CN102560675A - Nonpolar InN film growing on LiGao2 substrate and preparation method of nonpolar InN film - Google Patents

Nonpolar InN film growing on LiGao2 substrate and preparation method of nonpolar InN film Download PDF

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CN102560675A
CN102560675A CN2012100568519A CN201210056851A CN102560675A CN 102560675 A CN102560675 A CN 102560675A CN 2012100568519 A CN2012100568519 A CN 2012100568519A CN 201210056851 A CN201210056851 A CN 201210056851A CN 102560675 A CN102560675 A CN 102560675A
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inn
nonpolar
substrate
ligao
face
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李国强
杨慧
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention discloses a nonpolar InN film growing on a LiGao2 substrate. The nonpolar InN film comprises a nonpolar a surface InN buffer layer growing on the LiGao2 substrate, and a nonpolar a surface InN layer growing on the nonpolar a surface InN buffer layer, wherein the nonpolar a surface InN buffer layer is an InN film growing on the substrate at 300-350 DEG C; and the nonpolar a surface InN layer is an InN film growing on the substrate at 500-550 DEGC. The invention further discloses a preparation method of the nonpolar a surface InN film. Compared with the prior art, the InN film has the advantages of simple growing process and low preparation cost; the contradiction between the decomposition temperature and the reactivity of InN materials is overcome; and the prepared nonpolar InN film has low defect density and good crystallization quality.

Description

Be grown in LiGaO 2Nonpolar InN film on the substrate and preparation method thereof
Technical field
The present invention relates to nonpolar InN film, particularly be grown in LiGaO 2Nonpolar InN film on the substrate and preparation method thereof.
Background technology
III hi-nitride semiconductor material GaN; AlN and InN are the novel semiconductor materials of superior performance; Existing important use aspect opto-electronic device also has very wide application prospect on, ultra-high speed microelectronic device integrated at photoelectricity and the ultra-high frequency Microwave Device and Circuitry.
The InN material has the highest saturated electron drift velocity in the III hi-nitride semiconductor material, electronic migration speed and the effective electron mass with minimum.Therefore the InN material is ideal high speed, high-frequency crystal tube material, the great potential of in following high-speed high frequency microwave electronic device field, using.Though the material of high-frequency electron device commonly used is GaAs at present; And the same gallium arsenide of the transport property of InN (GaAs) is compared; Little to temperature and adulterated susceptibility; InN does not have the poison gas that has of GaAs and the generation of gallium phosphide (GaP) base device, is suitable for having very high radiation or the very strong environment of chemical corrosion.So InN is a kind of very promising material aspect high-frequency electron device.
Secondly, because the InN material is the direct band gap material, the current research result shows that its band gap magnitude is 0.6~0.7eV, and this makes In xGa 1-xThe energy gap scope of N ternary-alloy material can be with the variation of Ga component x in the alloy 3.4eV free adjustment from the 0.7eV of InN energy gap to the GaN energy gap, and corresponding wavelength is from 1771nm to 365nm.It provides corresponding to the almost ideal correspondence coupling energy gap of solar spectral, and this provides great possibility for design high efficiency solar battery.Because the material behavior of InN itself; Make the InGaN alloy can also resist the severe radiation of high-energy electron; Can the slow down process of cooling of hot carrier in the solar cell of unique phonon bottleneck effect; And can be with can autoregistration, thereby has eliminated the naturally occurring compound obstacle of silica-based solar cell, and these characteristics make it be particularly suitable for the high-level efficiency multijunction solar cell material as SPACE APPLICATION.Simultaneously, because InN has special band gap properties and other high-performance, make it at LED, also there is huge application potential aspects such as LD and special detector.
In order to satisfy the high performance needs of device, the research of being devoted to the InN sill more and more seems important, but problems such as being separated in the particular difficulty property of InN growth and the InGaN alloy have hindered the preparation of high-quality InN sill.At present, the InN sill mainly is to prepare on sapphire or GaN template through MOCVD or MBE method.There are two hang-ups in preparation InN material.Be not have suitable substrate on the one hand.Because the InN monocrystalline also is very difficult the acquisition; So must lean on heteroepitaxial growth, this just is difficult to avoided the problem than the macrolattice coupling, common substrate such as sapphire; Two kinds of aligning directions are arranged between InN and sapphire usually; A kind of is c face InN [1010] || c surface sapphire [1120], and this moment, lattice mismatch was up to 25%, if InN mismatch degree after sapphire (0001) direction is rotated 30 ° can be reduced to 13%; A kind of in addition extensional mode is a face InN (11-20) || a surface sapphire (11-20), its lattice mismatch is then up to 28%.Secondly, the Sapphire Substrate price is very expensive, makes the device production cost very high.
Be that the InN material has the highest balance nitrogen pressure in the III group-III nitride on the one hand in addition; Under given temperature; The InN material is than high tens times of GaN and AlN; This means that any InN that is deposited on the substrate takes off very possible at once the branch, the In metal that stays is evaporation subsequently also, so the sample of preparing often has a lot of textural defect.The InN decomposition temperature is only 600 ℃ simultaneously, and so low decomposition temperature has determined the InN material to grow at low temperatures; And as the NH of nitrogenous source 3Decomposition temperature about 1000 ℃, make the surface lack active N atom, the growth of InN is restricted, thereby has produced contradiction, therefore adopts general method to be difficult to prepare the single crystal material of InN.
This shows, make the extensive widespread use of the real realization of InN base device, raise the efficiency, and reduce its manufacturing cost, the most basic way is exactly that the employing novel method of researching and developing on the novel substrate prepares the InN sill.Therefore the epitaxy indium nitride is the focus and the difficult point of research always on the novel substrate.
Summary of the invention
For the above-mentioned shortcoming and deficiency that overcome prior art, one of the object of the invention is to provide a kind of LiGaO of being grown in 2Nonpolar InN film on the substrate has that defect concentration is low, the measured advantage of crystalline, and preparation cost is cheap.Two of the object of the invention is to provide the preparation method of above-mentioned nonpolar InN film.
The object of the invention is realized through following technical scheme:
Be grown in LiGaO 2Nonpolar InN film on the substrate comprises being grown in LiGaO 2Nonpolar a face InN impact plies on the substrate and be grown in the nonpolar a face InN epitaxial film on the nonpolar a face InN impact plies; Said nonpolar a face InN impact plies is the InN layer of growth when underlayer temperature is 300-350 ℃; Said nonpolar a face InN layer is the InN layer of growth when underlayer temperature is 500-550 ℃.
The thickness of said nonpolar a face InN impact plies is 50-100nm.
The above-mentioned LiGaO that is grown in 2The preparation method of the nonpolar InN film on the substrate may further comprise the steps:
(1) chooses substrate and crystalline orientation: adopt LiGaO 2Substrate, the crystalline orientation of selection are (001) crystal face;
(2) substrate is carried out anneal: with substrate behind 900-1000 ℃ of following high bake 3-5h air cooling to room temperature;
(3) substrate being carried out cleaning surfaces handles;
(4) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN impact plies, processing condition are: underlayer temperature is 300-350 ℃, and chamber pressure is 4-5 * 10 -5Pa, V/III ratio are 0.5-0.7ML/s for 35-50, the speed of growth;
(5) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN epitaxial film, processing condition are: underlayer temperature rises to 500-550 ℃, and chamber pressure is 3-5 * 10 -5Pa, V/III ratio are 0.7-0.9ML/s for 30-40, the speed of growth.
The thickness of said nonpolar a face InN impact plies is 50-100nm.
Step (3) is said carries out the cleaning surfaces processing to substrate, is specially: with LiGaO 2Substrate was put under the deionized water room temperature ultrasonic cleaning 5-10 minute, removed LiGaO 2Substrate surface pickup particle more successively through persalt, acetone, washing with alcohol, is removed surface organic matter; LiGaO after the cleaning 2Substrate dries up with high-purity drying nitrogen; Afterwards with LiGaO 2Substrate is put into the low temperature molecular beam epitaxy growth room, under UHV condition, underlayer temperature is risen to 850-900 ℃, high bake 20-30 minute, removes lining LiGaO 2The impurity that basal surface is remaining.
Said UHV condition is that pressure is less than 6 * 10 -7Pa.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention uses LiGaO 2As substrate, adopt the low temperature molecular beam epitaxy technology simultaneously at LiGaO 2(001) the nonpolar a face of elder generation's growth one deck InN impact plies on the substrate; Obtain very low lattice mismatch between substrate and nonpolar a face (11-20) the InN epitaxial film; Hang down and reach 3.6%, help depositing the nonpolar a face InN epitaxial film of low defective, improved InN base device efficient greatly.
(2) adopt the method for low temperature molecular beam epitaxy (MBE) growth InN material, both realized the condition of low-temperature epitaxy InN, avoided adopting NH again 3As nitrogenous source, thereby well solved the contradiction between InN material breakdown temperature and the reactive behavior.
(3) the nonpolar InN film of the present invention has been eliminated the quantum constraint stark effect that polar surface InN brings, and has improved the radiative recombination efficient of current carrier, can increase substantially the efficient of nitride device such as semiconductor laser, photodiode and solar cell.
(4) use LiGaO 2As substrate, obtain easily, low price helps reducing production costs.
In sum; Technology growth substrate of the present invention is unconventional; Growth technique is unique and simple, has repeatability, epitaxially grown a face InN film defects density is low, crystal mass is high, advantages such as electricity and optical property excellence; Can be widely used in HEMT device, high-frequency electron device, and field such as solar cell, easy to utilize.
Description of drawings
Fig. 1 be the present invention prepared be grown in LiGaO 2The schematic cross-section of the nonpolar InN film on the substrate;
Fig. 2 be the present invention prepared be grown in LiGaO 2The TEM Electronic Speculum figure of the nonpolar InN film on the substrate.
Fig. 3 be the present invention prepared be grown in LiGaO 2The XRD test pattern of the nonpolar InN film on the substrate.
Fig. 4 be the nonpolar a face of the prepared high quality of the present invention InN film be PL spectrum test pattern under the 77K in temperature.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is done to specify further, but embodiment of the present invention is not limited thereto.
Embodiment 1
Present embodiment is grown in LiGaO 2The preparation method of the nonpolar InN film on the substrate may further comprise the steps:
(1) chooses substrate and crystalline orientation: adopt LiGaO 2Substrate, the crystalline orientation of selection are (001) crystal face.
(2) substrate is carried out anneal: with substrate behind 900 ℃ of following high bake 3h air cooling to room temperature.
(3) substrate being carried out cleaning surfaces handles: with LiGaO 2Substrate was put under the deionized water room temperature ultrasonic cleaning 5 minutes, removed LiGaO 2Substrate surface pickup particle more successively through persalt, acetone, washing with alcohol, is removed surface organic matter; LiGaO after the cleaning 2Substrate dries up with high-purity drying nitrogen; Afterwards with LiGaO 2Substrate is put into the low temperature molecular beam epitaxy growth room, 6 * 10 -7Under the UHV condition of Pa, underlayer temperature is risen to 850 ℃, high bake 20 minutes is removed lining LiGaO 2The impurity that basal surface is remaining.
(4) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN impact plies, processing condition are: underlayer temperature is 300 ℃, and chamber pressure is 4 * 10 -5Pa, V/III ratio are 35, the speed of growth is 0.5ML/s.
(5) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN epitaxial film, processing condition are: underlayer temperature rises to 500 ℃, and chamber pressure is 3 * 10 -5Pa, V/III ratio are 30, the speed of growth is 0.7ML/s.
Fig. 1 be present embodiment prepared be grown in LiGaO 2The schematic cross-section of the nonpolar InN film on the substrate; Comprise LiGaO2 substrate 11, nonpolar a face InN impact plies 12, nonpolar a face InN film 13.Nonpolar a face InN impact plies 12 is on LiGaO2 substrate 11, and nonpolar a face InN film 13 is at nonpolar a face InN impact plies 12.Wherein, the thickness of nonpolar a face InN impact plies is 50nm.
Fig. 2 be the present invention prepared be grown in LiGaO 2The TEM Electronic Speculum figure of the nonpolar InN film on the substrate.Show that epitaxial substrate adopts LiGaO 2Substrate, the crystalline orientation of selection are (001) crystal face, obtain interface nonpolar clearly a face InN film.Wherein 0.54nm is LiGaO 2Substrate is along the lattice parameter of (100), and 0.57nm is the lattice parameter along the InN of (0001) direction, LiGaO 2The crystal face of growing on substrate relation be InN [0001] //LiGaO 2[100].
Fig. 3 be present embodiment prepared be grown in LiGaO 2The XRD figure spectrum of the nonpolar InN film on the substrate.Can know diffraction angle pairing a face InN and the substrate LiGaO of XRD by figure 2(001) diffraction peak position and intensity explain that crystal mass is good.
Fig. 4 for the present invention prepared be grown in LiGaO 2Nonpolar InN film on the substrate be PL spectrum test pattern under the 77K in temperature.It is 0.80eV that temperature PL spectrum test under 77K obtains interband exciton recombination luminescence peak, and this shows, uses the present invention at LiGaO 2(001) the nonpolar a face InN epitaxial film that grows on the substrate has extraordinary performance on optical property.
Utilize the LiGaO that is grown in of present embodiment preparation 2The step of field-effect transistor (FET) device of preparation InN/AlN is following on the substrate: earlier at LiGaO 2Substrate epitaxial growth (000-1) AlN layer, the nonpolar a face InN film that obtains according to above-mentioned steps again, regrowth SiNx insulation layer, last electron beam evaporation forms the Ti/Al source electrode, grid, and drain electrode.Wherein AlN thickness is 100nm, and the InN extension is 25nm, and the SiNx thickness of insulating layer is 25nm, source electrode, and grid and drain electrode are adopted as Ti (30nm)/Al (200nm).
Embodiment 2
Present embodiment is grown in LiGaO 2The preparation method of the nonpolar InN film on the substrate may further comprise the steps:
(1) chooses substrate and crystalline orientation: adopt LiGaO 2Substrate, the crystalline orientation of selection are (001) crystal face.
(2) substrate is carried out anneal: with substrate behind 1000 ℃ of following high bake 5h air cooling to room temperature.
(3) substrate being carried out cleaning surfaces handles: with LiGaO 2Substrate was put under the deionized water room temperature ultrasonic cleaning 10 minutes, removed LiGaO 2Substrate surface pickup particle more successively through persalt, acetone, washing with alcohol, is removed surface organic matter; LiGaO after the cleaning 2Substrate dries up with high-purity drying nitrogen; Afterwards with LiGaO 2Substrate is put into the low temperature molecular beam epitaxy growth room, 4 * 10 -7Under the UHV condition of Pa, underlayer temperature is risen to 900 ℃, high bake 30 minutes is removed lining LiGaO 2The impurity that basal surface is remaining.
(4) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN impact plies, processing condition are: underlayer temperature is 350 ℃, and chamber pressure is 5 * 10 -5Pa, V/III ratio are 50, the speed of growth is 0.7ML/s.
(5) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN epitaxial film, processing condition are: underlayer temperature rises to 550 ℃, and chamber pressure is 5 * 10 -5Pa, V/III ratio are 40, the speed of growth is 0.9ML/s.
Present embodiment is prepared is grown in LiGaO 2Nonpolar InN film on the substrate comprises LiGaO 2Substrate, nonpolar a face InN impact plies, nonpolar a face InN film.Nonpolar a face InN impact plies is on the LiGaO2 substrate, and nonpolar a face InN film is at nonpolar a face InN impact plies.Wherein, the thickness of nonpolar a face InN impact plies is 100nm.
Utilize the LiGaO that is grown in of present embodiment preparation 2The InGaN solar cell device step for preparing on the nonpolar a face InN film of preparation on the substrate is following: on the nonpolar a face InN epitaxial film that above-mentioned steps obtains, growing successively has the In of component gradient xGa 1-xThe N impact plies, the n type is mixed silicon In xGa 1-xN, In xGa 1-xThe N multiple quantum well layer, the p type is mixed the In of magnesium xGa 1-xThe N layer.Form ohmic contact through electron beam evaporation again; Pass through at N at last 2Anneal under the atmosphere, to improve the carrier concentration and the mobility of p type GaN film.Wherein, the thickness that the n type is mixed silicon GaN epitaxial film is 5 μ m, and the concentration of current carrier is 1 * 10 19Cm - 3In xGa 1-xN MQW layer thickness is about 300nm, and cycle life is 20, wherein In 0.2Ga 0.8N trap layer thickness is 3nm, In 0.08Ga 0.92It is 10nm that N builds layer; Mg doped p type In xGa 1-xThe thickness of N layer is about 200nm, and carrier concentration is 2 * 10 16Cm -3
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not limited by the examples; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (6)

1. be grown in LiGaO 2Nonpolar InN film on the substrate is characterized in that, comprises being grown in LiGaO 2Nonpolar a face InN impact plies on the substrate and be grown in the nonpolar a face InN epitaxial film on the nonpolar a face InN impact plies; Said nonpolar a face InN impact plies is the InN layer of growth when underlayer temperature is 300-350 ℃; Said nonpolar a face InN layer is the InN layer of growth when underlayer temperature is 500-550 ℃.
2. the LiGaO that is grown in according to claim 1 2Nonpolar InN film on the substrate is characterized in that, the thickness of said nonpolar a face InN impact plies is 50-100nm.
3. be grown in LiGaO 2The preparation method of the nonpolar InN film on the substrate is characterized in that, may further comprise the steps:
(1) chooses substrate and crystalline orientation: adopt LiGaO 2Substrate, the crystalline orientation of selection are (001) crystal face;
(2) substrate is carried out anneal: with substrate behind 900-1000 ℃ of following high bake 3-5h air cooling to room temperature;
(3) substrate being carried out cleaning surfaces handles;
(4) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN impact plies, processing condition are: underlayer temperature is 300-350 ℃, and chamber pressure is 4-5 * 10 -5Pa, V/III ratio are 0.5-0.7ML/s for 35-50, the speed of growth;
(5) adopt low temperature molecular beam epitaxy technology growing nonpolar a face InN epitaxial film, processing condition are: underlayer temperature rises to 500-550 ℃, and chamber pressure is 3-5 * 10 -5Pa, V/III ratio are 0.7-0.9ML/s for 30-40, the speed of growth.
4. the LiGaO that is grown in according to claim 3 2The preparation method of the nonpolar InN film on the substrate is characterized in that, the thickness of said nonpolar a face InN impact plies is 50-100nm.
5. the LiGaO that is grown in according to claim 3 2The preparation method of the nonpolar InN film on the substrate is characterized in that, step (3) is said carries out the cleaning surfaces processing to substrate, is specially: with LiGaO 2Substrate was put under the deionized water room temperature ultrasonic cleaning 5-10 minute, removed LiGaO 2Substrate surface pickup particle more successively through persalt, acetone, washing with alcohol, is removed surface organic matter; LiGaO after the cleaning 2Substrate dries up with high-purity drying nitrogen; Afterwards with LiGaO 2Substrate is put into the low temperature molecular beam epitaxy growth room, under UHV condition, underlayer temperature is risen to 850-900 ℃, high bake 20-30 minute, removes lining LiGaO 2The impurity that basal surface is remaining.
6. the LiGaO that is grown in according to claim 5 2The preparation method of the nonpolar InN film on the substrate is characterized in that, said UHV condition is that pressure is less than 6 * 10 -7Pa.
CN2012100568519A 2012-03-06 2012-03-06 Nonpolar InN film growing on LiGao2 substrate and preparation method of nonpolar InN film Pending CN102560675A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103334088A (en) * 2013-07-17 2013-10-02 辽宁太阳能研究应用有限公司 Method for low-temperature deposition of InN film on glass substrate
CN103996756A (en) * 2014-05-30 2014-08-20 广州市众拓光电科技有限公司 Film coating method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
G. SHIKATA 等: "Improvement of the surface morphology of a–plane InN using low-temperature InN buffer layers", 《PHY. STAT. SOL. (C)》 *
GUOQIANG LI 等: "Epitaxial growth of high quality nonpolar InN films on LiGaO2 substrates", 《CRYSTAL GROWTH & DESIGN》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103334088A (en) * 2013-07-17 2013-10-02 辽宁太阳能研究应用有限公司 Method for low-temperature deposition of InN film on glass substrate
CN103334088B (en) * 2013-07-17 2016-02-24 辽宁太阳能研究应用有限公司 The method of low temperature depositing InN film on a glass substrate
CN103996756A (en) * 2014-05-30 2014-08-20 广州市众拓光电科技有限公司 Film coating method and application thereof
CN103996756B (en) * 2014-05-30 2017-01-18 广州市众拓光电科技有限公司 Film coating method and application thereof

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Application publication date: 20120711