CN114657533A - 一种在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法 - Google Patents
一种在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法 Download PDFInfo
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Abstract
一种在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，本发明是为了解决现有以金属衬底，采用CVD法制备纳米金刚石得到的纳米金刚石数量少、形状不规则的问题。制备具有规则晶型的纳米金刚石颗粒的方法：一、清洗Mo片及Mo托；二、将Mo片放置在MPCVD装置的沉积系统腔体内，Mo托放置在Mo片上，抽真空后通入H2和CH4，调节微波功率，进行气相沉积，得到带有纳米金刚石的Mo片；三、关闭沉积系统，冷却后将带有纳米金刚石的Mo片放入去离子水中超声，得到纳米金刚石分散液。本发明通过Mo托将等离子体位置提高，使等离子体边缘远离Mo片，减小H等离子体刻蚀，在Mo衬底上制备得到了具有规则晶型的纳米金刚石颗粒。
Description
技术领域
本发明属于纳米材料生长领域，具体涉及一种制备具有规则晶型的分散纳米金刚石颗粒的方法。
背景技术
纳米金刚石是一种一维的碳材料，具有生物相容性，抗菌性等优点，且其内部包含的色心，如NV色心，SiV色心等，特别是在量子光学、纳米尺度磁力计、生物标记与跟踪、磁成像、药物运输等方面具有不可小觑的应用前景。减小金刚石的尺寸，增加色心浓度等均是提高色心荧光强度努力的方向，同时具有规则晶型的表层结构也有利于提高荧光收集效率。然而目前制备纳米金刚石的方法主要包括爆轰法、高温高压法(HPHT)和化学气相沉积法(CVD)。爆轰法过程剧烈不易控制，生产的纳米金刚石一般含有较多的石墨成分。HPHT法纳米金刚石通过将大块金刚石破碎获得，形状各异。CVD法生长纳米金刚石一般结构为膜层结构。目前在制备纳米金刚石时，一般会选择硅片、碳化硅等，也有部分选择金属作为衬底，缺点是纳米金刚石数量少、形状不规则、价格偏高或形成纳米金刚石膜。因此，开发一种经济的、可批量的制备具有规则晶型的分散的高质量的纳米金刚石颗粒的方法是非常重要的。
发明内容
本发明的目的是为了解决现有以金属衬底，采用CVD法制备纳米金刚石得到的纳米金刚石数量少、形状不规则的问题，而提供一种在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法。
本发明在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法按照以下步骤实现：
一、Mo衬底处理：将Mo片及Mo托分别在丙酮、酒精和水中超声清洗，得到清洗后的Mo片和Mo托；
二、微波等离子体化学气相沉积(MPCVD)：将Mo片放置在MPCVD装置的沉积系统腔体内，Mo托放置在Mo片上，腔体抽真空后，通入H2和CH4，控制H2的流量为180～200sccm，CH4的流量为8～15sccm，微波功率为2～4KW，进行气相沉积，得到带有纳米金刚石的Mo片；
三、取样：关闭沉积系统，冷却后将步骤二中带有纳米金刚石的Mo片放入去离子水中超声，取出Mo片，得到纳米金刚石分散液。
本发明以CH4和H2作为气源，使用Mo作为衬底，采用等离子体化学气相沉积法，在温度680℃，压力约14KPa条件下沉积，制备颗粒尺寸约300纳米的具有八面体晶型的纳米金刚石颗粒。本发明通过Mo托将等离子体位置提高，使等离子体边缘远离Mo片，减小H等离子体刻蚀。本发明在Mo衬底上制备得到了具有规则晶型的纳米金刚石颗粒。
本发明具有操作简单、晶型规则，数量多，质量高，颗粒分散等优点，得到的纳米金刚石颗粒在量子光学、纳米尺度磁力计、生物标记与跟踪、磁成像、药物运输等方面具有良好的应用前景。
附图说明
图1为本发明所述生长纳米金刚石的舱体内的结构图；
图2为实施例中生长12h的纳米金刚石的低倍数扫描电镜图片；
图3为实施例中生长12h的纳米金刚石的高倍数扫描电镜图片；
图4为实施例得到的纳米金刚石悬浮液的照片。
具体实施方式
具体实施方式一：本实施方式在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法按照以下步骤实施：
一、Mo衬底处理：将Mo片及Mo托分别在丙酮、酒精和水中超声清洗，得到清洗后的Mo片和Mo托；
二、微波等离子体化学气相沉积(MPCVD)：将Mo片放置在MPCVD装置的沉积系统腔体内，Mo托放置在Mo片上，腔体抽真空后，通入H2和CH4，控制H2的流量为180～200sccm，CH4的流量为8～15sccm，微波功率为2～4KW，进行气相沉积，得到带有纳米金刚石的Mo片；
三、取样：关闭沉积系统，冷却后将步骤二中带有纳米金刚石的Mo片放入去离子水中超声，取出Mo片，得到纳米金刚石分散液。
本实施方式使用的衬底为Mo衬底，由Mo片和Mo托组成，沉积时Mo托在Mo片上。
具体实施方式二：本实施方式与具体实施方式一不同的是步骤一Mo片及Mo托分别在丙酮、酒精和水中超声清洗15min。
具体实施方式三：本实施方式与具体实施方式一或二不同的是步骤一中Mo片的厚度为4mm，Mo托的高度为1.5mm。
具体实施方式四：本实施方式与具体实施方式三不同的是Mo片的直径为40～60mm，Mo托的直径为8～15mm。
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是步骤二中控制H2的流量为180～200sccm，CH4的流量为8～15sccm，微波功率为3KW。
具体实施方式六：本实施方式与具体实施方式五不同的是步骤二中控制H2的流量为190sccm，CH4的流量为10sccm，微波功率为3KW。
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是步骤二中控制沉积系统腔体内压力为12～16KPa。
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是步骤二中Mo片上温度为660～700℃。
具体实施方式九：本实施方式与具体实施方式一至八之一不同的是步骤二中气相沉积时间为10h～16h。
具体实施方式十：本实施方式与具体实施方式一至九之一不同的是步骤三中超声处理时间为10～30min。
实施例：本实施例在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法按照以下步骤实施：
一、Mo衬底处理：将Mo片及Mo托分别在丙酮、酒精和水中超声清洗15min，不使用任何晶种处理，得到清洗后的Mo片和Mo托，其中Mo片的厚度为4mm，Mo托的高度为1.5mm，Mo片的直径为50mm，Mo托的直径为10mm；
二、微波等离子体化学气相沉积(MPCVD)：将Mo片(作为衬底)放置在MPCVD装置的沉积系统腔体内，Mo托放置在Mo片上，腔体抽真空后，通入H2和CH4，控制H2的流量为190sccm，CH4的流量为10sccm，微波功率为3KW，压力为14KPa，Mo片上温度为680℃，进行气相沉积12h，得到带有纳米金刚石的Mo片；
三、取样：关闭沉积系统，冷却后将步骤二中带有纳米金刚石的Mo片放入去离子水中超声15min，取出Mo片，将表面沉积的纳米金刚石颗粒制备得到悬浮液。
根据图1所示，本发明MPCVD装置中Mo片和Mo托放置的结构示意图，以Mo片作为衬底，Mo托将等离子体位置提高1.5mm，使等离子体边缘远离Mo片，减小H等离子体刻蚀，通过提高等离子体位置的方法是十分重要且独特的。通入190sccmH2和10sccmCH4，功率为3KW，压力在14KPa左右，Mo片上温度为680℃，沉积时间为12h。沉积结束后取出Mo片，放入大烧杯的去离子水中，超声15min，将表面沉积的纳米颗粒制备成悬浮液后保存。图2为本发明的生长12h的纳米金刚石的低倍数扫描电镜图片，可见不需要特殊处理即可获得分散颗粒，尺寸在300nm左右。由图3可见，为具有规则晶型具有全(111)面的正八面体纳米金刚石。NV色心在(111)面定向，同时(111)面在掺杂方面很有优势，是具有磷和硼掺杂浓度最高的面，正八面体纳米金刚石的制备将促进纳米金刚石器件等领域的发展。由图4(a)可见，为本实施例使用Mo托获得的分散液，图4(b)为不使用钼托获得的分散液，有明显差别。
Claims (10)
1.在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于该方法按照以下步骤实现：
一、Mo衬底处理：将Mo片及Mo托分别在丙酮、酒精和水中超声清洗，得到清洗后的Mo片和Mo托；
二、微波等离子体化学气相沉积：将Mo片放置在MPCVD装置的沉积系统腔体内，Mo托放置在Mo片上，腔体抽真空后，通入H2和CH4，控制H2的流量为180～200sccm，CH4的流量为8～15sccm，微波功率为2～4KW，进行气相沉积，得到带有纳米金刚石的Mo片；
三、取样：关闭沉积系统，冷却后将步骤二中带有纳米金刚石的Mo片放入去离子水中超声，取出Mo片，得到纳米金刚石分散液。
2.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤一Mo片及Mo托分别在丙酮、酒精和水中超声清洗15min。
3.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤一中Mo片的厚度为4mm，Mo托的高度为1.5mm。
4.根据权利要求3所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于Mo片的直径为40～60mm，Mo托的直径为8～15mm。
5.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤二中控制H2的流量为180～200sccm，CH4的流量为8～15sccm，微波功率为3KW。
6.根据权利要求5所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤二中控制H2的流量为190sccm，CH4的流量为10sccm，微波功率为3KW。
7.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤二中控制沉积系统腔体内压力为12～16KPa。
8.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤二中Mo片上温度为660～700℃。
9.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤二中气相沉积时间为10h～16h。
10.根据权利要求1所述的在Mo衬底上制备具有规则晶型的纳米金刚石颗粒的方法，其特征在于步骤三中超声处理时间为10～30min。
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