CN112846199A - 利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法 - Google Patents

利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法 Download PDF

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CN112846199A
CN112846199A CN202110025521.2A CN202110025521A CN112846199A CN 112846199 A CN112846199 A CN 112846199A CN 202110025521 A CN202110025521 A CN 202110025521A CN 112846199 A CN112846199 A CN 112846199A
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袁鹏
申凤鸽
陈玉明
张应花
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Abstract

本发明涉及一种利用加热‑冷冻‑研磨‑超声制备超薄铋烯纳米片的方法，适用于制备少层铋烯纳米片。所述方法包括以下步骤：(1)取铋粉加入研钵，150‑180℃加热；(2)冷冻研钵中研磨；(3)重复步骤(1)和(2)；(4)称取步骤(3)处理后的铋粉，加入乙醇，配制浓度为10mg/mL的混悬液；(5)探针超声30min，每超声3s，间歇3s，功率300W；(6)水浴超声300min，功率400‑600W；(7)5000rpm离心10min，收集上清液，即为铋烯纳米片分散液。本发明采用加热‑冷冻‑研磨‑超声法制备铋烯纳米片，制备方法简单，可以制备超薄铋烯纳米片。

Description

利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法
技术领域
本发明涉及二维纳米材料制备技术领域，具体涉及一种利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法。
背景技术
自从Novoselov等人在2004年成功使用胶带法从石墨中剥离石墨烯以来，石墨烯和石墨烯样二维纳米材料出现快速发展。近年来，二维纳米材料因其独特、优异的化学和物理性能，使其在储能和转化装置、催化、传感器、生物医学和环境保护等领域得到了广泛的应用。除石墨烯系列外，二硫化钼、二硫化钨、磷烯、砷烯、锑烯、铋烯等一系列二维纳米材料相继被发现和制备。由于金属铋储量丰富，在常温空气中稳定，并且毒性小，生物相容性强，因此二维材料铋烯有着广阔的应用前景，特别是在生物医学领域。
到目前为止，铋烯的制备方法主要是液相超声剥离法，及在有机溶剂中通过长时间的超声剥离获得。液相超声剥离法能制备出高晶体质量的铋烯纳米片，但是现有制备铋烯纳米片的方法中，超声时间过长，并且制备出的纳米片厚度较厚。
发明内容
鉴于现有技术中存在的问题，本发明目的在于克服现有技术的不足，提出一种基于加热-冷冻-研磨-超声制备超薄铋烯纳米片及其制备方法。
本发明的技术方案是利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法，采用加热-冷冻-研磨-超声制备，具体步骤如下：
(1)取铋粉加入研钵，150-180℃加热；
(2)冷冻研钵中铋粉,研磨；
(3)重复步骤(1)和(2)；
(4)称取步骤(3)处理后的铋粉，加入乙醇，配制成混悬液；
(5)探针间歇超声；
(6)水浴超声；
(7)离心，收集上清液，即为铋烯纳米片分散液。
进一步，研钵中加入液氮作为冷冻剂。
进一步，加热-冷冻-研磨重复次数为5-10次。
进一步，混悬液的浓度为10mg/mL。
进一步，探针超声30min，每超声3s，间歇3s，功率为300W。
进一步，水浴超声300min，功率400-600W。
进一步，其特征在于，离心转速5000rpm，时间10min。
进一步，其特征在于，重复次数的增多，铋烯纳米片横向尺寸变小，厚度变薄
本发明的第二个技术方案是采用前述制备方法制得的铋烯纳米片，所述纳米片的横向尺寸在50nm以下，所述纳米片的厚度在2nm以下。
有益效果：
本发明制备铋烯纳米片的方法采用的是“自上而下”的策略，能制备出超薄纳米片，且操作简单。
附图说明
图1为实施例1(A)和实施例2(B)所制备的铋烯纳米片的的透射电子显微镜图片。
图2为实施例1(A)和实施例2(B)所制备的铋烯纳米片的原子原子力显微镜图片。
具体实施方式
为了使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明作进一步的详细描述。
实施例1
取5g铋粉加入研钵，在150-180℃温箱加热5min，然后在研钵中加入液氮研磨5min，重复加热-冷冻-研磨步骤5次。称取以上步骤处理后的铋粉1g，加入100mL乙醇，配制成浓度为10mg/mL的混悬液。探针超声30min，每超声3s，间歇3s,功率为300W。然后水浴超声300min，功率400W，最后室温5000rpm离心10min，收集上清液，即为铋烯纳米片分散液。
由图1A的透射电子显微镜图片可知，实施例1制得的铋烯纳米片横向尺寸为49.80±7.84nm，由图2A的原子力显微镜图像可知所制备的铋烯纳米片厚度约为1.91±0.30nm。
实施例2
取5g铋粉加入研钵，在150-180℃温箱加热5min，然后在研钵中加入液氮研磨5min，重复加热-冷冻-研磨步骤10次。称取以上步骤处理后的铋粉1g，加入100mL乙醇，配制成浓度为10mg/mL的混悬液。探针超声30min，每超声3s，间歇3s,功率为300W。然后水浴超声300min，功率400W，最后室温5000rpm离心10min，收集上清液，即为铋烯纳米片分散液。
由图1B的透射电子显微镜图片可知，实施例1制得的铋烯纳米片横向尺寸为26.80±5.39nm，由图2B的原子力显微镜图像可知所制备的铋烯纳米片厚度为1.52±0.29nm。
实施例1与实施例2的不同之处在于加热-冷冻-研磨重复的次数不同，从表征来看，随着重复次数的增多，铋烯纳米片横向尺寸变小，厚度变薄。本发明适用于制备超薄铋烯纳米片。

Claims (9)

1.利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法，其特征在于，采用加热-冷冻-研磨-超声制备，具体步骤如下：
(1)取铋粉加入研钵，150-180℃加热；
(2)冷冻研钵中铋粉,研磨；
(3)重复步骤(1)和(2)；
(4)称取步骤(3)处理后的铋粉，加入乙醇，配制成混悬液；
(5)探针间歇超声；
(6)水浴超声；
(7)离心，收集上清液，即为铋烯纳米片分散液。
2.根据权利要求1所述的方法，其特征在于，研钵中加入液氮作为冷冻剂。
3.根据权利要求1所述的方法，其特征在于，加热-冷冻-研磨重复次数为5-10次。
4.根据权利要求1所述的方法，其特征在于，混悬液的浓度为10mg/mL。
5.根据权利要求1所述的方法，其特征在于，探针超声30min，每超声3s，间歇3s，功率为300W。
6.根据权利要求1所述的方法，其特征在于，水浴超声300min，功率400-600W。
7.根据权利要求1所述的方法，其特征在于，离心转速5000rpm，时间10min。
8.根据权利要求1所述的方法，其特征在于，重复次数的增多，铋烯纳米片横向尺寸变小，厚度变薄。
9.根据权利要求1-8中任一项所述的方法制得的铋烯纳米片，其特征在于，所述纳米片的横向尺寸在50nm以下，所述纳米片的厚度在2nm以下。
CN202110025521.2A 2021-01-08 2021-01-08 利用加热-冷冻-研磨-超声制备超薄铋烯纳米片的方法 Active CN112846199B (zh)

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