CN104213090A - Method for preparing molybdenum-doped zinc oxide film by magnetron sputtering method - Google Patents
Method for preparing molybdenum-doped zinc oxide film by magnetron sputtering method Download PDFInfo
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Abstract
The invention relates to a method for preparing a molybdenum-doped zinc oxide film by a magnetron sputtering method. The method comprises the following steps: (1) a glass substrate is put on a substrate tray of a magnetron sputtering instrument for fixing; (2) a ZnO target and a Mo target are respectively put in a radio-frequency target position and a direct-current target position; the target positions are adjusted, so that the axes of a direct-current target is parallel to the surface of the substrate; and an included angle between the axes of a radio-frequency target and the horizontal plane is 70-80 degrees; and (3) a ZnO: Mo transparent conducting film is prepared by sputtering. The molybdenum-doped zinc oxide film prepared by the method generally has excellent quality and photoelectric performance; the resistivity of the film can reach 3.829*10-4 omega.cm; and the transmittance of the film in a light visible area reaches above 87%. The method is simple and feasible in preparation process, and is high in resource utilization rate.
Description
technical field
The present invention relates to a kind of magnetron sputtering preparation method of zinc-oxide film, particularly relate to a kind of magnetron sputtering preparation method of double target co-sputtering of doping molybdenum zinc oxide transparent conductive film, belong to technical field of electronic materials.
background technology
Transparent conductive film, because of its high permeability in visible region and good conductivity, has a wide range of applications at solar cell, display device and microelectronics technology.Transparent conductive film the most frequently used is at present ITO(In
2o
3: Sn), but because of phosphide element less at occurring in nature content, its extensive application is restricted.Transparent conductive film based on ZnO, because it is nontoxic, it is extensive to exist at occurring in nature, obtains more and more many concerns.In recent years, the ZnO film mixing the elements such as Al, B, Zr, In, Ga is prepared, as sol-gel method, chemical Vapor deposition process, pulsed laser deposition, spray heating decomposition, radio-frequency magnetron sputter method etc. by the various method of use.The film that above-mentioned various method is prepared has same scarcely on structure and properties.Magnetron sputtering method because of its can plated film at a lower temperature, and sedimentation rate is high, film adhesion is good, be easy to the advantages such as control, becomes the major technique preparing high-quality ZnO film in recent years.
At present, prepare the many employings of doping transparent conductive film first by doped element or its oxide compound to be doped thing and carry out being mixed with into the target containing corresponding doped element, then carry out the method that sputters.For the molybdenum doping zinc oxide transparent conductive film that research is relatively less, its disclosed method adopting magnetron sputtering to prepare also mostly is this type of, as ZL 200610043274.4 discloses a kind of zinc oxide transparent conductive film mixing molybdenum and preparation method thereof, the method is first by ZnO powder and MoO
3powder is mixed with into target, then adopts radio-frequency magnetron sputter method to prepare film; A kind of preparation method of molybdenum doping zinc-oxide film disclosed in CN 101158028A adopts reactive d.c.magnetron sputtering method, makes sputtering target, at Ar and O to inlay Mo in Zn
2on simple glass, ZnO:Mo transparent conductive film is deposited in atmosphere.The content that aforesaid method often adjusts a hotchpotch just must prepare a kind of corresponding target again, and not only experimental period is long, and causes the waste of resource.In addition to the above methods, when preparing film with magnetron sputtering, also someone employs dual-target sputtering method, and employing double oxide target as disclosed in ZL 201010616147.5, carries out experiment respectively and prepared CoTiO on two radio frequency targets
3film, because it uses double oxide target, so two radio frequency targets must be used just can to realize, adds experiment difficulty; CN 101768728A is disclosed adopts dual-target sputtering, but it uses layering to sputter, and then by anneal, use submolecule layering doping techniques to realize the doping of film, this method increases the difficulty of experimental period and experiment condition.Hereto also do not have a kind of cycle short, experiment condition simply prepares the magnetically controlled sputter method of doping transparent conductive film.
summary of the invention
The object of this invention is to provide a kind of film quality better and the simple magnetron sputtering method of preparation technology prepares the method for molybdenum doping zinc-oxide film.
Magnetron sputtering method of the present invention prepares the method for molybdenum doping zinc-oxide film, and step is as follows:
1) glass substrate after cleaning-drying is placed on the substrate pallet of magnetic control sputtering device, fixing;
2) by purity be 99.99% ZnO target and purity be after the Mo target cleaning-drying of 99.99%, be placed on radio frequency target position and direct current target position respectively, adjustment target position, make the axis of direct current target and substrate surface be parastate, between the axis of radio frequency target and horizontal plane, angle is 70 ~ 80 °;
3) Slag coating ZnO:Mo transparent conductive film, sputtering instrument back end vacuum tightness is higher than 2 × 10
-4pa, sputter gas is argon gas, and sputtering pressure is 0.5Pa, and underlayer temperature is 100 ~ 300 DEG C, and the sputtering power of ZnO target is the power of 285 ~ 326W, Mo target is 0.75W, sputters 40 ~ 60 minutes simultaneously.
The purity of the sputter gas argon gas of step 3) described in technique scheme is 99.99%.
Compared with prior art, beneficial effect of the present invention is: the method that the present invention adopts radio frequency target and direct current target jointly to sputter prepares the zinc oxide transparent conductive film of molybdenum doping, by the position of fixing molybdenum target, make its axis parallel with substrate surface, only regulate the angle of ZnO target and horizontal plane, can realize the Effective Doping of molybdenum in zinc-oxide film, and its incorporation can be controlled in 1-6at%, the film doping obtained within the scope of this doping is even and quality is better.ZnO:Mo film prepared by the present invention generally has good photoelectric properties, and the resistivity of film can reach 3.829 × 10
-4Ω cm, reaches more than 87% in the transmitance of visible region.Compared with the method preparing doping transparent conductive film with other magnetron sputtering methods, method preparation technology simple possible of the present invention, and resource utilization is high.
accompanying drawing explanation
Fig. 1 is the XRD figure of molybdenum doping zinc oxide.
embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1:
1) glass substrate after cleaning-drying is placed on the substrate pallet of magnetic control sputtering device, fixing;
2) by purity be 99.99% ZnO target and purity be after the Mo target cleaning-drying of 99.99%, be placed on radio frequency target position and direct current target position respectively, adjustment target position, make the axis of direct current target and substrate surface be parastate, between the axis of radio frequency target and horizontal plane, angle is 80 °;
3) Slag coating ZnO:Mo transparent conductive film, sputtering instrument back end vacuum tightness is higher than 2 × 10
-4pa, sputter gas is argon gas, and sputtering pressure is 0.5Pa, and underlayer temperature is 300 DEG C, and the sputtering power of ZnO target is the power of 285W, Mo target is 0.75W, sputters 40 minutes simultaneously.
The molybdenum doping zinc-oxide film thickness that this example obtains is 270nm, and the resistivity of film is 8.31 × 10 after tested
-4Ω cm, through EDS test, recording its molybdenum, to mix concentration be 5.63at%.
Embodiment 2:
1) glass substrate after cleaning-drying is placed on the substrate pallet of magnetic control sputtering device, fixing;
2) by purity be 99.99% ZnO target and purity be after the Mo target cleaning-drying of 99.99%, be placed on radio frequency target position and direct current target position respectively, adjustment target position, make the axis of direct current target and substrate surface be parastate, between the axis of radio frequency target and horizontal plane, angle is 70 °;
3) Slag coating ZnO:Mo transparent conductive film, sputtering instrument back end vacuum tightness is higher than 2 × 10
-4pa, sputter gas is argon gas, and sputtering pressure is 0.5Pa, and underlayer temperature is 100 DEG C, and the sputtering power of ZnO target is the power of 326W, Mo target is 0.75W, sputters 60 minutes simultaneously.
As shown in Figure 1, the ZnO:Mo film prepared as can be seen from Figure has significantly (002) peak to the XRD of the molybdenum doping zinc oxide that this example is obtained, and illustrate that film has hexagonal wurtzite structure, crystalline quality is good.Film thickness is 400nm, and the resistivity of film is 3.829 × 10 after tested
-4Ω cm.Through EDS test, recording its molybdenum, to mix concentration be 2.12at%.
Case study on implementation 3:
1) glass substrate after cleaning-drying is placed on the substrate pallet of magnetic control sputtering device, fixing;
2) by purity be 99.99% ZnO target and purity be after the Mo target cleaning-drying of 99.99%, be placed on radio frequency target position and direct current target position respectively, adjustment target position, make the axis of direct current target and substrate surface be parastate, between the axis of radio frequency target and horizontal plane, angle is 75 °;
3) Slag coating ZnO:Mo transparent conductive film, sputtering instrument back end vacuum tightness is higher than 2 × 10
-4pa, sputter gas is argon gas, and sputtering pressure is 0.5Pa, and underlayer temperature is 200 DEG C, and the sputtering power of ZnO target is the power of 300W, Mo target is 0.75W, sputters 50 minutes simultaneously.
The molybdenum doping zinc oxide thickness that this example obtains is 340nm, and the resistivity of film is 5.08 × 10 after tested
-4Ω cm.Through EDS test, recording its molybdenum, to mix concentration be 3.52at%.
Claims (2)
1. magnetron sputtering method prepares a method for molybdenum doping zinc-oxide film, it is characterized in that comprising the steps:
1) glass substrate after cleaning-drying is placed on the substrate pallet of magnetic control sputtering device, fixing;
2) by purity be 99.99% ZnO target and purity be after the Mo target cleaning-drying of 99.99%, be placed on radio frequency target position and direct current target position respectively, adjustment target position, make the axis of direct current target and substrate surface be parastate, between the axis of radio frequency target and horizontal plane, angle is 70 ~ 80 °;
3) Slag coating ZnO:Mo transparent conductive film, sputtering instrument back end vacuum tightness is higher than 2 × 10
-4pa, sputter gas is argon gas, and sputtering pressure is 0.5Pa, and underlayer temperature is 100 ~ 300 DEG C, and the sputtering power of ZnO target is the power of 285 ~ 326W, Mo target is 0.75W, sputters 40 ~ 60 minutes simultaneously.
2. magnetron sputtering method according to claim 1 prepares the method for molybdenum doping zinc-oxide film, it is characterized in that the purity of sputter gas argon gas in described step 3) is 99.99%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110416413A (en) * | 2019-07-26 | 2019-11-05 | 陕西师范大学 | A kind of perovskite solar cell and preparation method thereof of high-performance gradient electron transfer layer |
| CN116083852A (en) * | 2022-12-29 | 2023-05-09 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of molybdenum film with novel surface structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101158028A (en) * | 2007-10-11 | 2008-04-09 | 复旦大学 | Method for preparing polycrystalline doping molybdenum zinc oxide transparent conductive film |
| CN104004990A (en) * | 2014-06-03 | 2014-08-27 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
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2014
- 2014-08-29 CN CN201410431213.XA patent/CN104213090A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101158028A (en) * | 2007-10-11 | 2008-04-09 | 复旦大学 | Method for preparing polycrystalline doping molybdenum zinc oxide transparent conductive film |
| CN104004990A (en) * | 2014-06-03 | 2014-08-27 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
Non-Patent Citations (1)
| Title |
|---|
| CHING-MING HSU，ET AL.: "Surface textured molybdenum zinc oxide for light diffusion enhancement", 《THIN SOLID FILMS》, vol. 517, no. 13, 1 May 2009 (2009-05-01), pages 3717 - 3720, XP026052805, DOI: doi:10.1016/j.tsf.2008.12.038 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110416413A (en) * | 2019-07-26 | 2019-11-05 | 陕西师范大学 | A kind of perovskite solar cell and preparation method thereof of high-performance gradient electron transfer layer |
| CN116083852A (en) * | 2022-12-29 | 2023-05-09 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of molybdenum film with novel surface structure |
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Application publication date: 20141217 |