CN107354447A - 一种低导热氮化硼‑碳化硅薄膜的制备方法 - Google Patents
一种低导热氮化硼‑碳化硅薄膜的制备方法 Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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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
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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Abstract
本发明提供一种碳纳米管‑SiC薄膜的制备方法,包括以下步骤:将过渡金属衬底和碳纳米管粉体置于真空反应系统中,碳纳米管粉末颗粒尺寸为10纳米‑20纳米,采用氩气分别作为碳纳米管粉体载气体和三氯甲基硅烷载气体,氢气作为反应气体,在除去真空腔内氧气的情况下,维持室内真空度1‑1000Pa,并升温至800‑1200℃,将氢气注入真空腔中,流量为100‑500mL/min,分别将载有碳纳米管粉末和三氯甲基硅烷的氩气体通入真空腔中,流量分别为10‑100ml/min和100‑500ml/min,碳纳米管粉末供给速度为10‑100mg/min,同时保持氢气流量,保温1‑5h,降温速率为5‑20℃/min。本发明有益效果主要在于提高了SiC薄膜的高温抗氧化,抗烧蚀性能。
Description
技术领域
本发明涉及一种低导热碳化硅薄膜的制备方法,特别是涉及一种低导热氮化硼-碳化硅薄膜的制备方法。
背景技术
碳化硼的大部分性能比碳素材料更优。对于六方氮化硼:摩擦系数很低、高温稳定性很好、耐热震性很好、强度很高、导热系数很高、膨胀系数较低、电阻率很大、耐腐蚀、可透微波或透红外线。专利申请公开号为CN 102417375 A的发明公开了一种炭/ 炭复合材料碳化硅/ZrB2-碳化硅/碳化硅 涂层及其制备方法。包括内涂层、外涂层和中间涂层,内涂层的厚度为20 ~ 50μm,外涂层的厚度为30 ~ 80μm,中间涂层的厚度为50 ~ 80μm。通过包埋发法制备碳化硅 内涂层,降低中间层ZrB2-碳化硅与C/C复合材料的热应力。通过超音速等离子喷涂制备ZrB2-碳化硅 中间层,ZrB2-碳化硅为C/C复合材料提供良好的高温烧蚀、中低温抗氧化及隔热性能。通过沉积法制备碳化硅 外涂层,有效愈合涂层表面缺陷,阻止氧气的渗入,为C/C 复合材料提供良好的高温氧化保护。同时在中低温氧化过程中,ZrB2的氧化产物B 2O3可有效愈合涂层中的缺陷,为涂层试样提供良好的中温氧化保护。
专利申请公开号为CN 103722849 A的发明公开了一种SiC/Ta/C/Ta/SiC多层抗氧化耐高温涂层及其制备方法。由碳化硅 层、Ta 层和C 层叠层组成,其特征在于叠层的次序依次为SiC层、Ta 层、C 层、Ta 层、SiC层,循环1~3次,C层两侧均为Ta层,最内层和最外层均为碳化硅层,通过化学气相沉积法在所制备的碳化硅层上依次沉积Ta层,C层,Ta层和碳化硅层,得到SiC/Ta/C/Ta/SiC多层防氧化耐高温涂层。外层碳化硅在高温有氧环境中形成一层SiO2膜,能有效阻止氧原子的扩散,同时在Ta 层和C 层的接触面,可形成TaC层进一步提高抗氧化性能。涂层的交替沉积能够有效缓解涂层之间热膨胀系数差异,可显著提高涂层的热震性能,通过控制沉积时间和沉积次数可控制基体的厚度和层数,可实现对复合涂层微观结构的控制。
发明内容
本发明的目的旨在提高碳化硅薄膜的高温抗氧化,抗烧蚀性能,提供一种能有效提高基体表面高温抗氧化、抗烧蚀性能的氮化硼-碳化硅薄膜的制备方法。
为实现本发明的目的,所采用的技术方案是:一种氮化硼-碳化硅薄膜的制备方法,其特征在于将过渡金属衬底和氮化硼粉体置于真空反应系统中,氮化硼粉末颗粒尺寸为10-20nm,采用氩气分别作为氮化硼粉体载气体和三氯甲基硅烷载气体,氢气作为反应气体,在除去真空腔内氧气的情况下,维持室内真空度1-500Pa,并升温至1000-1200℃,将氢气注入真空腔中,流量为200-500mL/min,分别将载有氮化硼粉末和三氯甲基硅烷的氩气体通入真空腔中,流量分别为10-100ml/min和100-500ml/min,氮化硼粉末供给速度为10-100mg/min,同时保持氢气流量,保温1-5h,降温速率为5-20℃/min。
本发明的有益效果:1.工艺简单,可实现大面积生长;2.所制备的氮化硼薄膜具有较好的抗化学侵蚀和无机酸侵蚀的性能;3.所制备的氮化硼薄膜在硬度强度较高的同时,具有较高的韧性;4.具有较低的导热性能。
具体实施方式
下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
一种低导热氮化硼-碳化硅薄膜的制备方法,其特征在于将过渡金属衬底和氮化硼粉体置于真空反应系统中,氮化硼粉末颗粒尺寸为10纳米,采用氩气分别作为氮化硼粉体载气体和三氯甲基硅烷载气体,氢气作为反应气体,在除去真空腔内氧气的情况下,维持室内真空度1Pa,并升温至1000℃,将氢气注入真空腔中,流量为100mL/min,分别将载有氮化硼粉末和三氯甲基硅烷的氩气体通入真空腔中,流量分别为10ml/min和100ml/min,氮化硼粉末供给速度为10mg/min,同时保持氢气流量,保温1h,降温速率为5℃/min。
所制备的氮化硼薄膜具有较好的抗化学侵蚀和无机酸侵蚀的性能;在硬度强度较高的同时,具有较高的韧性,具有较低的导热性能。
实施例2
一种低导热氮化硼-碳化硅薄膜的制备方法,其特征在于将过渡金属衬底和氮化硼粉体置于真空反应系统中,氮化硼粉末颗粒尺寸为20纳米,采用氩气分别作为氮化硼粉体载气体和三氯甲基硅烷载气体,氢气作为反应气体,在除去真空腔内氧气的情况下,维持室内真空度500Pa,并升温至1200℃,将氢气注入真空腔中,流量为500mL/min,分别将载有氮化硼粉末和三氯甲基硅烷的氩气体通入真空腔中,流量分别为100ml/min和500ml/min,氮化硼粉末供给速度为100mg/min,同时保持氢气流量,保温5h,降温速率为20℃/min。
所制备的氮化硼薄膜具有较好的抗化学侵蚀和无机酸侵蚀的性能;在硬度强度较高的同时,具有较高的韧性,具有较低的导热性能。
上述仅为本发明的两个具体实施方式,但本发明的设计构思并不局限于此,凡利用此构思对本发明进行非实质性的改动,均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (1)
1.一种低导热氮化硼-碳化硅薄膜的制备方法,其特征在于将过渡金属衬底和氮化硼粉体置于真空反应系统中,氮化硼粉末颗粒尺寸为10-20nm,采用氩气分别作为氮化硼粉体载气体和三氯甲基硅烷载气体,氢气作为反应气体,在除去真空腔内氧气的情况下,维持室内真空度1-500Pa,并升温至1000-1300℃,将氢气注入真空腔中,流量为200-500mL/min,分别将载有氮化硼粉末和三氯甲基硅烷的氩气体通入真空腔中,流量分别为10-100ml/min和100-500ml/min,氮化硼粉末供给速度为10-100mg/min,同时保持氢气流量,保温1-5h,降温速率为5-20℃/min。
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CN108588675A (zh) * | 2018-04-24 | 2018-09-28 | 苏州宏久航空防热材料科技有限公司 | 一种金刚石切割线及其制备方法 |
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CN103722849A (zh) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | 一种SiC/Ta/C/Ta/SiC多层抗氧化耐高温涂层及其制备方法 |
CN105970185A (zh) * | 2016-04-22 | 2016-09-28 | 苏州派欧技术咨询服务有限公司 | 一种碳纳米管-SiC薄膜的制备方法 |
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CN103722849A (zh) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | 一种SiC/Ta/C/Ta/SiC多层抗氧化耐高温涂层及其制备方法 |
CN105970185A (zh) * | 2016-04-22 | 2016-09-28 | 苏州派欧技术咨询服务有限公司 | 一种碳纳米管-SiC薄膜的制备方法 |
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CN108588675A (zh) * | 2018-04-24 | 2018-09-28 | 苏州宏久航空防热材料科技有限公司 | 一种金刚石切割线及其制备方法 |
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