CN117587381A - 一种纳米草金刚石膜的制备方法及作为高灵敏度电化学电极应用 - Google Patents
一种纳米草金刚石膜的制备方法及作为高灵敏度电化学电极应用 Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 97
- 239000010432 diamond Substances 0.000 title claims abstract description 97
- 244000025254 Cannabis sativa Species 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical compound [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000004050 hot filament vapor deposition Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002086 nanomaterial Substances 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000005530 etching Methods 0.000 abstract description 3
- 238000010900 secondary nucleation Methods 0.000 abstract description 2
- 239000002070 nanowire Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000008351 acetate buffer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- -1 nanotextures Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 238000003631 wet chemical etching Methods 0.000 description 1
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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
本发明制备了一种通过空气中高温退火刻蚀掉纳米草金刚石/非金刚石碳复合结构中的非金刚石碳部分，形成纳米草金刚石，属于功能纳米结构及其制备的技术领域。在制备硼氮共掺杂金刚石/非金刚石复合结构薄膜时，氮气是至关重要的，氮的掺杂导致金刚石形成柱状生长，同时高的甲烷浓度和氮的加入会加剧金刚石二次成核，形成的金刚石晶粒非常小，同时含有大量非金刚石碳，这正是我们想要的结果。去除非金刚石，该金刚石传感器的高密度纳米草结构大大提高了电极的表面积，为检测痕量分子提供更多反应位点。以镉离子为例，在1—100μgL‑1的溶液中具有良好的线性度，可以实现0.28μgL‑1的低检测限。纳米草金刚石传感器具有较好稳定性和可重复使用性，并且制备方法工艺简单，便于大规模制备。
Description
技术领域
本发明属于金刚石纳米结构及其制备的技术领域，涉及一种新型纳米结构金刚石膜的制备方法及作为高灵敏度电化学电极应用
背景技术
金刚石是一种具有超硬度、高导热系数、化学惰性、稳定性等优良性能的功能材料。通过掺入杂质(如硼)使其导电，可以制作高性能的电化学电极。而功能性电极可以通过金刚石的纳米结构(例如纳米织构、纳米线和多孔金刚石等)促进更好的性能。但是，由于极高的硬度和化学惰性，不便于能通过机械加工或湿化学腐蚀来改变金刚石的形貌。金刚石纳米结构的可通过等离子体蚀刻实现，刻蚀出的表面纳米结构增大表面积。中国发明专利申请CN 104709872A公开了一种金刚石纳米线阵列、其制备方法及用于电化学分析的电极，所公开的制备方法是在金刚石膜表面设置掩膜层，暴露待形成纳米线的顶端，采用电感耦合式等氧等离子刻蚀，形成柱状金刚石纳米线，去除顶端掩膜材料，得到深宽比更高的金刚石纳米线阵列，但是这种方法制备纳米结构金刚石存在成本高的问题。
发明内容
为了解决上述问题，本发明通过空气中高温退火刻蚀掉纳米草金刚石/非金刚石碳复合结构中的非金刚石碳部分，处理得到纳米草金刚石，
本发明所采用的技术方案如下：
一种纳米草金刚石膜的制备方法，具体步骤为：
1)采用化学气相沉积(CVD)方法制备硼氮共掺杂金刚石/非金刚石复合结构薄膜：
将氢气、甲烷、硼酸三甲酯、氮气为制备气体，其中，硼酸三甲酯由氢气携带进入腔体，设置氢气流量为150～200sccm；甲烷流量为15～20sccm；携带硼酸三甲酯的氢气流量为2～5sccm；氮气流量为0.5～1sccm，腔体工作气压为7～8KPa，在基底上生长得到硼氮共掺杂金刚石/非金刚石复合结构薄膜；
2)将步骤1)所得硼氮共掺杂金刚石/非金刚石复合结构薄膜置于管式炉中空气气氛下800℃高温退火15～20分钟，刻蚀掉非金刚石部分，形成纳米草金刚石。
所述的化学气相沉积方法包括：微波等离子体化学气相沉积(MPCVD)、热丝化学气相沉积(HFCVD)、热阴极直流等离子体化学气相沉积(DCCVD)等方法。微波等离子体化学气相沉积法中微波功率设定为350～400W。
可以是以在硅、钛等基底上异质外延生长多晶膜薄膜，薄膜必须是氮掺杂的。
本发明所制备的纳米草金刚石膜可作为高灵敏度探测器的电化学电极。
本发明的有益效果：
本发明制备了一种通过空气中高温退火刻蚀掉纳米草金刚石/非金刚石碳复合结构中的非金刚石碳部分，形成高密度的纳米草金刚石。
并用于探测器电化学电极，该探测器的高密度纳米结构大大提高了电极的表面积，为检测痕量分子提供更多反应位点，可大幅提升检测重金属离子的性能，以镉离子为例，在1到100g·L-1的溶液中具有良好的线性度，可以实现0.28g·L-1的低检测限。并具有非常好的稳定性和可重复性。对金刚石传感器在广泛的工业领域中检测低浓度和痕量化学和生物分子具有重要意义。
本发明制备方法工艺简单，便于大规模制备。
附图说明
图1(a)为硼氮共掺杂金刚石/非金刚石复合结构薄膜,(b)为纳米草金刚石的形貌图，(c)、(d)分别为(a)、(b)的高倍放大图。
图2(a)是从1到100g·L-1的不同浓度的镉离子溶液的差分常规脉冲伏安图。(b)是氧化峰值电流值与镉离子浓度之间的拟合线性关系图。
图3纳米草金刚石电极选择性的柱状图。
具体实施方式
以下结合附图与实施例对本申请作进一步详细描述，需要指出的是，以下所述实施例旨在便于对本申请的理解，而对其不起任何限定作用。
实施例1：硅片衬底硼氮共掺杂金刚石/非金刚石复合结构薄膜的制备
选取1cm×1cm大小的硅片作为生长衬底，首先将硅片清洗，去除表面污染物。为了提高生长过程的成核密度，将其生长面放在含金刚石粉的砂纸上研磨15分钟，并放入含有金刚石粉的酒精中超声处理1小时，最后经过丙酮、酒精、去离子水依次超声清洗，用氮气吹干后放入CVD反应室沉积金刚石膜。气相沉积过程中，以氢气、甲烷、携带硼酸三甲酯的氢气、氮气为反应气体，对应的气体流量分别为200sccm、20sccm、2sccm、1sccm，微波功率350W，腔体气压8KPa，生长时间6小时。复合薄膜沉积厚度约为15μm。
在制备硼氮共掺杂金刚石/非金刚石复合结构薄膜时，氮气是至关重要的，氮的掺杂导致金刚石形成柱状生长，同时高的甲烷浓度和氮的加入会加剧金刚石二次成核，形成的金刚石晶粒非常小，同时含有大量非金刚石碳，这正是我们想要的结果。
实施例2：制备纳米草金刚石结构
将硼氮共掺杂金刚石/非金刚石复合结构薄膜置于管式电阻炉800℃空气中高温退火15分钟，快速取出，非金刚石碳在空气中快速氧化消失，剩下金刚石相，同时由于实施例1中氮气的加入，使金刚石纳米草呈现直立柱状生长，制备出高密度硼氮共掺杂纳米草金刚石。
实施例3：用于检测镉离子的电化学测试
用pH＝5.5的醋酸盐缓冲液将镉离子稀释为不同浓度溶液待测。在最优的沉积条件下(沉积时间为270s,沉积电位为-1.0V)，图2(a)是从1到100g·L-1的不同浓度的镉离子溶液的差分脉冲阳极溶出伏安图。显然，随着镉离子浓度的增加，氧化峰电流增加，表明峰电流对低浓度镉离子的响应敏感。图2(b)揭示了氧化峰值电流值与镉离子浓度之间的拟合线性关系，其中相关系数(R2)为0.998。根据三倍信噪比，计算出的检测限为0.28g·L-1，低于欧盟推荐的镉离子标准(水中不超过3g·L-1)。优异的检测能力是因为纳米草硼氮共掺杂金刚石具有较多的反应位点，优良的电催化能力和较高信噪比。此外，相比于其他相关金刚石材料例如硼掺杂金刚石、氮掺杂金刚石、金属颗粒修饰金刚石、石墨修饰金刚石等电极，其检测限分别为1.6、1.1、0.51和0.47g·L-1。纳米草硼氮共掺杂金刚石电极的检测极限比上述报道的电极材料要小，因此纳米草硼氮共掺杂金刚石是一种很有前途的电极材料，用于构建高性能的电化学传感器。
实施例4：用于检测镉离子(Cd2+)的纳米草金刚石电极选择性测试
图3显示了纳米草硼氮共掺杂金刚石电极将包括Pb2+、Zn2+、Ca2+、Cu2+、Mg2+和Na+在内的几种干扰离子分别加入到具有十倍Cd2+浓度的Cd2+标准溶液中。如图3所示，当加入Pb2 +、Zn2+、Ca2+、Cu2+、Mg2+和Na+离子时，Cd2+的信号略有变化。说明纳米草硼氮共掺杂金刚石电极对上述六种离子具有较好的抗干扰性能。
Claims (7)
1.一种纳米草金刚石膜的制备方法，其特征在于，该方法的具体步骤为：
1)采用化学气相沉积方法制备硼氮共掺杂金刚石/非金刚石复合结构薄膜：
将氢气、甲烷、硼酸三甲酯、氮气为制备气体，其中，硼酸三甲酯由氢气携带进入腔体，设置氢气流量为150～200sccm；甲烷流量为15～20sccm；携带硼酸三甲酯的氢气流量为2～5sccm；氮气流量为0.5～1sccm，腔体工作气压为7～8KPa，在基底上生长得到硼氮共掺杂金刚石/非金刚石复合结构薄膜；
2)将步骤1)所得硼氮共掺杂金刚石/非金刚石复合结构薄膜置于管式炉中空气气氛下800℃高温退火15～20分钟，刻蚀掉非金刚石部分，形成纳米草金刚石。
2.根据权利要求1所述的纳米草金刚石膜的制备方法，其特征在于，所述的化学气相沉积方法包括：微波等离子体化学气相沉积、热丝化学气相沉积和热阴极直流等离子体化学气相沉积法。
3.根据权利要求2所述的纳米草金刚石膜的制备方法，其特征在于，微波等离子体化学气相沉积法中微波功率设定为350～400W。
4.根据权利要求1所述的纳米草金刚石膜的制备方法，其特征在于，所述基底为硅、钛材质。
5.根据权利要求1所述的纳米草金刚石膜的制备方法，其特征在于，氢气、甲烷、携带硼酸三甲酯的氢气、氮气的气体流量分别为200sccm、20sccm、2sccm和1sccm。
6.一种根据权利要求1～5任意一项所述方法制备得到的纳米草金刚石膜。
7.如权利要求6所述的纳米草金刚石膜作为高灵敏度探测器的电化学电极的用途。
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