CN102820211A - Non-polar A-plane GaN film preparation method - Google Patents
Non-polar A-plane GaN film preparation method Download PDFInfo
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- CN102820211A CN102820211A CN2012103137257A CN201210313725A CN102820211A CN 102820211 A CN102820211 A CN 102820211A CN 2012103137257 A CN2012103137257 A CN 2012103137257A CN 201210313725 A CN201210313725 A CN 201210313725A CN 102820211 A CN102820211 A CN 102820211A
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Abstract
The invention provides a non-polar A-plane GaN film preparation method including: growing a non-polar A-plane InGaN flexible layer on a substrate; growing a non-polar A-plane GaN buffer layer on the non-polar A-plane InGaN flexible layer; annealing the non-polar A-plane InGaN flexible layer and the non-polar A-plane GaN buffer layer to form a self-assembly laterally epitaxial template; and growing a non-polar A-plane GaN film on the self-assembly laterally epitaxial template. By the aid of the self-assembly nanoscale laterally epitaxial template, film quality can be improved, and non-polar GaN films high in crystalline quality are obtained.
Description
Technical field
The present invention relates to the semiconductive thin film preparing technical field, relate in particular to a kind of method for preparing nonpolar GaN film.
Background technology
Between decades in the past, GaN and relevant InGaN, alloy semiconductor materials such as AlGaN have been obtained great success.This has also promoted the light-emitting diode (LEDs) of semiconductor applications, the fast development of laser diode (LDs) and HEMT (HEMT) simultaneously.
Though the GaN field of semiconductor materials has obtained significant achievement; But in traditional C is looked unfamiliar the nitride material of long hexagonal crystal system, cause the serious further raising that hampers the related device performance of the stronger internal electric field of material internal to the spontaneous polarization and the piezoelectric polarization that exist along C.In order to reduce the influence of polarized electric field to quantum well radiation efficient, growing nonpolar A face GaN becomes the emphasis of research at present.Therefore Sapphire Substrate adopts R surface sapphire substrate growing nonpolar A face GaN film also to receive increasing attention because the advantage on the price has satisfied the requirement of industrialization in enormous quantities.
Yet; Owing to have bigger lattice mismatch and thermal mismatching between non polarity A side GaN and the R surface sapphire substrate; Be grown in the A face GaN film on the R surface sapphire substrate and often have highdensity stacking fault and dislocation; Quality of materials is relatively poor, and to be applied in the nonpolar A face GaN film effect unsatisfactory and existing much being used for improves the method for C face GaN defective.
Summary of the invention
The technical problem that (one) will solve
For solving above-mentioned one or more problems, the invention provides a kind of method for preparing nonpolar GaN film, to improve the crystalline quality of nonpolar GaN film.
(2) technical scheme
According to an aspect of the present invention, a kind of method for preparing the non polarity A face GaN film is provided.This method comprises: growing nonpolar A face InGaN flexible layer on substrate; At non polarity A side InGaN flexible layer growing nonpolar A face GaN resilient coating; Non polarity A side InGaN flexible layer and non polarity A side GaN resilient coating are annealed, form self assembly horizontal extension template; And on self assembly horizontal extension template growing nonpolar A face GaN film.
(3) beneficial effect
Can find out that from technique scheme the method that the present invention prepares nonpolar GaN film has following beneficial effect:
(1) research before shows that directly two-step method epitaxial growth nonpolar GaN film is difficult to obtain high-quality epitaxial film on the R surface sapphire; And adopt the horizontal extension template of self-assembled nanometer yardstick of the present invention can improve film quality, obtain to have nonpolar GaN film than high-crystal quality;
(2) than the MBE growing technology, MOCVD material growing technology is owing to its relative less cost, shirtsleeve operation; In suitability for industrialized production, be widely used; Method of the present invention has the high speed of growth, reaches 1 μ m/hr, and growth quality is better simultaneously.
Description of drawings
Fig. 1 is the flow chart according to the preparation non polarity A face GaN film of the embodiment of the invention;
Fig. 2 is the sketch map according to variations in temperature in the preparation non polarity A side GaN thin-film process of the embodiment of the invention;
Fig. 3 is the cross-sectional view according to the non polarity A face GaN film of embodiment of the invention preparation;
Fig. 4 is for adopting conventional two-step method (A) and utilizing the SEM of the non polarity A face GaN film of method shown in Figure 1 (B) preparation to scheme;
Fig. 5 waves the curve chart of half-breadth with azimuthal variation for what adopt conventional two-step method and the non polarity A face GaN film that utilizes method preparation shown in Figure 1.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
In one exemplary embodiment of the present invention, a kind of method for preparing nonpolar GaN film is provided.As shown in Figure 1, this method may further comprise the steps:
Steps A: get a substrate, and in the reative cell of metal organic chemical vapor deposition (MOCVD) equipment, substrate is carried out high-temperature ammonolysis and handle;
The R surface sapphire substrate is placed metal organic chemical vapor deposition MOCVD reative cell; Under 1100 ℃ of conditions of carrying out and feeding nitrogen, substrate was toasted 20 minutes earlier; Re-use the mixed carrier gas nitrogenize substrate 3 minutes of nitrogen and ammonia, its temperature is similarly 1100 ℃, and is as shown in Figure 2.
Need to prove that what present embodiment adopted is Sapphire Substrate, for other substrate, like silicon or carborundum, as long as the lattice match degree that satisfies itself and non polarity A side GaN also can adopt less than 20%.
Step B: on substrate, utilize MOCVD technology growth non polarity A side InGaN flexible layer;
Substrate base temperature after the nitrogenize is reduced to 750 ℃, feed trimethyl indium, trimethyl gallium and ammonia as reaction source to reative cell, nitrogen is under the condition of 200torr as carrier gas keeping reative cell pressure, growth A face InGaN flexible layer.
The growth time of non polarity A side InGaN flexible layer is 2 to 16 minutes.The thickness of this layer non polarity A side InGaN flexible layer is between 10 to 90nm.
Step C: utilize MOCVD technology growth non polarity A side GaN resilient coating;
The substrate temperature of the InGaN flexible layer of having grown is reduced to 550 ℃, feeds trimethyl gallium and nitrogen as reaction source to reative cell, nitrogen is carrier gas, under the condition of maintenance reative cell pressure 50torr, and growing nonpolar A face low temperature GaN resilient coating.The non polarity A side low temperature GaN buffer growth time is 3 minutes, and the thickness of the non polarity A side low temperature GaN resilient coating of generation is between 30 to 50nm.
Step D: non polarity A side InGaN flexible layer and non polarity A side GaN resilient coating are carried out high annealing formation self assembly horizontal extension template;
The substrate temperature of grown non polarity A side InGaN flexible layer and low temperature GaN resilient coating is increased to 1100 ℃; Keep under the constant situation of flow and the reative cell pressure of nitrogen; Anneal and formed the horizontal extension template of self-assembled nanometer yardstick in 5 minutes; Wherein, annealing temperature is 1100 ℃, annealing time 5 minutes.
Certainly, also can adjust annealing parameter as required, but need to satisfy, annealing temperature should be greater than 1000 ℃, and anneal environment is nitrogen environment or other inert gas environments, and pressure is greater than 30torr, and annealing time was greater than 3 minutes.
Step e is utilized the MOCVD technology, with carrier gas gallium source and nitrogenous source is fed reative cell, growing nonpolar A face GaN film on the horizontal extension template;
The horizontal extension die plate temperature that forms the self-assembled nanometer yardstick is remained on 1100 ℃; Feed gallium source and nitrogen as reaction source to reative cell; Pure nitrogen gas or nitrogen/hydrogen relaxes gas as carrier gas, growing high-quality nonpolar GaN film under the condition that keeps reative cell pressure 50torr.
Step F is closed the gallium source, and reative cell drops to below 300 ℃ and closes ammonia, and the effect that continues the feeding ammonia is to suppress the elevated temperature heat of GaN material to decompose;
Step G continues cooling, and reaction chamber temperature after dropping to room temperature by 300 ℃ takes out sample.
Fig. 2 is the sketch map according to variations in temperature in the preparation non polarity A side GaN thin-film process of the embodiment of the invention.At first under 1100 ℃, substrate is toasted; Nitrogenize is 3 minutes under ammonia atmosphere; Growing InGaN film when temperature drops to 750 ℃ then at 3 minutes low temperature GaN buffer (LT GaN) of 550 ℃ of growths, utilizes the time of heating up that the InGaN film of previous growth and the GaN of low temperature are annealed after the InGaN film growth is intact at last; At the GaN of 1100 ℃ of high temperature of growing down, wait to grow to finish to lower the temperature and get sheet after 5 minutes.
Fig. 3 is the cross-sectional view according to the non polarity A face GaN film of embodiment of the invention preparation.As shown in Figure 3; Growing InGaN and low temperature GaN resilient coating on the R surface sapphire substrate of thickness 430 μ m; After annealing, form the horizontal extension template of the self-assembled nanometer yardstick of thickness 30-120nm; This template is loose porous, can realize discharging the purpose of upper strata GaN membrane stress, subsequently growth 1 μ m left and right sides high-quality non polarity A face GaN film on the horizontal extension template.
Need to prove; Non polarity A side InGaN flexible layer, non polarity A side low temperature GaN resilient coating and non polarity A face GaN film all are method preparations of adopting MOCVD; In fact; This three-layer thin-film also can adopt other modes to prepare, and for example: electron beam evaporation, chemical vapour deposition (CVD), magnetron sputtering or the like should be included within protection scope of the present invention equally.
Fig. 4 is for adopting conventional two-step method (A) and utilizing the SEM of the non polarity A face GaN film of method shown in Figure 1 (B) preparation to scheme.As shown in Figure 4, adopt the sample (A) of conventional method growth, film surface is more coarse, is the growth pattern of typical island, and with the increase of thickness, film surface appearance does not improve.Adopt sample (B) face of present technique growth to reveal the trend in film Lianping preferably, it is more smooth that surface topography just becomes when film thickness reaches 1um, shows between the film island all to merge, and realizes two-dimensional growth.
Fig. 5 waves the curve chart of half-breadth with azimuthal variation for what adopt conventional two-step method and the non polarity A face GaN film that utilizes method preparation shown in Figure 1.As shown in Figure 5, the minimum when numerical value of halfwidth is 0 ° at the azimuth, maximum when being 90 ° at the azimuth shows tangible anisotropy.Obviously the halfwidth than the sample (A) of traditional handicraft growth is little to have adopted the halfwidth of sample (B) of the inventive method growth.This shows that our technology can improve the crystal mass of film significantly.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (12)
1. a method for preparing the non polarity A face GaN film is characterized in that, comprising:
Growing nonpolar A face InGaN flexible layer on substrate;
At said non polarity A side InGaN flexible layer growing nonpolar A face GaN resilient coating;
Said non polarity A side InGaN flexible layer and non polarity A side GaN resilient coating are annealed, form self assembly horizontal extension template; And
Growing nonpolar A face GaN film on said self assembly horizontal extension template.
2. the method for preparing the non polarity A face GaN film according to claim 1 is characterized in that, in the said step that non polarity A side InGaN flexible layer and non polarity A side GaN resilient coating are annealed: annealing temperature is greater than 1000 ℃; Environment is nitrogen environment or inert gas environment; Annealing time was greater than 3 minutes.
3. the method for preparing the non polarity A face GaN film according to claim 2 is characterized in that, annealing temperature is 1100 ℃; Environment is a nitrogen environment, and pressure is 50torr; Annealing time is 5 minutes.
4. the method for preparing the non polarity A face GaN film according to claim 1 is characterized in that, adopts the metal-organic chemical vapor deposition equipment mocvd method said non polarity A side GaN resilient coating of growing.
5. the method for preparing the non polarity A face GaN film according to claim 4 is characterized in that, in the step of said employing mocvd method growing nonpolar A face GaN resilient coating: reaction source is trimethyl gallium and nitrogen; Carrier gas is a nitrogen.
6. the method for preparing the non polarity A face GaN film according to claim 4 is characterized in that, in the step of said employing mocvd method growing nonpolar A face GaN resilient coating: growth temperature is 550 ℃; Reative cell pressure 50torr; Growth time is 3 minutes.
7. the method for preparing the non polarity A face GaN film according to claim 1 is characterized in that, adopts the mocvd method said non polarity A side InGaN flexible layer of growing.
8. the method for preparing the non polarity A face GaN film according to claim 7 is characterized in that, in the step of said employing mocvd method growing nonpolar A face InGaN flexible layer: reaction source is trimethyl indium, trimethyl gallium and ammonia, and carrier gas is a nitrogen.
9. the method for preparing the non polarity A face GaN film according to claim 8 is characterized in that, in the step of said employing mocvd method growing nonpolar A face InGaN flexible layer: growth temperature is 750 ℃; Environment is a nitrogen environment, and pressure is 200torr.
10. according to each described method for preparing the non polarity A face GaN film in the claim 1 to 9, it is characterized in that, saidly on substrate, also comprise before the step of growing nonpolar A face InGaN flexible layer:
Said substrate is carried out high-temperature ammonolysis to be handled.
11. the method for preparing the non polarity A face GaN film according to claim 10 is characterized in that, saidly substrate is carried out the high-temperature ammonolysis processed steps comprises:
At 1100 ℃, under the condition of feeding nitrogen substrate was toasted 20 minutes;
At 1100 ℃, under the condition of the mixed carrier gas of feeding nitrogen and ammonia substrate was toasted 3 minutes.
12., it is characterized in that said substrate is R surface sapphire, SiC or Si according to each described method for preparing the non polarity A face GaN film in the claim 1 to 9.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198867A (en) * | 2017-12-29 | 2018-06-22 | 杭州电子科技大学 | A kind of low-power consumption GaN/AlGaN resonance tunnel-through diodes |
| CN108428621A (en) * | 2018-03-29 | 2018-08-21 | 太原理工大学 | One kind is in amorphous Si O2The method of Grown GaN film |
| CN110364420A (en) * | 2019-07-16 | 2019-10-22 | 北京工业大学 | A kind of insertion InGaN/GaN superlattice structure improves the epitaxial growth method of non-polar GaN quality of materials |
| CN110429019A (en) * | 2019-06-24 | 2019-11-08 | 北京工业大学 | A kind of insertion InGaN layer improves the epitaxial growth method of non-polar GaN quality of materials |
| CN111948235A (en) * | 2020-08-07 | 2020-11-17 | 广西大学 | Method for measuring semipolar plane III group nitride film defect density and application thereof |
| CN113628953A (en) * | 2021-06-17 | 2021-11-09 | 中国电子科技集团公司第十三研究所 | Method for preparing nitride material and nitride semiconductor device |
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| CN101831628A (en) * | 2010-04-21 | 2010-09-15 | 中国科学院半导体研究所 | Method for growing high-quality In ingredient enriched InGaN thin film material |
| CN101901757A (en) * | 2010-06-24 | 2010-12-01 | 西安电子科技大学 | MOCVD growing method based on nonpolar a-surface GaN on a-surface 6H-SiC substrate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198867A (en) * | 2017-12-29 | 2018-06-22 | 杭州电子科技大学 | A kind of low-power consumption GaN/AlGaN resonance tunnel-through diodes |
| CN108428621A (en) * | 2018-03-29 | 2018-08-21 | 太原理工大学 | One kind is in amorphous Si O2The method of Grown GaN film |
| CN108428621B (en) * | 2018-03-29 | 2020-05-05 | 太原理工大学 | In amorphous SiO2Method for growing GaN film on substrate |
| CN110429019A (en) * | 2019-06-24 | 2019-11-08 | 北京工业大学 | A kind of insertion InGaN layer improves the epitaxial growth method of non-polar GaN quality of materials |
| CN110429019B (en) * | 2019-06-24 | 2021-11-19 | 北京工业大学 | Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN layer |
| CN110364420A (en) * | 2019-07-16 | 2019-10-22 | 北京工业大学 | A kind of insertion InGaN/GaN superlattice structure improves the epitaxial growth method of non-polar GaN quality of materials |
| CN110364420B (en) * | 2019-07-16 | 2021-10-26 | 北京工业大学 | Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN/GaN superlattice structure |
| CN111948235A (en) * | 2020-08-07 | 2020-11-17 | 广西大学 | Method for measuring semipolar plane III group nitride film defect density and application thereof |
| CN113628953A (en) * | 2021-06-17 | 2021-11-09 | 中国电子科技集团公司第十三研究所 | Method for preparing nitride material and nitride semiconductor device |
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