CN102560675A - Nonpolar InN Thin Film Grown on LiGaO2 Substrate and Its Preparation Method - Google Patents
Nonpolar InN Thin Film Grown on LiGaO2 Substrate and Its Preparation Method Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910010936 LiGaO2 Inorganic materials 0.000 title claims abstract description 8
- 239000010409 thin film Substances 0.000 title claims abstract 9
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
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- 229910001218 Gallium arsenide Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
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- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 description 1
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- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
本发明公开了生长在LiGaO2衬底上的非极性InN薄膜，包括生长在LiGaO2衬底上的非极性a面InN缓冲层及生长在非极性a面InN缓冲层上的非极性a面InN层；所述非极性a面InN缓冲层是在衬底温度为300-350℃时生长的InN膜层；所述非极性a面InN层是在衬底温度为500-550℃时生长的InN膜层。本发明还公开了上述非极性a面InN薄膜的制备方法。与现有技术相比，本发明具有生长工艺简单，制备成本低廉的优点，消除了InN材料分解温度与反应活性之间的矛盾问题，且制备的非极性InN薄膜缺陷密度低、结晶质量好。
The invention discloses a nonpolar InN thin film grown on a LiGaO2 substrate, including a nonpolar a-plane InN buffer layer grown on a LiGaO2 substrate and a nonpolar InN buffer layer grown on a nonpolar a-plane InN buffer layer. The non-polar a-plane InN layer; the non-polar a-plane InN buffer layer is an InN film layer grown when the substrate temperature is 300-350°C; the non-polar a-plane InN layer is grown at a substrate temperature of 500- InN film layer grown at 550°C. The invention also discloses a preparation method of the above-mentioned nonpolar a-plane InN thin film. Compared with the prior art, the present invention has the advantages of simple growth process and low preparation cost, and eliminates the contradiction between the decomposition temperature and reactivity of InN materials, and the prepared non-polar InN thin film has low defect density and good crystal quality .
Description
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)
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Cited By (2)
| 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 |
-
2012
- 2012-03-06 CN CN2012100568519A patent/CN102560675A/en active Pending
Non-Patent Citations (2)
| 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)
| 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 |