CN102208339B - Silicon-carbide-base compound substrate and manufacturing method thereof - Google Patents
Silicon-carbide-base compound substrate and manufacturing method thereof Download PDFInfo
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Abstract
The invention provides a silicon-carbide-base compound substrate and a manufacturing method thereof. The silicon-carbide-base compound substrate comprises a silicon-carbide-base monocrystal substrate, a compound stress covariant layer which is covered on the silicon-carbide-base monocrystal substrate and formed by alternatively stacking a titanium nitride monocrystal thin film material and a multi-layer aluminum nitride monocrystal thin film material, and a gallium nitride template layer which grows on the compound stress covariant layer and consists of a gallium nitride monocrystal thin film material. The invention also provides a method for manufacturing the silicon-carbide-base compound substrate. By the invention, the crystal lattice mismatch of the silicon-carbide-base gallium nitride material is relieved, and the heat dismatch of the silicon-carbide-base gallium nitride material is solved; therefore, the performance and the qualification rate of the gallium nitride light emitting diode (LED) epitaxial sheet prepared on the silicon-carbide-base compound substrate are enhanced greatly; and the silicon-carbide-base compound substrate is suitable for application and market popularization.
Description
Technical field
The present invention relates to the substrate for the epitaxial growth of semiconductor material growth, more specifically, relate to a kind of silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material.
Background technology
Nitride-based semiconductor, especially gallium nitride (GaN) are that Application and preparation is in the core material of light-emitting diode (LED) device in semiconductor lighting and display backlight field.Owing to lacking the homoplasmon monocrystal material, the device application of GaN material is carried out in heterogeneous substrate usually, and relatively more commonly used have a sapphire (a-Al
2O
3), carborundum (6H-SiC), silicon (Si) etc.Along with the progress of recent domestic SiC monocrystal material technology of preparing, the price of SiC single crystal substrates reduces gradually, and this has created condition for the production cost that reduces preparation gallium nitride based LED epitaxial wafer material in the SiC substrate.But all there are larger difference in SiC substrate and GaN material in lattice constant and thermal coefficient of expansion, can run into thus the problem of two aspects: (1) lattice mismatch issue: because of the lattice constant (a=0.3189nm of GaN, c=0.5185nm) and the lattice constant (a=0.3073nm of 6H-SiC, c=1.0053nm) difference, 3.77% lattice mismatch caused at the GaN epitaxial loayer epitaxial growth initial stage can produce very large lattice mismatch stress, (several nm are thick to hundreds of nm when the thickness of the GaN epitaxial loayer of growth surpasses a certain critical thickness, specifically decide on the intermediate layer situation of introducing) after, this Macrolattice mismatch stress that accumulates in the GaN epitaxial loayer will be to discharge the performance that this will cause the deterioration of GaN epitaxial loayer crystalline quality and then reduce follow-up LED device architecture in the form that produces at the interface dislocation and defective; (2) thermal mismatch problem: because of thermal coefficient of expansion (a:5.59 * 10 of GaN
-6K) and the thermal coefficient of expansion of 6H-SiC (a:3.54 * 10
-6K) also there is larger difference, this causes GaN epitaxial loayer or LED device architecture can gather very large thermal stress from very high growth temperature (such as 800～1100 ℃) drops to the process of room temperature, and this thermal stress is a kind of tensile stress for the GaN epitaxial loayer and then easily causes the GaN epitaxial film materials to produce be full of cracks or crooked.Employing is gathered larger hot tensile stress and is had crackle or crooked GaN epitaxial film materials to prepare the LED device, certainly will affect the raising of LED device performance and yields.The common method that shifts at present and coordinate to discharge the mismatch stress of the GaN epitaxial film materials for preparing in the SiC substrate has: stress covariant layer (comprising resilient coating, flexible layer, insert layer etc.) and graph substrate.Existing stress covariant layer, such as low temperature GaN resilient coating, AlN resilient coating, AlGaN component-gradient buffer layer, thin InAlGaN flexible layer etc., although have better effects aspect transfer and the coordination release lattice mismatch stress, effect is limited aspect transfer and coordination releasing heat mismatch stress.And the graph substrate method need to be done mask and litho pattern (figure of nanometer or micro-meter scale) in SiC substrate or GaN epitaxial loayer, because being difficult to reduce, window place dislocation density needs repeatedly mask and litho pattern, complex process and further raised the material preparation cost, also be difficult to simultaneously obtain the uniform large scale GaN epitaxial film materials of crystalline quality, such as the GaN epitaxial film materials more than the 2 inches diameter.
Summary of the invention
The object of the invention is to for the lattice mismatch and thermal mismatch problem and the deficiencies in the prior art that prepare in carborundum (SiC) substrate in gallium nitride (GaN) the base LED epitaxial wafer material, a kind of silicon-carbide-base compound substrate for the preparation of gallium nitrate based (GaN) LED epitaxial wafer material is provided.
The invention provides a kind of silicon-carbide-base compound substrate, comprise: a single-crystal silicon carbide substrate; One combined stress covariant layer covers in the described single-crystal silicon carbide substrate, is replaced by nitride multilayer ti single crystal thin-film material and nitride multilayer aluminium monocrystal thin films material stackingly to consist of; One gallium nitride template layer is grown on the described combined stress covariant layer, is made of monocrystalline GaN film material.
The thickness of every layer of titanium nitride (TiN) monocrystal thin films material is 5～30nm in the combined stress covariant layer.
The thickness of every layer of aluminium nitride (AlN) monocrystal thin films material is not less than 3 times of every layer of titanium nitride (TiN) monocrystal thin films material thickness in the combined stress covariant layer.
Layer with the single-crystal silicon carbide substrate contact in combined stress covariant layer is titanium nitride monocrystal thin films material.
The layer that contacts with the gallium nitride template layer in combined stress covariant layer is the aluminum nitride single crystal film material.
The number of plies of titanium nitride monocrystal thin films material is 1～10 layer, and the number of plies of aluminum nitride single crystal film material is identical with the number of plies of titanium nitride monocrystal thin films material.
TiN monocrystal thin films material is used for transfer and thin aluminium nitride (AlN) layer and the lattice mismatch stress of uppermost gallium nitride (GaN) template layer and the effect of thermal stress of coordination on titanium nitride (TiN) layer, to reduce dislocation density and elimination crackle and crooked.The effect of AlN layer is the lattice mismatch stress for auxiliary titanium nitride (TiN) monocrystal thin films material transfer and the coordination suprabasil gallium nitride of carborundum (SiC) (GaN) material.
The thickness of gallium nitride (GaN) template layer is not less than 2 μ m, and the rate of temperature fall that drops to room temperature from 800～1100 ℃ growth temperature during growing gallium nitride (GaN) template layer is 5～20 ℃/minute.
Material growth technique for the preparation of gallium nitride (GaN) monocrystal thin films material in titanium nitride (TiN) monocrystal thin films in the combined stress covariant layer and aluminium nitride (AlN) monocrystal thin films material and gallium nitride (GaN) template layer includes but not limited to metal-organic chemical vapor deposition equipment (MOCVD), ion beam epitaxy (IBE), molecular beam epitaxy (MBE), pulsed laser deposition (PLD), plasma auxiliary chemical vapor deposition (PE-CVD) and magnetron sputtering deposition (MSD).
Silicon-carbide-base compound substrate can be used for the preparation growth of the nitride semiconductor single-crystal thin-film material such as gallium nitride (GaN), aluminium nitride (AlN), indium nitride (InN), aluminum gallium nitride (AlGaN), indium gallium nitrogen (InGaN), aluminium gallium nitrogen (InAlGaN) and nitride semiconductor LED device architecture.
The present invention also provides a kind of method of making silicon-carbide-base compound substrate, and this silicon-carbide-base compound substrate is characterized in that for the preparation of the nitride semiconductor epitaxial material, comprises:
Get a single-crystal silicon carbide substrate;
Form a combined stress covariant layer in the single-crystal silicon carbide substrate, combined stress covariant layer is replaced by aluminum nitride single crystal film material and titanium nitride monocrystal thin films material and stackingly consists of;
Form a gallium nitride template layer at combined stress covariant layer, the gallium nitride template layer is made of monocrystalline GaN film material.
The combined stress covariant layer that replaces stacking formation by nitride multilayer titanium (TiN) and aluminium nitride (AlN) monocrystal thin films material of the present invention can be alleviated the thermal stress that causes because of the lattice mismatch stress between substrate and the epitaxial loayer and thermal expansion coefficient difference.The present invention can improve performance and the yields of nitride semiconductor LED epitaxial wafer material on the silicon carbide substrate, is fit to use and marketing.
Description of drawings
Fig. 1 is the basic composite substrate structure schematic diagram of carborundum (SiC) for the preparation of nitride semiconductor LED epitaxial wafer material.
Embodiment
Elaborate preferred implementation of the present invention below in conjunction with accompanying drawing.
Fig. 1 is used for the basic composite substrate structure schematic diagram of carborundum (SiC) of gallium nitride (GaN) LED epitaxial wafer material preparation.As shown in the figure, the basic compound substrate 1 of carborundum (SiC) the combined stress covariant layer 12 and gallium nitride (GaN) the monocrystal thin films template layer 13 that comprise a carborundum (SiC) single crystal substrates 11 and set gradually from carborundum (SiC) single crystal substrates 11 sides.
Carborundum (SiC) single crystal substrates 11 plays a supportive role.
Combined stress covariant layer 12 covers on carborundum (SiC) single crystal substrates 11, and ultra-thin titanium nitride (TiN) monocrystal thin films material 121 and multilayer 15～90nm thick thin aluminium nitride (AlN) the monocrystal thin films material 122 thick by multilayer 5～30nm replace stacking formation.As shown in Figure 1, the layer that contacts with carborundum (SiC) single crystal substrates in the combined stress covariant layer 12 is preferably TiN layer 121, the lattice constant of the lattice constant of TiN layer and SiC is more approaching like this, and this can improve the effect of the alleviation lattice mismatch power of combined stress covariant layer 12.Yet the present invention is not limited to situation shown in Figure 1, and the subgrade with carborundum (SiC) substrate contact in the combined stress covariant layer also can be AlN.The thickness of each AlN layer is not less than 3 times of thickness of each TiN layer.Ultra-thin TiN layer 121 is used for shifting and coordinate to discharge lattice mismatch stress and the thermal stress between carborundum (SiC) substrate and gallium nitride (GaN) monocrystal thin films template layer 13 (will be described later) of growing on it.AlN layer 122 is used for assisting ultra-thin TiN layer 121 to shift and coordinate to discharge gallium nitride (GaN) monocrystal thin films template layer 13 (will be described later) of SiC substrate and growth on it at the lattice mismatch stress of epitaxial process generation.The preparation method of TiN layer 121 and AlN layer includes but not limited to metal-organic chemical vapor deposition equipment, ion beam epitaxy, molecular beam epitaxy, pulsed laser deposition, plasma auxiliary chemical vapor deposition and magnetron sputtering deposition.
Gallium nitride (GaN) monocrystal thin films template layer 13 covers on the combined stress covariant layer 12, thickness is not less than 2 μ m, can be by ultra-thin TiN layer 121 and the thickness of thin AlN layer 122 and the dislocation density that the number of plies reduces GaN monocrystal thin films in the GaN template layer 13 in the regulation and control combined stress covariant layer 12, the rate of temperature fall when thickness that also can be by the ultra-thin TiN monocrystal thin films material 121 in the regulation and control combined stress covariant layer 12 and the number of plies and control growing GaN template layer 13 is eliminated crackle in the GaN template layer 13 with crooked.In addition, because the lattice constant of AlN layer and the lattice constant of gallium nitride (GaN) monocrystal thin films template layer 13 are more approaching, as shown in Figure 1, the layer that contacts with gallium nitride (GaN) monocrystal thin films template layer 13 in the combined stress covariant layer 12 is preferably AlN layer 122.The preparation method of gallium nitride (GaN) monocrystal thin films template layer 13 includes but not limited to metal-organic chemical vapor deposition equipment, ion beam epitaxy, molecular beam epitaxy, pulsed laser deposition, plasma auxiliary chemical vapor deposition and magnetron sputtering deposition.
The basic compound substrate 1 of carborundum (SiC) that above-mentioned three combines formation can prepare the homogeneity single crystalline substrate template that low-dislocation-density, flawless and bending are provided for follow-up nitride semiconductor epitaxial sheet material.Although above-mentionedly be illustrated as example for the preparation of gallium nitride (GaN) take the basic compound substrate of carborundum (SiC), yet, will be appreciated that on the basic compound substrate 1 of this carborundum (SiC), can also prepare lamination and the nitride semiconductor LED device architecture of the nitride semi-conductor materials such as growing aluminum nitride, indium nitride, aluminum gallium nitride, indium gallium nitrogen, aluminium gallium nitrogen monocrystal thin films material, above-mentioned various monocrystal thin films materials.
Combined stress covariant layer among the present invention is compared existing stress covariant layer technology (comprising resilient coating, flexible layer, insert layer etc.) and is had better stress transfer and coordinate releasing effect.Be embodied in following three aspects:
1) select with carborundum (SiC) and aluminium nitride (AlN) have better Lattice Matching relation and the very large nitride multilayer titanium of thermal coefficient of expansion (TiN) monocrystal thin films material as the transfer of lattice mismatch stress and thermal stress with coordinate releasing layer.
The lattice mismatch of cube TiN (111) face and 6H-SiC (002) face is 2.22%, with the lattice mismatch of six side AlN (0002) faces be 3.45%.But the stress transfer thought based on the covariant intermediate layer of compliant substrate, in AlN layer epitaxially grown process, the TiN layer will be subject to SiC substrate and thin AlN layer and impose on its tensile stress, because TiN is very thin, this lattice mismatch stress can be transferred to first and coordinate in the TiN layer to discharge; And in GaN template layer growth course, the lattice mismatch stress between SiC substrate and the GaN material just will be transferred in the combined stress covariant layer that TiN layer and AlN layer combine and coordinate to discharge.Thereby be reduced in the probability of introducing dislocation and defective in the GaN template layer, also be first at the interface introducing at SiC substrate and AlN monocrystal thin films material even introduce dislocation, and can not produce more bad impact to top GaN template layer.Particularly, the alternately stacked structure of the multilayer TiN of the present invention's employing and AlN, more interfaces of introducing are played again and are stoped following threading dislocation upwards to breed the effect of extending, thereby further reduce dislocation density.
2) thermal coefficient of expansion of TiN is 9.35 * 10
-6K compares thermal coefficient of expansion (a:5.59 * 10 of GaN
-6K), the thermal coefficient of expansion of AlN (a:4.15 * 10
-6K) and the thermal coefficient of expansion of SiC (a:3.54 * 10
-6K) all much larger, adding the TiN layer, to compare AlN layer and GaN template layer and SiC single crystal substrates all much thin, but the stress transfer thought based on the covariant intermediate layer of compliant substrate, drop to the thermal stress of gathering because of the thermal expansion coefficient difference generation the room temperature process from 800～1100 ℃ growth temperatures, can transfer to first in each TiN layer with the form of tensile stress by the regulation and control rate of temperature fall and coordinate to discharge, and then realize the GaN template layer and the AlN layer is unstressed, crackle and bending.
3) TiN and the AlN combined stress covariant layer that replaces stacking formation had both had and compares existing stress covariant layer (comprising resilient coating, flexible layer and low temperature insert layer) better lattice mismatch stress and thermal stress shift trade-off effect, also can adopt the Material growth technique identical with the GaN template layer successively preparation on same equipment, therefore compare existing graph substrate technology, preparation technology is simpler also more practical.
The present invention is only by the thickness of the TiN in the regulation and control combined stress covariant layer and AlN layer and the silicon-carbide-base compound substrate that the rate of temperature fall behind the overlapping number of plies and the epitaxial growth GaN template layer just can obtain low-dislocation-density and flawless and bending, with this kind large-sized substrate epitaxial growth GaN material or other nitride semi-conductor materials and preparation LED device architecture, will certainly increase substantially performance and the yields of nitride semiconductor LED epitaxial wafer material on the existing silicon carbide substrate.Therefore, be fit to use and marketing.
The below introduces the preparation method of preparation above-mentioned carborundum (SiC) compound substrate.Should be appreciated that, preparation method described below is only for preparing an instantiation of carborundum of the present invention (SiC) compound substrate.Those skilled in the art can make change according to design needs and other factors under instruction of the present invention.
Adopt metal-organic chemical vapor deposition equipment (MOCVD) technique as follows for the preparation of the technological process of the basic compound substrate of carborundum (SiC) of nitride semiconductor LED epitaxial wafer material preparation:
Step 1: get one 2 inch silicon carbides (6H-SiC) single crystal substrates 11;
Step 2: the 6H-SiC single crystal substrates 11 that will clean is put into the MOCVD equipment reaction chamber;
Step 3: on 6H-SiC single crystal substrates 11, prepare first the ultra-thin TiN monocrystal thin films material 121 of growth 1 bed thickness 10nm as the stress covariant layer of lattice mismatch stress and thermal stress with MOCVD technique;
Step 4: the thin AlN monocrystal thin films material 122 of using again MOCVD technique epitaxial growth 1 bed thickness 50nm on the thick ultra-thin TiN layer 121 of 10nm;
Step 5: repeating step 3 and step 4 prepare by 3 layers of thick ultra-thin TiN layer 121 of 10nm and 3 layers of thick AlN layer 122 of 50nm with MOCVD technique and to replace the stacking combined stress covariant layer material 12 that consists of;
Step 6: on combined stress covariant layer material 12, prepare again the thick GaN monocrystal thin films material of 1 layer of 2 μ m of growth as GaN template layer 13 with MOCVD technique;
Step 7: the rate of temperature fall of regulation and control GaN template layer 13, drop to 750 ℃ with 10 ℃/minute rate of temperature fall from 1050 ℃ first, drop to 250 ℃ with 20 ℃/minute rate of temperature fall from 750 ℃ again, naturally drop to room temperature at last;
Step 8: taking-up comprises carborundum (6H-SiC) single crystal substrates 11, combined stress covariant layer 12 from the MOCVD equipment reaction chamber, low-dislocation-density is unstressed and the basic compound substrate 1 of carborundum (6H-SiC) of the GaN template layer 13 of bending;
Step 9: do GaN homogeneity single crystalline substrate template with the basic compound substrate 1 of 2 inch silicon carbides (6H-SiC), adopt MOCVD technique to prepare the GaN base blue-ray LED epitaxial wafer material of High Efficiency Luminescence.
It should be noted that at last above example is only in order to technical scheme of the present invention to be described but not limit it.Although with reference to given example the present invention is had been described in detail, those of ordinary skill in the art can make amendment to technical scheme of the present invention as required or be equal to replacement, and does not break away from the spirit and scope of technical solution of the present invention.
Claims (11)
1. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material is characterized in that, comprises:
One single-crystal silicon carbide substrate;
One combined stress covariant layer covers in the described single-crystal silicon carbide substrate, is replaced by nitride multilayer ti single crystal thin-film material and nitride multilayer aluminium monocrystal thin films material stackingly to consist of;
One gallium nitride template layer is grown on the described combined stress covariant layer, is made of monocrystalline GaN film material.
2. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1 is characterized in that, the thickness of every layer of described titanium nitride monocrystal thin films material is 5～30nm in the described combined stress covariant layer.
3. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1, it is characterized in that, the thickness of every layer of described aluminum nitride single crystal film material is not less than 3 times of thickness of every layer of described titanium nitride monocrystal thin films material in the described combined stress covariant layer.
4. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1 is characterized in that, the layer with described single-crystal silicon carbide substrate contact in described combined stress covariant layer is described titanium nitride monocrystal thin films material.
5. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1 is characterized in that, the layer that contacts with described gallium nitride template layer in described combined stress covariant layer is described aluminum nitride single crystal film material.
6. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1, it is characterized in that, the number of plies of described titanium nitride monocrystal thin films material is 3～10 layers, and the number of plies of described aluminum nitride single crystal film material is identical with the number of plies of described titanium nitride monocrystal thin films material.
7. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1 is characterized in that, the thickness of described gallium nitride template layer is not less than 2 μ m.
8. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1, it is characterized in that, be 5～20 ℃/minute from the rate of temperature fall that 800～1100 ℃ growth temperature drops to room temperature in growth during described gallium nitride template layer.
9. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1, it is characterized in that, comprise metal-organic chemical vapor deposition equipment, ion beam epitaxy, molecular beam epitaxy, pulsed laser deposition, plasma auxiliary chemical vapor deposition and magnetron sputtering deposition for the preparation of the Material growth technique of the titanium nitride monocrystal thin films material in the described combined stress covariant layer and aluminum nitride single crystal film material and gallium nitride template layer.
10. the silicon-carbide-base compound substrate for the preparation of the nitride semiconductor epitaxial material according to claim 1, it is characterized in that, described silicon-carbide-base compound substrate is used for gallium nitride, aluminium nitride, indium nitride, aluminum gallium nitride, indium gallium nitrogen, aluminium gallium nitrogen monocrystal thin films material, reaches the preparation growth of nitride semiconductor LED device architecture.
11. the manufacture method of a silicon-carbide-base compound substrate, this silicon-carbide-base compound substrate is characterized in that for the preparation of the nitride semiconductor epitaxial material, comprises:
Get a single-crystal silicon carbide substrate;
Form a combined stress covariant layer in described single-crystal silicon carbide substrate, described combined stress covariant layer is replaced by aluminum nitride single crystal film material and titanium nitride monocrystal thin films material and stackingly consists of;
Form a gallium nitride template layer at described combined stress covariant layer, described gallium nitride template layer is made of monocrystalline GaN film material.
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| WO2014015458A1 (en) * | 2012-07-23 | 2014-01-30 | 东莞市中镓半导体科技有限公司 | Composite substrate with protective layer for preventing metal from diffusing |
| CN103579471B (en) * | 2012-07-23 | 2016-06-15 | 东莞市中镓半导体科技有限公司 | A kind of compound substrate with preventing metal diffusing protective layer |
| CN103882526B (en) * | 2014-03-25 | 2016-06-01 | 山东大学 | Direct growth is from the method for peeling GaN monocrystalline on sic substrates |
| CN107170861A (en) * | 2017-06-02 | 2017-09-15 | 王荣华 | A kind of LED gallium nitride substrates and preparation method thereof |
| CN109786218A (en) * | 2019-02-13 | 2019-05-21 | 保定中创燕园半导体科技有限公司 | A kind of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate |
| CN113981532A (en) * | 2021-08-30 | 2022-01-28 | 华灿光电（浙江）有限公司 | Substrate for epitaxial growth of silicon carbide and method for manufacturing substrate |
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