CN101798672A - Method for preparing P-type zinc oxide film from in situ low-pressure oxidized aluminum-doped zinc nitride - Google Patents
Method for preparing P-type zinc oxide film from in situ low-pressure oxidized aluminum-doped zinc nitride Download PDFInfo
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- CN101798672A CN101798672A CN 200910214084 CN200910214084A CN101798672A CN 101798672 A CN101798672 A CN 101798672A CN 200910214084 CN200910214084 CN 200910214084 CN 200910214084 A CN200910214084 A CN 200910214084A CN 101798672 A CN101798672 A CN 101798672A
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Abstract
The invention discloses a method for preparing a P-type zinc oxide film from in situ low-pressure oxidized aluminum-doped zinc nitride; an ultra-high vacuum magnetron sputtering system is adopted to prepare an aluminum-doped zinc nitride film on a quartz substrate as a precursor, wherein the select purity of a target is 99.999 percent high-purity zinc; and a high-purity aluminum sheet is put on the surface of the target to control the aluminum content in a sample. After the precursor is prepared, the background of a reaction chamber is vacuumized to be 10 to 4Pa, and 99.999 percent high-purity oxygen is fed in to oxidize the precursor at low pressure. The method improves the active nitrogen content in the zinc oxide with nitrogen and aluminum doping, improves the concentration and the mobility of a hole carrier, and reduces the resistivity of the zinc oxide film. When the oxidation temperature is 550DEG C, the resistivity is low to 19.8(ohm.cm), the concentration of the carrier reaches +4.6E1018cm-3. An optical band gap is 3.27Ev, and the film has excellent crystalline state and optical properties.
Description
Technical field
The present invention relates to photoelectric technology, refer to that especially the low-pressure oxidized aluminum-doped zinc nitride of a kind of original position prepares the method for p type zinc-oxide film
Background technology
Because fields such as information technology, photoelectron technology, aerospace are to the tight demand of short-wave long light-emitting device, zinc oxide, gan, wide bandgap semiconductors such as silicon carbide become the research focus in the our times scope.Compare with other semiconductor material with wide forbidden band, zinc oxide has numerous advantages: exciton bind energy helps obtaining the room-temperature exciton radiation of efficient stable up to 60meV; Can prepare at a lower temperature, impurity and the defective introduced when reducing material preparation, and can simplify production technique greatly; Have higher thermostability and chemical stability; Have stronger radiation hardness ability, can satisfy the requirement of aeronautical and space technology; Its abundant raw materials and nontoxic helps reducing cost and protecting environment.Therefore the further investigation utmost point of zinc oxide material is hopeful to solve the bottleneck problem of multiple technologies such as semiconductor lighting, ultraviolet semiconductor laser.What need to be resolved hurrily in the zinc oxide research at present is p type doping problem, and the stable and controlled p section bar material of performance is the basis of preparation junction device, also is the key of zinc oxide material practicability.The intrinsic zinc oxide material is n type conduction, there are a lot of intrinsic alms giver's defectives such as oxygen room (Vo), gap zinc (Zni) and hydrogen impurity, can produce the height auto-compensation, be difficult to realize that the p type mixes acceptor doping, greatly limited the Application and Development of Zinc oxide-base photoelectric device, resistivity is up to 10
12Ω cm.Since people such as Minegish i in 1997 successfully prepare p type zinc-oxide film first, existing many investigators have realized that the p type of zinc oxide mixes, yet the carrier mobility of the p type zinc oxide that is obtained is very low, and resistivity is higher, can not satisfy the application requiring of high-quality light electrical part.Some investigators attempt preparation Zinc oxide-base homogeneous pn junction device, but are in the preliminary research stage on the p type to zinc oxide mixes the basis of studying.Select suitable dopant material and suitable preparation technology, realize the doping of low resistance p type zinc oxide, preparation is stablized and the p section bar material and the junction device of dependable performance have become most important, the most urgent task in the current zinc oxide material application, and correlative study in this respect is for promoting information technology, photoelectron technology, development of aviation and aerospace technology to have very important significance.
After people such as Yan predicted that the nitrogen element is the desirable dopant material of p type zinc oxide, a lot of research groups had carried out the research work of nitrogen doping preparation p type ZnO.They utilize metal organic chemical vapor deposition (MOCVD) respectively, pulsed laser deposition (PLD), and laser molecular beam epitaxy (LMBE), technologies such as direct current reaction magnetron sputtering adopt nitrogenous gas to prepare p type zinc oxide as doped source: the N film.Yet these technologies can't provide enough active nitrogen conducts to be subjected to the master to compensate intrinsic alms giver defective, and the p type zinc-oxide film carrier mobility for preparing is lower, and resistivity is higher, and performance does not also reach the requirement of photoelectric device.In order to solve the low problem of nitrogen solid solubility in zinc oxide, people such as C.Wang and Kaminska as presoma, go out p type zinc-oxide film by the film preparation of thermooxidizing zinc nitride with the zinc nitride film of sputtering method preparation.Although this method can provide enough active nitrogen doped source, the pollution of carbon and hydrogen can appear in zinc nitride film preparation and oxidising process, and the resistivity of sample is higher, and crystalline quality is also not ideal enough.T.Yamamoto shows the Theoretical Calculation of zinc oxide electronic band structure: n type doped source can reduce crystalline Madelung energy, and the doping of p type can make it to raise.Active alms giver is subjected to the main codoped of implementing with activity, can be with the alms giver with original being led of the replacement of the gravitation between being led between repulsion, the doping content of increase acceptor atom obtains more acceptor impurity.Theoretical Calculation shows that the polarization of donor impurity can be followed successively by: indium＜gallium＜aluminium, aluminium are more suitable for being used for the p type zinc oxide of codoping technology growth low-resistance, so III-V family element codoped has become the adulterated main path of present acquisition p type.Nitrogen, aluminium are mixed the obvious p type zinc-oxide film resistivity that reduced altogether.But under general technology, be difficult to effectively control the content of active nitrogen in the sample.
Summary of the invention
Main purpose of the present invention is in order to remedy the deficiency that prior art exists, provide the low-pressure oxidized aluminum-doped zinc nitride of a kind of original position to prepare the method for p type zinc-oxide film, this method utilizes the method for nitrogen aluminium codoped to prepare p type zinc-oxide film, obtain to improve the content of active nitrogen in the zinc oxide, improve the concentration and the mobility of hole carrier, reduce the effective way of zinc-oxide film resistivity.To carry out original position low-pressure oxidized to mixing aluminium zinc nitride film first, comes the controlled oxidation process by the oxygen partial pressure that reduces in the oxidizing atmosphere, realized the effective control to active nitrogen content in the sample.Because presoma does not have ingress of air, effectively reduces the pollution of elements such as carbon, hydrogen, has also suppressed the hydrolysis reaction of zinc nitride simultaneously, the electricity and the optical property of p type zinc-oxide film are largely increased.
For achieving the above object, the technical scheme that the present invention takes is: the low-pressure oxidized aluminum-doped zinc nitride of this original position prepares the method for p type zinc-oxide film, adopt ultrahigh vacuum(HHV) multi-target magnetic control sputtering systems produce to contain aluminium zinc nitride film as presoma, it is low-pressure oxidized to carry out original position then, wherein target selection purity is 99.999% high purity zinc, on target surface, place high-purity aluminium flake of different area, the content of aluminium in the control sample, realize nitrogen aluminium codoped, the target meanwhile distance of substrate is adjustable, after the presoma preparation was finished, it was 10 that the reaction chamber background is vacuumized
-4Pa, feeding 99.999% high purity oxygen gas, that precursor thin-film is carried out original position is low-pressure oxidized, comes the controlled oxidation process by the oxygen partial pressure that reduces in the oxidizing atmosphere, has realized the effective control to active nitrogen content in the sample.
Described substrate is selected sheet glass, monocrystalline silicon piece, silica glass or single-crystal zinc-oxide.
Described precursor thin-film is carried out in-situ oxidation, oxidizing temperature is 450 ℃～550 ℃, and oxidation pressure is 10
3Pa, oxidization time are 2 hours.
After adopting such scheme, it is fine and close that the zinc nitride membrane structure becomes, and the nitrogen element is difficult for diffusing out after the oxidation, thereby more active nitrogen can be provided, and the content and structure of state of aluminium element in film can keep and improve the content of active nitrogen, reduces the resistivity of p type film.Utilize nitrogen aluminium codoped to improve the content of active nitrogen in the zinc oxide, the concentration and the mobility of increase hole carrier reduce zinc-oxide film resistivity.Oxidizing temperature is 550 o'clock, and resistivity is low to moderate 19.8 (Ω cm), and carrier concentration reaches+4.632E+18.It is good that thin film crystallization state and optical property keep.
Embodiment
The low-pressure oxidized aluminum-doped zinc nitride of original position of the present invention prepares the method for p type zinc-oxide film, the zinc nitride film that adopts ultrahigh vacuum(HHV) multi-target magnetic control sputtering systems produce is as presoma, the target village is that diameter is the high purity zinc (99.999%) of 60mm, place high-purity aluminium flake of different area on the target surface, control the content of aluminium in the sample, the distance of target and substrate is adjustable.Substrate is selected silica glass.Underlayer temperature is 200 ℃.RF source frequencies is 12.56MHz, and power input is 50W.Working gas is nitrogen (99.999%) and argon gas (99.999%).The reaction chamber base vacuum is 10
-4Pa, before the reactive sputtering, first butterfly covers substrate, utilizes the pollutent on the argon plasma cleaning target, and the flow of argon gas is 20cm
3/ min, air pressure are 1.2Pa.Feed nitrogen (20cm behind the 30min
3/ min), the reaction chamber vacuum degree control is carried out reactive sputtering at 2Pa, time 30min.After containing the preparation work of aluminium zinc nitride film presoma and finishing, base vacuum is extracted into 10
-4Pa, feeding high purity oxygen gas (99.999%) and argon gas again, that presoma is carried out original position is low-pressure oxidized.Oxidation pressure is adjusted to 10
3Pa, oxidizing temperature is chosen at 550 ℃, and the time is 2 hours.
Adopt above-mentioned prepared nitrogen aluminium codoped zinc-oxide film.The result shows that when oxidizing temperature was 550 ℃, it was 19.8 Ω cm that oxidization time can reach resistivity in 2 hours, and hole is+4.6E10
18Cm
-3P type zinc-oxide film.Its percent of pass in visible-range is about 88%.Optical band gap is at 3.27eV.
Claims (3)
1. the low-pressure oxidized aluminum-doped zinc nitride of original position prepares the method for p type zinc-oxide film, it is characterized in that: adopt ultrahigh vacuum(HHV) multi-target magnetic control sputtering systems produce to contain aluminium zinc nitride film as presoma, it is low-pressure oxidized to carry out original position then, wherein target selection purity is 99.999% high purity zinc, on target surface, place high-purity aluminium flake of different area, the content of aluminium in the control sample, realize nitrogen aluminium codoped, the target meanwhile distance of substrate is adjustable, after the presoma preparation was finished, it was 10 that the reaction chamber background is vacuumized
-4Pa, feeding 99.999% high purity oxygen gas, that precursor thin-film is carried out original position is low-pressure oxidized, comes the controlled oxidation process by the oxygen partial pressure that reduces in the oxidizing atmosphere, has realized the effective control to active nitrogen content in the sample.
2. prepare the method for p type zinc-oxide film according to the low-pressure oxidized aluminum-doped zinc nitride of the described original position of claim 1, it is characterized in that: described substrate is selected sheet glass, monocrystalline silicon piece, silica glass or single-crystal zinc-oxide.
3. prepare the method for p type zinc-oxide film according to the low-pressure oxidized aluminum-doped zinc nitride of the described original position of claim 1, it is characterized in that: precursor thin-film is carried out in-situ oxidation, and oxidizing temperature is 450 ℃～550 ℃, and oxidation pressure is 103Pa, and oxidization time is 2 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104409337A (en) * | 2014-11-05 | 2015-03-11 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sulphur and silver co-doped p type zinc oxide optoelectronic thin film |
| CN104818452A (en) * | 2015-04-20 | 2015-08-05 | 岭南师范学院 | Method for preparing nitrogen aluminum co-doping p type zinc oxide thin film |
| CN106086797A (en) * | 2016-07-12 | 2016-11-09 | 京东方科技集团股份有限公司 | Indium tin oxide films and preparation method thereof, containing its array base palte, display device |
| CN108914078A (en) * | 2018-08-07 | 2018-11-30 | 泉州市康馨化工科技有限公司 | The preparation method of the zinc nitride system laminated film of performance improvement |
-
2009
- 2009-12-18 CN CN 200910214084 patent/CN101798672A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104409337A (en) * | 2014-11-05 | 2015-03-11 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sulphur and silver co-doped p type zinc oxide optoelectronic thin film |
| CN104409337B (en) * | 2014-11-05 | 2017-10-27 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of sulphur and silver-colored codoped p type zinc oxide optoelectronic film |
| CN104818452A (en) * | 2015-04-20 | 2015-08-05 | 岭南师范学院 | Method for preparing nitrogen aluminum co-doping p type zinc oxide thin film |
| CN104818452B (en) * | 2015-04-20 | 2018-10-19 | 岭南师范学院 | A method of preparing nitrogen aluminium codoped p type zinc-oxide film |
| CN106086797A (en) * | 2016-07-12 | 2016-11-09 | 京东方科技集团股份有限公司 | Indium tin oxide films and preparation method thereof, containing its array base palte, display device |
| CN106086797B (en) * | 2016-07-12 | 2018-12-11 | 京东方科技集团股份有限公司 | Indium tin oxide films and preparation method thereof, the array substrate containing it, display device |
| CN108914078A (en) * | 2018-08-07 | 2018-11-30 | 泉州市康馨化工科技有限公司 | The preparation method of the zinc nitride system laminated film of performance improvement |
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Open date: 20100811 |