CN100464393C - A manufacture method for GaN insulation or semi-insulation epitaxy layer - Google Patents
A manufacture method for GaN insulation or semi-insulation epitaxy layer Download PDFInfo
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- CN100464393C CN100464393C CNB2007100521672A CN200710052167A CN100464393C CN 100464393 C CN100464393 C CN 100464393C CN B2007100521672 A CNB2007100521672 A CN B2007100521672A CN 200710052167 A CN200710052167 A CN 200710052167A CN 100464393 C CN100464393 C CN 100464393C
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Abstract
The provided preparation method for high-quality GaN insulation or semi-insulation epitaxial layer comprises: selecting Al2O3, SiC or Si as the substrate to nitrogenize at high-temperature; in turns, growing the AlN nucleation layer at 750-780Deg, 3D growing GaN nucleation layer at 720-730Deg, 2D growing GaN epitaxial layer at 750-780Deg, and doping Fe, Cr or Mg; then, using AlGaN/GaN superlattice or multi-cycle intermittent atomic-layer pulse deposition method to grow GaN transient layer, and growing the final product on high III/V ratio condition at 720-730Deg. This invention can be used to microwave device.
Description
Technical field
The present invention relates to the preparation method of a kind of GaN insulation or semi-insulation epitaxy layer.
Background technology
Gallium nitride (GaN) is the third generation semiconductor after Si, GaAs, has broad stopband (3.5eV), high disruptive field intensity (3 * 10
6V/cm), high electronics saturation drift velocity (3 * 10
7Cm/s), high heat conductance.In addition, the GaN material is very hard, and stable chemical property is arranged, and is high temperature resistant, corrosion-resistant, and thermal conductivity is good, has good radioresistance characteristic and excellent hot operation characteristic.That this makes GaN become to work under adverse circumstances is high-power, at a high speed, the good base material of high frequency (microwave), high-temperature electronic device.But the growth of insulation GaN material has individual difficult point, and GaN material back of the body bottom electron is dense usually, is difficult to directly obtain insulation or semi-insulated GaN epitaxial loayer.As power device, GaN insulated substrate performance does not with great difficulty cause puncture voltage reduction, high frequency electric leakage, causes component failure.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-performance, high quality GaN insulation or semi-insulation epitaxy layer, the preparation method that the present invention adopts is the in-situ doped method of molecular beam epitaxy, can reach with the GaN insulation of this method preparation or the performance parameter of semi-insulation epitaxy layer: carrier concentration≤1 * 10
14Cm
-2, halfwidth≤0.15 of X-ray diffraction (002) face swing curve °, 5 μ m * 5 mu m range inner surface evenness≤0.3nm.
The technical scheme that realizes the object of the invention is the preparation method of a kind of GaN insulation or semi-insulation epitaxy layer, promptly adopts the in-situ doped method of molecular beam epitaxy, and its concrete steps are as follows:
(1) in the reaction growth room, with Al
2O
3, SiC or Si be substrate, under 800～850 ℃ of temperature substrate carried out high-temperature ammonolysis 10～30 minutes;
(2) in the AlN of 750～780 ℃ of following high growth temperature 10～20nm resilient coating.
(3) in the three-dimensional GaN nucleating layer of 720～730 ℃ of following low-temperature epitaxy 20～40nm;
(4) in the two-dimentional GaN epitaxial loayer of 750～780 ℃ of following high growth temperature 100～150nm;
Implement in-situ doped metal Fe, Cr or Mg when (5) continuing epitaxial growth GaN, growing coarse relatively, thickness is the GaN insulating barrier of 0.5～2 μ m;
(6) grown behind the GaN insulating barrier, preparation AlGaN/GaN superlattice structure or employing batch type atomic layer sedimentation growing GaN transition zone on this GaN insulating barrier, then at 720～730 ℃, high III/V than growing high-crystal quality, ganoid GaN epitaxial loayer under the condition, its thickness is no more than 1 μ m.
Wherein, the AlN resilient coating adopts the atomic layer deposition method growth.Can reduce the lattice parameter mismatch ratio between substrate and the GaN like this, improve the crystal mass of GaN epitaxial loayer.And the growth of AlN resilient coating is the monoatomic layer Al polarity of modulation of growing earlier on the substrate behind the high-temperature ammonolysis, and N, Al alternately enter reaction growth room growing AIN resilient coating then.
Above-mentioned used batch type atomic layer sedimentation or atomic layer deposition method be Ga or Al source metal and N source respectively with pulse mode, successively enter the reaction growth room and grow GaN layer or AlN layer.
And in the method for implementing to adopt when in-situ doped local δ doping and/or undoped spacer and/or mixing continuously.Preferred in-situ doped metal Fe, Cr or Mg implement to circulate at interval in-situ doped under 500～730 ℃ circulating temperature state, mix when temperature is reduced to 500～600 ℃ of scopes, and temperature then stops when rising to 600～730 ℃ of scopes mixing, and circulation is carried out.
And, in preparation process, behind 720～730 ℃ of following growing three-dimensional GaN nucleating layers, carry out the transition to 750～780 ℃ of two-dimentional GaN epitaxial loayers of growth down gradually.
As shown from the above technical solution, the present invention at substrate behind high-temperature ammonolysis, high growth temperature AlN nucleating layer successively, the three-dimensional GaN nucleating layer of low-temperature epitaxy, high growth temperature two dimension GaN epitaxial loayer when continuing epitaxial growth GaN, is implemented original position transition metal (Fe and Cr) and is mixed again, the preparation high dislocation density, coarse relatively GaN insulation epitaxial loayer.On this GaN insulating barrier, prepare the AlGaN/GaN superlattice structure then or adopt batch type atomic layer sedimentation growing GaN transition zone.At last, at high III/V than two-dimensional growth low-dislocation-density, ganoid GaN epitaxial loayer under the condition.And with this GaN insulation or semi-insulation epitaxy layer is substrate, the microwave device structure of can growing.
The atomic layer deposition method of in said process, using, be that Ga or Al source metal and N source are respectively with pulse mode, successively enter the reaction growth room and grow GaN layer or AlN layer, can strengthen of the migration of III family metallic atom like this at growing surface, with find the energy minimum point before the N atom combines, thereby help the two-dimensional growth of film, effectively improve the crystal mass of each layer material, can also both reduce simultaneously the stress of GaN insulation epitaxial loayer, stop the dislocation extension again.
After tested, can reach with the GaN insulation of the inventive method preparation or the performance parameter of semi-insulation epitaxy layer: carrier concentration≤1 * 10
14Cm
-2, the halfwidth (FWHM)≤0.15 of XRD (002) swing curve °, high-quality GaN insulation or the semi-insulation epitaxy layer of 5 μ m * 5 mu m range inner surface evenness (RMS)≤0.3nm.
Description of drawings
Fig. 1 is with the GaN insulation of the inventive method preparation or the schematic diagram of semi-insulation epitaxy layer.
Fig. 2 is the atomic force microscope picture of the GaN insulating barrier of in-situ doped Fe metallic element acquisition.
Fig. 3 has grown to adopt the transition of AlGaN/GaN superlattice again, the atomic force microscope picture of the high quality GaN epitaxial loayer of growth behind the GaN insulating barrier.
Fig. 4 is cross section transmission electron microscope (TEM) picture of the high-crystal quality insulation GaN epitaxial loayer of the inventive method preparation.
Fig. 5 is cross section high-resolution-ration transmission electric-lens (HRTEM) picture of the high-crystal quality insulation GaN epitaxial loayer of the inventive method preparation.
Embodiment
Select two inches Al
2O
3, SiC or Si be as substrate, substrate is 810 ℃ of cleanings 10 minutes down before growth.Substrate is placed the reaction growth room, high-temperature ammonolysis is 10～30 minutes under arbitrary temperature of substrate in 800～850 ℃ of temperature ranges, present embodiment is specially 810 ℃, the AlN of high growth temperature 10～20nm under arbitrary temperature in 750～780 ℃ of temperature ranges (Al/N〉1) resilient coating then, present embodiment is the 10nm AlN resilient coating of having grown under 765 ℃, the three-dimensional GaN nucleating layer of low-temperature epitaxy 20～40nm under arbitrary temperature in 720～730 ℃ of temperature ranges again, present embodiment is the GaN nucleating layer of 20nm of having grown under 720 ℃, then temperature is elevated to gradually the two-dimentional GaN epitaxial loayer of high growth temperature 100～150nm under the arbitrary temperature in 750～780 ℃ of temperature ranges, present embodiment is the two-dimentional GaN epitaxial loayer that is elevated to 760 ℃ of 100nm that grown gradually.Implement in-situ doped metal Fe, Cr or Mg (present embodiment is example with Fe) when then continuing epitaxial growth GaN, grow coarse relatively, thickness and be the GaN insulating barrier (referring to Fig. 2) of 0.5～2 μ m (embodiment grown 1 μ m), in the method for implementing to adopt when in-situ doped local δ doping and/or undoped spacer and/or mixing continuously.Be to carry out continuous in-situ at 550 ℃ to mix in the present embodiment.By experiment, also can carry out under 500～730 ℃ circulating temperature state and circulate at interval in-situ dopedly, mix when temperature is reduced to 500～600 ℃ of scopes, temperature then stops when rising to 600～730 ℃ of scopes mixing, and circulation is carried out.Grown behind the GaN insulating barrier, on this GaN insulating barrier preparation AlGaN/GaN superlattice structure or adopt the batch type atomic layer sedimentation grow the GaN transition zone, extend to epitaxial loayer (embodiment has adopted the AlGaN/GaN superlattice structure) with the threading dislocation that stops and reduce in the insulating barrier.At last, than growing high-crystal quality, ganoid GaN epitaxial loayer (referring to Fig. 3, RMS=0.2nm, prior art is generally about 0.3nm) under the condition, its thickness is no more than 1 μ m at 720～730 ℃, high III/V.Adopt the prepared GaN insulation of the present invention or the schematic diagram of semi-insulation epitaxy layer to see Fig. 1, among Fig. 1 from bottom to up each layer be respectively substrate 7, AlN resilient coating 6, the three-dimensional GaN nucleating layer 5 of low-temperature epitaxy, the two-dimentional GaN epitaxial loayer 4 of high growth temperature, GaN insulating barrier 3, AlGaN/GaN superlattice 2, high-crystal quality, ganoid GaN epitaxial loayer 1.Fig. 4, Fig. 5 are respectively the cross section transmission electron microscope (TEM) and high-resolution-ration transmission electric-lens (HRTEM) pictures of the high-crystal quality insulation GaN epitaxial loayer of the inventive method preparation, and picture shows with preparation method of the present invention can obtain high-crystal quality, ganoid GaN insulation or semi-insulation epitaxy layer.
Claims (7)
1. the preparation method of GaN insulation or semi-insulation epitaxy layer, it is characterized in that: adopt the in-situ doped method preparation of molecular beam epitaxy, concrete steps are as follows:
(1) in the reaction growth room, with Al
2O
3, SiC or Si be substrate, under 800～850 ℃ of temperature substrate carried out high-temperature ammonolysis 10～30 minutes;
(2) in the AlN of 750～780 ℃ of following high growth temperature 10～20nm resilient coating;
(3) in the three-dimensional GaN nucleating layer of 720～730 ℃ of following low-temperature epitaxy 20～40nm;
(4) in the two-dimentional GaN epitaxial loayer of 750～780 ℃ of following high growth temperature 100～150nm;
Implement in-situ doped metal Fe, Cr or Mg when (5) continuing epitaxial growth GaN, growing coarse relatively, thickness is the GaN insulating barrier of 0.5～2 μ m;
(6) grown behind the GaN insulating barrier, preparation AlGaN/GaN superlattice structure or employing batch type atomic layer sedimentation growing GaN transition zone on this GaN insulating barrier, then at 720～730 ℃, high III/V than growing high-crystal quality, ganoid GaN epitaxial loayer under the condition, its thickness is no more than 1 μ m.
2. the preparation method of GaN insulation according to claim 1 or semi-insulation epitaxy layer is characterized in that: the AlN resilient coating adopts the atomic layer deposition method growth.
3. the preparation method of GaN insulation according to claim 2 or semi-insulation epitaxy layer, it is characterized in that: the growth of AlN resilient coating is the monoatomic layer A1 polarity of modulation of growing earlier on the substrate behind the high-temperature ammonolysis, and N, Al alternately enter reaction growth room growing AIN resilient coating then.
4. the preparation method of GaN insulation according to claim 1 and 2 or semi-insulation epitaxy layer, it is characterized in that: used batch type atomic layer sedimentation or atomic layer deposition method be Ga or Al source metal and N source respectively with pulse mode, successively enter the reaction growth room and grow GaN layer or AlN layer.
5. the preparation method of GaN insulation according to claim 1 or semi-insulation epitaxy layer is characterized in that: the method that adopts local δ doping and/or undoped spacer and/or mix continuously when enforcement is in-situ doped.
6. the preparation method of GaN insulation according to claim 5 or semi-insulation epitaxy layer, it is characterized in that: wherein in-situ doped metal Fe, Cr or Mg implement the interval to circulate in-situ doped under 500～730 ℃ circulating temperature state, when reducing to 500～600 ℃ of scopes, temperature mixes, temperature then stops when rising to 600～730 ℃ of scopes mixing, and circulation is carried out.
7. the preparation method of GaN insulation according to claim 1 or semi-insulation epitaxy layer is characterized in that: carry out the transition to 750～780 ℃ of two-dimentional GaN epitaxial loayers of growth down behind 720～730 ℃ of following growing three-dimensional GaN nucleating layers gradually.
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Cited By (2)
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| TWI575602B (en) * | 2013-09-23 | 2017-03-21 | 烏翠泰克股份有限公司 | Method and apparatus for forming device quality gallium nitride layers on silicon substrates |
| US9666432B2 (en) | 2013-07-02 | 2017-05-30 | Ultratech, Inc. | Method and apparatus for forming device quality gallium nitride layers on silicon substrates |
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| CN101515543B (en) * | 2008-02-20 | 2010-08-25 | 中国科学院半导体研究所 | Gallium nitride membrane structure grown on silicon substrate and growing method thereof |
| CN101807523A (en) * | 2010-03-17 | 2010-08-18 | 中国科学院半导体研究所 | Method for growing GaN film without crack on surface on large mismatch substrate |
| CN101924021B (en) * | 2010-07-02 | 2012-07-04 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Semiconductor device, as well as manufacture method and luminescent device thereof |
| JP2012199398A (en) * | 2011-03-22 | 2012-10-18 | Sumitomo Electric Ind Ltd | COMPOUND GaN SUBSTRATE, MANUFACTURING METHOD OF THE SAME, GROUP III NITRIDE SEMICONDUCTOR DEVICE AND MANUFACTURING METHOD OF THE SAME |
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Cited By (3)
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