CN116606149A - 一种高强高纯氮化硅坩埚及其制备方法和应用 - Google Patents
一种高强高纯氮化硅坩埚及其制备方法和应用 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 223
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 223
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims description 55
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 42
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 41
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- 239000011230 binding agent Substances 0.000 claims description 18
- 239000011863 silicon-based powder Substances 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 15
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims description 11
- 239000012159 carrier gas Substances 0.000 claims description 11
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
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- 229910052710 silicon Inorganic materials 0.000 abstract description 9
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- 238000010998 test method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
本发明涉及多晶硅铸锭技术领域,具体涉及一种高强高纯氮化硅坩埚及其制备方法和应用。本发明采用反应烧结结合化学气相沉积法制备氮化硅坩埚,解决现有反应烧结制备的氮化硅坩埚中,因具有杂质导致的不适合应用于硅晶制备的技术问题。本发明采用化学气相沉积法制备高纯度Si3N4涂层,通过采用此涂层作为坩埚内层,以阻隔氮化硅陶瓷基体中杂质的扩散,避免单晶硅生产中基体内的杂质与硅进行反应。反应烧结的氮化硅基体具有较高的强度,而且CVD Si3N4纯度高无杂质,二者结合后所制备的氮化硅坩埚能够很好地满足单晶硅的制备要求,具有广阔的市场应用前景。
Description
技术领域
本发明涉及多晶硅铸锭技术领域,具体来说是一种高强高纯氮化硅坩埚及其制备方法和应用。
背景技术
以太阳能利用为目的光伏能源具有清洁、环保、可再生等特点,随着工业发展带来的环境污染和破坏问题,太阳能利用已经成为国际大力发展的新能源和战略性新兴产业之一。光伏产业的主导产品有晶体硅太阳能电池等,其中单晶硅电池更是凭借比其他晶体硅太阳能电池更高的转换效率和稳定性,占据重要地位。
在单晶硅生产中,坩埚是熔硅和晶体生长的关键材料,对单晶硅的生产成本和产品产量、质量都有直接的重要影响。传统的石英坩埚在单晶硅制备领域虽然已经广泛应用,但是仍存在很多性能上的不足,如:熔融石英高温性能不足,易导致坩埚破裂;另外石英坩埚易被熔融硅侵蚀,污染产物的同时也可能产生残余应力导致坩埚开裂等问题。
氮化硅陶瓷是一种高温结构特种陶瓷材料,具有强度高、耐高温、抗氧化、抗腐蚀、耐磨损、化学稳定性好、导热系数大和热膨胀系数低等优点,以及与熔融硅不润湿的特性,作为可重复使用的硅晶体冶炼用坩埚材料得到了各国的大力研发。郭大为在“一种反应烧结制备氮化硅坩埚的方法”(CN 104744047A)中提到了以硅粉、粘结剂和溶剂为原料或者以硅粉、氮化硅粉、粘结剂和溶剂为原料,采用反应烧结法制备氮化硅坩埚,而由于粘结剂在烧结时,不可避免的会使得氧、碳积存于氮化硅中,那么在单晶硅的生产制备过程中随温度的升高,氧、碳等杂质不可避免的会进入至单晶硅中,致使单晶硅中不可避免地引入杂质,难以保证单晶硅的纯度要求,即便上述技术方案达到了杂质含量低的技术目的,但是无法从根本上解决在单晶硅生产中保证单晶硅纯度的问题。
发明内容
针对上述现有技术存在的不足,本发明提供了一种高强高纯氮化硅坩埚及其制备方法和应用,本发明采用反应烧结(RS)结合化学气相沉积法(CVD)制备氮化硅坩埚,解决现有反应烧结制备的氮化硅坩埚中,因具有杂质导致的不适合应用于硅晶制备的技术问题。
为实现上述目的,本发明的技术方案如下:
一种高强高纯氮化硅坩埚的制备方法,包括以下步骤:
步骤1、氮化硅基体的制备:
S1、将30~70wt.%的硅粉与20~60wt.%的高纯去离子水混合并球磨8~12h,然后加入分散剂、粘结剂以及烧结助剂继续球磨8~12h混合均匀制得浆料;将浆料浇注到模具中,抽真空30~60min以除去其中气泡,之后在20~40℃下自然干燥24~48h后,得到坩埚坯体;
S2、将步骤1的坩埚坯体于氮气气氛中进行致密烧结,得到氮化硅基体;
将氮化硅基体采用200~600目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面粗糙度控制在0.4~0.8mm;表面粗糙度指表面粗糙的程度,表面略粗糙有利于氮化硅涂层的结合;
步骤2、高强高纯氮化硅坩埚的制备,于步骤S2的氮化硅基体表面沉积氮化硅涂层:
以四氯化硅、氨气为反应源,以氢气为载气,采用鼓泡法、即采用氢气(H2)带出SiCl4,以氩气为稀释气体,采用化学气相沉积法在步骤S2的氮化硅基体表面制备高纯Si3N4涂层,得到高强高纯氮化硅坩埚。
优选的,所述步骤S1中粘结剂为聚乙烯醇缩丁醛或聚乙烯醇;分散剂为磷酸三乙酯或正硅酸乙酯;烧结助剂选自Al2O3、Y2O3、钇铝石榴石中的一种或多种的混合。
优选的,所述步骤S1中硅粉为30~70wt.%、粘结剂为2~3wt.%、分散剂为2~3wt.%、烧结助剂为6~15wt.%、高纯去离子水为20~60wt.%,各原料的质量百分比之和为100%;其中硅粉的粒径为5~40μm。
优选的,所述步骤S2中致密烧结的条件为:于温度为1500~2000℃、压力为0.1~10MPa条件下烧结2~5h。
优选的,所述步骤2中化学气相沉积法的具体操作为:先在沉积温度为800~1000℃下沉积1~3h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在900~1200℃下沉积2~3h,提高氮化硅涂层的厚度至40~150μm。
优选的,所述步骤2中四氯化硅流量为15~60mL/min,氨气流量为20~90mL/min,氢气流量为60~200mL/min,氩气流量为20~300mL/min。
本发明还保护了上述制备方法制得的高强高纯氮化硅坩埚,所述高强高纯氮化硅坩埚的氮化硅基体厚度为3~40mm,所述高纯Si3N4涂层的厚度为40~150μm。
本发明还保护了高强高纯氮化硅坩埚在制备单晶硅生产坩埚中的应用。
与现有技术相比,本发明的有益效果:
1、本发明提出一种高强高纯氮化硅坩埚的制备方法,通过反应烧结结合化学气相沉积法,制备一种具有强度高、耐高温、可保证硅晶生产产物纯净、可长期重复使用的氮化硅坩埚,用以弥补传统反应烧结制备的氮化硅坩埚存在杂质的技术缺陷,本发明的原理在于:采用化学气相沉积法制备高纯度Si3N4涂层,通过采用此涂层作为坩埚内层,以阻隔氮化硅陶瓷基体中杂质的扩散(杂质源于烧结助剂),避免单晶硅生产中基体内的杂质与硅进行反应。反应烧结的氮化硅基体具有较高的强度,而且CVD Si3N4纯度高无杂质,二者结合后所制备的氮化硅坩埚能够很好地满足单晶硅的制备要求,具有广阔的市场应用前景。
2、本发明通过将烧结氮化硅基体的密度、表面粗糙度与CVD Si3N4涂层的沉积温度、沉积时间等参数相结合,氮化硅基体的密度为2.8-3.0g/cm3,表面粗糙度为0.4~0.8mm,进而调控涂层的制备工艺,使涂层封填基体表面残余孔隙的同时,实现涂层和基体的结合,获得一种可保证硅晶生产产物纯净的氮化硅坩埚。
附图说明
图1为本发明实施例1反应烧结制得的氮化硅基体形貌的扫描电镜图;
图2为本发明实施例1化学气相沉积工艺后于氮化硅基体表面沉积的氮化硅涂层表面形貌的扫描电镜图;
图3为本发明实施例1反应烧结结合化学气相沉积工艺制得的高强高纯氮化硅坩埚的横截面形貌的扫描电镜图,即氮化硅基体表面沉积氮化硅涂层后的横截面形貌;
具体实施方式
下面对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。基于本发明中的实施例,本领域普通技术人员在没有做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。本发明各实施例中所述实验方法,如无特殊说明,均为常规方法。
下述实验方法和检测方法,如没有特殊说明,均为常规方法;下述试剂和原料,如没有特殊说明,均为市售。
实施例1
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将30wt.%、粒径为10μm的硅粉与50wt.%的高纯去离子水混合并球磨12h,然后加入3wt.%的分散剂(磷酸三乙酯)、2wt.%的粘结剂(聚乙烯醇缩丁醛)以及各5wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在40℃下自然干燥24h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1500℃、压力为5MPa、时间为2h,得到烧结致密坩埚;
S13、采用200目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.4mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为800℃下沉积3h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1100℃下沉积2h,提高氮化硅涂层的厚度至100μm,氮化硅基体厚度为30mm,得到高强高纯氮化硅坩埚。
实施例2
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将40wt.%、粒径为8μm的硅粉与40wt.%的高纯去离子水混合并球磨12h,然后加入3wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及5wt.%的Al2O3、5wt.%的Y2O3、4wt.%的钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在30℃下自然干燥32h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1600℃、压力为2MPa、时间为4h,得到烧结致密坩埚;
S13、采用300目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.5mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为850℃下沉积2.5h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1000℃下沉积2.5h,提高氮化硅涂层的厚度至120μm,氮化硅基体厚度为25mm,得到高强高纯氮化硅坩埚。
实施例3
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将50wt.%、粒径为5μm的硅粉与30wt.%的高纯去离子水混合并球磨12h,然后加入2wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及各5wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在20℃下自然干燥36h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1800℃、压力为0.1MPa、时间为5h,得到烧结致密坩埚;
S13、采用400目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.6mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为900℃下沉积2h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在900℃下沉积3h,提高氮化硅涂层的厚度至50μm,氮化硅基体厚度为25mm,得到高强高纯氮化硅坩埚。
实施例4
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将50wt.%、粒径为5μm的硅粉与30wt.%的高纯去离子水混合并球磨12h,然后加入2wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及各5wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在20℃下自然干燥24h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为2000℃、压力为5MPa、时间为2h,得到烧结致密坩埚;
S13、采用400目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.6mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为1000℃下沉积2h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1200℃下沉积2h,提高氮化硅涂层的厚度至100μm,氮化硅基体厚度为30mm,得到高强高纯氮化硅坩埚。
实施例5
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将60wt.%、粒径为8μm的硅粉与20wt.%的高纯去离子水混合并球磨12h,然后加入3wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及5wt.%的Al2O3、4wt.%的Y2O3、5wt.%的钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在30℃下自然干燥18h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1700℃、压力为10MPa、时间为5h,得到烧结致密坩埚;
S13、采用500目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.7mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为900℃下沉积2.5h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1100℃下沉积2.5h,提高氮化硅涂层的厚度至80μm,氮化硅基体厚度为32mm,得到高强高纯氮化硅坩埚。
实施例6
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将70wt.%、粒径为10μm的硅粉与20wt.%的高纯去离子水混合并球磨12h,然后加入2wt.%的分散剂(磷酸三乙酯)、2wt.%的粘结剂(聚乙烯醇缩丁醛)以及各2wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在40℃下自然干燥12h后,得到坩埚坯体;
S12、将步骤S11的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1700℃、压力为10MPa、时间为5h,得到烧结致密坩埚;
S13、采用600目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.8mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为800℃下沉积3h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1000℃下沉积3h,提高氮化硅涂层的厚度至150μm,氮化硅基体厚度为35mm,得到高强高纯氮化硅坩埚。
实施例7
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将50wt.%、粒径为5μm的硅粉与30wt.%的高纯去离子水混合并球磨12h,然后加入2wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及各5wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在20℃下自然干燥24h后,得到坩埚坯体;
S12、将步骤S11制得的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1500℃、压力为10MPa、时间为2h,得到烧结致密坩埚;
S13、采用400目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.6mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为800℃下沉积2h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1200℃下沉积2h,提高氮化硅涂层的厚度至40μm,氮化硅基体厚度为3mm,得到高强高纯氮化硅坩埚。
实施例8
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将60wt.%、粒径为8μm的硅粉与20wt.%的高纯去离子水混合并球磨12h,然后加入3wt.%的分散剂(磷酸三乙酯)、3wt.%的粘结剂(聚乙烯醇缩丁醛)以及5wt.%的Al2O3、4wt.%的Y2O3、5wt.%的钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在30℃下自然干燥18h后,得到坩埚坯体;
S12、将步骤S11制得的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为1700℃、压力为7MPa、时间为4h,得到烧结致密坩埚;
S13、采用500目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.7mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为850℃下沉积1.5h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在1100℃下沉积2.5h,提高氮化硅涂层的厚度至80μm,氮化硅基体厚度为32mm,得到高强高纯氮化硅坩埚。
实施例9
一种高强高纯氮化硅坩埚的制备方法,包括如下步骤:
步骤1、氮化硅基体的制备:
S11、将70wt.%、粒径为10μm的硅粉与20wt.%的高纯去离子水混合并球磨12h,然后加入2wt.%的分散剂(磷酸三乙酯)、2wt.%的粘结剂(聚乙烯醇缩丁醛)以及各2wt.%的Al2O3、Y2O3、钇铝石榴石(烧结助剂)继续球磨12h混合均匀制得稳定浆料,然后将浆料浇注到模具中,抽真空30min以除去其中气泡,然后在40℃下自然干燥12h后,得到坩埚坯体;
S12、将步骤S11制得的坩埚坯体置于反应烧结炉中进行烧结致密,烧结气氛为N2,温度为2000℃、压力为5MPa、时间为5h,得到烧结致密坩埚;
S13、采用600目的砂轮进行平整度调整,将步骤S12的烧结致密坩埚打磨光滑,使坩埚表面的粗糙度控制在0.8mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
于氮化硅基体表面沉积氮化硅涂层,具体为:将步骤1的氮化硅基体于沉积炉中进行氮化硅涂层的沉积,沉积工艺如下:
以四氯化硅(SiCl4)、氨气(NH3)为反应源,采用鼓泡法、即采用氢气(H2)为载气带出SiCl4,氩气(Ar)为稀释气体,四氯化硅与氨气的流量比为3:4,采用化学气相沉积法在氮化硅坩埚表面制备高纯Si3N4涂层,先在沉积温度为900℃下沉积1h,使CVD Si3N4能渗透进入氮化硅表面,渗透至烧结工艺造成的未致密孔洞并修饰加工粗糙度,同时与氮化硅坩埚形成良好的结合;然后在900℃下沉积3h,提高氮化硅涂层的厚度至60μm,氮化硅基体厚度为40mm,得到高强高纯氮化硅坩埚。
本发明实施例1-9均制得具有强度高、耐高温、可保证产物纯净、可长期重复使用的氮化硅坩埚,下面以实施例2中的氮化硅坩埚为例,对氮化硅坩埚的性能进行研究,具体研究方法和结果如下所示:
图1为反应烧结制备的氮化硅基体形貌图,图1的测试方法为扫描电子显微镜,结果表明,本发明采用的反应烧结制备的氮化硅基体具有很高的致密化程度。
图2为采用化学气相沉积工艺在氮化硅基体表面沉积的氮化硅涂层表面形貌图,图2的测试方法为扫描电子显微镜,结果表明,CVD工艺制备的氮化硅涂层表面平整且完全致密。
图3为氮化硅基体表面沉积氮化硅涂层后的横截面形貌图,图3的测试方法为扫描电子显微镜,结果表明,基体和涂层基本致密,且基体和涂层结合紧密,完全没有分界。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (8)
1.一种高强高纯氮化硅坩埚的制备方法,其特征在于,包括以下步骤:
步骤1、氮化硅基体的制备:
S1、将硅粉、粘结剂、分散剂、烧结助剂与高纯去离子水混合并球磨,球磨至浆料中硅粉粒径为1~5μm,将浆料置于模具中并去除气泡,然后室温下自然干燥,得到坩埚坯体;
S2、将步骤1的坩埚坯体于氮气气氛中进行致密烧结后,打磨至坩埚表面粗糙度为0.4~0.8mm,得到氮化硅基体;
步骤2、高强高纯氮化硅坩埚的制备:
以四氯化硅、氨气为反应源,以氢气为载气,以氩气为稀释气体,采用化学气相沉积法在步骤S2的氮化硅基体表面制备高纯Si3N4涂层,得到高强高纯氮化硅坩埚。
2.根据权利要求1所述的一种高强高纯氮化硅坩埚的制备方法,其特征在于,所述步骤S1中粘结剂为聚乙烯醇缩丁醛或聚乙烯醇;分散剂为磷酸三乙酯或正硅酸乙酯;烧结助剂选自Al2O3、Y2O3、钇铝石榴石中的一种或多种的混合。
3.根据权利要求1所述的一种高强高纯氮化硅坩埚的制备方法,其特征在于,所述步骤S1中硅粉为30~70wt.%、粘结剂为2~3wt.%、分散剂为2~3wt.%、烧结助剂为6~15wt.%、高纯去离子水为20~60wt.%,各原料的质量百分比之和为100%;其中硅粉的粒径为5~40μm。
4.根据权利要求1所述的一种高强高纯氮化硅坩埚的制备方法,其特征在于,所述步骤S2中致密烧结的条件为:于温度为1500~2000℃、压力为0.1~10MPa条件下烧结2~5h。
5.根据权利要求1所述的一种高强高纯氮化硅坩埚的制备方法,其特征在于,所述步骤2中化学气相沉积法的具体操作为:先在沉积温度为800~1000℃下沉积1~3h,然后在900~1200℃下沉积2~3h。
6.根据权利要求1所述的一种高强高纯氮化硅坩埚的制备方法,其特征在于,所述步骤2中四氯化硅流量为15~60mL/min,氨气流量为20~90mL/min,氢气流量为60~200mL/min,氩气流量为20~300mL/min。
7.一种权利要求1-6任一项所述制备方法制得的高强高纯氮化硅坩埚,其特征在于,所述高强高纯氮化硅坩埚的氮化硅基体厚度为3~40mm,所述高纯Si3N4涂层的厚度为40~150μm。
8.一种权利要求7所述的高强高纯氮化硅坩埚在制备单晶硅生产坩埚中的应用。
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