CN1317749C - Three-dopant contained P-type zinc oxide film and method for making same - Google Patents
Three-dopant contained P-type zinc oxide film and method for making same Download PDFInfo
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- CN1317749C CN1317749C CNB2005100630562A CN200510063056A CN1317749C CN 1317749 C CN1317749 C CN 1317749C CN B2005100630562 A CNB2005100630562 A CN B2005100630562A CN 200510063056 A CN200510063056 A CN 200510063056A CN 1317749 C CN1317749 C CN 1317749C
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Abstract
The present invention discloses a zinc oxide film containing three dopants and a preparation method thereof. A backing containing lithium successively comprises a ZnO buffer layer, a ZnO epitaxial layer and a P-shaped ZnO ternary codoping layer, whereinthe ternary codoping layer comprises three dopants which are lithium, nitrogen, aluminum or gallium. The present invention has the advantages that the backing containing lithium adopts a high-temperature diffusion method to make lithium enter the ZnO thin film through a heterogeneity interface for preparing the p-shaped ZnO thin film, the film containing the three dopants which are lithium, aluminum or gallium and nitrogen can make the hole concentration of the film be at least 5*10<17>cm<-3>, make resistivity be lower than 3cm and make Hall mobility be within 0.1 to 10cm<2>/Vs. The p-shaped thin film with the properties can be used for p-n homojunction in photoproduction volt type elements and electroluminescence type elements.
Description
Technical field
The present invention relates to a kind of p type zinc oxide (ZnO) film and manufacture method thereof that is used to prepare opto-electronic device such as light-emitting diode, laser diode, field effect transistor and photo-detector etc.
Background technology
ZnO has multiple superior function, has a wide range of applications at aspects such as nesa coating, surface acoustic wave device and piezoelectric ceramic.ZnO also is an a kind of direct transition type II-VI family semiconductor, and the room temperature energy gap is 3.37eV.Because its very high free exciton binding energy (60meV), ZnO has become another important semiconductor material with wide forbidden band behind GaN, aspect the low threshold value of preparation, the high efficiency short-wavelength light electronic device very wide application prospect is being arranged.
The realization that high-quality ZnO intrinsic film and stable p-type are mixed is the basic point of zno-based optoelectronic device applications.Though progress is huge aspect the preparation of high-quality ZnO epitaxial film, the exploitation of stable repeatably ZnO p type doping techniques relatively lags behind, thereby has seriously influenced the commercialization paces of zinc oxide opto-electronic device.People utilize single element (Li, N, P and As) to mix and Ga (Al or In), and the common doping method of N binary has all run into difficulty in various degree, is summarized as follows:
(1) to be entrained in be more feasible scheme to lithium (Li) in theory, prophesy Li atom substitutes the Zn atom and can form a shallow acceptor thereby become p type dopant (C.H.Park, S.B.Zhang, and S.H.Wei in the ZnO lattice, Phys.Rev.B 66,073202 (2002) .).Yet experimental results show that the ZnO film of mixing Li becomes semi insulating material bar none.D.C.Look etc. have reported with Li doping ZnO material and have obtained semi-insulating ZnO; Wherein reason is explained (D.C.Look et al., Appl.Phys.Lett.81,1830 (2002) .) as yet completely.
(2) nitrogen (N) doping is the p-type doping method that is expected most, thereby people have found also that really the nitrogen-atoms of displacement can form shallow acceptor and realize that the p type mixes; Yet the admittedly molten rate of nitrogen in ZnO is extremely low, obtain very difficulty of high-concentration dopant.The Kawasaki of metal material research institute of northeastern Japan university group has been reported and has been utilized the temperature modulation legal system to be equipped with N doping p-ZnO film recently, and its room temperature hole concentration only is 2 * 10
16Cm
-3Though, also made light-emitting diode, also have suitable distance from practicality, also illustrate the limitation that the N single element mixes (A.Tsukazaki, A.Ohtomo, T.Onuma, etal:Nature Materials 4,42 (2005) .).
(3) the ratio of ionic radii oxonium ion of phosphorus (P) element wants big, so will generate deep acceptor after the displacement of theoretical prophesy.Yet nearest experiment shows, utilizes P
2O
5But formed shallow acceptor P type ZnO film as dopant, mechanism is wherein explored (K.-K.Kim, H.-S.Kim, D.-K.Hwang, J.-H.Lim, and S.-J.Park, Appl.Phys.Lett.83,63 (2003) .).Can this method develop into effective p type doping techniques, still do not have final conclusion at present.
(4) the ratio of ionic radii oxonium ion of arsenic (As) element is bigger, so should generate more being led of deep energy level after the displacement.Yet nearest experiment shows equally, utilizes the diffusion of As from substrate, has obtained shallow acceptor P type ZnO film equally, and reason is not wherein understood (J.Cryst.Growth 216,330 (2000) for Y.R.Ryu, et al) equally as yet.
(5) the miserable altogether technology of the Ga of ZnO (Al or In), N obtains extensive studies.Because the admittedly molten rate of N in ZnO is very low, the N singly technology of mixing is restricted, in order to solve this difficulty, Yamamoto etc. have proposed Ga (Al or In), N in 1999 miserable altogether theoretical, form compound by Ga, N and ZnO, reduce the energy of doping system, thereby improve doping content (the T.Yamamoto and H.Katayama-Yoshida of N, Jpn.J.Appl.Phys.38, L166 (1999)).Experimental results show that Ga (Al or In), the method that N is miserable altogether have certain effect, nearest leaf will town etc. utilizes magnetron sputtering to prepare the ZnO film that Al, N mix altogether (Ye Zhi town etc., patent publication No.: CN 1588623A).Yet it is quite limited to the raising of the molten admittedly rate of N that Al, N mix method altogether, and in addition, the method for mixing need be controlled the ratio of Al (Ga or In) and N altogether, and too much Al (Ga or In) can become isolated substitutional impurity, and becomes the alms giver, and this can influence the doping effect greatly.Therefore, the doping window of this method is narrower, is difficult for implementing, and this also is the reason that only this method is really used as yet over 5 years.
Indulge the above, ZnO p type mixes and has obtained certain progress in recent years, but industrial needed high electricity is led, the ZnO p type doping techniques of high stability still lacks.
Summary of the invention
Problem at prior art exists the object of the present invention is to provide a kind of high hole concentration of three kinds of dopants, the zinc-oxide film and manufacture method thereof of high stability of containing.
For achieving the above object, a kind of technical scheme that contains the zinc-oxide film of three kinds of dopants provided by the invention is: comprise ZnO resilient coating, ZnO epitaxial loayer and P type ZnO ternary codoping layer on the lithium substrate successively containing, wherein, three kinds of dopants that the ternary codoping layer is comprised are: lithium, and nitrogen and aluminium or gallium, the thickness of described ZnO resilient coating is 5～50nm, the thickness of described ZnO epitaxial loayer is 50～200nm, and the thickness of described P type ZnO film is 300～500nm.
Further, described substrate comprises lithium niobate, lithium tantalate, lithium gallium oxide or lithium aluminate for containing the lithium substrate, also comprises rich lithium lithium niobate, lithium tantalate, lithium gallium oxide or the lithium aluminate of lithium content more than stoichiometric(al).
A kind of manufacture method that contains the zinc-oxide film of three kinds of dopants provided by the invention comprises the steps:
1. carry out chemical cleaning to containing the lithium substrate, use deionized water rinsing then, send into the growth room of molecular beam epitaxy system after drying up with nitrogen;
2. underlayer temperature is increased between 120～750 ℃ and heat-treats, to obtain the clean surface;
3. underlayer temperature is controlled at the thick ZnO resilient coating of 5～50nm of growing between 120～550 ℃, growth between underlayer temperature to the 350～700 ℃ epitaxial loayer of 50～200nm then raises, stop growing then and carry out annealing in process, allow lithium fully diffuse to the ZnO resilient coating from substrate;
4. 300～the 500nm that grows between 350～700 ℃ comprises aluminium or gallium and active nitrogen doped P-type ZnO film, wherein, the diffusion furnace of metallic aluminium or gallium is adopted in aluminium or gallium source, and activated nitrogen source adopts the radio frequency plasma body source of the gas or the nitrogenous element that contain nitric oxide or nitrogen dioxide.
Further, also comprise step 5.: close activated nitrogen source, regulate the line of aluminium or gallium, the 100～1000nm that grows between 350～700 ℃ comprises the n type ZnO film of aluminium or gallium dopant.
Further, described substrate comprises conventional lithium niobate, lithium tantalate, lithium gallium oxide or lithium aluminate for containing the lithium substrate, also comprises rich lithium lithium niobate, lithium tantalate, lithium gallium oxide or the lithium aluminate of lithium content more than stoichiometric(al).
Beneficial effect of the present invention is: allow lithium enter into ZnO film preparation p type ZnO film by heterogeneous interface in the way that contains employing High temperature diffusion on the lithium substrate, this film contains lithium, aluminium or gallium and three kinds of dopants of nitrogen, can make the hole concentration of film be at least 5 * 10
17Cm
-3, resistivity is lower than 3cm, and Hall mobility is at 0.1～10cm
2Between/the Vs, these performances allow p type film to be used for the p-n homojunction of photogenic voltage and electroluminescence type device.
Description of drawings
Fig. 1 is the process chart of the embodiment of the invention 1.
Fig. 2 be the embodiment of the invention 1 structure as the intention.
The home position observation pattern of the reflection high energy electron diffraction (RHEED) when Fig. 3 prepares p type ZnO monocrystal thin films for the embodiment of the invention 1 ternary method of mixing altogether on rich lithium lithium niobate (0001) substrate.
Fig. 4 is cross section transmission electron microscope (TEM) figure of the prepared p type ZnO film of the embodiment of the invention 1.
Fig. 5 is the process chart of the embodiment of the invention 2.
The home position observation pattern of the reflection high energy electron diffraction (RHEED) when Fig. 6 prepares the p-n junction that contains p type ZnO layer and n type ZnO layer for the embodiment of the invention 2 ternarys method of mixing altogether on rich lithium lithium tantalate (0001) substrate.
Fig. 7 is the zinc oxide p-n knot of embodiment 2 preparations and the schematic diagram of corresponding metal electrode structure.
Fig. 8 is the ZnO p-n homojunction volt-ampere characteristic of embodiment 2 preparations.
Embodiment
The present invention is described in detail below in conjunction with preparation method of the present invention and accompanying drawing.
Adopt process chart as shown in Figure 1, the ternary method of mixing altogether prepares p type ZnO monocrystal thin films on rich lithium lithium niobate (0001) substrate concrete steps are as follows:
1. adopt the lithium niobate that is rich in lithium (0001) substrate that departs from stoichiometric(al), lithium more than needed in the substrate is easy to enter into epitaxial film by thermal diffusion, thereby helps the high dose lithium doping.
2. above-mentioned substrate is carried out chemical cleaning, use deionized water rinsing then, send into the growth room of molecular beam epitaxy system after drying up with high pure nitrogen.
3. underlayer temperature is increased to 450 ℃, carries out 20 minutes heat treatment, is cooled to 200 ℃ then and carries out oxygen plasma treatment 20 minutes, to obtain the clean surface that oxygen stops.The oxygen flow that is adopted during oxygen plasma treatment is 2sccm, and radio-frequency power is 350 watts.
4. underlayer temperature is at 200 ℃ of growth 20nm thick ZnO resilient coatings, and underlayer temperature to 400 ℃ then raises.Reflected high energy electron diffraction in temperature-rise period (RHEED) pattern displaying is clearly because 6 * 6 structures again that lithium is induced show that lithium diffuses to the ZnO film from lithium niobate substrate.Epitaxial loayer at 400 ℃ of growth 200nm stops growing then and carries out annealing in process, and annealing time is 20 minutes.RHEED pattern displaying epitaxial film surface keeps clearly because 6 * 6 structures again that lithium is induced show that lithium is doped in the ZnO film under this temperature.
5. the flat p type ZnO film that comprises aluminium and active nitrogen doping at 400 ℃ of growth 300nm.The diffusion furnace of metallic aluminium is adopted in the aluminium source, and activated nitrogen source adopts the radio frequency Nitrogen plasma source.The temperature of aluminium stove is 600 ℃, and nitrogen flow is 0.5sccm, and radio-frequency power is 150 watts.The whole doping process of RHEED pattern displaying surface keeps because 6 * 6 structures again that lithium is induced, and has so just realized in ZnO film that lithium, aluminium and nitrogen ternary mix altogether.
The structure of the film for preparing according to the method described above is rich lithium lithium niobate substrate 1 as shown in Figure 2 successively, the low temperature buffer layer 2 that 20nm is thick, epitaxial loayer 3 and the p type layer 4 that contains lithium, aluminium and three kinds of dopants of nitrogen that 200nm is thick.In above-mentioned film preparation process, we utilize reflection high energy electron diffraction instrument (RHEED) that sample is carried out home position observation, its result as shown in Figure 3, (a) lithium niobate substrate surface wherein for cleaning after the oxygen plasma treatment, this surface is very smooth; (b) be the surface of the ZnO resilient coating that just length is good; (c) the zinc bloom buffer layer surface when being warming up to 400 ℃, 6 * 6 structures again of inducing by lithium of clear display, the such structure again of zinc oxide surface is that we observe for the first time; (d) mix zinc oxide surface in the process altogether for ternary, this surface has kept 6 * 6 structures again of being induced by lithium.RHEED result is presented at 400 ℃ of growth phases, and lithium can be diffused in the ZnO film to high concentration, thereby has realized the high concentration lithium doping of ZnO monocrystal thin films.But the film of singly mixing lithium does not show p type characteristic, but presents semi-insulating.Therefore mix in this high concentration and carry out aluminium nitrogen on the lithium basis more simultaneously and mix altogether, promptly carry out lithium, aluminium and nitrogen ternary and mix altogether, the result has realized that the p type of high hole concentration mixes.Fig. 4 is cross section transmission electron microscope (TEM) figure of this sample, has shown sharp keen ZnO/LiNbO
3Interface, and good crystallinity.Table 1 is the test result of ear suddenly of specimen electric property: hole concentration is 3.6 * 10
18Cm
-3, mobility is 2cm
2/ Vs, resistivity is 0.78cm.The electric property of this film shows that we have prepared the preparation of the p type ZnO film of device quality.
Table 1 is the ear test result suddenly:
| The measuring current pattern | Target voltage (mV) | Electric current I (μ A) | Film thickness (μ m) | Face resistance (K Ω/sq) |
| AC | 100 | 10 | 0.5 | -15.6715 |
| Volume resistance (Ω cm) | Hall coefficient (m 2/C) | Mobility [mu] h (cm 2/Vs) | Face carrier concentration (cm -2) | Body carrier concentration (cm -3) |
| -0.78357 | 3.459 | -2 | 1.81×10 14 | 3.61×10 18 |
Adopt process chart as shown in Figure 5, the concrete steps that prepare zinc oxide p-n homojunction on rich lithium lithium tantalate (0001) substrate are as follows:
1. adopt the lithium tantalate that is rich in lithium (0001) substrate that departs from stoichiometric(al), lithium more than needed in the substrate is easy to enter into epitaxial film by thermal diffusion, thereby helps the high dose lithium doping.
2. above-mentioned substrate is carried out chemical cleaning, use deionized water rinsing then, the growth room of the molecular beam epitaxy system of sending into after drying up with high pure nitrogen.
3. underlayer temperature is increased to 500 ℃, carries out 20 minutes heat treatment, is cooled to 250 ℃ then and carries out oxygen plasma treatment 20 minutes, to obtain the clean surface that oxygen stops.The oxygen flow that is adopted during oxygen plasma treatment is 2sccm, and radio-frequency power is 350 watts.
4. underlayer temperature is at 250 ℃ of growth 20nm thick ZnO resilient coatings, and underlayer temperature to 450 ℃ then raises.(the RHEED pattern displaying is clearly because 6 * 6 structures again that lithium is induced show that lithium diffuses to the ZnO film from lithium niobate substrate to reflected high energy electron diffraction in temperature-rise period.Epitaxial loayer at 450 ℃ of growth 100nm stops growing then and carries out annealing in process, and annealing time is 20 minutes.RHEED pattern displaying epitaxial film surface keeps clearly because 6 * 6 structures again that lithium is induced show that lithium is doped in the ZnO film under this temperature.
5. comprise aluminium and active nitrogen doped P-type ZnO film at 450 ℃ of growth 500nm.The diffusion furnace of metallic aluminium is adopted in the aluminium source, and activated nitrogen source adopts the radio frequency Nitrogen plasma source.The temperature of aluminium stove is 600 ℃, and nitrogen flow is 0.5sccm, and radio-frequency power is 150 watts.The whole doping process of RHEED pattern displaying surface keeps because 6 * 6 structures again that lithium is induced, and has so just realized in ZnO film that lithium, aluminium and nitrogen ternary mix altogether.
6. the ZnO ternary that stops growing codoping layer is closed activated nitrogen source, closes the aluminium stove, and annealing is 20 minutes under 450 ℃ of oxygen atmospheres.
7. regulate the line of aluminium, and comprise the n-type ZnO film of aluminium dopants at 350 ℃ of 500nm that grow down.Wherein the resistivity of this layer is by the doping decision of aluminium, and when the aluminium furnace temperature was 560 ℃, the electron concentration of this layer ZnO was 2 * 10
18Cm
-3
In above-mentioned preparation thin-film process, we utilize reflection high energy electron diffraction instrument (RHEED) that sample is carried out home position observation, its result as shown in Figure 6, wherein (a) is through the lithium tantalate substrate surface after the oxygen plasma treatment, sharp keen diffracted ray shows through after the in-situ treatment, substrate surface cleaning and smooth, (b) be the surface of the ZnO resilient coating that just length is good, (c) the zinc bloom buffer layer surface when being warming up to 450 ℃, 6 * 6 structures again of inducing by lithium of clear display, (d) mix zinc oxide surface in the process altogether for ternary, this surface has kept 6 * 6 structures again of being induced by lithium.(e) surface of n-ZnO film, 6 * 6 disappear, and this is because growth temperature reduces the diffusion hindered of lithium.Fig. 7 is the schematic diagram of this zinc oxide p-n knot and corresponding metal electrode structure, is rich lithium lithium tantalate substrate 1 successively, the thick n type layer 5 that contains aluminium dopants of epitaxial loayer 3 that low temperature buffer layer 2,100nm that 20nm is thick are thick, the p type layer 4 that contains lithium, aluminium and three kinds of dopants of nitrogen for 500nm is thick and 500nm, titanium/gold electrode 6 that n type zinc oxide forms ohmic contact and p type zinc oxide nickel/gold electrode 7 of forming ohmic contact.According to the structure of Fig. 7, the volt-ampere characteristic that we have tested this sample as shown in Figure 8, small reverse current and the forward current that rises rapidly show that this sample has good p-n junction characteristic.In addition, under forward voltage, we have observed the basket violet light, show that this zinc oxide p-n knot can be applicable to the making of opto-electronic devices such as light-emitting diode, laser diode, photo-detector.
Claims (5)
1. zinc-oxide film that contains three kinds of dopants, it is characterized in that, comprise ZnO resilient coating, ZnO epitaxial loayer and P type ZnO ternary codoping layer on the lithium substrate successively containing, wherein, three kinds of dopants being comprised of ternary codoping layer are: lithium, and nitrogen, with aluminium or gallium, the thickness of described ZnO resilient coating is 5～50nm, and the thickness of described ZnO epitaxial loayer is 50～200nm, and the thickness of described P type ZnO film is 300～500nm.
2. the zinc-oxide film that contains three kinds of dopants according to claim 1, it is characterized in that, described substrate comprises lithium niobate, lithium tantalate, lithium gallium oxide or lithium aluminate for containing the lithium substrate, also comprises rich lithium lithium niobate, lithium tantalate, lithium gallium oxide or the lithium aluminate of lithium content more than stoichiometric(al).
3. a manufacture method that contains the zinc-oxide film of three kinds of dopants is characterized in that, comprises the steps:
1. carry out chemical cleaning to containing the lithium substrate, use deionized water rinsing then, send into the growth room of molecular beam epitaxy system after drying up with nitrogen;
2. underlayer temperature is increased between 120～750 ℃ and heat-treats, to obtain the clean surface;
3. underlayer temperature is controlled at the thick ZnO resilient coating of 5～50nm of growing between 120～550 ℃, growth between underlayer temperature to the 350～700 ℃ epitaxial loayer of 50～300nm then raises, stop growing then and carry out annealing in process, allow lithium fully diffuse to the ZnO resilient coating from substrate;
4. 300～the 500nm that grows between 350～700 ℃ comprises aluminium or gallium and active nitrogen doped P-type ZnO film, wherein, the diffusion furnace of metallic aluminium or gallium is adopted in aluminium or gallium source, and activated nitrogen source adopts the radio frequency plasma body source of the gas or the nitrogenous element that contain nitric oxide or nitrogen dioxide.
4. the manufacture method that contains the zinc-oxide film of three kinds of dopants according to claim 3, it is characterized in that, also comprise step 5.: close activated nitrogen source, regulate the line of aluminium or gallium, the 300～1000nm that grows between 350～700 ℃ comprises the n type ZnO film of aluminium or gallium dopant.
5. according to claim 3 or the 4 described manufacture methods that contain the zinc-oxide film of three kinds of dopants, it is characterized in that, the described lithium substrate that contains comprises lithium niobate, lithium tantalate, lithium gallium oxide or lithium aluminate, also comprises rich lithium lithium niobate, lithium tantalate, lithium gallium oxide or the lithium aluminate of lithium content more than stoichiometric(al).
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| CN101148781B (en) * | 2007-07-27 | 2010-07-28 | 北京大学 | Process for preparing zinc oxide ferro-electricity film |
| CN102496578A (en) * | 2011-12-07 | 2012-06-13 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing p-type zinc oxide (ZnO) based thin film in lithium-nitrogen (Li-N) double-acceptor co-doping mode |
| CN102605317B (en) * | 2012-03-30 | 2013-12-11 | 哈尔滨工业大学 | Preparation method of multi-luminous-region luminous Ag, Ga and N doping ZnO film |
| CN104480427B (en) * | 2014-12-02 | 2017-01-25 | 中国科学院上海硅酸盐研究所 | Preparation method of zinc oxide based diluted magnetic semiconductor thin film and in-situ regulation and control method of charge concentration of zinc oxide based diluted magnetic semiconductor thin film |
| CN113120949A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Zinc oxide nano material, preparation method thereof, thin film and photoelectric device |
| CN117832347B (en) * | 2024-03-04 | 2024-05-14 | 江西兆驰半导体有限公司 | Micro-LED epitaxial wafer, preparation method thereof and LED chip |
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| US6448585B1 (en) * | 1999-02-19 | 2002-09-10 | Murata Manufacturing Co., Ltd. | Semiconductor luminescent element and method of manufacturing the same |
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