CN1219334C - γ－LiAlO2/α－Al2O3Flexible substrate material and preparation method thereof - Google Patents
γ－LiAlO2/α－Al2O3Flexible substrate material and preparation method thereof Download PDFInfo
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- CN1219334C CN1219334C CNB031419038A CN03141903A CN1219334C CN 1219334 C CN1219334 C CN 1219334C CN B031419038 A CNB031419038 A CN B031419038A CN 03141903 A CN03141903 A CN 03141903A CN 1219334 C CN1219334 C CN 1219334C
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- flexible substrate
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- 239000000758 substrate Substances 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910010092 LiAlO2 Inorganic materials 0.000 title 1
- 229910010093 LiAlO Inorganic materials 0.000 claims abstract description 42
- 238000004549 pulsed laser deposition Methods 0.000 claims abstract description 30
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 3
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003746 solid phase reaction Methods 0.000 claims description 9
- 230000005284 excitation Effects 0.000 claims description 6
- 230000003760 hair shine Effects 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000012876 topography Methods 0.000 claims 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract 6
- 229910018068 Li 2 O Inorganic materials 0.000 abstract 4
- 229910052594 sapphire Inorganic materials 0.000 abstract 1
- 239000010980 sapphire Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007648 laser printing Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
一种适合于GaN外延生长的γ-LiAlO2/α-Al2O3柔性衬底材料及其制备方法，该柔性衬底材料是在白宝石α-Al2O3上设有一层四方相的铝酸锂γ-LiAlO2构成。该柔性衬底材料的制备方法是：先将清洗的α-Al2O3衬底送入脉冲激光淀积(PLD)系统，在富锂的环境气氛下淀积Li2O薄膜，然后将上步骤中得到的Li2O/α-Al2O3样品放入退火炉中，在富锂的反应气氛下，Li2O与α-Al2O3在高温下发生固相反应得到γ-LiAlO2覆盖层，通过控制退火时间得到具有不同厚度的γ-LiAlO2覆盖层，再利用去离子水溶解清洗掉未反应的Li2O，从而得到γ-LiAlO2/α-Al2O3柔性衬底。
A γ-LiAlO 2 /α-Al 2 O 3 flexible substrate material suitable for GaN epitaxial growth and a preparation method thereof, wherein the flexible substrate material is composed of a layer of tetragonal lithium aluminate γ-LiAlO 2 arranged on white sapphire α-Al 2 O 3. The preparation method of the flexible substrate material is as follows: firstly, a cleaned α-Al 2 O 3 substrate is sent into a pulsed laser deposition (PLD) system, a Li 2 O film is deposited in a lithium-rich environment atmosphere, then the Li 2 O/α-Al 2 O 3 sample obtained in the above step is put into an annealing furnace, in a lithium-rich reaction atmosphere, Li 2 O and α-Al 2 O 3 react at high temperature to obtain a γ-LiAlO 2 covering layer, γ-LiAlO 2 covering layers with different thicknesses are obtained by controlling the annealing time, and then unreacted Li 2 O is dissolved and washed away by deionized water, thereby obtaining a γ-LiAlO 2 /α-Al 2 O 3 flexible substrate.
Description
Technical field
The present invention relates to a kind of γ-LiAlO
2/ α-Al
2O
3Flexible substrate material and preparation method.γ-LiAlO
2/ α-Al
2O
3Flexible substrate material is mainly as the epitaxial growth of InN-GaN base blue-light semiconductor.
Background technology
The broad-band gap III-V group iii v compound semiconductor material that with GaN is representative is receiving increasing concern, they will be at blue, green light LED (LEDs) and laser diode (LDs), high density information read-write, subsurface communication, deep quest, laser printing, biology and engineering in medicine, and ultrahigh speed microelectronic component and hyperfrequency microwave device aspect are with a wide range of applications.
Because GaN fusing point height, hardness is big, saturated vapor pressure is high, so want the GaN body monocrystalline of growing large-size to need high temperature and high pressure, Polish high pressure research center has made just under the high pressure of 1600 ℃ high temperature and 20kbar that bar is wide to be the GaN body monocrystalline of 5mm.Current, the technology of GaN body monocrystalline of growing large-size more immature, and growth is with high costs, from practical application quite long distance is arranged still.
White gem crystal (α-Al
2O
3), be easy to preparation, low price, and have the good characteristics such as high-temperature stability, α-Al
2O
3It is at present the most frequently used InN-GaN base epitaxial substrate material (referring to Jpn.J.Appl.Phys., the 36th volume,, the 1568th page in 1997).
Lithium aluminate (γ-LiAlO
2) be the InN-GaN base epitaxial substrate material that just came into one's own in recent years, because the lattice mismatch of itself and GaN epitaxial film is quite little, have only 1.4%, this makes it be expected to become a kind of quite desirable GaN epitaxial substrate material (referring to U.S. Pat P6218280, Kryliouk Olga, Anderson Tim, Chai Bruce, " Method and apparatus forproducing group-III nitrides ").
Above-mentioned formerly technology substrate (α-Al
2O
3Or γ-LiAlO
2) the remarkable shortcoming that exists is: (1) is with α-Al
2O
3Make substrate, α-Al
2O
3And the lattice mismatch between the GaN makes the GaN film of preparation have higher dislocation density and a large amount of point defects up to 13.8%; (2) because LiAlO
2The non-stoichiometric volatilization easily takes place under the melt high temperature, and crystal growth difficulty is difficult to obtain large scale, high-quality LiAlO
2Monocrystal, and the process of substrate has caused a large amount of raw-material wastes.
Summary of the invention
The objective of the invention is: utilize Li
2O and α-Al
2O
3Solid phase reaction preparation have LiAlO
2Tectal α-Al
2O
3Flexible substrate γ-LiAlO
2/ α-Al
2O
3, be used for the high-quality GaN of epitaxial growth.
The epitaxial growth of GaN is mainly at α-Al at present
2O
3Carry out on the foreign substrate.Yet α-Al
2O
3And have bigger lattice mismatch and thermal mismatching between the GaN, cause producing in the GaN epitaxial film higher dislocation density and a large amount of point defects.In order to reduce the dislocation density in the GaN epitaxial film, a kind of so-called flexible substrate technology is arisen at the historic moment.Flexible substrate is to propose according to distribution and the equilibrium relation of elastic strain energy between " substrate " and epitaxial loayer.Concerning the infinite thickness substrate, carry out heteroepitaxy under mismatch condition, there is a critical value in the thickness of epitaxial loayer, when the thickness of epitaxial loayer during less than critical value, lattice mismatch in the system is mainly by the epitaxial loayer elastic strain, and storage elasticity can compensate in epitaxial loayer.When epitaxy layer thickness during greater than critical value, the lattice mismatch in the system then can cause the generation of epitaxial loayer Dislocations.If the thickness of substrate is limited, then the critical thickness of epitaxial loayer can increase.So-called " flexible substrate " be very little " substrate " of thickness just, and this thickness is more little, and the critical thickness of epitaxial loayer is big more.If substrate is very thin, then owing to the effect of " image force ", even dislocation has taken place in the system, dislocation also mainly is distributed in " substrate ".Recently, the LiAlO of Tetragonal
2(be γ-LiAlO
2) obtained widely research, γ-LiAlO as the epitaxial substrate of GaN
2With the lattice mismatch of GaN epitaxial film littler (1.4%), well below α-Al
2O
3With the lattice mismatch (13.8%) of GaN epitaxial film, this so that it be expected to become and be better than α-Al
2O
3The GaN epitaxial substrate.Based on above consideration, in key of the present invention be: utilize pulsed laser deposition (PLD:pulsed laser deposition) technology and Li
2O and α-Al
2O
3Between solid phase reaction, at α-Al
2O
3Generate γ-LiAlO on the substrate
2Cover layer, the recycling deionized water dissolving washes unreacted Li
2O, thus γ-LiAlO obtained
2/ α-Al
2O
3Flexible substrate.Here, α-Al
2O
3Both participate in solid phase reaction as reactant, worked again the γ-LiAlO that supports on it
2The effect of thin layer.Flexible substrate (γ-the LiAlO of this kind structure
2/ α-Al
2O
3) be suitable for the epitaxial growth of high-quality GaN.
The present invention mainly comprises two steps: at first be α-Al
2O
3Li on the substrate
2The O thin film technology is α-Al then
2O
3γ-LiAlO on the substrate
2Tectal preparation.
Fig. 1 is the schematic diagram of pulsed laser deposition (PLD) system.The mechanism of PLD method be at first with KrF excimer laser (excitation wavelength the is 248nm) scioptics of pulsewidth 25-30ns (nanosecond) with about 10J/cm
2Energy density optically focused, the Li in optical window shines device
2The O target, behind the target absorbing laser, owing to Electron Excitation becomes high temperature fused state, material surface tens nanometer (nm) is evaporated, gasiform particulate is released and is diffused with column, from the opposed suitable heated α-Al of the surperficial number centimeters of target
2O
3Adhere on the substrate, thereby the accumulation deposit becomes Li
2The O film.
Pulsed laser deposition of the present invention (PLD) technology prepares flexible substrate material γ-LiAlO
2/ α-Al
2O
3The concrete technology flow process as follows:
Earlier with the α-Al that cleans
2O
3Substrate is sent into pulsed laser deposition (PLD) system, at a-Al
2O
3Prepare Li on the substrate
2The O film, the high-purity Li more than 99.999% is adopted in the Li source
2The O target.System adopts the KrF excimer laser of pulsewidth 25-30ns (nanosecond), and excitation wavelength is 248nm, and scioptics are with about 10J/cm
2Energy density optically focused, the Li in optical window shines device
2The O target, deposit Li under the ambiance of rich lithium
2The O film.Then with the Li that obtains in the upper step
2O/ α-Al
2O
3Sample is put into annealing furnace, and annealing about 1100 ℃ is in order to suppress Li
2The reaction atmosphere of rich lithium, Li are still adopted in the volatilization of O
2O and α-Al
2O
3Obtained γ-LiAlO in the lower solid phase reaction that takes place of high temperature (about 1100 ℃)
2Cover layer obtains having the γ-LiAlO of different-thickness by the control annealing time
2Cover layer, the recycling deionized water dissolving washes unreacted Li
2O, thus γ-LiAlO obtained
2/ α-Al
2O
3Flexible substrate.The flexible substrate of this kind structure is suitable for epitaxial growth of high quality GaN.
Technical characterstic of the present invention is:
1, adopt pulsed laser deposition (PLD) technology to prepare Li
2The O film.Li
2The fusing point height of O (greater than 1700 ℃), pulsed laser deposition (PLD) technology can be evaporated materials with high melting point.Because the energy height of laser beam is concentrated, power density is enough big, and the speed of heat temperature raising is fast, can in the extremely short time, the state of aggregation of target material be changed rapidly, thereby obtain very high evaporation rate, the growth rate of film is very fast, and thickness also is easy to accurate control.Pulsed laser deposition (PLD) technology adopts contactless heating, is difficult for introducing impurity in preparation process.In addition, the ambiance flexibility and changeability of pulsed laser deposition (PLD) system, initialization system is or vacuum or inert atmosphere or active atmosphere as required, this has just in time satisfied the requirement that needs in this patent adopt the ambiance of rich lithium.
2, preparing Li with pulsed laser deposition (PLD) technology
2During the O film, in order to suppress Li
2The volatilization of O, the pulsed laser deposition system adopts the ambiance of rich lithium; At follow-up Li
2O and α-Al
2O
3Between high-temperature annealing process solid phase reaction process in, in order to suppress Li
2The reaction atmosphere of rich lithium is still adopted in the volatilization of O.
3, at γ-LiAlO
2/ α-Al
2O
3In the structure of flexible substrate, α-Al
2O
3Both participate in solid phase reaction as reactant, worked again the γ-LiAlO that supports on it
2The effect of thin layer.The flexible substrate of this kind structure is suitable for epitaxial growth of high quality GaN.
Description of drawings
Fig. 1 is the schematic diagram of pulsed laser deposition (PLD) system.
Among the figure: 1-KrF excimer laser (excitation wavelength is 248nm), 2-target, 3-substrate.
Embodiment
Prepare γ-LiAlO with above-mentioned pulsed laser deposition (PLD) experimental provision and concrete technological process
2/ α-Al
2O
3Flexible substrate material.
Earlier with the α-Al that cleans
2O
3Substrate is sent into pulsed laser deposition (PLD) system, at α-Al
2O
3Prepare Li on the substrate
2The O film, the high-purity Li more than 99.999% is adopted in the Li source
2The O target.System adopts the KrF excimer laser of pulsewidth 25-30ns (nanosecond), and excitation wavelength is 248nm, and scioptics are with about 10J/cm
2Energy density optically focused, the Li in optical window shines device
2The O target, deposit Li under the ambiance of rich lithium
2The O film.Then with the Li that obtains in the upper step
2O/ α-Al
2O
3Sample is put into annealing furnace, and annealing about 1100 ℃ is in order to suppress Li
2The reaction atmosphere of rich lithium, Li are still adopted in the volatilization of O
2O and α-Al
2O
3Obtained γ-LiAlO in the lower solid phase reaction that takes place of high temperature (about 1100 ℃)
2Cover layer obtains having the γ-LiAlO of different-thickness by the control annealing time
2Cover layer, the recycling deionized water dissolving washes unreacted Li
2O, thus γ-LiAlO obtained
2/ α-Al
2O
3Flexible substrate.
Claims (4)
1, a kind of epitaxially grown γ-LiAlO of GaN that is suitable for
2/ α-Al
2O
3Flexible substrate material is characterized in that at white stone α-Al
2O
3Be provided with the lithium aluminate γ-LiAlO of one deck Tetragonal
2, consist of γ-LiAlO
2/ α-Al
2O
3Flexible substrate.
2, the described γ-LiAlO of claim 1
2/ α-Al
2O
3The preparation method of flexible substrate material is characterized in that earlier with the α-Al that cleans
2O
3Substrate is sent into the pulsed laser deposition system, at α-Al
2O
3Prepare Li on the substrate
2The O film, the high-purity Li more than 99.999% is adopted in the Li source
2The O target, system adopts the KrF excimer laser of pulsewidth 25-30ns, and excitation wavelength is 248nm, and scioptics are with about 10J/cm
2Energy density optically focused, the Li in optical window shines device
2The O target, deposit Li under the ambiance of rich lithium
2The O film is then with the Li that obtains in the upper step
2O/ α-Al
2O
3Sample is put into annealing furnace, and annealing about 1100 ℃ is in order to suppress Li
2The reaction atmosphere of rich lithium, Li are still adopted in the volatilization of O
2O and α-Al
2O
3Solid phase reaction at high temperature takes place obtained γ-LiAlO
2Cover layer obtains having the γ-LiAlO of different-thickness by the control annealing time
2Cover layer through cleaning, thereby has obtained γ-LiAlO
2/ α-Al
2O
3Flexible substrate.
3, γ-LiAlO according to claim 2
2/ α-Al
2O
3Flexible substrate material preparation method is characterized in that Li
2O and α-Al
2O
3In 1100 ℃ of lower solid phase reactions that take place of high temperature, the reaction time is 10-20 minute, obtains single (100) spinelle γ-LiAlO orientation, that have the island surface topography this moment
2Cover layer.
4, γ-LiAlO according to claim 2
2/ α-Al
2O
3Flexible substrate material preparation method is characterized in that utilizing deionized water dissolving to fall unreacted Li
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031419038A CN1219334C (en) | 2003-07-29 | 2003-07-29 | γ－LiAlO2/α－Al2O3Flexible substrate material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031419038A CN1219334C (en) | 2003-07-29 | 2003-07-29 | γ－LiAlO2/α－Al2O3Flexible substrate material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1482688A CN1482688A (en) | 2004-03-17 |
| CN1219334C true CN1219334C (en) | 2005-09-14 |
Family
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|---|---|---|---|
| CNB031419038A Expired - Fee Related CN1219334C (en) | 2003-07-29 | 2003-07-29 | γ－LiAlO2/α－Al2O3Flexible substrate material and preparation method thereof |
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|---|---|
| CN (1) | CN1219334C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100373548C (en) * | 2006-06-13 | 2008-03-05 | 中国科学院上海光学精密机械研究所 | Method for growing non-polar GaN thick film on lithium aluminate wafer |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322176C (en) * | 2004-09-28 | 2007-06-20 | 中国科学院上海光学精密机械研究所 | Having gamma-LiAlO2Method for preparing single crystal film covering layer substrate |
| CN1322175C (en) * | 2004-09-28 | 2007-06-20 | 中国科学院上海光学精密机械研究所 | Preparation of gamma-LiAlO by pulsed laser deposition2Method for covering substrate with single crystal thin film |
| CN100378255C (en) * | 2005-09-01 | 2008-04-02 | 南京大学 | A controlled growth method of a-plane and m-plane GaN thin film materials |
| CN100457630C (en) * | 2006-12-18 | 2009-02-04 | 天津理工大学 | Prepn process of lithium aluminate substrate material |
| CN101330117B (en) * | 2007-06-18 | 2012-04-18 | 周明奇 | Method for preparing illuminating device using zinc oxide |
-
2003
- 2003-07-29 CN CNB031419038A patent/CN1219334C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100373548C (en) * | 2006-06-13 | 2008-03-05 | 中国科学院上海光学精密机械研究所 | Method for growing non-polar GaN thick film on lithium aluminate wafer |
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|---|---|
| CN1482688A (en) | 2004-03-17 |
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