CN101603172A - The method of a kind of growing AIN or AlGaN film - Google Patents
The method of a kind of growing AIN or AlGaN film Download PDFInfo
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- CN101603172A CN101603172A CNA2008101145981A CN200810114598A CN101603172A CN 101603172 A CN101603172 A CN 101603172A CN A2008101145981 A CNA2008101145981 A CN A2008101145981A CN 200810114598 A CN200810114598 A CN 200810114598A CN 101603172 A CN101603172 A CN 101603172A
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Abstract
The invention provides the method for a kind of growing AIN or AlGaN film, is to feed an amount of TMIn improves AlN and AlGaN film as promoting agent crystal mass and surface finish when adopting conventional growing AIN of mocvd method or AlGaN.Usually adopt hydrogen as carrier gas, TMGa, TMAl and NH
3As Ga source, Al source and N source, TMIn and other raw materials feed reaction chamber together simultaneously, grow at 1050-1200 ℃ respectively, and wherein the flow of TMIn is generally 40-400sccm.Characterize the surfaceness of sample and adopt X-ray diffraction three brilliant rocking curve peak width at half heights to characterize the crystal mass of sample by the atomic power microscopic method, as can be seen, adopt the AlN of the inventive method gained to compare with the sample of prior art growth with the AlGaN sample, surfaceness obviously descends, and crystal mass improves.
Description
Technical field
The present invention relates to metal organic chemical vapor deposition (MOCVD) technical field, the preparation method of particularly a kind of AlN and high Al component AlGaN film.
Background technology
III group-III nitride semiconductor ternary alloy AlGaN material is because its band gap is adjustable continuously between can be from 3.42eV to 6.2eV, can be widely used in that short wavelength deep (UV) is luminous, among detection and the white-light illuminating LEDs.The ultraviolet detection technology is the another dual-use detecting technique that grows up after infrared and laser acquisition technology.The blind deep ultraviolet detector of sunlight can effectively detect the airbound target that discharges a large amount of uv-radiations in those wake flames or the plumage flame, for example guided missile, jet plane etc.In flight course, inevitably can discharge a large amount of uv-radiations in wake flame or the plumage flame, this just provides a kind of extremely effectively means for the detection of guided missile, opportunity of combat.Specifically can be applied in aspects such as the ultraviolet guidance of guided missile and ultraviolet alarm.Aspect civilian, the supervision that ultraviolet detector can be used for fire and combustion processes and detection relevant etc. with biochemistry.The LEDs of the near ultraviolet of emission wavelength between 200-365nm, ultraviolet, deep ultraviolet wave band has very big application prospect in high-density optical data storage, water and air purification and sterilization and white-light illuminating field.High-quality AlN and high Al component Al
xGa
1-xThe N material is the critical material among deep ultraviolet detector and the LEDs.AlN be widely used in the substrate template layer, and AlGaN is important active area materials because of its greater band gap.High-quality Al
xGa
1-xThe N material is the key that realizes deep-UV light-emitting and improve deep ultraviolet detector detection performance.Compare the Al of hetero epitaxy AlN and high Al component on Sapphire Substrate with GaN
xGa
1-xThe N monocrystalline is more harsh to the requirement of growth conditions.Because the sticking coefficient of Al atomic ratio Ga atom is big, surface transport is lower, and the transverse growth speed of AlN is slow, causes accurate two-dimensional layer growth pattern to be difficult to form, and is difficult to obtain slick surface.This just requires AlN growth for Thin Film temperature greater than 1200 ℃, and for the MOCVD equipment that adopts the heater strip heating of three districts, this is a limit growth temperature.And, aluminium source trimethyl aluminium (TMAl) and nitrogenous source ammonia (NH
3) between have the intensive pre-reaction, the solid affixture that pre-reaction forms can be deposited on the growth surface of sample and can not fully decompose, and causes that magazine mixes in the epitaxial film, causes the polycrystalline growth of epitaxial film.These reasons cause the surface irregularity of AlN or AlGaN epitaxial film and exist up to 10
10Cm
-2Dislocation desity.Therefore, improve extension AlN and high Al component Al
xGa
1-xN crystal mass and surface topography are one of focuses of research.
Improve the crystal mass and the surface finish of AlGaN film as the low temperature high temperature composite buffering layer method of Chinese patent application 200610019545.2 report, but the process of growth of this method is comparatively complicated, comparatively harsh to the conditional request of buffer layer.
Summary of the invention
The object of the present invention is to provide a kind of simple surface topography that improves AlN and high Al component AlGaN and improve the method for crystal mass,, improve the surface finish of film with the dislocation desity in effective reduction epitaxial film.
Technical scheme of the present invention is as follows:
The method of a kind of growing AIN or AlGaN film feeds trimethyl indium (TMIn) as promoting agent when using metal organic chemical vapor deposition (MOCVD) method in 1050-1200 ℃ of growing AIN or AlGaN film.
In the aforesaid method, AlN and AlGaN film generally are epitaxys on Sapphire Substrate, adopt high-purity hydrogen (H
2) as carrier gas, trimethyl-gallium (TMGa), trimethyl aluminium (TMAl) and ammonia (NH
3) respectively as Ga source, Al source and N source, TMGa, TMAl, TMIn and NH
3Feed reaction chamber simultaneously, wherein the flow of TMIn is generally 40-400sccm, is preferably 150-300sccm.
Aforesaid method in AlN or AlGaN growth for Thin Film process, usually control pressure between 20-200torr, preferred 50-100torr; V/III is preferably 50-1000 between 40-2000.
For the quality of high AlN and AlGaN epitaxial film further is provided, can with hydrogen carrier gas, 1050 ℃-1200 ℃ of temperature, pressure 100-200torr, under the condition of V/III 400-800, the AlN layer in 50-150 cycle of growth is as buffer layer earlier on Sapphire Substrate to adopt the pulse mode that alternately feeds trimethyl aluminium (TMAl) and NH3, and specifically each cycle feeds 3-10s TMAl successively, the 3-10s carrier gas, 3-10s NH
3With the 3-10s carrier gas.Preferred 1100 ℃-1200 ℃ of the growth temperature of this pulse AlN buffer layer, the preferred 150-200torr of pressure, the preferred 400-600 of V/III.
The present invention is by feeding an amount of TMIn improves AlN and AlGaN film as promoting agent crystal mass and surface finish when conventional growing AIN and the AlGaN.TMIn has been widely used in the GaN material as promoting agent, not only can improve the characteristics of luminescence of hetero epitaxy GaN layer, but also can improve surface topography.In experimental technique of the present invention, growth temperature is 1050-1200 ℃, is higher than the decomposition temperature of InN, so In does not participate in forming component in AlN or AlGaN, only play the effect of promoting agent.
Characterize the surfaceness of sample by atomic power micro-(AFM) method, adopt X-ray diffraction (XRD) three brilliant rocking curve peak width at half heights to characterize the crystal mass of sample, as can be seen, adopt the AlN of this special methods gained to compare with the sample of usual conditions growth with the AlGaN sample, surfaceness obviously descends, and crystal mass improves.
Description of drawings
To be embodiment 1 containing TMIn atmosphere and do not containing XRD (002) face 2 θ-ω scanning result comparison diagram of the AlN that is grown in the TMIn atmosphere Fig. 1.
Fig. 2 a has shown that embodiment 1 contains the AFM surface topography of the AlN that grows in the TMIn atmosphere;
Fig. 2 b has shown the AFM surface topography of the AlN that embodiment 1 does not grow in containing TMIn atmosphere.
Fig. 3 a has shown that embodiment 2 contains the AFM surface topography of the AlN that grows in the TMIn atmosphere;
Fig. 3 b has shown the AFM surface topography of the AlN that embodiment 2 does not grow in containing TMIn atmosphere.
The AlGaN that Fig. 4 embodiment 3 grows in containing TMIn atmosphere and do not containing XRD (002) the face peak width at half height comparison diagram of the AlGaN that grows in the TMIn atmosphere.
Fig. 5 a is XRD (102) the face rocking curve figure of the AlGaN that grows in containing TMIn atmosphere of embodiment 4;
Fig. 5 b is that embodiment 4 is not at the XRD that contains the AlGaN that grows under the TMIn atmosphere (102) face rocking curve figure.
Embodiment
Also further specify the present invention in conjunction with the accompanying drawings below by embodiment, but the scope that does not limit the present invention in any way.
Prepare the AlN film according to following steps:
1) reaction chamber temperature is elevated to 1060 ℃, sapphire (0001) substrate is toasted 15min under nitrogen atmosphere;
2) be warming up to 1200 ℃, the flow set of TMIn is 180sccm, and pressure 50torr, V/III are 400, with the 600nm AlN film of growing on Sapphire Substrate of the speed of growth of 400nm per hour.
Prepare the AlN film according to following steps:
1) reaction chamber temperature is elevated to 1060 ℃, sapphire (001) substrate is toasted 15min under nitrogen atmosphere;
2) be warming up to 1200 ℃, adopt the pulse atom-layer-epitaxial method on Sapphire Substrate with the AlN buffer layer in 100 cycles of growth of 200nm per hour, thickness is 100nm, growth conditions is: pressure 150torr, V/III is 600, and each cycle feeds 5s TMAl, 3s hydrogen, 5s NH successively
3, 3s hydrogen;
3) keep temperature-resistant, in step 2) the basis on, the flow set of TMIn is 180sccm, adopts TMAl, TMIn and NH
3Feed the method for reaction chamber simultaneously, with the growth AlN film of 400nm per hour, thickness is 600nm, and concrete growth conditions is: pressure 50torr, V/III are 400.
Adopt the AFM of the AlN sample of this special methods gained AlN sample and common growth to show that pattern relatively sees Fig. 3 a and Fig. 3 b.As can be seen from Figure, (Fig. 3 surfaceness (rms=1.67nm) a) will be starkly lower than not and to contain the AlN sample (Fig. 3 b) of growing under the TMIn atmosphere (rms=36.58nm) the present embodiment AlN film of growing.
Prepare the AlGaN film according to following steps:
1) reaction chamber temperature is elevated to 1060 ℃, sapphire (0001) substrate is toasted 15min under nitrogen atmosphere;
2) reaction chamber temperature is elevated to 1200 ℃, with speed of growth direct growth 320nm AlN film on Sapphire Substrate of 1.4 μ m per hour,, growth conditions is: pressure 50torr, V/III are 400;
3) in step 2) the basis on, keep temperature-resistant, 10 cycle AlN/Al grow
xGa
1-xThe N superlattice, wherein, the thickness at trap and base all is 5nm in the superlattice, and Al component x is controlled at 0.8, and in this process of growth, pressure is 75torr, and V/III is 600;
4) keep growth temperature constant, on the basis of step 3), the flow set of TMIn is 240sccm, adopts TMAl, TMGa, TMIn and NH
3Feed the method for reaction chamber simultaneously, with the growth Al of 1 μ m per hour
0.6Ga
0.4N film, thickness are 1 μ m, and growth conditions is: pressure 75torr, V/III are 1000.
Adopt the AlGaN sample of this special methods gained AlGaN sample and common growth to compare, crystal mass improves greatly.Characterize the variation of crystal mass by the peak width at half height of XRD (002) face rocking curve relatively, as shown in Figure 4, as can be seen, the Al that present embodiment is grown
0.6Ga
0.4The peak width at half height of the XRD of N film (002) face rocking curve is than not containing the Al that obtains under the TMIn atmosphere
0.6Ga
0.4The N film is little, this means the Al that adopts the inventive method growth
xGa
1-xThe N crystal mass is far better.
Prepare the AlGaN film according to following steps:
1) reaction chamber temperature is elevated to 1060 ℃, sapphire (0001) substrate is toasted 15min under nitrogen atmosphere,
2) reaction chamber temperature is elevated to 1200 ℃, adopt the pulse atom-layer-epitaxial method on Sapphire Substrate with the AlN buffer layer in 100 cycles of growth of 200nm per hour, thickness is 100nm, growth conditions is: pressure 150torr, V/III is 600, and each cycle feeds 5s TMAl, 3s hydrogen, 5s NH successively
3, 3s hydrogen;
3) keep temperature-resistant, with speed of growth direct growth 320nm AlN film on Sapphire Substrate of 1.4 μ m per hour, growth conditions is: pressure 50torr, V/III are 400;
4) on the basis of step 3), keep temperature-resistant, 10 cycle AlN/Al grow
xGa
1-xThe N superlattice, wherein, the thickness at trap and base all is 5nm in the superlattice, and Al component x is controlled at 0.8, and in this process of growth, pressure is 75torr, and V/III is 600;
5) keep growth temperature constant, on the basis of step 4), the flow set of TMIn is 240sccm, adopts TMAl, TMGa, TMIn and NH3 to feed the method for reaction chamber simultaneously, with the growth Al of 1 μ m per hour
0.6Ga
0.4N film, thickness are 1 μ m, and growth conditions is: pressure 75torr, V/III are 1000.
Adopt the AlGaN sample of this special methods gained AlGaN sample and common growth to compare, crystal mass improves greatly.Characterize the variation of crystal mass by XRD (102) face rocking curve peak width at half height relatively, shown in Fig. 5 a and Fig. 5 b, as can be seen, the Al that present embodiment is grown
0.6Ga
0.4(peak width at half height of Fig. 5 XRD (102) face rocking curve a) is 968arcsec to the N film, than not containing the Al that grows under the TMIn atmosphere
0.6Ga
0.4The peak width at half height 1200arcsec of N film (Fig. 5 b) is little, this means to adopt Al of the present invention
xGa
1-xThe N crystal mass will be good many.
Claims (9)
1. the method for growing AIN or AlGaN film feeds trimethyl indium as promoting agent in 1050-1200 ℃ during with mocvd method growing AIN or AlGaN film.
2. the method for claim 1 is characterized in that: carry out epitaxy on Sapphire Substrate, adopt hydrogen as carrier gas, trimethyl-gallium, trimethyl aluminium and NH
3Respectively as Ga source, Al source and N source.
3. method as claimed in claim 2 is characterized in that: trimethyl indium and other raw materials feed reaction chamber together simultaneously.
4. method as claimed in claim 3 is characterized in that: the flow of trimethyl indium is 40-400sccm.
5. method as claimed in claim 4 is characterized in that: the flow of trimethyl indium is 150-300sccm.
6. method as claimed in claim 2 is characterized in that: in AlN or AlGaN growth for Thin Film process, control pressure is 20-200torr, and V/III is 40-2000.
7. method as claimed in claim 6 is characterized in that: control pressure is 50-100torr in the process of growth, and V/III is 50-1000.
8. method as claimed in claim 2 is characterized in that: before epitaxy AlN or AlGaN film, be carrier gas with hydrogen, 1050 ℃-1200 ℃ of temperature, pressure 100-200torr under the condition of V/III 400-800, adopts alternately to feed trimethyl aluminium and NH
3Pulse mode earlier the AlN layer in 50-150 cycle of growth is as buffer layer on Sapphire Substrate, specifically each cycle feeds the 3-10s trimethyl aluminium successively, 3-10s carrier gas, 3-10s NH
3With the 3-10s carrier gas.
9. method as claimed in claim 8 is characterized in that: the growth temperature of AlN buffer layer is 1100 ℃-1200 ℃, and pressure is 150-200torr, and V/III is 400-600.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903615A (en) * | 2012-10-18 | 2013-01-30 | 中山大学 | Preparation method of p type GaN and AlGaN semiconductor material |
| CN103695999A (en) * | 2013-12-02 | 2014-04-02 | 中国电子科技集团公司第五十五研究所 | Nitride single crystal membrane prepared by alternate source supply and method |
| CN103710747A (en) * | 2013-12-02 | 2014-04-09 | 中国电子科技集团公司第五十五研究所 | N source intermittent transportation prepared nitride single-crystal film and method |
| CN105543969A (en) * | 2016-01-25 | 2016-05-04 | 南通同方半导体有限公司 | Growth method for improving quality of AlN thin film crystal |
| TWI577842B (en) * | 2016-05-30 | 2017-04-11 | 光鋐科技股份有限公司 | Growth method of aluminum gallium nitride |
| CN111690907A (en) * | 2019-03-15 | 2020-09-22 | 马鞍山杰生半导体有限公司 | Aluminum nitride film and preparation method and application thereof |
| CN113548648A (en) * | 2020-04-23 | 2021-10-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aluminum nitride nanoparticles and method for preparing same |
-
2008
- 2008-06-10 CN CNA2008101145981A patent/CN101603172A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903615A (en) * | 2012-10-18 | 2013-01-30 | 中山大学 | Preparation method of p type GaN and AlGaN semiconductor material |
| CN102903615B (en) * | 2012-10-18 | 2018-02-06 | 中山大学 | P-type GaN and AlGaN semiconductor material a kind of preparation method |
| CN103695999A (en) * | 2013-12-02 | 2014-04-02 | 中国电子科技集团公司第五十五研究所 | Nitride single crystal membrane prepared by alternate source supply and method |
| CN103710747A (en) * | 2013-12-02 | 2014-04-09 | 中国电子科技集团公司第五十五研究所 | N source intermittent transportation prepared nitride single-crystal film and method |
| CN103695999B (en) * | 2013-12-02 | 2016-04-27 | 中国电子科技集团公司第五十五研究所 | Nitride single crystal film prepared by a kind of alternately supply source and method |
| CN103710747B (en) * | 2013-12-02 | 2016-06-08 | 中国电子科技集团公司第五十五研究所 | Nitride single crystal film and method are prepared in the conveying of a kind of interval, N source |
| CN105543969A (en) * | 2016-01-25 | 2016-05-04 | 南通同方半导体有限公司 | Growth method for improving quality of AlN thin film crystal |
| CN105543969B (en) * | 2016-01-25 | 2018-05-01 | 南通同方半导体有限公司 | A kind of growing method of improvement AlN film crystal quality |
| TWI577842B (en) * | 2016-05-30 | 2017-04-11 | 光鋐科技股份有限公司 | Growth method of aluminum gallium nitride |
| CN111690907A (en) * | 2019-03-15 | 2020-09-22 | 马鞍山杰生半导体有限公司 | Aluminum nitride film and preparation method and application thereof |
| CN113548648A (en) * | 2020-04-23 | 2021-10-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aluminum nitride nanoparticles and method for preparing same |
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Open date: 20091216 |