缺点。本发明的制备方法工艺简单、高效,陶瓷纤维的直径和界面层厚度可调可控;所制备的纤维坯体具有一定的柔性和强度,方便后续排布;本发明在采用相转化法制备纤维独石结构氮化硅陶瓷制备的过程中,可采用冷等静压+无压烧结的方法,生产效率高,能同时制备多个样品。
Description
技术领域
本发明属于高温透波陶瓷材料技术领域,具体涉及相转化法制备纤维独石结构氮化硅陶瓷材料。
背景技术
陶瓷材料以其优异的高温性能成为高温透波领域的主要候选材料之一。目前常见的高温透波陶瓷主要包括氮化硅(Si3N4)、氮化硼(BN)、氧化铝(Al2O3)、石英以及磷酸盐陶瓷等。与其它陶瓷材料相比,Si3N4陶瓷具有较优异的综合性能,它不仅具有高的强度和模量、良好的抗热震性能、优异的抗雨蚀性能,还具有高的热稳定性、良好的高温力学性能以及高温抗氧化性能等,是当前最有前景的高温透波陶瓷材料之一,也是近年来氮化物陶瓷中的研究热点。
然而,由于Si3N4陶瓷由强的共价键组成,其断裂韧性较低,在外来载荷的作用下,无法承受一定程度的缺陷,往往会发生灾难性的破坏,从而使其实际应用受到了限制。而向Si3N4陶瓷中引入如颗粒、晶须以及纤维等增强体是对Si3N4陶瓷增强补韧的主要手段。其中,纤维的增韧效果最好,但是纤维品种较少,价格昂贵,加之编织工艺复杂,在应用和产业化上受到了极大的限制。
在仿竹木结构的纤维独石结构中,将强度较高的纤维状胞体材料和弱结合胞界面材料按照一定的方式排列,由于在材料断裂过程中可以诱导裂纹偏转,使裂纹钝化、增大断裂表面、消耗断裂能,从而可以获得具有优异断裂韧性的复合材料。但当前尚未有利用稀土硅酸盐作为界面层材料制备仿竹木结构的Si3N4纤维独石陶瓷材料的报道。因此,有必要开发一种简单、有效的相转化来制备仿竹木结构的Si3N4纤维独石陶瓷材料。
发明内容
为了克服上述现有技术的不足,本发明提出了一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,制备所得的Si3N4纤维独石陶瓷材料具有仿竹木结构的纤维独石结构特征,克服了现有氮化硅基陶瓷材料断裂韧性低的缺点。
为了实现上述目的,本发明所采用的技术方案是:
本发明提供了一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,该方法包括以下步骤:
S1、将Si3N4粉末、BN粉末和烧结助剂一起进行湿法球磨后经干燥、过筛后制得陶瓷粉末;
S2、将聚醚砜或聚砜加入到N-甲基吡咯烷酮中,完全溶解后制得聚合物溶液;
S3、将稀土硅酸盐粉末、粘结剂和去离子水或酒精一起进行球磨后获得稀土硅酸盐界面层材料的涂覆浆料;
S4、将步骤S1中制备的陶瓷粉末加入到步骤S2所制备的聚合物溶液中,经脱泡处理后将陶瓷浆料抽取到注射器中,并利用注射泵将浆料以一定的直径挤入到水中,经浸泡和干燥后制得纤维坯体;
S5、利用浸渍法或者喷涂法将步骤S3中制备的稀土硅酸盐界面层涂覆浆料涂覆到步骤S4制得的纤维坯体上;
S6、将步骤S5的纤维坯体裁切成所需要的长度并进行排布,然后相继进行冷压成型、冷等静压,高温排胶以及无压烧结或热压烧结,最后制得纤维独石结构氮化硅陶瓷。
优选地,所述Si3N4粉末、BN粉末和烧结助剂的质量百分比为:30-100wt.%、0-50wt.%、0-20wt.%。
优选地,所述烧结助剂的种类包括Y2O3+Al2O3,Yb2O3等,在所述Y2O3+Al2O3中,所述Y2O3与Al2O3的质量比为1.5-3。
优选地,所述冷压成型的压强为10-30MPa,保压时间为1-5min;冷等静压的压力为50-250MPa,保压时间为5-30min;高温排胶的温度为650-800℃,时间为2-6小时;无压烧结的温度为1600-1900℃,保温时间为1-6小时。
优选地,步骤S2中,聚合物溶液的浓度为0.01-0.5g/mL。
优选地,稀土硅酸盐粉末中的稀土元素包括La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y和Sc共17种元素中的一种或几种。
优选地,稀土硅酸盐界面层涂覆浆料的浓度为2-40wt.%,并且粘结剂的浓度为0-5wt.%。进一步地,所述粘结剂包括但不限于甲基纤维素。
优选地,步骤S4中,每毫升聚合物溶液加入0.5-1.5g陶瓷粉末;浆料的挤入直径为0.1-2mm。
优选地,步骤S6中,排布方式分为随机排布和定向排布,定向排布为纤维层间自下而上的堆叠角度为0-90°。
本发明还提供了采用上述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法制备得到的纤维独石结构氮化硅陶瓷材料。
优选地,步骤S1中湿法球磨的时间为6-24h,转速为100-360r/min;步骤S3的球磨时间为6-24h。
优选地,步骤S5中,浸渍法涂覆为将步骤S5所制备的纤维坯体放入步骤S3所制备的界面层涂覆浆料中,浆料完全浸没纤维坯体,停留5-300s后取出干燥。
优选地,步骤S5中,喷涂法涂覆为将步骤S3所制备的界面层涂覆浆料通过喷枪喷涂到步骤S5所制备的纤维坯体表面,然后干燥。
与现有技术相比,本发明的有益效果是:
本发明以Si3N4陶瓷为胞体材料,稀土硅酸盐(RE2SiO5、RE2Si2O7,RE=稀土元素)为新型胞界面材料,开发一种简单、有效的相转化方法,成功制备得到仿竹木结构的Si3N4纤维独石陶瓷材料,克服了现有氮化硅基陶瓷材料断裂韧性低的缺点。本发明的制备方法工艺简单、高效,陶瓷纤维的直径和界面层厚度可调可控;所制备的纤维坯体具有一定的柔性和强度,方便后续排布;本发明在采用相转化法制备纤维独石结构氮化硅陶瓷制备的过程中,采用冷等静压+无压烧结的方法,生产效率高,能同时制备多个样品。
附图说明
图1为氮化硅纤维坯体表面和截面的SEM图(a为纤维坯体的表面形貌,b为纤维坯体的截面形貌);
图2为直径分别为0.3mm、0.5mm、0.8mm以及1mm的Si3N4基体纤维坯体的宏观形貌;
图3为Si3N4基纤维独石陶瓷材料垂直于(a)和平行于(b)纤维排布方向的断面SEM图。
具体实施方式
下面对本发明的具体实施方式作进一步说明。在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
下述实施例中的实验方法,如无特殊说明,均为常规方法,下述实施例中所用的试验材料,如无特殊说明,均为可通过常规的商业途径购买得到。
实施例1一种相转化法制备纤维独石结构氮化硅陶瓷的制备方法
该方法包括以下步骤:
(1)称取65wt.%的Si3N4粉末、25wt.%的BN粉末和10wt.%的烧结助剂【Y2O3+Al2O3,m(Y2O3):m(Al2O3)=2】,利用行星式球磨机湿法球磨18h,转速为200r/min,之后于70℃烘箱中进行干燥,干燥之后的陶瓷粉末过100目筛备用。
(2)以聚醚砜(PES)作为聚合物基体粘结剂,N-甲基吡咯烷酮(NMP)作为溶剂,将一定量的PES加入到NMP中,充分搅拌直到完全溶解,作为聚合物溶液,聚合物溶液的浓度为0.10g/mL。
(3)将20wt.%的稀土硅酸盐Yb2Si2O7粉末以及2wt.%的甲基纤维素粘结剂和去离子水或酒精球磨18h,转速为260r/min,获得浓度为20wt.%的稀土硅酸盐界面层涂覆浆料。
(4)将步骤1中制备的陶瓷粉末加入到步骤2所制备的聚合物溶液中(每毫升聚合物溶液加入1.0g陶瓷粉末),充分搅拌得到陶瓷浆料,浆料经15min脱泡处理后,抽取到注射器中。
(5)将步骤4装有浆料的注射器安装到注射泵上,利用注射泵将浆料以一定的直径(0.3,0.5,0.8,1.0mm)挤入到装有去离子水的结晶皿中,浸泡24h,之后将纤维坯体从水中取出后进行干燥。
对制备所得的纤维坯体进行扫描电子显微镜(SEM)分析,由图1可以看出,用相转化法制备的基体纤维直径非常均与,在纤维外表面,Si3N4被聚醚砜包裹而沉积下来,表面比较平整。
同时,由图2可以看出,所制备的纤维坯体直径是可以调控的,从而有利于对材料的性能进行优化。此外,该方法也可以实现连续基体纤维坯体的制备,且所制备的基体纤维具有一定的强度和柔性,可弯曲打圈,为接下来的涂覆和排布提供了便捷。
(6)利用浸渍或者喷涂的方法对干燥后的纤维坯体进行稀土硅酸盐界面层材料涂覆:在采用浸渍法涂覆时,将步骤(5)所制备的纤维坯体放入步骤(3)所制备的界面层涂覆浆料中,浆料完全浸没纤维坯体,停留45s后取出干燥;或者在采用喷涂法涂覆时,将步骤(3)所制备的界面层涂覆浆料通过喷枪喷涂到步骤(5)所制备的纤维坯体表面,然后干燥。
(7)将干燥后的纤维坯体裁切成所需要的长度并进行排布。排布方式分为短切纤维随机排布,或纤维定向排布,所述定向排布即纤维层间自下而上的堆叠角度为0-90°(本实施采用45°);
(8)将排布好的纤维放入冷压模具中在24T手动分体式压片机(深圳市科晶智达科技有限公司,型号:YLJ-24T-SJ)上进行冷压成型,压强为20MPa,保压时间为3min,随后放入电动冷等静压机(深圳市科晶智达科技有限公司,型号:YLJ-CIP-60A)中进行冷等静压,压力为200MPa,保压时间为20min;将冷压后的坯体放入1200度管式炉(深圳市科晶智达科技有限公司,型号:OTF-1200X)中,在700℃下保温4小时进行排胶,将排胶后的陶瓷坯体放入1900度真空烧结炉(长沙市开福区同达真空机械厂,型号:TDS/25/40/1900)中进行无压烧结,烧结温度为1750℃,保温时间是4小时;最后制备得到纤维独石结构氮化硅陶瓷。
对制备得到的纤维独石结构氮化硅陶瓷进行断面SEM分析。如图3所示的Si3N4基纤维独石陶瓷材料垂直于和平行于纤维排布方向的断面SEM图,可以很清楚的看出其具有仿竹木结构的纤维独石结构特征,同时,断面明显显示出裂纹在界面处有偏转的现象。
实施例2一种相转化法制备纤维独石结构氮化硅陶瓷的制备方法
该方法包括以下步骤:
(1)称取70wt.%的Si3N4粉末、10wt.%的BN粉末和20wt.%的烧结助剂【Y2O3+Al2O3,m(Y2O3):m(Al2O3)=3】,利用行星式球磨机湿法球磨24h,转速为100r/min,之后于100℃烘箱中进行干燥,干燥之后的陶瓷粉末过200目筛备用。
(2)以聚醚砜(PES)作为聚合物基体粘结剂,N-甲基吡咯烷酮(NMP)作为溶剂,将一定量的PES加入到NMP中,充分搅拌直到完全溶解,作为聚合物溶液,聚合物溶液的浓度为0.25g/mL。
(3)将5wt.%的稀土硅酸盐粉末Y2SiO5+Yb2Si2O7(其中Y2SiO5和Yb2Si2O7的质量比为1:1)以及5wt.%的甲基纤维素粘结剂和去离子水或酒精球磨24h,转速为300r/min,获得浓度为5wt.%的稀土硅酸盐界面层涂覆浆料。
(4)将步骤1中制备的陶瓷粉末加入到步骤2所制备的聚合物溶液中(每毫升聚合物溶液加入1.5g陶瓷粉末),充分搅拌得到陶瓷浆料,浆料经20min脱泡处理后,抽取到注射器中。
(5)将步骤4装有浆料的注射器安装到注射泵上,利用注射泵将浆料以一定的直径(0.3,0.5,0.8,1.0mm)挤入到装有去离子水的结晶皿中,浸泡48h,之后将纤维坯体从水中取出后进行干燥。
(6)利用浸渍或者喷涂的方法对干燥后的纤维坯体进行稀土硅酸盐界面层材料涂覆:在采用浸渍法涂覆时,将步骤(5)所制备的纤维坯体放入步骤(3)所制备的界面层涂覆浆料中,浆料完全浸没纤维坯体,停留60s后取出干燥;或者在采用喷涂法涂覆时,将步骤(3)所制备的界面层涂覆浆料通过喷枪喷涂到步骤(5)所制备的纤维坯体表面,然后干燥。
(7)将干燥后的纤维坯体裁切成所需要的长度并进行排布。排布方式分为短切纤维随机排布,或纤维定向排布,所述定向排布即纤维层间自下而上的堆叠角度为0-90°(本实施例采用60°);
(8)将排布好的纤维放入冷压模具中在24T手动分体式压片机(深圳市科晶智达科技有限公司,型号:YLJ-24T-SJ)上进行冷压成型,压强为30MPa,保压时间为1min,随后放入电动冷等静压机(深圳市科晶智达科技有限公司,型号:YLJ-CIP-60A)中进行冷等静压,压力为250MPa,保压时间为5min;将冷压后的坯体放入1200度管式炉(深圳市科晶智达科技有限公司,型号:OTF-1200X)中,在800℃下保温2小时进行排胶,将排胶后的陶瓷坯体放入1900度真空烧结炉(长沙市开福区同达真空机械厂,型号:TDS/25/40/1900)中进行无压烧结,烧结温度为1900℃,保温时间是1小时;最后制备得到纤维独石结构氮化硅陶瓷。
实施例3一种相转化法制备纤维独石结构氮化硅陶瓷的制备方法
该方法包括以下步骤:
(1)称取48wt.%的Si3N4粉末、45wt.%的BN粉末和15wt.%的烧结助剂【Y2O3+Al2O3,m(Y2O3):m(Al2O3)=1.5】,利用行星式球磨机湿法球磨6h,转速为360r/min,之后于50℃烘箱中进行干燥,干燥之后的陶瓷粉末过40目筛备用。
(2)以聚醚砜(PES)作为聚合物基体粘结剂,N-甲基吡咯烷酮(NMP)作为溶剂,将一定量的PES加入到NMP中,充分搅拌直到完全溶解,作为聚合物溶液,聚合物溶液的浓度为0.05g/mL。
(3)将10wt.%的稀土硅酸盐粉末Ho2SiO5+Lu2SiO+Er2SiO5(三者的质量比为1:1:
1)以及0.5wt.%的甲基纤维素粘结剂和去离子水或酒精球磨6h,转速为200r/min,获得浓度为10wt.%的稀土硅酸盐界面层涂覆浆料。
(4)将步骤1中制备的陶瓷粉末加入到步骤2所制备的聚合物溶液中(每毫升聚合物溶液加入0.5g陶瓷粉末),充分搅拌得到陶瓷浆料,浆料经5min脱泡处理后,抽取到注射器中。
(5)将步骤4装有浆料的注射器安装到注射泵上,利用注射泵将浆料以一定的直径(0.3,0.5,0.8,1.0mm)挤入到装有去离子水的结晶皿中,浸泡12h,之后将纤维坯体从水中取出后进行干燥。
(6)利用浸渍或者喷涂的方法对干燥后的纤维坯体进行稀土硅酸盐界面层材料涂覆:在采用浸渍法涂覆时,将步骤(5)所制备的纤维坯体放入步骤(3)所制备的界面层涂覆浆料中,浆料完全浸没纤维坯体,停留5s后取出干燥;或者在采用喷涂法涂覆时,将步骤(3)所制备的界面层涂覆浆料通过喷枪喷涂到步骤(5)所制备的纤维坯体表面,然后干燥。
(7)将干燥后的纤维坯体裁切成所需要的长度并进行排布。排布方式分为短切纤维随机排布,或纤维定向排布,所述定向排布即纤维层间自下而上的堆叠角度为0-90°(本实施例采用90°);
(8)将排布好的纤维放入冷压模具中在24T手动分体式压片机(深圳市科晶智达科技有限公司,型号:YLJ-24T-SJ)上进行冷压成型,压强为10MPa,保压时间为5min,随后放入电动冷等静压机(深圳市科晶智达科技有限公司,型号:YLJ-CIP-60A)中进行冷等静压,压力为50MPa,保压时间为30min;将冷压后的坯体放入1200度管式炉(深圳市科晶智达科技有限公司,型号:OTF-1200X)中,在650℃下保温6小时进行排胶,将排胶后的陶瓷坯体放入1900度真空烧结炉(长沙市开福区同达真空机械厂,型号:TDS/25/40/1900)中进行无压烧结,烧结温度为1600℃,保温时间是6小时;最后制备得到纤维独石结构氮化硅陶瓷。
以上对本发明的实施方式作了详细说明,但本发明不限于所描述的实施方式。对于本领域的技术人员而言,在不脱离本发明原理和精神的情况下,对这些实施方式进行多种变化、修改、替换和变型,仍落入本发明的保护范围内。
Claims (10)
1.一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,包括以下步骤:
S1、将Si3N4粉末、BN粉末和烧结助剂一起进行湿法球磨后经干燥、过筛后制得陶瓷粉末;
S2、将聚醚砜或聚砜加入到N-甲基吡咯烷酮中,完全溶解后制得聚合物溶液;
S3、将稀土硅酸盐粉末、粘结剂和去离子水或酒精一起进行球磨后获得稀土硅酸盐界面层材料的涂覆浆料;
S4、将步骤S1中制备的陶瓷粉末加入到步骤S2所制备的聚合物溶液中,经脱泡处理后将陶瓷浆料抽取到注射器中,并利用注射泵将浆料以一定的直径挤入到水中,经浸泡和干燥后制得纤维坯体;
S5、利用浸渍法或者喷涂法将步骤S3中制备的稀土硅酸盐界面层涂覆浆料涂覆到步骤S4制得的纤维坯体上;
S6、将步骤S5的纤维坯体裁切成所需要的长度并进行排布,然后相继进行冷压成型、冷等静压,高温排胶以及无压烧结或热压烧结,最后制得纤维独石结构氮化硅陶瓷。
2.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,所述Si3N4粉末、BN粉末和烧结助剂的质量百分比为:30-100wt.%、0-50wt.%、0-20wt.%。
3.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,所述烧结助剂的种类包括Y2O3+Al2O3,Yb2O3,在所述Y2O3+Al2O3中,所述Y2O3与Al2O3的质量比为1.5-3。
4.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,所述冷压成型的压强为10-30MPa,保压时间为1-5min;冷等静压的压力为50-250MPa,保压时间为5-30min;高温排胶的温度为650-800℃,时间为2-6小时;无压烧结的温度为1600-1900℃,保温时间为1-6小时。
5.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,步骤S2中,聚合物溶液的浓度为0.01-0.5g/mL。
6.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,稀土硅酸盐粉末中的稀土元素包括La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y和Sc共17种元素。
7.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,稀土硅酸盐界面层涂覆浆料的浓度为2-40wt.%,并且粘结剂的浓度为0-5wt.%。
8.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,步骤S4中,每毫升聚合物溶液加入0.3-2.0g陶瓷粉末;浆料的挤入直径为0.05-2mm。
9.根据权利要求1所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法,其特征在于,步骤S6中,排布方式分为随机排布和定向排布,定向排布为纤维层间自下而上的堆叠角度为0-90°。
10.采用权利要求1-9任一项所述的一种通过相转化法制备纤维独石结构氮化硅陶瓷材料的方法制备得到的纤维独石结构氮化硅陶瓷材料。
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