CN102593239B - Preparation method of latticed textured azo compound (AZO) transparent conductive membrane - Google Patents
Preparation method of latticed textured azo compound (AZO) transparent conductive membrane Download PDFInfo
- Publication number
- CN102593239B CN102593239B CN201110305886.7A CN201110305886A CN102593239B CN 102593239 B CN102593239 B CN 102593239B CN 201110305886 A CN201110305886 A CN 201110305886A CN 102593239 B CN102593239 B CN 102593239B
- Authority
- CN
- China
- Prior art keywords
- film
- azo
- transparent conductive
- preparation
- network
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title claims description 15
- -1 azo compound Chemical class 0.000 title 1
- 239000012528 membrane Substances 0.000 title 1
- 239000010408 film Substances 0.000 claims abstract description 65
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000010409 thin film Substances 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 10
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 238000003980 solgel method Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000000411 transmission spectrum Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Surface Treatment Of Glass (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Photovoltaic Devices (AREA)
- Chemically Coating (AREA)
Abstract
本发明提供了一种具有网络状绒面的AZO透明导电膜的制备方法，其特征是：采用溶胶–凝胶法制备AZO薄膜；选择一定的Al掺杂浓度，采用适当的热处理工艺获得具有网络状绒面的AZO透明导电膜。本发明具有能耗小、设备简单、重复性好、易于工业化生产的优点。由本方法制备的网络状绒面AZO透明导电膜可应用于气敏传感器、吸波、光催化、薄膜太阳能电池等领域。
The invention provides a method for preparing an AZO transparent conductive film with a network texture, which is characterized in that: a sol-gel method is used to prepare an AZO film; a certain Al doping concentration is selected, and an appropriate heat treatment process is adopted to obtain a film with a network Suede-like AZO transparent conductive film. The invention has the advantages of low energy consumption, simple equipment, good repeatability and easy industrial production. The network-like suede AZO transparent conductive film prepared by the method can be applied to the fields of gas sensor, wave absorption, photocatalysis, thin film solar cell and the like.
Description
技术领域 technical field
本发明涉及AZO透明导电膜的制备方法，特别涉及一种具有网络状绒面的AZO透明导电膜的制备方法。 The invention relates to a preparation method of an AZO transparent conductive film, in particular to a preparation method of an AZO transparent conductive film with a network suede surface.
背景技术 Background technique
透明导电氧化物(TCO)薄膜作为一种同时具备高可见光透过率和低电阻的光电信息材料，广泛用于薄膜太阳能电池、平板显示器、传感器以及各种光电器件，Al掺杂ZnO透明导电薄膜(ZnO: Al，简称AZO)，是近几年研究较多的TCO之一，AZO与传统的TCO膜如ITO (In2O3: Sn)、FTO (SnO2: F)具有可比拟的光电性能，且具有易得、环境友好、在氢等离子体中性能稳定等优点。 Transparent conductive oxide (TCO) film, as a photoelectric information material with high visible light transmittance and low resistance, is widely used in thin-film solar cells, flat panel displays, sensors and various optoelectronic devices. Al-doped ZnO transparent conductive film (ZnO: Al, referred to as AZO), is one of the TCOs that have been studied more in recent years. AZO and traditional TCO films such as ITO (In 2 O 3 : Sn) and FTO (SnO 2 : F) have comparable photoelectric properties. performance, and has the advantages of easy availability, environmental friendliness, and stable performance in hydrogen plasma.
AZO薄膜在用于薄膜太阳能电池时，在要求其具有高可见光透过率和低电阻的同时，还要求薄膜表面具有一定的粗糙度(绒度)，以达到减反增透的目的，目前绒面AZO薄膜主要利用溅射后腐蚀和金属有机物化学气相沉积(MOCVD)制备获得，相比气相沉积，湿化学法是一类工艺简单、成本低廉的薄膜制备方法，适用于大面积衬底上的均匀沉积，其中，溶胶－凝胶法可在分子级水平控制掺杂，是制备掺杂ZnO透明导电薄膜较为理想的方法，然而通常采用溶胶–凝胶法制备的AZO膜呈平整、光滑的表面，不能获得绒面结构，文献及专利检索表明，目前尚无有关利用溶胶–凝胶法制备绒面AZO膜的报道。 When AZO film is used in thin-film solar cells, it is required to have high visible light transmittance and low resistance, and at the same time, it is also required to have a certain roughness (velvet) on the surface of the film to achieve the purpose of reducing reflection and anti-reflection. Surface AZO thin films are mainly prepared by post-sputtering corrosion and metal-organic chemical vapor deposition (MOCVD). Compared with vapor deposition, wet chemical method is a kind of thin film preparation method with simple process and low cost, which is suitable for large-area substrates. Uniform deposition, among which, the sol-gel method can control the doping at the molecular level, which is an ideal method for preparing doped ZnO transparent conductive films, but the AZO film usually prepared by the sol-gel method has a flat and smooth surface , the textured structure cannot be obtained. Literature and patent searches show that there is no report on the preparation of textured AZO films by the sol-gel method.
发明内容 Contents of the invention
本发明的目的在于提供一种网络状绒面AZO透明导电膜的制备方法，该方法能耗小、设备简单、重复性好、易于工业化生产。 The object of the present invention is to provide a method for preparing a network-like suede AZO transparent conductive film, which has low energy consumption, simple equipment, good repeatability and is easy for industrial production.
为达到上述目的，本发明的技术方案中，采用溶胶–凝胶法制备网络状绒面AZO透明导电膜。 In order to achieve the above object, in the technical solution of the present invention, a sol-gel method is used to prepare a network-shaped suede AZO transparent conductive film.
上述的一种网络状绒面AZO透明导电膜的制备方法，具体步骤为： The preparation method of above-mentioned a kind of network shape suede AZO transparent conductive film, concrete steps are:
1、ZnO:Al胶体溶液的配制 1. Preparation of ZnO:Al colloidal solution
将一定量分析纯醋酸锌和硝酸铝在搅拌下加入无水乙醇/乙二醇甲醚，并加入适量二乙醇胺/单乙醇胺。继续搅拌1~2小时，得到透明稳定的胶体溶液。 Add a certain amount of analytically pure zinc acetate and aluminum nitrate to absolute ethanol/ethylene glycol methyl ether under stirring, and add an appropriate amount of diethanolamine/monoethanolamine. Continue stirring for 1-2 hours to obtain a transparent and stable colloidal solution.
2、衬底清洗 2. Substrate cleaning
将玻璃衬底置于去离子水、丙酮、无水乙醇中依次进行超声清洗，然后用去离子水冲洗，最后将衬底置于烘箱中晾干。 Place the glass substrate in deionized water, acetone, and absolute ethanol for ultrasonic cleaning in sequence, then rinse with deionized water, and finally place the substrate in an oven to dry.
3、薄膜制备 3. Film preparation
将预先清洗好的玻璃衬底（石英、蓝宝石等）浸渍到上述透明胶体溶液中，然后以恒定速度缓慢上升，从而在衬底上涂覆一层均匀的胶体膜，将胶体膜在400°C进行预处理以除去膜中的有机溶剂，重复上述步骤若干次，获得不同厚度的AZO薄膜。 Immerse the pre-cleaned glass substrate (quartz, sapphire, etc.) Pretreatment is carried out to remove the organic solvent in the film, and the above steps are repeated several times to obtain AZO films with different thicknesses.
4、薄膜的热处理 4. Heat treatment of thin film
将获得的AZO薄膜置于箱式炉中在空气中热处理1 h，然后将样品置于管式炉中，在还原气氛下热处理1 h，然后缓慢冷却至室温。 The obtained AZO film was heat-treated in a box furnace in air for 1 h, then the sample was placed in a tube furnace, heat-treated in a reducing atmosphere for 1 h, and then slowly cooled to room temperature.
上述制备方法中，步骤1中Zn2+摩尔浓度为0.5 mol/L；Al/Zn原子浓度比为4%~6%：1；Zn2+与二乙醇胺/单乙醇胺的摩尔比为1：1。 In the above preparation method, the molar concentration of Zn 2+ in step 1 is 0.5 mol/L; the atomic concentration ratio of Al/Zn is 4%~6%:1; the molar ratio of Zn 2+ to diethanolamine/monoethanolamine is 1:1 .
上述制备方法中，步骤3中所述的恒定速度为6cm/min，胶体膜在400°C的预处理时间为10~20分钟；重复次数为10~16次；薄膜厚度为300~600 nm。 In the above preparation method, the constant speed described in step 3 is 6cm/min, the pretreatment time of the colloidal film at 400°C is 10-20 minutes; the number of repetitions is 10-16 times; the film thickness is 300-600 nm.
上述制备方法中，步骤4中在空气中和还原气氛下的热处理温度均为400°C，所用还原气体为Ar/H2、N2/H2或H2，Ar、N2气流速为1~8 L/min，H2气流速为0.2~2 L/min。 In the above preparation method, the heat treatment temperature in step 4 in the air and under the reducing atmosphere is 400 ° C, the reducing gas used is Ar/H 2 , N 2 /H 2 or H 2 , and the flow rate of Ar and N 2 is 1 ~8 L/min, H 2 flow rate is 0.2~2 L/min.
本发明的优点在于通过选择合适的Al掺杂浓度以及热处理气氛和温度，利用溶胶－凝胶法制备出具有网络状绒面的AZO透明导电膜，该网络状绒面AZO透明导电膜可用于气敏传感器、吸波、光催化、薄膜太阳能电池等领域。 The advantage of the present invention is that by selecting the appropriate Al doping concentration and heat treatment atmosphere and temperature, the AZO transparent conductive film with a network texture is prepared by using the sol-gel method, and the network texture AZO transparent conductive film can be used for gas Sensitive sensors, microwave absorption, photocatalysis, thin film solar cells and other fields.
附图说明 Description of drawings
图1为实施例1制备的网络状绒面AZO透明导电膜的AFM图； Fig. 1 is the AFM figure of the network-shaped suede AZO transparent conductive film prepared by embodiment 1;
图2为实施例1制备的网络状绒面AZO透明导电膜的AFM图； Fig. 2 is the AFM figure of the network-shaped suede AZO transparent conductive film prepared in embodiment 1;
图3为实施例1制备的网络状绒面AZO透明导电膜的透过率谱； Fig. 3 is the transmittance spectrum of the network-shaped suede AZO transparent conductive film prepared in embodiment 1;
图4为实施例2制备的网络状绒面AZO透明导电膜的AFM图； Fig. 4 is the AFM figure of the network-shaped suede AZO transparent conductive film prepared in embodiment 2;
图5为实施例2制备的网络状绒面AZO透明导电膜的AFM图； Fig. 5 is the AFM figure of the network-shaped suede AZO transparent conductive film prepared in embodiment 2;
图6为实施例2制备的网络状绒面AZO透明导电膜的透过率谱。 FIG. 6 is the transmittance spectrum of the network-shaped suede AZO transparent conductive film prepared in Example 2.
具体实施方式 Detailed ways
下面的实施例是对本发明的进一步说明，而不是限制本发明的范围。 The following examples are to further illustrate the present invention, but not to limit the scope of the present invention.
实施例1： Example 1:
称取Zn(Ac)2·2H2O（分析纯）10.9745g，Al(NO3)3·2H2O（分析纯）0.9380g；将上述药品在搅拌的条件下先后添加到100mL无水乙醇中；量取4.8mL二乙醇胺，在搅拌的条件下添加到上述溶液中，溶液逐渐由浑浊变为无色透明；继续搅拌2小时，得到透明稳定的溶胶；将清洗干净的玻璃衬底浸渍到上述前躯体溶胶中，然后以6cm/min的恒定速度将玻璃衬底缓慢提出液面，从而在玻璃上涂覆一层均匀的溶胶膜，将溶胶膜在400°C进行预处理20分钟，然后重复前面的浸渍、提拉、预处理步骤共16次；将获得的AZO薄膜置于箱式炉中在空气中400°C热处理1 h，然后将样品置于管式炉中，在流速为3：0.3 L/min的Ar/H2气氛下热处理1 h，然后缓慢冷却至室温。 Weigh 10.9745g of Zn(Ac) 2 2H 2 O (analytical grade), 0.9380g of Al(NO 3 ) 3 2H 2 O (analytical grade); medium; measure 4.8mL diethanolamine and add it to the above solution under stirring, the solution gradually changes from turbid to colorless and transparent; continue stirring for 2 hours to obtain a transparent and stable sol; dip the cleaned glass substrate into In the above-mentioned precursor sol, then the glass substrate is slowly lifted out of the liquid surface at a constant speed of 6 cm/min, thereby coating a uniform sol film on the glass, and the sol film is pretreated at 400 ° C for 20 minutes, and then Repeat the previous impregnation, pulling, and pretreatment steps for a total of 16 times; place the obtained AZO film in a box furnace for heat treatment at 400°C in air for 1 h, and then place the sample in a tube furnace at a flow rate of 3 : Heat treatment in 0.3 L/min Ar/H 2 atmosphere for 1 h, then slowly cooled to room temperature.
所得AZO膜的方块电阻为149 Ω/□；图1，图2为AZO膜的AFM图，由图可见薄膜具有规则的网络状绒面，其沟道宽约400 nm，由“沟”底到“坝”顶的高度平均约20 nm，图3为AZO膜的透过率谱，显示薄膜在可见光区的透过率在85%左右。 The sheet resistance of the obtained AZO film is 149 Ω/□; Figure 1 and Figure 2 are the AFM images of the AZO film. It can be seen from the figure that the film has a regular network-like suede surface, and the channel width is about 400 nm. The average height of the top of the "dam" is about 20 nm. Figure 3 shows the transmittance spectrum of the AZO film, which shows that the transmittance of the film in the visible light region is about 85%.
实施例2： Example 2:
称取Zn(Ac)2·2H2O（分析纯）10.9745g，Al(NO3)3·9H2O（分析纯）0.9380g；将上述药品在搅拌的条件下先后添加到100mL乙二醇甲醚中；量取3mL单乙醇胺，在搅拌的条件下添加到上述溶液中，溶液逐渐由浑浊变为无色透明；继续搅拌2小时，得到透明稳定的溶胶；将清洗干净的玻璃衬底浸渍到上述前躯体溶胶中，然后以6cm/min的恒定速度将玻璃衬底缓慢提出液面，从而在玻璃上涂覆一层均匀的溶胶膜，将溶胶膜在400°C进行预处理20分钟，然后重复前面的浸渍、提拉、预处理步骤共16次；将获得的AZO薄膜置于箱式炉中在空气中400°C热处理1 h，然后将样品置于管式炉中，在流速为0.3 L/min的H2气氛下于400°C热处理1 h，然后缓慢冷却至室温。 Weigh 10.9745g of Zn(Ac) 2 2H 2 O (analytically pure), 0.9380g of Al(NO 3 ) 3 9H 2 O (analytical pure); add the above drugs to 100mL ethylene glycol under stirring in methyl ether; measure 3mL of monoethanolamine and add it to the above solution under stirring, the solution gradually changes from turbid to colorless and transparent; continue stirring for 2 hours to obtain a transparent and stable sol; dip the cleaned glass substrate into the above-mentioned precursor sol, then slowly lift the glass substrate out of the liquid surface at a constant speed of 6cm/min, thereby coating a uniform sol film on the glass, and pretreating the sol film at 400°C for 20 minutes, Then repeat the previous impregnation, pulling, and pretreatment steps a total of 16 times; the obtained AZO film was placed in a box furnace and heat-treated at 400°C in the air for 1 h, and then the sample was placed in a tube furnace at a flow rate of Heat treatment at 400°C for 1 h under 0.3 L/min H2 atmosphere, and then slowly cool to room temperature.
所得AZO膜的方块电阻为85 Ω/□，图4，图5为所得AZO膜的AFM图，由图可见薄膜具有规则的网络状绒面，其“沟”宽约1μm，“坝”宽约400 nm，从“沟”底到“坝”顶的高度平均约80 nm，图6为AZO膜的透过率谱，显示薄膜在可见光区的透过率在85%左右。 The sheet resistance of the obtained AZO film is 85 Ω/□. Figure 4 and Figure 5 are the AFM images of the obtained AZO film. It can be seen from the figure that the film has a regular network-like suede surface, and its "groove" is about 1 μm wide, and the "dam" is about The average height from the bottom of the "ditch" to the top of the "dam" is about 80 nm. Figure 6 shows the transmittance spectrum of the AZO film, which shows that the transmittance of the film in the visible light region is about 85%.
实施例3： Example 3:
称取Zn(Ac)2·2H2O（分析纯）10.9745g，Al(NO3)3·9H2O（分析纯）0.7504g；将上述药品在搅拌的条件下先后添加到100mL无水乙醇中；量取3mL单乙醇胺，在搅拌的条件下添加到上述溶液中，溶液逐渐由浑浊变为无色透明；继续搅拌2小时，得到透明稳定的溶胶；将清洗干净的玻璃衬底浸渍到上述前躯体溶胶中，然后以6cm/min的恒定速度将玻璃衬底缓慢提出液面，从而在玻璃上涂覆一层均匀的溶胶膜，将溶胶膜在400°C进行预处理10分钟，然后重复前面的浸渍、提拉、预处理步骤共12次；将获得的AZO薄膜置于箱式炉中在空气中400°C热处理1 h。然后将样品置于管式炉中，在流速为8：0.8 L/min的N2/H2气氛下于400°C热处理1 h，然后缓慢冷却至室温。 Weigh 10.9745g of Zn(Ac) 2 2H 2 O (analytical grade), 0.7504g of Al(NO 3 ) 3 9H 2 O (analytical grade); medium; measure 3mL of monoethanolamine, add it to the above solution under the condition of stirring, the solution gradually changes from turbid to colorless and transparent; continue to stir for 2 hours to obtain a transparent and stable sol; dip the cleaned glass substrate into the above In the precursor sol, the glass substrate was slowly lifted out of the liquid surface at a constant speed of 6 cm/min, thereby coating a uniform sol film on the glass, and the sol film was pretreated at 400 ° C for 10 minutes, and then repeated The previous impregnation, pulling, and pretreatment steps were 12 times in total; the obtained AZO film was heat-treated in a box furnace at 400°C for 1 h in air. The samples were then placed in a tube furnace, heat-treated at 400 °C for 1 h in a N 2 /H 2 atmosphere with a flow rate of 8:0.8 L/min, and then slowly cooled to room temperature.
所得AZO膜的方块电阻为105 Ω/□，在可见光区的透过率在85%左右。 The sheet resistance of the obtained AZO film is 105 Ω/□, and the transmittance in the visible light region is about 85%.
实施例4 ： Example 4:
称取Zn(Ac)2·2H2O（分析纯）10.9745g，Al(NO3)3·9H2O（分析纯）1.1254g；将上述药品在搅拌的条件下先后添加到100mL乙二醇甲醚中；量取4.8mL二乙醇胺，在搅拌的条件下添加到上述溶液中，溶液逐渐由浑浊变为无色透明；继续搅拌2小时，得到透明稳定的溶胶；将清洗干净的玻璃衬底浸渍到上述前躯体溶胶中，然后以6cm/min的恒定速度将玻璃衬底缓慢提出液面，从而在玻璃上涂覆一层均匀的溶胶膜，将溶胶膜在400°C进行预处理20分钟，然后重复前面的浸渍、提拉、预处理步骤共16次；将获得的AZO薄膜置于箱式炉中在空气中400°C热处理1 h。然后将样品置于管式炉中，在流速为2 L/min的H2气氛下于400°C热处理1 h，然后缓慢冷却至室温。 Weigh 10.9745g of Zn(Ac) 2 2H 2 O (analytical grade), 1.1254g of Al(NO 3 ) 3 9H 2 O (analytical grade); in methyl ether; measure 4.8mL diethanolamine and add it to the above solution under stirring, the solution gradually changes from turbid to colorless and transparent; continue stirring for 2 hours to obtain a transparent and stable sol; clean the glass substrate Immerse in the above-mentioned precursor sol, then slowly lift the glass substrate out of the liquid surface at a constant speed of 6cm/min, thereby coating a uniform sol film on the glass, and pretreat the sol film at 400°C for 20 minutes , and then repeated the previous impregnation, pulling, and pretreatment steps for a total of 16 times; the obtained AZO film was placed in a box furnace and heat-treated at 400°C in air for 1 h. The samples were then placed in a tube furnace, heat-treated at 400 °C for 1 h under H2 atmosphere at a flow rate of 2 L/min, and then slowly cooled to room temperature.
所得AZO膜的方块电阻为95 Ω/□，在可见光区的透过率在85%左右。 The sheet resistance of the obtained AZO film is 95 Ω/□, and the transmittance in the visible light region is about 85%. the
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110305886.7A CN102593239B (en) | 2011-10-11 | 2011-10-11 | Preparation method of latticed textured azo compound (AZO) transparent conductive membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110305886.7A CN102593239B (en) | 2011-10-11 | 2011-10-11 | Preparation method of latticed textured azo compound (AZO) transparent conductive membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102593239A CN102593239A (en) | 2012-07-18 |
| CN102593239B true CN102593239B (en) | 2015-04-15 |
Family
ID=46481646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110305886.7A Expired - Fee Related CN102593239B (en) | 2011-10-11 | 2011-10-11 | Preparation method of latticed textured azo compound (AZO) transparent conductive membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102593239B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998721B (en) * | 2012-12-28 | 2015-02-11 | 江苏宇迪光学股份有限公司 | Method for coating diffusion film coating |
| CN104376895B (en) * | 2014-11-13 | 2016-12-07 | 南通华盛高聚物科技股份有限公司 | Transparent conductive film and its preparation method and application |
| CN106847378A (en) * | 2017-03-31 | 2017-06-13 | 东莞市纳利光学材料有限公司 | A kind of flexible transparent conductive film and preparation method thereof |
| CN107602156B (en) * | 2017-10-13 | 2020-10-16 | 四川航天机电工程研究所 | Wave-absorbing ceramic and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560059B (en) * | 2009-05-27 | 2012-09-12 | 中南大学 | Aluminum-doped zinc oxide film coating and nano-rod array material as well as preparation method thereof |
| KR101069066B1 (en) * | 2010-04-23 | 2011-09-29 | 전북대학교산학협력단 | Method for manufacturing a transparent conductive substrate of aluminum doped zinc oxide nanorod based silicon solar cell |
-
2011
- 2011-10-11 CN CN201110305886.7A patent/CN102593239B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102593239A (en) | 2012-07-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lee et al. | Fabrication of tin oxide film by sol–gel method for photovoltaic solar cell system | |
| Liu et al. | Preparation of ZnO porous thin films by sol–gel method using PEG template | |
| CN110002767B (en) | Preparation method of high-transmittance hydrophobic coating film for photovoltaic glass | |
| EP2717320B1 (en) | Preparation method for surface-textured conductive glass and its application for solar cells | |
| CN103508406B (en) | AZO thin film, preparation method and include its MEMS | |
| CN105731821B (en) | Method for constructing super-hydrophilic, anti-reflection and moisture-proof composite film on glass substrate | |
| CN102943253A (en) | Aluminum-doped zinc oxide (AZO) transparent conducting film and preparation method thereof | |
| CN102157575A (en) | Novel transparent conducting oxide thin film with multi-layer film structure and manufacturing method thereof | |
| CN102593239B (en) | Preparation method of latticed textured azo compound (AZO) transparent conductive membrane | |
| CN102603202A (en) | Method for preparing tin selenide photoelectric thin film | |
| CN103451637A (en) | Aluminum-doped zinc oxide film and preparation method thereof | |
| CN102094191B (en) | Method for preparing copper tin sulfur film with preferred orientation | |
| CN102664215B (en) | Method for preparing zinc selenide photoelectric film | |
| Kanmaz et al. | Silicon dioxide thin films prepared by spin coating for the application of solar cells | |
| CN1949546A (en) | Method for preparing p type copper sulfide transparent conducting film | |
| CN105870260B (en) | A kind of preparation method of antireflection structure and Graphene compound transparent electricity conductive film | |
| CN106435533A (en) | Method for preparing high-performance AZO transparent conductive thin film | |
| CN102877049B (en) | Preparation method of co-doped transparent conductive thin film | |
| WO2006098185A1 (en) | Process for producing substrate for thin-film photoelectric transducer, and thin-film photoelectric transducer | |
| CN102400123B (en) | A kind of preparation method of Na-Mg weak doping p-type ZnO film | |
| CN116371703B (en) | Preparation method of ITO film suitable for flexible substrate and ITO film | |
| CN104498916B (en) | Method used for preparing aluminium-doped zinc oxide thin film via electroless deposition | |
| CN103928564A (en) | A method for preparing aluminum oxide passivation film on the surface of crystalline silicon solar cell | |
| CN108374162B (en) | A kind of preparation method of aluminum-doped zinc oxide transparent conductive film | |
| Premalal et al. | Development of quality FTO films by spray pyrolysis for dye-sensitized solar cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150415 Termination date: 20171011 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |