CN104628025A - Solvothermal Preparation of CeO2 Nanorod Thin Films Vertically Assembled on Silicon Surface - Google Patents
Solvothermal Preparation of CeO2 Nanorod Thin Films Vertically Assembled on Silicon Surface Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 239000002073 nanorod Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010409 thin film Substances 0.000 title claims abstract description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title abstract description 11
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000010408 film Substances 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000758 substrate Substances 0.000 abstract description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 abstract description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 11
- 238000001816 cooling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
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Abstract
本发明涉及一种硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，该方法是以洁净的硅片为基体，以CeCl 3和CO(NH2)2为原料、以乙醇为溶剂配制前躯体溶液、在160-200℃的溶剂热条件下反应，在硅片表面制备由CeO2纳米棒垂直组装而形成的薄膜。本发明方法设备简单，制膜成本低，不需要对硅基质和薄膜进行高温处理，制得的膜薄是由CeO2纳米棒垂直组装而成，均匀、可见光透明度高、附着性好、抗紫外线性能强，并在380-390nm有很强的发射峰，在晶硅太阳能电池抗紫外线性能方面有广泛应用。
The invention relates to a solvothermal preparation method for vertically assembling CeO2 nanorod films on a silicon surface. The method uses a clean silicon chip as a substrate, uses CeCl3 and CO( NH2 ) 2 as raw materials, and ethanol as a solvent before preparation. The body solution is reacted under 160-200°C solvothermal conditions, and a thin film formed by vertical assembly of CeO 2 nanorods is prepared on the surface of a silicon wafer. The method of the invention has simple equipment, low cost of film making, and does not need high-temperature treatment of the silicon substrate and film, and the prepared film is composed of CeO2 nanorods vertically assembled, uniform, high in visible light transparency, good in adhesion, and UV-resistant It has strong performance and has a strong emission peak at 380-390nm, and is widely used in the anti-ultraviolet performance of crystalline silicon solar cells.
Description
技术领域 technical field
本发明涉及一种在硅片基体上垂直组装CeO2纳米棒薄膜的溶剂热制备方法，属于新型结构纳米材料研究技术领域。 The invention relates to a solvothermal preparation method for vertically assembling a CeO2 nanorod thin film on a silicon chip substrate, and belongs to the technical field of research on new structure nanometer materials.
背景技术 Background technique
在高海拔地区，由于臭氧层稀薄、紫外线强，导致一般平均寿命为15年左右的太阳能电池，在高海拔地区的使用寿命降低到5年左右。在太阳能电池表面增加抗紫外薄膜提高太阳能电池使用寿命的有效途径，另一方面对于晶硅太阳能电池，有占太阳光总能量43%的紫外光和红外光不能被吸收利用，人们寻求既能转光，又能对紫外线有屏蔽作用的功能材料。纳米CeO2具有可见光透过率高，紫外线吸收能力强等优点倍受关注。 In high-altitude areas, due to the thin ozone layer and strong ultraviolet rays, the average lifespan of solar cells is about 15 years, but the service life in high-altitude areas is reduced to about 5 years. Adding an anti-ultraviolet film on the surface of solar cells is an effective way to improve the service life of solar cells. On the other hand, for crystalline silicon solar cells, ultraviolet light and infrared light, which account for 43% of the total solar energy, cannot be absorbed and utilized. It is a functional material that can shield ultraviolet rays. Nano-CeO 2 has the advantages of high visible light transmittance and strong ultraviolet absorption ability, which has attracted much attention.
邹云玲等（蛋清蛋白辅助水热法制备CeO2纳米棒及其发光性能[J].化学研究与应用，2010.22（3）：316-319.）以氯化铈和氢氧化钠为反应原料，以新鲜的蛋清为络合剂，在水热体系中制备出长度为200nm、直径约为几十纳米的CeO2纳米棒，并且在紫蓝色发光区具有较强的发光。Yong Chen等（Synthesis and characterization of CeO2 nano-rods[J].Ceramics International，2013.39（6）：6607-6610）以六水合硝酸铈和磷酸钠为原料采用水热法合成了直径为30nm长度为100nmCeO2纳米棒，以水合醋酸铈和磷酸氢钠为原料合成了直径为10nm长度为400nmCeO2纳米棒，与其它不规则的CeO2颗粒相比，这两种纳米棒有更好的紫外线吸收能力。 Zou Yunling et al. (Preparation of CeO 2 nanorods and their luminescent properties by egg white protein-assisted hydrothermal method [J]. Chemical Research and Application, 2010.22 (3): 316-319.) Using cerium chloride and sodium hydroxide as reaction raw materials, with Fresh egg white is a complexing agent, and CeO 2 nanorods with a length of 200nm and a diameter of about tens of nanometers are prepared in a hydrothermal system, and have strong luminescence in the purple-blue luminescent region. Yong Chen et al. (Synthesis and characterization of CeO 2 nano-rods[J]. Ceramics International, 2013.39 (6): 6607-6610) synthesized nano-rods with a diameter of 30nm and a length of 100nm CeO 2 nanorods, CeO 2 nanorods with a diameter of 10nm and a length of 400nm were synthesized from hydrated cerium acetate and sodium hydrogen phosphate. Compared with other irregular CeO 2 particles , these two nanorods have better UV absorption capacity .
周丽等（水热法制纳米 CeO2膜及紫外吸收性能研究[J].化学研究与应用，2012.24（2）：237-241.）以硝酸铈和尿素为原料，采用水热法在玻璃基质上以130℃ 加热7h的条件制备出了厚度达到100nm，晶型较好，膜表面平整度较高，且具有优异的可见光透过性和紫外吸收特性的纳米薄膜。 Zhou Li et al. (Study on nano-CeO 2 film prepared by hydrothermal method and its ultraviolet absorption properties[J]. Chemical Research and Application, 2012.24 (2): 237-241.) Using cerium nitrate and urea as raw materials, the hydrothermal method was used to form a glass substrate. The nano-thin film with a thickness of 100nm, a good crystal form, a high surface smoothness, and excellent visible light transmittance and ultraviolet absorption properties was prepared by heating at 130°C for 7 hours.
但硅片在水热体系下被严重侵蚀，故不能用水热法在硅片表面制备纳米CeO2薄膜。目前国内外尚未见采用溶剂热法在硅片表面垂直组装CeO2纳米棒薄膜的报道。 However, the silicon wafer is severely corroded under the hydrothermal system, so the nano- CeO2 film cannot be prepared on the surface of the silicon wafer by the hydrothermal method. At present, there is no report on the vertical assembly of CeO 2 nanorod films on the surface of silicon wafers by solvothermal method at home and abroad.
发明内容 Contents of the invention
发明目的： Purpose of the invention:
本发明提出了一种硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，其目的在于把对紫外线吸收能力强、发光性强的CeO2纳米棒组装在硅片上，以使得纳米棒晶型较好，膜表面平整。 The present invention proposes a solvothermal preparation method for vertically assembling CeO2 nanorod films on a silicon surface. The shape is better, and the surface of the film is smooth.
技术方案： Technical solutions:
本发明是通过以下技术方案实施的： The present invention is implemented through the following technical solutions:
一种硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，其特征在于：步骤如下： A kind of solvothermal preparation method of CeO2nanorod film vertically assembled on silicon surface, it is characterized in that: the steps are as follows:
（1）将原料CeCl3·7H2O溶于无水乙醇中，得到0.01-0.02mol/L CeCl3的无水乙醇溶液，加入0.02-0.04mol /L的CO(NH2)2，搅拌均匀，得到前躯体溶液； (1) Dissolve the raw material CeCl 3 7H 2 O in absolute ethanol to obtain a 0.01-0.02mol/L CeCl 3 absolute ethanol solution, add 0.02-0.04mol/L CO(NH 2 ) 2 and stir well , to obtain the precursor solution;
（2）将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液，密封，置于烘箱中，在160-200℃温度下反应2-6h；反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 (2) Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution, seal it, place it in an oven, and react at 160-200°C for 2-6h; after the reaction is complete, cool down naturally to After room temperature, take out the silicon chip, wash it with ethanol and water respectively, and dry it to obtain the product.
步骤（2）中前驱液的填充度为70-80%。 The filling degree of the precursor solution in step (2) is 70-80%.
步骤（1）中尿素与CeCl3的摩尔比为2:1。 The molar ratio of urea to CeCl3 in step (1) is 2:1.
优点和效果： Advantages and effects:
本发明提供一种硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，具有如下优点和有益效果： The present invention provides a kind of solvothermal preparation method of CeO nanorod film vertically assembled on silicon surface, has following advantage and beneficial effect:
该方法设备简单，制膜成本低廉，不需要对硅基质和薄膜进行高温处理，制得的膜薄是由CeO2纳米棒垂直组装而成，均匀、可见光透明度高、附着性好、抗紫外线性能强，并在380-390nm有很强的发射峰（见图4），在晶硅太阳能电池抗紫外线性能方面有广泛应用。 The method has simple equipment, low cost of film production, and does not require high-temperature treatment of the silicon substrate and film. The prepared film is composed of CeO2 nanorods vertically assembled, uniform, high transparency of visible light, good adhesion, and UV resistance. Strong, and has a strong emission peak at 380-390nm (see Figure 4), it is widely used in the anti-ultraviolet performance of crystalline silicon solar cells.
附图说明 Description of drawings
图1所得CeO2纳米棒薄膜的SEM照片。 Fig. 1 SEM photograph of the obtained CeO2 nanorod film.
图2所得CeO2纳米棒薄膜的XRD谱图。 Figure 2 XRD spectrum of the obtained CeO2 nanorod film.
图3所得CeO2纳米棒薄膜的紫外光谱图；图中a为样品片的曲线；b为空硅片的曲线。 The ultraviolet spectrogram of the obtained CeO nanorod thin film in Fig. 3; among the figure a is the curve of the sample sheet; b is the curve of the empty silicon sheet.
图4所得CeO2纳米棒薄膜的发射光谱图（激发波长310nm）。 Figure 4. The emission spectrum of the obtained CeO2 nanorod film (excitation wavelength 310nm).
具体实施方式 Detailed ways
本发明提供一种硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，设备简单，制膜成本低，不需要对硅基质和薄膜进行高温处理，把对紫外线吸收能力强、发光性强的CeO2纳米棒组装在硅片上，制得的膜薄是由CeO2（薄膜的XRD谱图如图2所示）纳米棒垂直组装而成（薄膜的SEM照片如图1所示），均匀、可见光透明度高、附着性好、抗紫外线性能强（紫外光谱图如图3所示），并在380-390nm有很强的发射峰（发射光谱图如图4所示），在晶硅太阳能电池抗紫外线性能方面有广泛应用。硅片表面垂直组装的CeO2纳米棒薄膜，直径为30-50nm，薄膜厚度可达170 nm左右，晶型较好，膜表面平整。 The invention provides a solvothermal preparation method for vertically assembling a CeO2 nanorod film on a silicon surface, which has simple equipment, low cost of film production, and does not require high-temperature treatment of the silicon substrate and film, and can be made of a material with strong ultraviolet absorption ability and strong luminescence CeO 2 nanorods are assembled on a silicon wafer, and the prepared film is composed of CeO 2 (XRD spectrum of the film is shown in Figure 2) nanorods are vertically assembled (SEM photo of the film is shown in Figure 1), uniform , High transparency of visible light, good adhesion, strong UV resistance (ultraviolet spectrum as shown in Figure 3), and a strong emission peak at 380-390nm (emission spectrum as shown in Figure 4), in crystalline silicon solar energy The anti-ultraviolet performance of the battery has a wide range of applications. The CeO 2 nanorod film vertically assembled on the surface of the silicon wafer has a diameter of 30-50nm, a film thickness of about 170 nm, a good crystal form, and a smooth film surface.
上述硅表面垂直组装CeO2纳米棒薄膜的溶剂热制备方法，步骤如下： Above-mentioned silicon surface vertical assembly CeO The solvothermal preparation method of nanorod film, the steps are as follows:
（1）将原料CeCl3·7H2O溶于无水乙醇中，得到0.01-0.02mol/L CeCl3的无水乙醇溶液，加入0.02-0.04mol /L的CO(NH2)2，搅拌均匀，得到前躯体溶液； (1) Dissolve the raw material CeCl 3 7H 2 O in absolute ethanol to obtain a 0.01-0.02mol/L CeCl 3 absolute ethanol solution, add 0.02-0.04mol/L CO(NH 2 ) 2 and stir well , to obtain the precursor solution;
（2）将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液，密封，置于烘箱中，在160-200℃温度下反应2-6h；反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 (2) Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution, seal it, place it in an oven, and react at 160-200°C for 2-6h; after the reaction is complete, cool down naturally to After room temperature, take out the silicon chip, wash it with ethanol and water respectively, and dry it to obtain the product.
步骤（2）中前驱液的填充度为70-80%。 The filling degree of the precursor solution in step (2) is 70-80%.
步骤（1）中尿素（CO(NH2)2）与CeCl3的摩尔比为2:1。 The molar ratio of urea (CO(NH 2 ) 2 ) to CeCl 3 in step (1) is 2:1.
下面结合具体实施例对本发明进行具体说明： The present invention is specifically described below in conjunction with specific embodiment:
实施例1Example 1
将原料CeCl3·7H2O溶于无水乙醇中，得到0.01mol/L CeCl3的无水乙醇溶液，加入0.02mol /L CO(NH2)2，尿素与CeCl3的摩尔比为2:1，搅拌均匀，得到前躯体溶液。将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液（填充度为70%），密封，置于烘箱中，在200℃温度下反应3h。反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 Dissolve the raw material CeCl 3 7H 2 O in absolute ethanol to obtain a 0.01mol/L CeCl 3 absolute ethanol solution, add 0.02mol/L CO(NH 2 ) 2 , and the molar ratio of urea to CeCl 3 is 2: 1. Stir evenly to obtain the precursor solution. Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution (filling degree is 70%), seal it, place it in an oven, and react at 200°C for 3 hours. After the reaction is finished, the silicon chip is taken out after naturally cooling down to room temperature, washed with ethanol and water respectively, and dried to obtain the product.
实施例2Example 2
将原料CeCl3·7H2O溶于无水乙醇中，得到0.015mol/LCeCl3的无水乙醇溶液，加入0.03mol /L CO(NH2)2，尿素与CeCl3的摩尔比为2:1，搅拌均匀，得到前躯体溶液。将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液（填充度为70%），密封，置于烘箱中，在180℃温度下反应4h。反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 Dissolve the raw material CeCl 3 7H 2 O in absolute ethanol to obtain a 0.015mol/LCeCl 3 absolute ethanol solution, add 0.03mol/L CO(NH 2 ) 2 , and the molar ratio of urea to CeCl 3 is 2:1 , and stir evenly to obtain a precursor solution. Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution (filling degree is 70%), seal it, place it in an oven, and react at 180°C for 4 hours. After the reaction is finished, the silicon chip is taken out after naturally cooling down to room temperature, washed with ethanol and water respectively, and dried to obtain the product.
实施例3Example 3
将原料CeCl3·7H2O溶于一定体积的无水乙醇中，得到0.02mol/L CeCl3的无水乙醇溶液，加入0.04mol /L CO(NH2)2，尿素与CeCl3的摩尔比为2:1，搅拌均匀，得到前躯体溶液。将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液（填充度为80%），密封，置于烘箱中，在160℃温度下反应6h。反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 Dissolve the raw material CeCl 3 7H 2 O in a certain volume of dehydrated ethanol to obtain a 0.02mol/L CeCl 3 dehydrated ethanol solution, add 0.04mol/L CO(NH 2 ) 2 , the molar ratio of urea to CeCl 3 2:1, stir evenly to obtain precursor solution. Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution (filling degree is 80%), seal it, place it in an oven, and react at 160°C for 6h. After the reaction is finished, the silicon chip is taken out after naturally cooling down to room temperature, washed with ethanol and water respectively, and dried to obtain the product.
实施例4Example 4
将原料CeCl3·7H2O溶于无水乙醇中，得到0.02mol/L CeCl3的无水乙醇溶液，加入0.04mol /L CO(NH2)2，尿素与CeCl3的摩尔比为2:1，搅拌均匀，得到前躯体溶液。将洁净的硅片放入内衬为聚四氟乙烯反应釜中，加入前驱液（填充度为75%），密封，置于烘箱中，在200℃温度下反应2h。反应结束，自然降温至室温后取出硅片，分别用乙醇、水洗涤干净，干燥即得产品。 Dissolve the raw material CeCl 3 7H 2 O in absolute ethanol to obtain a 0.02mol/L CeCl 3 absolute ethanol solution, add 0.04mol/L CO(NH 2 ) 2 , and the molar ratio of urea to CeCl 3 is 2: 1. Stir evenly to obtain the precursor solution. Put the clean silicon wafer into a polytetrafluoroethylene-lined reactor, add the precursor solution (filling degree is 75%), seal it, place it in an oven, and react at 200°C for 2 hours. After the reaction is finished, the silicon chip is taken out after naturally cooling down to room temperature, washed with ethanol and water respectively, and dried to obtain the product.
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| CN105000586A (en) * | 2015-08-03 | 2015-10-28 | 攀钢集团攀枝花钢铁研究院有限公司 | One-step synthesizing method of high-dispersion and weak-agglomeration doped ceria |
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