CN112142479B - 一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法 - Google Patents
一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法 Download PDFInfo
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Abstract
本发明公开了一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法,包括如下步骤:(1)将硫酸氧钛溶于蒸馏水中,获得硫酸氧钛水溶液;(2)将SiC粉末、有机溶剂和蒸馏水混合分散,获得混合溶液;(3)在上述混合溶液中加入碳氮原料,同时加入上述硫酸氧钛水溶液,水浴搅拌至沉淀全部析出后,室温静置;(4)将步骤(3)所得的物料进行离心,获得沉淀,用蒸馏水和无水乙醇充分洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;(5)将上述SiC@Ti(C,N)前驱体粉末于氮气气氛下煅烧,再经高温退火,即得。本发明简便易操作,具有制备温度低,成本较低,节能环保等优点。
Description
技术领域
本发明属于材料合成技术领域,具体涉及一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法。
背景技术
碳化硅具有各种优异的性能,如超硬耐磨、高热导率和机械强度、低热膨胀系数、耐化学腐蚀、高温稳定性(直到2500℃的分解温度)、有用的电阻特性等。碳化硅作为一种结构材料被广泛应用于各个领域。但是碳化硅材料韧性较低,脆性大,碳化硅晶片的断裂韧性一般在2.5~3MPa.m1/2之间;反应烧结纯碳化硅粉体的烧结温度在1450-1700℃之间,纯碳化硅粉体在1450℃以下结合性较差。
发明内容
本发明的目的在于克服现有技术缺陷,提供一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法。
本发明的技术方案如下:
一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法,包括如下步骤:
(1)将硫酸氧钛溶于蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,获得硫酸氧钛水溶液;
(2)将SiC粉末、有机溶剂和蒸馏水混合,并超声(频率20kHZ功率300W)分散,获得混合溶液;
(3)在上述混合溶液中加入碳氮原料搅拌均匀,同时缓慢加入上述硫酸氧钛水溶液,水浴搅拌至沉淀全部析出后,室温静置24-48h;上述碳氮原料为三聚氰胺、尿素和石墨相氮化碳中的至少一种;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇充分洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末于氮气气氛下煅烧,再经高温退火,即得所述SiC@Ti(C,N)核壳结构陶瓷粉体。
在本发明的一个优选实施方案中,所述步骤(1)中,所述硫酸氧钛和蒸馏水的比例为1.5-2.5g∶45-55mL。
进一步优选的,所述步骤(1)中,所述硫酸氧钛和蒸馏水的比例为2g∶50mL。
在本发明的一个优选实施方案中,所述步骤(2)中,所述SiC粉末、有机溶剂和蒸馏水的比例为1.5-2.5g∶15-25mL∶90-110mL。
进一步优选的,所述步骤(2)中,所述SiC粉末、有机溶剂和蒸馏水的比例为2g∶20mL: 100mL。
在本发明的一个优选实施方案中,所述SiC、碳氮原料和硫酸氧钛的质量比为 2∶3-8∶0.4-1。
在本发明的一个优选实施方案中,所述硫酸氧钛和蒸馏水的比例为2g∶50mL,所述SiC粉末、有机溶剂和蒸馏水的比例为2g∶20mL∶100mL,所述SiC、碳氮原料和硫酸氧钛的质量比为2∶3-8∶0.4-1。
在本发明的一个优选实施方案中,所述有机溶剂为乙二醇、异丙醇或正丙醇。
在本发明的一个优选实施方案中,所述煅烧的温度为600-800℃,时间为1-2h。
在本发明的一个优选实施方案中,所述高温退火的温度为1200-1400℃。
本发明的有益效果是:
1、本发明简便易操作,具有制备温度低,成本较低,节能环保等优点。
2、本发明通过制备出核壳结构的SiC@Ti(C,N)陶瓷材料,提高了碳化硅基体材料的断裂韧性。
3、本发明制备的SiC@Ti(C,N)核壳结构陶瓷粉体的壳层厚度为10-100nm,具有包裹性良好,壳层厚度可控等优点。
附图说明
图1为本发明实施例1至5制备的SiC@Ti(C,N)陶瓷粉体材料(a)与纯碳化硅(b) 的扫描电镜照片。
图2为本发明实施例2、4制备的SiC@Ti(C,N)陶瓷粉体材料的粉末衍射图。
图3为本发明实施例1至5制备的SiC@Ti(C,N)陶瓷粉体材料的扫描电镜照片。
图4为本发明实施例4制备的SiC@Ti(C,N)陶瓷粉体的显微维氏硬度压痕图。
具体实施方式
以下通过具体实施方式对本发明的技术方案进行进一步的说明和描述。
实施例1
(1)将2.00g硫酸氧钛溶于50mL蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,稀释至0.01g/mL,获得硫酸氧钛水溶液;
(2)将2.00g SiC粉末、20mL乙二醇和100mL蒸馏水混合,并超声(频率20kHZ 功率300W)分散20-60min,获得混合溶液;
(3)在上述混合溶液中加入4.00g CO(NH2)2搅拌均匀,同时缓慢加入80mL上述硫酸氧钛水溶液,水浴搅拌24h至沉淀全部析出后,室温静置48h;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇反复超声和离心洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末置于管式炉中,于氮气气氛下800℃煅烧2h,再经1400℃高温退火,即得如图1和3所示的所述SiC@Ti(C,N)核壳结构陶瓷粉体,其壳层厚度约为100±1nm,在型号为ZHV-1MDXS高级半自动显微维氏硬度计 (Semi-automaticmicrophotometer)上对样品进行了显微硬度测定。测试仪器采用正四棱锥体金刚石压头,在1.96N试验力作用下压入试样表面,保荷时间10s后,样品最大显微硬度高达1642HV,采用压痕法测出断裂韧性最高5.88MPa.m1/2,相比于纯碳化硅材料的断裂韧性提高了96%。
实施例2
(1)将2.00g硫酸氧钛溶于50mL蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,稀释至0.01g/mL,获得硫酸氧钛水溶液;
(2)将2.00g SiC粉末、20mL乙二醇和100mL蒸馏水混合,并超声(频率20kHZ 功率300W)分散20-60min,获得混合溶液;
(3)在上述混合溶液中加入3.00g CO(NH2)2搅拌均匀,同时缓慢加入30mL上述硫酸氧钛水溶液,水浴搅拌24h至沉淀全部析出后,室温静置48h;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇反复超声和离心洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末置于管式炉中,于氮气气氛下800℃煅烧2h,再经1250℃高温退火,即得如图1、2和3所示的所述SiC@Ti(C,N)核壳结构陶瓷粉体,壳层厚度约为52±1nm,样品最大显微硬度高达1434HV,采用压痕法测出断裂韧性最高5.55MPa.m1/2,相比于纯碳化硅材料的断裂韧性提高了85%。
实施例3
(1)将2.00g硫酸氧钛溶于50mL蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,稀释至0.01g/mL,获得硫酸氧钛水溶液;
(2)将2.00g SiC粉末、20mL乙二醇和100mL蒸馏水混合,并超声(频率20kHZ 功率300W)分散20-60min,获得混合溶液;
(3)在上述混合溶液中加入6.00gCO(NH2)2和2.00g g-C3N4搅拌均匀,同时缓慢加入100mL上述硫酸氧钛水溶液,水浴搅拌24h至沉淀全部析出后,室温静置48h;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇反复超声和离心洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末置于管式炉中,于氮气气氛下800℃煅烧2h,再经1200℃高温退火,即得如图1和3所示的所述SiC@Ti(C,N)核壳结构陶瓷粉体,壳层厚度约为100±1nm,样品最大显微硬度高达1025HV,采用压痕法测出断裂韧性最高 3.50MPa·m1 /2,相比于纯碳化硅材料的断裂韧性提高了17%。。
实施例4
(1)将2.00g硫酸氧钛溶于50mL蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,稀释至0.01g/mL,获得硫酸氧钛水溶液;
(2)将2.00g SiC粉末、20mL乙二醇和100mL蒸馏水混合,并超声(频率20kHZ 功率300W)分散20-60min,获得混合溶液;
(3)在上述混合溶液中加入6.00g CO(NH2)2搅拌均匀,同时缓慢加入60mL上述硫酸氧钛水溶液,水浴搅拌24h至沉淀全部析出后,室温静置48h;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇反复超声和离心洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末置于管式炉中,于氮气气氛下800℃煅烧2h,再经1250℃高温退火,即得如图1、2和3所示的所述SiC@Ti(C,N)核壳结构陶瓷粉体,壳层厚度约为82±1nm,测出硬度值高达2587HV,采用压痕法测出断裂韧性最高 3.23MPa.m1/2,相比于纯碳化硅材料的断裂韧性提高了7%(如图4所示)。
实施例5
(1)将2.00g硫酸氧钛溶于50mL蒸馏水中,于30℃水浴搅拌直至澄清,过滤除去不溶物后,稀释至0.01g/mL,获得硫酸氧钛水溶液;
(2)将2.00g SiC粉末、20mL乙二醇和100mL蒸馏水混合,并超声(频率20kHZ 功率300W)分散20-60min,获得混合溶液;
(3)在上述混合溶液中加入2.00g CO(NH2)2搅拌均匀,同时缓慢加入10mL上述硫酸氧钛水溶液,水浴搅拌24h至沉淀全部析出后,室温静置48h;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇反复超声和离心洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末置于管式炉中,于氮气气氛下600℃煅烧2h,再经1250℃高温退火,即得如图1和3所示的所述SiC@Ti(C,N)核壳结构陶瓷粉体,壳层厚度约为34±1nm,样品最大显微硬度高达988HV,采用压痕法测出断裂韧性最高 3.02MPa·m1/2,相比于纯碳化硅材料的断裂韧性提高了0.7%。
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (7)
1.一种SiC@Ti(C,N)核壳结构陶瓷粉体的制备方法,其特征在于:包括如下步骤:
(1)将硫酸氧钛溶于蒸馏水中,于水浴搅拌直至澄清,过滤除去不溶物后,获得硫酸氧钛水溶液;
(2)将SiC粉末、有机溶剂和蒸馏水混合,并超声分散,获得混合溶液,有机溶剂为乙二醇、异丙醇或正丙醇;
(3)在上述混合溶液中加入碳氮原料搅拌均匀,同时缓慢加入上述硫酸氧钛水溶液,水浴搅拌至沉淀全部析出后,室温静置24-48h;上述碳氮原料为三聚氰胺和尿素,或尿素和三聚氰胺,或三聚氰胺、尿素和石墨相氮化碳;
(4)将步骤(3)所得的物料进行离心,除去上层清液,获得沉淀,将该沉淀用蒸馏水和无水乙醇充分洗涤后,经干燥和研磨,获得SiC@Ti(C,N)前驱体粉末;
(5)将上述SiC@Ti(C,N)前驱体粉末于氮气气氛下煅烧,再经高温退火,即得所述SiC@Ti(C,N)核壳结构陶瓷粉体,该煅烧的温度为600-800℃,时间为1-2h,该高温退火的温度为1200-1400℃。
2. 如权利要求1所述的制备方法,其特征在于:所述步骤(1)中,硫酸氧钛和蒸馏水的比例为1.5-2.5g: 45-55mL。
3. 如权利要求2所述的制备方法,其特征在于:所述步骤(1)中,硫酸氧钛和蒸馏水的比例为2g: 50mL。
4. 如权利要求1所述的制备方法,其特征在于:所述步骤(2)中,所述SiC粉末、有机溶剂和蒸馏水的比例为1.5-2.5g: 15-25mL: 90-110mL。
5. 如权利要求4所述的制备方法,其特征在于:所述步骤(2)中,所述SiC粉末、有机溶剂和蒸馏水的比例为2g: 20mL: 100mL。
6.如权利要求1所述的制备方法,其特征在于:所述SiC、碳氮原料和硫酸氧钛的质量比为2:3-8:0.4-1。
7.如权利要求1所述的制备方法,其特征在于:所述硫酸氧钛和蒸馏水的比例为2g:50mL,所述SiC粉末、有机溶剂和蒸馏水的比例为2g: 20mL: 100mL,所述SiC、碳氮原料和硫酸氧钛的质量比为2:3-8:0.4-1。
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