CN105140332B - 一种石墨烯‑ZnxAg（1‑x）NyO（1‑y）紫外探测器及其制备方法 - Google Patents
一种石墨烯‑ZnxAg（1‑x）NyO（1‑y）紫外探测器及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯‑ZnxAg(1‑x)NyO(1‑y)紫外探测器及其制备方法，该紫外探测器为光电导型紫外探测器，光电导型紫外探测器包括设置在基底上的光敏层和电极，其特征在于，所述的光敏层中含有石墨烯和ZnxAg(1‑x)NyO(1‑y)，按摩尔比计，x＝0.40～0.99，y＝0.01～0.60；制备方法包括石墨烯粉末与乙酸锌、硝酸银和乙酸铵混合溶液制成复合物胶体，随后将胶体旋涂、热处理、紫外臭氧联合处理和共溅射得到石墨烯‑ZnxAg1‑xNyO1‑y紫外探测器。测试结果表明该石墨烯‑ZnxAg1‑xNyO1‑y探测器对波长小于360nm的紫外光辐射具有良好的响应度和响应速度，是一种综合性能优秀的紫外探测器。
Description
技术领域
本发明涉及光电材料与器件领域，具体涉及一种石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器及其制备方法。
背景技术
紫外探测器在很多应用场合均有很高的应用价值。军用方面可用于宇航探测、战斗机尾焰跟踪、导弹尾焰跟踪等；民用方面可用于高压电晕检测、紫外指纹检测、火焰探测等。制造紫外探测器的一类主流材料是半导体材料，半导体紫外探测器体积小、性能稳定、使用方便。半导体紫外探测器可分为光电导效应探测器和光伏效应探测器两大类，其中光电导型紫外探测器具有较好的响应电流，GaN、SiC、ZnO、AlxGa1-xN等化合物半导体紫外探测器已经广泛应用于生产和生活中。
发明内容
本发明的目的在于，提供一种制备石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的制备方法，所需设备简单成本低廉，且具有优秀的紫外光响应性能，可以作为军用和民用紫外探测器件，有非常大的应用前景。
为了实现上述任务，本发明采取如下的技术解决方案：
一种石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器，该紫外探测器为光电导型紫外探测器，光电导型紫外探测器包括设置在基底上的光敏层和电极，所述的光敏层中含有石墨烯和ZnxAg(1-x)NyO(1-y)，按摩尔比计，x＝0.40～0.99，y＝0.01～0.60。
具体的，按摩尔比计，石墨烯中碳原子与ZnxAg(1-x)NyO(1-y)中锌原子加银原子之和的比为(1～10):(10～1)。
更具体的，所述光敏层的基底为玻璃，所述的电极为Au/Ti电极。
制备所述的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法，包括将石墨烯与含锌化合物、含银化合物和含氮化合物的混合溶液通过溶胶凝胶法制备成胶体，胶体经旋涂处理、热处理、紫外臭氧联合处理和共溅射处理后即得石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器。
具体的，所述的含锌化合物为乙酸锌，含银化合物为硝酸银，含氮化合物为乙酸铵；
混合溶液中乙酸锌的浓度为0.01mol/L、硝酸银的浓度为0.001～0.01mol/L和乙酸铵的浓度为0.01～0.1mol/L；
胶体中含有石墨烯的碳原子的浓度为0.001～0.1mol/L。
更具体的，所述的旋涂处理包括将胶体旋涂在玻璃上；
所述的热处理包括将旋涂胶体的玻璃在氩气氛围下进行400℃热处理；
所述的紫外臭氧联合处理为将热处理后的旋涂胶体的玻璃置于臭氧氛围中254nm紫外辐射处理；
所述的共溅射处理包括将紫外联合臭氧处理后的带有胶体的玻璃利用Au靶和Ti钯在氩气氛围及气压20Pa的条件下共溅射做成Au/Ti电极。
另外，所述的石墨烯的制备方法包括配制50g/L石墨粉末和20g/L高锰酸钾的浓硫酸混合溶液，将混合溶液依次在10℃、30℃和90℃下各搅拌1小时后加入等体积的质量浓度为30％的双氧水，静置后将沉淀物烘干并在1000℃和氩气下热处理得到石墨烯粉末。
本发明的有益效果为：
(1)本发明制备的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器和无石墨烯的基于单一ZnxAg(1-x)NyO(1-y)材料的紫外探测器相比，对波长小于360nm的紫外光辐射具有更好的响应度和响应速度；
(2)本发明制备的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器和石墨烯-ZnxAg1-xO、石墨烯-ZnNyO1-y、石墨烯-ZnO等基于石墨烯和三元、二元化合物 半导体结合得到的紫外探测器相比，对波长小于360nm的紫外光辐射具有更好的响应度。
附图说明
图1是实施例一制备的石墨烯材料的Raman光谱图；
图2是实施例一制备的石墨烯-ZnxAg(1-x)NyO(1-y)探测器的响应光谱曲线；
以下结合说明书附图和具体实施方式对本发明做具体说明。
具体实施方式
本发明制备的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器为光电导型紫外探测器，光电导型紫外探测器包括设置在基底上的光敏层和电极。该探测器的光敏层中含有石墨烯和ZnxAg(1-x)NyO(1-y)材料，以摩尔比计，石墨烯中碳原子与ZnxAg(1-x)NyO(1-y)材料中锌原子与银原子之和的比例为1:10～10:1，其中ZnxAg(1-x)NyO(1-y)化合物下标摩尔比例为x＝0.40～0.99，y＝0.01～0.60；玻璃为光敏层的基底，Au/Ti作为本发明紫外探测器的电极。
ZnxAg(1-x)NyO(1-y)是一种四元化合物半导体材料，测试表明其对波长小于360nm的紫外光辐射具有较好的响应度。石墨烯可以看作被剥离的单原子层石墨，其电子迁移率高达105cm2/Vs量级，其透光率超过97％，已被学术界公认为一种革命性的新材料。
发明人的测试表明将ZnxAg(1-x)NyO(1-y)和石墨烯相结合，可以实现更好的紫外探测性能。本发明给出了一套完整的制备石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法：先独立制备出石墨烯粉末，再将石墨烯粉末加入乙酸锌、硝酸银和乙酸铵混合溶液并搅拌形成石墨烯-ZnxAg(1-x)NyO(1-y)复合物胶体，以该胶体为基础通过后续的旋涂、热处理、紫外臭氧联合处理和共溅射四个步骤制备出石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器。
实施例1：
步骤1：利用氧化还原法制备石墨烯粉末，步骤如下：在98％浓硫酸中加入50g/L石墨粉末，20g/L高锰酸钾，依次在10/30/90摄氏度下各搅拌1小时后加入等体积的30％双氧水，静置5天后取出沉淀物，再超声处理2小时离心过滤后烘干得到固体物，在1000摄氏度氩气下热处理1小时得到石墨烯粉末；
步骤2：利用溶胶凝胶法制备石墨烯-ZnxAg(1-x)NyO(1-y)复合物胶体：配置含有0.01mol/L乙酸锌、0.001mol/L硝酸银和0.01mol/L乙酸铵混合溶液，搅拌均匀后将步骤1中制成的石墨烯粉末加入其中，配置成碳原子浓度0.01mol/L的混合悬浊液，加热至90摄氏度后加入PVA至浓度0.5g/L，搅拌2小时再静置至常温搅拌1小时，形成石墨烯-ZnxAg(1-x)NyO(1-y)复合物胶体；
步骤3：将胶体旋涂在玻璃上烘干并重复5次，得到石墨烯-ZnxAg(1-x)NyO(1-y)复合物薄膜，在氩气氛围下400摄氏度热处理1小时后取出薄膜，置于臭氧氛围中用254nm紫外辐射处理30分钟；
步骤4：将石墨烯-ZnxAg(1-x)NyO(1-y)薄膜和玻璃一起放入溅射系统，利用Au靶和Ti钯在氩气氛围下共溅射，气压20Pa，做成顶部的Au/Ti电极，从而完成石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的制备。
图1是本发明方法制备的石墨烯材料的Raman光谱图，图中可以看出石墨烯的典型G/D/2D特征峰。图2是石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器光谱响应曲线，可以看出其对波长低于360nm的紫外光辐射有很强的响应，但对波长大于400nm的可见光几乎没有响应，说明其具有优秀的光谱选择针对性的紫外探测功能。表1给出了本实施例的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器在360nm处的响应度和对360nm紫外辐射95％峰值响应时间的具体数值，从表1中可以看出和其它实施例相比，本实施例的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器具有最高的响应度和最低的响应时间，说明了 其优秀的紫外响应性能。
实施例2：
制备方法与测试同实施例1，但是步骤2中所配制溶液浓度变化为0.01mol/L乙酸锌、0.01mol/L硝酸银、0.01mol/L乙酸铵混合溶液。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例3：
制备方法与测试同实施例1，但是步骤2中所配制溶液浓度变化为0.01mol/L乙酸锌、0.001mol/L硝酸银、0.1mol/L乙酸铵混合溶液。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例4：
制备方法与测试同实施例1，但是步骤2中将石墨烯粉末加入ZnxAg1-xNyO1-y溶液，配置成碳原子浓度为0.001mol/L的混合悬浊液。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例5：
制备方法与测试同实施例1，但是步骤2中将石墨烯粉末加入ZnxAg1-xNyO1-y溶液，配置成碳原子浓度为0.1mol/L的混合悬浊液。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例6：
制备方法与测试同实施例1，但是省略了步骤1，且步骤2中不加入石墨烯粉末，最终制成的是无石墨烯的ZnxAg1-xNyO1-y探测器。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例 的紫外探测器的响应性能较实施例1差。
实施例7：
制备方法与测试同实施例1，但是步骤2中的溶液组分中不含硝酸银，最终制成的是石墨烯-ZnNyO1-y紫外探测器。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例8：
制备方法与测试同实施例1，但是步骤2中的溶液组分中不含乙酸铵，最终制成的是石墨烯-ZnxAg1-xO紫外探测器。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
实施例9：
制备方法与测试同实施例1，但是步骤2中的溶液组分中不含硝酸银和乙酸铵，最终制成的是石墨烯-ZnO紫外探测器。表1给出了本实时例制备的紫外探测器响应度和响应时间的数值，从表1可以看出本实施例的紫外探测器的响应性能较实施例1差。
表1
| 实施例 | 响应度(A/W) | 上升响应时间(s) | 下降响应时间(s) |
| 1 | 1.33 | 19.2 | 11.5 |
| 2 | 0.75 | 22.8 | 14.1 |
| 3 | 0.88 | 21.3 | 13.6 |
| 4 | 1.16 | 34.9 | 19.8 |
| 5 | 0.82 | 19.9 | 12.8 |
| 6 | 0.69 | 64.7 | 61.2 |
| 7 | 0.82 | 46.6 | 42.9 |
| 8 | 0.75 | 51.0 | 44.6 |
| 9 | 0.66 | 55.9 | 50.3 |
Claims (7)
1.一种石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器，该紫外探测器为光电导型紫外探测器，光电导型紫外探测器包括设置在基底上的光敏层和电极，其特征在于，所述的光敏层中含有石墨烯和ZnxAg(1-x)NyO(1-y)，按摩尔比计，x＝0.40～0.99，y＝0.01～0.60。
2.如权利要求1所述的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器，其特征在于，按摩尔比计，石墨烯中碳原子与ZnxAg(1-x)NyO(1-y)中锌原子加银原子之和的比为(1～10):(10～1)。
3.如权利要求1或2所述的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器，其特征在于，所述光敏层的基底为玻璃，所述的电极为Au/Ti电极。
4.制备权利要求1、2或3所述的石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法，其特征在于，包括将石墨烯与含锌化合物、含银化合物和含氮化合物的混合溶液通过溶胶凝胶法制备成胶体，胶体旋涂于基底上后经热处理和紫外臭氧联合处理，再通过共溅射制备电极即得石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器；
所述的基底为玻璃。
5.如权利要求4所述的制备石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法，其特征在于，所述的含锌化合物为乙酸锌，含银化合物为硝酸银，含氮化合物为乙酸铵；
混合溶液中乙酸锌的浓度为0.01mol/L、硝酸银的浓度为0.001～0.01mol/L和乙酸铵的浓度为0.01～0.1mol/L；
胶体中含有石墨烯的碳原子的浓度为0.001～0.1mol/L。
6.如权利要求4所述的制备石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法，其特征在于，所述的热处理包括将旋涂胶体的玻璃在氩气氛围下进行400℃热处理；所述的紫外臭氧联合处理包括将热处理后的旋涂胶体的玻璃置于臭氧氛围中254nm紫外辐射处理；
所述的共溅射包括将紫外联合臭氧处理后的旋涂胶体的玻璃利用Au靶和Ti钯在氩气氛围及气压20Pa的条件下制备Au/Ti电极。
7.如权利要求4所述的制备石墨烯-ZnxAg(1-x)NyO(1-y)紫外探测器的方法，其特征在于，所述的石墨烯的制备方法包括配制50g/L石墨粉末和20g/L高锰酸钾的浓硫酸混合溶液，将混合溶液依次在10℃、30℃和90℃下各搅拌1小时后加入等体积的质量浓度为30％的双氧水，静置后将沉淀物烘干并在1000℃和氩气下热处理得到石墨烯粉末。
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