CN1945858A - Preparing high conductivity suede non-blended ZnO film by MOCVD method - Google Patents
Preparing high conductivity suede non-blended ZnO film by MOCVD method Download PDFInfo
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- CN1945858A CN1945858A CNA2006100162514A CN200610016251A CN1945858A CN 1945858 A CN1945858 A CN 1945858A CN A2006100162514 A CNA2006100162514 A CN A2006100162514A CN 200610016251 A CN200610016251 A CN 200610016251A CN 1945858 A CN1945858 A CN 1945858A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 title abstract 4
- 239000011521 glass Substances 0.000 claims abstract description 7
- 230000001939 inductive effect Effects 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000010408 film Substances 0.000 claims description 51
- 239000010409 thin film Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 230000012010 growth Effects 0.000 claims description 11
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 claims description 8
- 230000005611 electricity Effects 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000008020 evaporation Effects 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- 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
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Abstract
This invention relates to a method for preparing high conductive rate and non-doped ZnO films of soft nap at super-low temperature with MOCVD technology, which first of all utilizes an electronic beam evaporation technology or sputter method to deposit a layer of 50-100nm high electric conducted ITO film as the seed inducing layer on a glass substrate with fine conductivity, then utilizes the MOCVD technology to grow non-doped ZnO film at low temperature. The method can prepare ZnO films of soft nop structure with fine light diffusion ability at very low temperature and reduce the resistivity of ZnO film grown by the MOCVD system greatly.
Description
[technical field]: the invention belongs to the transparent conductive oxide film field, particularly be fit to the preparation method of the transparent conductive film of thin film solar cell application.
[background technology]: in recent years, in Si thin film solar cell (Solar cell) application facet, because SnO
2Film has fabulous electricity and optical characteristics, is widely used as the nesa coating of solar cell.Yet their optical characteristics under the hydrogen plasma atmosphere environment worsen, and have limited its application as transparent conductive film in thin film solar cell.And ZnO film not only can have high stability in the hydrogen plasma environment, and can realize good photoelectric characteristic (low-resistivity, suede structure, high permeability) film growth, thus the transparent conductive film that has competitiveness in the thin film solar cell become.For silicon (Si) thin film solar cell, fall into the light path that light (light trapping) effect (being corresponding suede structure) can increase incident light, particularly important to improving device performance.
The method of growing ZnO thin-film is a lot of at present, comprise pulsed laser deposition (PLD), molecular beam epitaxy (MBE), metal-organic chemical vapor deposition equipment (MOCVD), radio frequency/direct current sputtering (RF/DCSputtering), electric beam evaporation (EBRE), spraying thermal decomposition (Spray Pyrolysis) and sol-gel processing (Sol-gel) etc.Being used for the ZnO film preparation of solar cell and assembly thereof, mainly be magnetron sputtering and MOCVD technology in the world.Utilize magnetron sputtering method to prepare the ZnO film that thin film solar cell is used, adopt Al to mix usually and obtain low resistivity (～10
-4Ω cm) mirror surface structure.People such as Jin Yoo utilize radio frequency sputtering method to grow high permeability (T on Corning 1737 glass substrate
400-800nm＞85%) low-resistivity (ρ～1.9 * 10
-4Ω cm) ZnO:Al film is (referring to JinsuYoo, Jeonghul Lee, Seokki Kim, etc.High transmittance and low resistive ZnO:Al films for thin film solar cells, ThinSolid Films, 2005,480-481:213), the growth technique of its film characteristics optimum: radio-frequency power 100W, underlayer temperature 573K, Ar dividing potential drop 0.27Pa.Be the sunken light action of electrode before the adaptation thin film solar cell, the ZnO film after the sputter must take wet etching could form suede structure, in the hope of obtaining good light scattering ability.During the modulation suede structure, wet etching plays a crucial role, and therefore, has high risk and cause waste of material (corrosion rear film thickness reduces) when large tracts of land corrosion ZnO film forms suede structure.
Yet, but MOCVD technology direct growth goes out the ZnO film of suede structure (referring to Baosheng Sang, Akira Yamada, Makoto Konagai, Growth of Boron doped ZnO thin films by atomiclayer deposition, Solar Energy Materials and Solar cells, 1997,46:19).The low-resistivity of MOCVD growth at present, the matte structure ZnO-underlayer temperature of TCO film and need B generally more than 423K
2H
6Doping (hypertoxic gas) could obtain the film of low-resistivity.
[summary of the invention]: the objective of the invention is to solve existing method and prepare ZnO film and need B
2H
6Mix (a kind of hypertoxic gas) and cause environmental pollution problems, provide a kind of " green " environment-friendly type mocvd method ultralow temperature to prepare the method for high conductivity, suede non-blended ZnO film.
The method that metal-organic chemical vapor deposition equipment provided by the invention (MOCVD) ultralow temperature prepares high conductivity, suede non-blended ZnO film, realized by following steps:
(a) utilize electron beam evaporation technique or the sputtering method ito thin film that the high electricity of deposition one deck 50-100nm is led on glass substrate earlier as the seed inducing layer;
(b) on above-mentioned inducing layer, utilize the non-blended ZnO film about metal-organic chemical vapor deposition equipment method growth 600-3000nm: reactant gas source diethyl zinc DEZn and water H
2O is contained in the bubbler respectively and is positioned in the temperature controlled water bath jar, enters reative cell via Ar gas bell source; DEZn and H
2The temperature controlled water bath jar of O is stabilized in 293-318K and 313-353K respectively; The flow of diethyl zinc and water is set at 100-300 μ mol/min and 300-600 μ mol/min respectively, and the vacuum chamber reaction pressure is 100-600Pa, and the underlayer temperature excursion is 398-413K, and the deposit film time is 20-60min.
Then, to obtaining the ZnO film H of deposition in (b) step
2The annealing of gas low pressure.Its annealing temperature is 443-503K, can effectively improve the electron mobility of ZnO film.
Advantage of the present invention and effect: the method on the one hand can cryogenic conditions obtains suede structure with light scattering feature down, improves growth rate; Secondly do not needing B
2H
6Can reduce significantly under the situation of mixing MOCVD system growing ZnO thin-film resistivity (can reduce to～10
-3Ω cm); By follow-up H
2The electron mobility that annealing can make film is from～18.6cm
2/ Vs brings up to～32.5cm
2/ Vs (improving～30%).In addition, method provided by the invention can not pollute environment, belongs to " green " Environmentally-sound technology.This method can be fit to the preparation of large tracts of land (for example S=20cm*20cm) ZnO transparent conductive film.
[description of drawings]:
Fig. 1 is the typical shape appearance figure of underlayer temperature ZnO film when being 408K;
Fig. 2 is the surface topography map (wherein ito thin film is 50nm) of underlayer temperature ZnO/ITO film when being 408K.
[embodiment]:
Embodiment 1
The present invention proposes the method for two growths " green " environment-friendly type ZnO-TCO film.
At first, utilize electron beam evaporation technique or sputtering method on glass substrate, to deposit earlier one deck
100nmThe ito thin film that high electricity is led is as seed inducing layer (Seed layer), and it has good conductivity (～10 usually
-4Ω cm); Utilize the unadulterated ZnO film of MOCVD technology low-temperature epitaxy then.The suede structure that this method can obtain to have the light scattering feature on the one hand, on the other hand, can reduce significantly MOCVD system growing ZnO thin-film resistivity (can reduce to～10
-3Ω cm).
The concrete manufacture process of film:
1, deposits one deck in the electron beam evaporation equipment
The ito thin film that the high electricity of 100nm is led
2, the MOCVD non-blended ZnO film about 1.2 μ m of growing.
Typical growth conditions is as follows: in the experiment, and reactant gas source diethyl zinc DEZn and water H
2O is contained in the bubbler respectively and is positioned in the temperature controlled water bath jar, enters reative cell via Ar gas bell source; DEZn and H
2The temperature controlled water bath jar of O is stabilized in 313K and 333K respectively; The flow of diethyl zinc and water is set at 202.1 μ mol/min and 447.75 μ mol/min respectively, and the vacuum chamber reaction pressure is 200Pa, and the underlayer temperature excursion is 398-413K, and the deposit film time is 30min.In addition, H
2Gas annealing (～the electron mobility that 473K) can improve ZnO film from 18.6 to 32.5cm
2/ Vs.Table 1 is that the ZnO film of preparation and the electrology characteristic of ZnO/ITO film compare.
The electrology characteristic of table 1 ZnO film and ZnO/ITO film relatively
| #Un-doped ZnO | 398K | 408K | 413K | 418K | |
| Without ITO | ρ(Ωcm) μ(cm 2/Vs) n(cm -3) d(nm) | 2.08×10 -1 2.17 1.38×10 19 850 | 8.92×10 -2 5.62 1.457×10 19 900 | 3.33×10 -2 11.2 1.35×10 19 1005 | 8.05×10 -3 24.3 3.19×10 19 1200 |
| With ITO | ρ(Ωcm) μ(cm 2/Vs) n(cm -3) d(nm) | 1.6×10 -3 20.5 1.8×10 20 980 | 2.1×10 -3 18.6 1.6×10 20 1400 | 1.8×10 -3 21.4 1.5×10 20 1500 |
ITO：d＝100nm，ρ＝3.5×10
-4Ωcm，μ＝12.21cm
2/Vs，n＝1.62×10
21cm
-3，T＞85％(in VIS-NIR region).
Embodiment 2
The concrete manufacture process of film:
1, utilize electron beam evaporation technique or sputtering method on glass substrate, to deposit earlier one deck
50nm is high, and electricity is led Ito thin filmAs the seed inducing layer;
2, the MOCVD non-blended ZnO film about 1.0 μ m of growing.
Typical growth conditions is as follows: in the experiment, and reactant gas source diethyl zinc DEZn and water H
2O is contained in the bubbler respectively and is positioned in the temperature controlled water bath jar, enters reative cell via Ar gas bell source; DEZn and H
2The temperature controlled water bath jar of O is stabilized in 313K and 333K respectively; The flow of diethyl zinc and water is set at 202.1 μ mol/min and 447.75 μ mol/min respectively, and the vacuum chamber reaction pressure is 200Pa, and the underlayer temperature excursion is 398-413K, and the deposit film time is 30min.Fig. 1 and Fig. 2 are respectively the textured ZnO membrane that the ZnO film of growing on the direct glass substrate and ITO go up low-temperature epitaxy.The resistivity of ZnO/ITO film is～4.5 * 10
-3Ω cm.
Claims (2)
1, a kind of metal-organic chemical vapor deposition equipment method ultralow temperature prepares the method for high conductivity, suede non-blended ZnO film, it is characterized in that this method is realized by following steps:
(a) utilize electron beam evaporation technique or the sputtering method ito thin film that the high electricity of deposition one deck 50-100nm is led on glass substrate earlier as the seed inducing layer;
(b) on above-mentioned inducing layer, utilize the non-blended ZnO film about metal-organic chemical vapor deposition equipment method growth 600-3000nm: reactant gas source diethyl zinc DEZn and water H
2O is contained in the bubbler respectively and is positioned in the temperature controlled water bath jar, enters reative cell via Ar gas bell source; DEZn and H
2The temperature controlled water bath jar of O is stabilized in 293-318K and 313-353K respectively; The flow of diethyl zinc and water is set at 100-300 μ mol/min and 300-600 μ mol/min respectively, and the vacuum chamber reaction pressure is 100-600Pa, and the underlayer temperature excursion is 398-413K, and the deposit film time is 20-60min.
2, method according to claim 1 is characterized in that last deposit film H in (b) step
2The annealing of gas low pressure, temperature 443-503K is to improve the electron mobility of ZnO film.
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| CNB2006100162514A CN100424899C (en) | 2006-10-24 | 2006-10-24 | Preparing high conductivity suede non-blended ZnO film by MOCVD method |
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|---|---|---|---|
| CNB2006100162514A CN100424899C (en) | 2006-10-24 | 2006-10-24 | Preparing high conductivity suede non-blended ZnO film by MOCVD method |
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|---|---|
| CN1945858A true CN1945858A (en) | 2007-04-11 |
| CN100424899C CN100424899C (en) | 2008-10-08 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100494486C (en) * | 2007-05-08 | 2009-06-03 | 中国科学院上海光学精密机械研究所 | Method for developing m-face or a-face ZnO film by metal organic chemical vapour deposition |
| US8034656B2 (en) | 2008-03-04 | 2011-10-11 | Kisco | Annealing method of zinc oxide thin film |
| CN105349966A (en) * | 2015-10-15 | 2016-02-24 | 南开大学 | Preparation method and application for ZnO-TCO film of suede composite structure |
| WO2018032874A1 (en) * | 2016-08-17 | 2018-02-22 | 佛山市中山大学研究院 | Ultraviolet-transparent electrically conductive thin film and manufacturing method therefor |
| CN114032525A (en) * | 2021-11-04 | 2022-02-11 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160192480A1 (en) * | 2014-12-30 | 2016-06-30 | Clemson University Research Foundation | Electronic device including transparent and flexible mica substrate and method for manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3408618B2 (en) * | 1994-04-12 | 2003-05-19 | 松下電器産業株式会社 | Solar cell manufacturing method |
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2006
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100494486C (en) * | 2007-05-08 | 2009-06-03 | 中国科学院上海光学精密机械研究所 | Method for developing m-face or a-face ZnO film by metal organic chemical vapour deposition |
| US8034656B2 (en) | 2008-03-04 | 2011-10-11 | Kisco | Annealing method of zinc oxide thin film |
| CN101527265B (en) * | 2008-03-04 | 2012-05-23 | 韩国铁钢株式会社 | Heat treatment method of zinc oxide thin film and manufacturing method of solar cell |
| CN105349966A (en) * | 2015-10-15 | 2016-02-24 | 南开大学 | Preparation method and application for ZnO-TCO film of suede composite structure |
| WO2018032874A1 (en) * | 2016-08-17 | 2018-02-22 | 佛山市中山大学研究院 | Ultraviolet-transparent electrically conductive thin film and manufacturing method therefor |
| CN114032525A (en) * | 2021-11-04 | 2022-02-11 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
| CN114032525B (en) * | 2021-11-04 | 2023-09-12 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
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| CN100424899C (en) | 2008-10-08 |
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Effective date of registration: 20090206 Address after: Jiangnan hi tech Zone, South Ring Road, Licheng District, Quanzhou, Fujian Patentee after: Fujian Golden Sun Solar Technic Co., Ltd. Address before: Nankai District Wei Jin Road, Tianjin City No. 94 Patentee before: Nankai University |
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Effective date of registration: 20111121 Address after: 362000 Jiangnan hi tech Zone, South Ring Road, Licheng District, Fujian, Quanzhou Co-patentee after: Beijing Jingcheng Boyang Optoelectronic Equipment Co.,Ltd. Patentee after: Fujian Golden Sun Solar Technic Co., Ltd. Address before: 362000 Jiangnan hi tech Zone, South Ring Road, Licheng District, Fujian, Quanzhou Patentee before: Fujian Golden Sun Solar Technic Co., Ltd. |
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