CN101270471A - Method for growing nonpolar face GaN thin-film material and uses thereof - Google Patents
Method for growing nonpolar face GaN thin-film material and uses thereof Download PDFInfo
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- CN101270471A CN101270471A CNA2008100988646A CN200810098864A CN101270471A CN 101270471 A CN101270471 A CN 101270471A CN A2008100988646 A CNA2008100988646 A CN A2008100988646A CN 200810098864 A CN200810098864 A CN 200810098864A CN 101270471 A CN101270471 A CN 101270471A
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Abstract
The invention relates to a growing control method for nonpolor surface GaN film material. Growing in a MOCVD system, the R surface sapphire of [1120] is selected as underlay material; firstly, material heat treatment under the temperature of 900 to 1100 DEG C is carried out on the growing R surface sapphire in the MOCVD system for 5 to 60 minutes; or then alkaline air is pumped in to be treated by surface ammoniation under the temperature of 900 to 1100 DEG C for 10 to 120 minutes, then pumped into H2 and/or N2 as carrier gas in the temperature range of 900 to 1100 DEG C; the alkaline air and metal organic gallium source are taken as growing gas source; the growing nonpolor surface of GaN material of a surface or a m surface is composed on the sapphire underlay of a certain crystal surface of the selected underlay through controlling the carrier gas, the gas flow of the growing air source and the growing temperature parameters.
Description
Technical field
The present invention relates to a kind of method of using metal organic-matter chemical vapour phase epitaxy (MOCVD) growing technology by substrate crystal face selection method control growing non-polar GaN, especially utilize the method for MOCVD technology growing nonpolar face GaN thin-film material on R surface sapphire substrate material.The nonpolar GaN film material of this method growth can be used for fields such as photodiode, laser apparatus, solar cell.Thereon according to the different different epitaxial structures of device application growth, as photodiode, laser apparatus, solar cell etc.The present invention can control the growth of nonpolar a face GaN material effectively, can improve the quantum yield and the luminous efficiency of device.
Background technology
Although gallium nitride base light-emitting device has been obtained very big success, their luminous efficiency, especially at ultraviolet and green light band, also not fully up to expectations.
[1]A major reason that influences its luminous efficiency is that there is spontaneous polarization in gan along conventional growth direction (i.e. [0001] direction), if at this graphic memory at shear stress, on [0001] direction, also have the piezoelectric polarization effect so.
[2]Gan hexagonal wurtzite structure and coordinate are selected as shown in Figure 1.Polarization field makes gallium nitride material inside produce powerful built in field, and has caused the highdensity two-dimensional electron gas in interface.Although this effect can be used to some electron device, High Electron Mobility Transistor (HEMT) for example, however its performance for light emitting semiconductor device is disadvantageous.
[3,4,5]Because common light emitting diode is to be active layer with the multiple quantum well structure, as Fig. 2 (a) with (b).Therefore the polarizing effect of the direction of growth is brought two disadvantageous effects at least.At first built in field has weakened the overlapping degree of electron hole spatial wave function,
[6]Make that the electron-hole recombination time is elongated,
[7]Cause low quantum yield thus; Secondly polarized electric field causes band curvature, and effective energy gap of multiple quantum well diminishes, therefore luminous wave band generation red shift, this just so-called quantum limit stark effect.
In addition, polarized electric field also brings a serious problem: along with the increase of injecting electric current, bigger blue shift also can take place in the luminous peak position of diode.
[8]
One of scheme that solves is a growth cubic structure nitride heterojunction.
[9,10]But owing to lack suitable substrate and the thermodynamic (al) metastable state character of cubic lattice structure self, though, have little effect therefore through long-time effort.
[11,12]On the other hand, theoretical investigation shows that the wurtzite gan is not have spontaneous polarization in vertical [0001] symmetry axis direction (for example [1 100], [1120] direction).If do not have shear stress simultaneously in growth plane, the piezoelectric polarization effect on these directions will not exist yet so, as shown in Figure 3.
Because being with of quantum well structures is flat rubber belting, therefore, the influence of built in field will not exist, and making efficient LED for us has great advantage.People such as Walterei adopt MBE first at LiAlO
2(100) extension obtains m face GaN/AlGaN multi-quantum pit structure on the substrate, and has verified that the quantum yield of edge [1100] direction quantum well is significantly improved.
[13]Recently, people such as Aran Chakraborty has realized nonpolar InGaN/GaN LED first on m face GaN self-supporting substrate.Meanwhile, people such as C.Q.Chen has realized on the r surface sapphire based on the visible light of InGaN/GaNMQW with based on the nonpolar LED of GaN/AlGaN MQW UV-light a face.
[14,15]The applicant seminar has also successfully obtained LiAlO
2(100) growth a face, M face GaN thin-film material and GaN/InGaN LED device on the substrate.
[16,17]At present, be in the starting stage about the material of nonpolar III group-III nitride and the research Buddhist monk of device, its performance with at c face α-Al
2O
3And the device for preparing is compared a certain distance is still arranged on the SiC substrate.Because the development of technology must make the growth conditions of epitaxial material be different from the growth in conventional substrate, the semiconductor material crystal mass is still needed and will further be improved, and research work remains further to be carried out in a deep going way.
Reference
[1]T.Deguchi，K.Sekiguchi，A.Nakamura，T.Sota，R.Matsuol，S.Chichibu，and S.Nakamura，Jpn.J.Appl.Phys.，Part 2 38，L914(1999)
[2]F.Bernardini，V.Fiorentini，and D.Vanderbilt，Phys.Rev.B 56，10024(R)(1997)
[3]A.Bykhovski，B.Gelmont，and M.Shur，J.Appl.Phys.74，6734(1993).
[4]S.Kaiser，M.Jakob，J.Zweck，W.Gebhardt，O.Ambacher，R.Dimitrov，A.T.Schremer，J.A.Smart，and J.R.Shealy，J.Vac.Sci.Tech.B 18，733(2000).
[5]S.Arulkumaran，T.Egawa，H.Ishikawa，and T.Jimbo，J.Vac.Sci.Tech.B 21，888(2003)
[6]N.Grandjean，B.Damilano，S.Dalmasso，M.Leroux，M.La··ugt，and J.Massies，J.Appl.Phys.86，3714(1999)
[7]R.Langer，J.Simon，V.Ortiz，N.T.Pelekanos，A.Barski，R.Andr e，and M.Godlewski，Appl.Phys.Lett.74，3827(1999)
[8]H.C.Ca sey et al.Appl.Phys.Lett.68：2867(1996)
[9]S.F.Chichibu，M.Sugiyama，T.Kuroda，A.Tackeuchi，T.Kitamura，H.Nakanishi，T.Sota，S.P.DenBaars，S.Nakamura，Y.Ishida，and H.Okumura，Appl.Phys.Lett.79，3600(2001).
[10]S.F.Chichibu，M.Sugiyama，T.Onuma，T.Kitamura，H.Nakanishi，T.Kuroda，A.Tackeuchi，T.Sota，Y.Ishida，and H.Okumura，Appl.Phys.Lett.79，4319(2001)
[11]O.Brandt，in Group III Nitride Semiconductor Compounds：Physical andApplications，edited by B.Gil(Oxford Univ.Press，New York，1998).
[12]Z.H.Feng，H.Yang，X.H.Zheng，Y.Fu，Y.P.Sun，X.M.Shen，and Y.T.Wang，Appl.Phys.Lett.82，206(2003)
[13]P.Waltereit，O.Brandt，A.Trampert，H.T.Grahn，J.Menniger，M.Ramsteiner，M.Reiche，and K.H.Ploog，Nature 406，865(2000)
[14]Ashay Chitnis，Changqing Chen，Vinod Adivarahan，Maxim Shatalov，Edmundas Kuokstis，Vasavi Mandavilli，Jinwei Yang，and M.Asif Khan，Appl.Phys.Lett.84，3663(2004).
[15]C.Q.Chen，V.Adivarahan，J.W.Yang，E.Kuokstis，and M.A.Khan，Jpn.J.Appl.Phys.，Part 2 42，L1039(2003).
[16] thank and rely on oneself; Zhang Rong; Liu Chengxiang etc., ZL200510094184.3, the control growing method of a kind of a face and m face GaN thin-film material
[17] thank and rely on oneself; Zhang Rong; Liu Chengxiang etc., ZL 200510094747.9, a kind of growth method of m face InGaN/GaN quantum well LED device architecture
The present invention relates to a kind of metal organic-matter chemical vapour phase epitaxy (MOCVD) growing technology of using by the method for substrate crystal face selection method control growing nonpolar GaN, especially utilize the method for MOCVD technology growing nonpolar face GaN thin-film material on R surface sapphire substrate material. The nonpolar GaN film material of the method growth can be used for the fields such as light emitting diode, laser instrument, solar cell. Thereon according to the different different epitaxial structures of device application growth, such as light emitting diode, laser instrument, solar cell etc. The present invention can control the growth of nonpolar a face GaN material effectively, can improve quantum efficiency and the luminous efficiency of device.
Summary of the invention
The present invention seeks to: utilize the MOCVD growing technology, control the technology of synthetically grown nonpolar GaN film material by the system of selection of substrate crystal face.Select for use the R surface sapphire of [1120] to do substrate material, handle substrate material, adopt low pressure by direct high temperature and desalination, low 53 than growth technique direct on substrate the growing GaN thin-film material.Acquisition has the nonpolar GaN film material of surface of good pattern and crystalline structure.
The object of the invention also is: by the system of selection control of substrate crystal face, adopt direct high temperature and nitriding treatment substrate material and low pressure, growth techniques such as low V/III ratio are growing nonpolar face GaN thin-film material on Sapphire Substrate directly.The nonpolar GaN film material of growth can be used for fields such as photodiode, laser apparatus, solar cell.Thereon according to the different different epitaxial structures of device application growth, as photodiode, laser apparatus, solar cell etc.The present invention can control the growth of GaN materials such as nonpolar a face effectively, can improve the quantum yield and the luminous efficiency of device.
Technical solution of the present invention: the control growing method of nonpolar face GaN thin-film material, in the MOCVD system, pass through to select the substrate of substrate crystal face, select the R surface sapphire of [1120] to do substrate material, at first, in the MOCVD system R surface sapphire substrate of growth is carried out material heat treatment under 900-1100 ℃ of temperature, the time is 5-60 minute; Probable back feeding ammonia carries out surfaces nitrided, is 10-120 minute 900-1100 ℃ of following time of temperature; Feed H 900-1100 ℃ of temperature range again
2And/or N
2As carrier gas, ammonia and metal organic gallium source as the growth source of the gas; By the control carrier gas, growth source of the gas gas flow and growth temperature parameter, a face or the m face GaN material of synthetically grown non-polar plane on the Sapphire Substrate of the substrate crystal face of selecting.
By the control carrier gas, parameters such as gallium source gas flow and growth temperature, the GaN material of synthetically grown non-polar plane on the Sapphire Substrate of the substrate crystal face of selecting.
The present invention also can feed carrier gas H
2, N
2Or H
2With N
2Mixed gas carries out material heat treatment to the R surface sapphire substrate under 900-1100 ℃ of temperature.
4, growing nonpolar face GaN thin-film material is used to the different epitaxial structure of growing, and uses on photodiode, laser apparatus, solar cell.
Mechanism of the present invention is: utilize MOCVD growing technology synthetically grown nonpolar GaN film material on the substrate through selecting crystal face.In the MOCVD system, select for use the R surface sapphire of [1120] to do substrate material, handle substrate material by direct high temperature and desalination, adopt low pressure, low 53 is more direct at growing GaN thin-film material on the substrate than growth technique: the Sapphire Substrate through selecting crystal face is fed carrier gas H under 900-1100 ℃ of temperature
2, N
2Or H
2And N
2Mixed gas carries out material heat treatment, then or feed ammonia and carry out surfaces nitridedly, feeds carrier gas in certain 500-1100 ℃ of temperature range again, ammonia and metal organic source, by control carrier gas, parameters such as source gas flow and growth temperature, synthetically grown nonpolar face GaN material.Detection through product shows that synthetically grown has gone out the GaN thin-film material of nonpolar a face on the R surface sapphire substrate.The GaN film of a face is at LED, and opto-electronic device aspects such as laser apparatus have better application and are worth, and film thickness can be controlled.
Key of the present invention is: select the employing of the Sapphire Substrate of crystal face, and the thermal anneal process before the substrate growth is very important.Certainly, the control of the temperature of thermal annealing temperature and growth material also is key of the present invention.
The invention has the beneficial effects as follows: the nonpolar GaN film material that has obtained to have surface of good pattern and crystalline structure.Technical matters of the present invention belongs to first on the material growing technology.The nonpolar GaN film material of growth can be used for fields such as photodiode, laser apparatus, solar cell.Thereon according to the different different epitaxial structures of device application growth, as photodiode, laser apparatus, solar cell etc.The present invention can control the growth of GaN materials such as nonpolar a face effectively, can improve the quantum yield and the luminous efficiency of device.
Description of drawings
Fig. 1 is that gan hexagonal wurtzite structure and coordinate are selected synoptic diagram.As can be seen from the figure, C axle GaN material is the hexagonal wurtzite structure.And be quadrilateral structure in the R face, M face.
Fig. 2 is the polarizing effect of c axle gan and being with of causing thereof.The C axle is because the existence of polarizing effect causes polarized electric field in material.And cause band curvature thus.2 (a) are the axial polarizing effects of c among the figure, and 2 (b) are the curves of the band curvature that causes of polarization.
Fig. 3 is the quantum well polarized electric field distribution of m face GaN Quito and can be with synoptic diagram.Avoided the polarizing effect that exists in the C shaft material in the M flooring, energy band structure also becomes parallel.
Fig. 4 has gone out the XRD scanning spectrum of the GaN thin-film material of nonpolar a face for the present invention's synthetically grown on the R surface sapphire substrate.Diffraction peak among the figure derives from GaN's (11-20) face, (1-102) of R surface sapphire substrate, (2-204) diffraction of face respectively.Do not observe (0002) or the diffraction peak of other faces of C face, this shows that the epitaxial material that we obtain is single-orientated A face (11-20) GaN.
Fig. 5 is the scanning electronic microscope (SEM) and atomic force microscope (AFM) the surface topography photo of the present invention's nonpolar a face GaN thin-film material that synthetically grown goes out on the R surface sapphire substrate.As seen from the figure, optimize the nonpolar a face GaN film surfacing that technology grows by the present invention, the AFM surface topography is at 5*5um
2The RMS=7.6nm of scope.And occurred with conventional jewel substrate on the different defective pattern of c face GaN thin-film material of growing.
Fig. 6 is the Raman spectrum of the nonpolar a face GaN thin-film material that synthetically grown goes out on the R surface sapphire substrate.X (y, y)-x configuration down, the A1 of GaN (TO) mould and E2 high frequency mould lay respectively at 532.5cm
-1And 569.9cm
-1X (z, y)-x configuration down, GaN has only E1 (TO) mould to occur, and is positioned at 567.5cm
-1X (z, z)-x configuration down, GaN A1 (TO) mould occurred being positioned at and has occurred, and is positioned at 532.5cm
-1In addition, the peak width at half height of E2 high frequency mould is 6.2cm
-1, showing that crystal strain inhomogeneous broadening effect is not obvious, sample quality is higher.Calculating in-plane stress is σ yy=-19Gpa, σ zz=18.6Gpa.
Embodiment
The present invention utilizes MOCVD growing technology nonpolar a face GaN thin-film material of synthetically grown on the R face substrate through selecting crystal face.Specifically comprise following a few step:
1) select the sapphire wafer of unconventional crystal orientation a face (11-20), R face (1-102) or M face (11-20) etc. to make substrate material, this experimental selection R surface sapphire is made substrate.
2) the unconventional crystal face sapphire of selecting with process in the MOCVD system is done the GaN material of substrate growing nonpolar, in the MOCVD system Sapphire Substrate through selecting crystal face is fed carrier gas H under 900-1100 ℃ of temperature
2, N
2Or H
2And N
2Mixed gas carries out 5-60 minute material heat treatment, then or feed ammonia and carry out 10-60 minute surfaces nitrided.
3) feed carrier gas in certain 500-1100 ℃ of temperature range again, ammonia and metal organic source are by control carrier gas, parameters such as source gas flow and growth temperature, synthetically grown nonpolar face GaN material.Growth time determines according to required film thickness.
4) the metal organic gallium source is that trimethyl-gallium stream is 1-50sccm.Carrier gas flux is 2-8slm.The ammonia flow that is added directly to substrate is 1-15slm.NH
3Flow is 3-8slm, and growth temperature is 900-1100 ℃.Time is 10-60 minute.
5) carrier band gas, H
2Or N
2Or H
2And N
2Mixed gas is as diluent gas, NH
3Gas is as nitrogenous source.H
2Or N
2Or H
2And N
2Air-fuel mixture enleanment airshed 2500-3500sccm; NH
3Gas 200-700sccm, especially 500-700sccm, the conversion zone temperature also can be 500-1100 ℃, growth time is can obtain A face GaN film completely under the condition of 8-20min.V/III refers to the mol ratio of N and Ga than being 200-3000.
Wherein, the sapphire wafer of unconventional crystal orientation a face (11-20), R face (1-102) or M face (11-20) etc. is done the employing of substrate material, and to the thermal anneal process before the substrate growth, the temperature control of control of thermal annealing temperature and growth material is key of the present invention.Fig. 1-Fig. 3 of the present invention has provided the performance that sample of the present invention reached.The present invention also relates to the control growing method of nonpolar GaN film materials such as a face or m face.
The optimization growth conditions scope of the present invention growing nonpolar a face G a N on the sapphire wafer substrate of a face (11-20) is shown in Table 1.
The optimization growth conditions scope of table 1. growing nonpolar a face G a N on the sapphire wafer substrate of a face (11-20)
| Grown layer | Growth temperature (℃ | Pressure (Torr | The V/III ratio | Material |
| Nucleating layer | 900-1100 | 0-500 | -- | Unconventional crystal orientation Sapphire Substrate |
| Or it is surfaces nitrided | 900-1100 | 0-500 | NH 3 | Unconventional crystal orientation Sapphire Substrate |
| Grown layer | 500-1100 | 0-500 | 200-300 | Non-polar GaN |
Nucleating layer or surfaces nitrided all adopting and 900-1100 ℃, the non-polar GaN grown layer can be selected 900-1100 ℃ for use at 500-1100 ℃; The non-polar GaN grown layer also can be chosen in 600-700 ℃, and this also is one of characteristics of the present invention.
Claims (5)
1, the control growing method of nonpolar face GaN thin-film material, in the MOCVD system, grow, it is characterized in that doing substrate material by the R surface sapphire of selecting [1120], at first, in the MOCVD system R surface sapphire substrate of growth is carried out material heat treatment under 900-1100 ℃ of temperature, the time is 5-60 minute; Probable back feeding ammonia carries out surfaces nitrided, is 10-120 minute 900-1100 ℃ of following time of temperature; Feed H 900-1100 ℃ of temperature range again
2And/or N
2As carrier gas, ammonia and metal organic gallium source as the growth source of the gas; By the control carrier gas, growth source of the gas gas flow and growth temperature parameter, a face or the m face GaN material of synthetically grown non-polar plane on the Sapphire Substrate of the substrate crystal face of selecting.
2, the control growing method of nonpolar face GaN thin-film material according to claim 1 is characterized in that feeding carrier gas H
2, N
2Or H
2With N
2Mixed gas carries out material heat treatment to the R surface sapphire substrate under 900-1100 ℃ of temperature.
3, the control growing method of nonpolar face GaN thin-film material according to claim 1 is characterized in that the metal organic gallium source is a trimethyl-gallium, and flow is 1-50sccm, and the time is 10-60 minute, NH
3Gas 200-700sccm, V/III is than being 200-3000, the i.e. mol ratio of N and Ga.
4, the control growing method of nonpolar face GaN thin-film material according to claim 1 is characterized in that the non-polar GaN grown layer is chosen in 600-700 ℃ or 900-1100 ℃ of temperature, and this also is one of characteristics of the present invention.
5, growing nonpolar face GaN thin-film material is used to the different epitaxial structure of growing, and uses on photodiode, laser apparatus, solar cell.
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