CN103794469A - Preparation method of gallium nitride film layer and substrate - Google Patents
Preparation method of gallium nitride film layer and substrate Download PDFInfo
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- CN103794469A CN103794469A CN201210424784.1A CN201210424784A CN103794469A CN 103794469 A CN103794469 A CN 103794469A CN 201210424784 A CN201210424784 A CN 201210424784A CN 103794469 A CN103794469 A CN 103794469A
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Abstract
The invention provides a preparation method of a gallium nitride film layer and a substrate. The preparation method of the gallium nitride film layer comprises the following steps: obtaining and cleaning an indirect substrate; forming a graphene film on the surface of the indirect substrate; and forming a gallium nitride film layer on the surface of the graphene film. The preparation method of the gallium nitride film layer can effectively reduce the dislocation density of the gallium nitride film layer in a process of growth, thereby improving performance of the gallium nitride film layer.
Description
Technical field
The present invention relates to a kind of preparation method and substrate of gallium nitride film layer.
Background technology
Metallo-organic compound chemical vapor deposition (Metal-organic Chemical Vapor Deposition, be called for short MOCVD) be a kind of Novel air phase epitaxy growing technology growing up on vapor phase epitaxial growth basis, it is mainly with III family, organic compound and the V of II family element, the hydride of VI family element etc. are as crystal growth source material, in pyrolysis mode at the enterprising promoting the circulation of qi phase epitaxy of substrate, the various III-V family of growing, the thin layer monocrystal material of II-VI compound semiconductor and their multivariate solid solution, as the GaN(gallium nitride in the normal use of semiconductor applications) film.
In the time utilizing MOCVD to prepare gallium nitride film layer, optimal substrate is and the gallium nitride substrate of gallium nitride film layer homogeneity, but gallium nitride fusing point is up to 2800 ℃, equilibrium vapour pressure reaches 4.5GPa, prepare very difficulty of gallium nitride body monocrystalline, therefore, substrate is mainly selected from sapphire (α-Al at present
2o
3), carborundum (4H/6H-SiC) or silicon (Si).
But there is larger lattice mismatch and thermal mismatching in Sapphire Substrate and gallium nitride material.Although by patterned surface substrate technology and diauxic growth method, can reduce to a certain extent the dislocation density of film inside, but still be difficult to control the quality of film; Meanwhile, because Sapphire Substrate is non-conductive, when packaged LED luminescent device, need to utilize the complicated technologies such as photoetching, etching, evaporation on epitaxial loayer, to prepare electrode, this has reduced efficient lighting area greatly, has lowered the utilance of epitaxial material; The lower thermal conductivity of Sapphire Substrate makes the heat radiation difficulty of device.
Although silicon carbide substrates is low with the lattice mismatch rate of gallium nitride material, and there is good heat conduction and conductivity,, before gallium nitride film growth layer, the AlGaN that need to grow under the high temperature of approximately 1000 ℃ is as conduction stratum nucleare; And SiC substrate is expensive.
Lattice mismatch and thermal mismatching between silicon substrate and gallium nitride material are larger, the far super Sapphire Substrate of the difficulty of gallium nitride film growth layer and silicon carbide substrates.
Summary of the invention
For solving one of the above-mentioned problems in the prior art, the invention provides a kind of preparation method of gallium nitride film layer, it is low that it prepares difficulty, and can reduce the dislocation density in growth course, thereby improve the performance of gallium nitride film layer.
In addition, the present invention also provides a kind of substrate, and the lattice mismatch between itself and gallium nitride film layer is little, and surperficial utilance is high, and production cost is low.
The technical scheme adopting solving the problems of the technologies described above is to provide a kind of gallium nitride film layer, comprises the following steps:
Obtain indirect substrate, and described indirect substrate is cleaned;
Surface at described indirect substrate forms graphene film layer;
Surface at described graphene film layer forms gallium nitride film layer.
Wherein, comprise in the step that described indirect substrate is cleaned:
Toluene, carbon tetrachloride, acetone, ethanol, deionized water are mixed to obtain and mix cleaning fluid;
Utilize described mixing cleaning fluid to carry out ultrasonic cleaning to described indirect substrate;
At the concentrated sulfuric acid and H
2o
2mixed liquor in soak described indirect substrate;
Utilize described in HF solution removal the native oxide of substrate surface indirectly;
Utilize described in deionized water rinsing substrate indirectly;
Remove the moisture of described indirect substrate surface.
Wherein, described indirect substrate ultrasonic cleaning 5～10min, described indirect substrate is at the concentrated sulfuric acid and H
2o
2mixed liquor in soak 3～6min, utilize described in deionized water rinsing indirectly substrate 3～8 times.
Wherein, utilizing mass concentration is the native oxide that 2.5～4.5% HF solution etches away described indirect substrate surface.
Wherein, utilize high pure nitrogen to dry up described indirect substrate, to remove the moisture of described indirect substrate surface.
Wherein, comprise in the step of the surface of described indirect substrate making graphene film layer:
Surface at described indirect substrate forms SiC thin layer;
Make the thermal decomposition of described SiC thin layer, thereby form graphene film layer on the surface of described indirect substrate.
Wherein, form SiC thin layer by high temperature distillation, liquid phase epitaxy, magnetron sputtering, pulsed laser deposition, chemical vapour deposition (CVD) or molecular beam epitaxial process on the surface of described indirect substrate.
Wherein, comprise in the step of the surface of described indirect substrate formation SiC thin layer:
At described indirect substrate surface uniform spreading Polycarbosilane;
At the temperature of 1050～1300 ℃, make described Polycarbosilane cracking form SiC thin layer.
Wherein, before forming graphene film layer, the surface of described indirect substrate also needs:
The described indirect substrate of original position baking 1～3 hour at the temperature of 500～900 ℃.
Wherein, it is in 1100 ℃ of above environment that the described indirect substrate that surface is formed with to described SiC thin layer is placed on temperature, makes the thermal decomposition of described SiC thin layer, thereby forms graphene film layer on the surface of described graphene film layer.
Wherein, form in the step of gallium nitride film layer on the surface of described indirect substrate, the described indirect substrate that surface is formed with to graphene film layer is placed in 900 ℃ of above environment, and passes into TMGa gas and NH
3gas, gas carrier is H
2gas, makes the two bond fissions of C=C in described graphene film layer, and is combined with NH2 and/or MMG and forms gallium nitride film layer.
Wherein, forming after gallium nitride film layer, also comprise annealing in process, in order to reduce the stress of described gallium nitride film layer.
Wherein, described indirect substrate is Sapphire Substrate, SiC substrate or Si substrate, LiAlO
3substrate or ZnO substrate.
The present invention also provides a kind of substrate, comprises indirect substrate and the gallium nitride layer that is arranged on described indirect substrate surface, between described indirect substrate and described gallium nitride layer, is also provided with graphene film layer.
Wherein, for making LED, blue laser and solar cell.
The present invention has following beneficial effect:
The preparation method of gallium nitride film layer provided by the invention, first forms graphene film on the surface of indirect substrate, then forms gallium nitride film layer on the surface of graphene film.Because the regional area in graphene film exists island or chain structure, and between carbon atom, connect fairly regular, pliable and tough, lattice mismatch is little, therefore can effectively reduce the dislocation density in gallium nitride film layer growth process, thereby improves the performance of gallium nitride film layer.
In addition, graphene film heat conduction is good, and high temperature resistant, can improve the radiating efficiency of device in later stage encapsulation, and then improves device useful life.
Gallium nitride film layer after graphene film superficial growth completes can be in cleavage under mechanicals efforts along lattice direction, and smooth surface, can directly contact with glass, plastics and metal material, therefore can carry out the preparation of multiple device.As, the gallium nitride after graphene film superficial growth completes can directly carry out the vertical encapsulation of LED after luminous extension cleavage.
Utilize substrate that this preparation method obtains compared with the direct substrate of sapphire, the surface that not be used in substrate is prepared electrode and can be realized vertical encapsulation, thereby makes the service efficiency of gallium nitride film layer at least improve 20%; Compared with the direct substrate of carborundum, can effectively reduce the cost of manufacture of gallium nitride film layer; Compared with the direct substrate of silicon materials, no longer make highly difficult Si-GaN resilient coating, and can effectively reduce the impact of stress on device.
Substrate provided by the invention, being indirectly provided with graphene film layer between substrate and gallium nitride layer, can reduce the lattice mismatch between indirect substrate and gallium nitride layer by graphene film layer, thereby can improve the performance of gallium nitride layer, and reduce stress; And graphene film has good thermal conductivity, can improve device useful life; This substrate conduction, the surface that not be used in substrate is prepared electrode and can be realized vertical encapsulation, thereby makes the service efficiency of gallium nitride film layer at least improve 20%.
Accompanying drawing explanation
Fig. 1 is the preparation method's of embodiment of the present invention gallium nitride film layer flow chart;
Fig. 2 is the flow chart that cleans the indirect substrate of Si;
Fig. 3 is the flow chart that forms SiC thin layer;
The structure chart of the substrate that Fig. 4 provides for the embodiment of the present invention.
Embodiment
For making those skilled in the art understand better technical scheme of the present invention, preparation method and substrate below in conjunction with accompanying drawing to gallium nitride film layer provided by the invention are described in detail.
The present embodiment provides a kind of preparation method of gallium nitride film layer.Fig. 1 is the preparation method's of embodiment of the present invention gallium nitride film layer flow chart.As shown in Figure 1, the preparation method of gallium nitride film layer comprises the following steps:
Step S1, obtains indirect substrate, and described indirect substrate is cleaned.
Substrate can adopt Sapphire Substrate, SiC substrate, Si substrate, LiAlO indirectly
3substrate or ZnO substrate.The present embodiment describes as an example of Si substrate example, and as shown in Figure 2, the concrete steps of cleaning the indirect substrate of Si comprise:
Step S11, mixes toluene, carbon tetrachloride, acetone, ethanol, deionized water to obtain and mixes cleaning fluid.
Step S12, utilizes described mixing cleaning fluid to carry out ultrasonic cleaning to described Si substrate.
Utilize and mix cleaning fluid ultrasonic cleaning Si substrate 5～10min, to remove spot and the dust of Si substrate surface.
Step S13, makes described Si substrate at the concentrated sulfuric acid and H
2o
2mixed liquor in soak.
By the concentrated sulfuric acid and H
2o
2mix according to a certain percentage, the ratio of mixing can be determined according to actual conditions; Then by Si substrate at the concentrated sulfuric acid and H
2o
2mixed liquor in soak 3～6min.
Step S14, utilizes the native oxide of Si substrate surface described in HF solution removal.
Utilizing mass concentration is the native oxide that 2.5～4.5% HF solution etches away Si substrate surface.
Step S15, utilizes Si substrate described in deionized water rinsing.
Utilize deionized water rinsing Si substrate 3～8 times, with by residual HF solution, the concentrated sulfuric acid and H
2o
2deng removal.
Step S16, removes the moisture of described Si substrate surface.
In step S16, utilize high pure nitrogen to dry up Si substrate, to remove the moisture of described Si substrate surface.
It should be noted that, step S11 has only been to provide a kind of method of the Si of cleaning substrate to step S16.In actual applications, also can adopt other cleaning method to clean Si substrate, as long as Si substrate can be cleaned up.
In order to make Si substrate more clean, preferably, before implementation step S2, the present embodiment is also included at the temperature of 500～900 ℃ original position baking Si substrate 1～3 hour.
Step S2, forms graphene film layer on the surface of described Si substrate.
The step that forms graphene film layer in step S2 comprises:
Step S21, forms SiC thin layer on the surface of described Si substrate.
SiC thin layer can form on the surface of Si substrate by high temperature distillation, liquid phase epitaxy, magnetron sputtering, pulsed laser deposition, chemical vapour deposition (CVD) or molecular beam epitaxial process.
The present embodiment SiC thin layer is only the source layer as graphene film, is not very high to the quality requirement of SiC thin layer.Therefore, as shown in Figure 3, the present embodiment obtains SiC thin layer by following steps:
Step S211, at described Si substrate surface uniform spreading Polycarbosilane.
Step S212 makes described Polycarbosilane cracking form SiC thin layer at the temperature of 1050～1300 ℃.
Lower to the cost that the mode of step S212 obtains SiC thin layer by step S211, therefore, can reduce the preparation cost of gallium nitride film layer.
Step S22, decomposes described SiC film thermal, thereby forms graphene film layer on the surface of described Si substrate, and this graphene film layer can be considered to two-dimentional graphene film layer.
In step S22, it is in 1100 ℃ of above environment that the described Si substrate that surface is formed with to described SiC thin layer is placed on temperature, preferably more than 1300 ℃, make the thermal decomposition of described SiC thin layer, thereby form graphene film layer on the surface of described graphene film.The thickness of graphene film layer is generally several thickness to tens atoms.
Step S3, forms gallium nitride film layer on the surface of described graphene film layer.
The described Si substrate that surface is formed with to graphene film layer is placed in hot environment, is generally in 900 ℃ of above environment, and passes into TMGa gas and NH
3gas, gas carrier is H
2gas, makes the two bond fissions of C=C in described graphene film, and is combined with NH2 and/or MMG and forms gallium nitride film layer.
Under hot conditions, TMGa gas (trimethyl is transferred gas) can be decomposed into DMG, and DMG decomposition activation energy is lower, easily generates MMG.NH
3the thermal stability of gas is very good, even have decomposition also can ignore at high temperature.But NH
3the CH that gas can discharge with the decomposition reaction of above-mentioned TMGa gas
3reaction, generates CH
4and NH
2.H
2under hot conditions, can be decomposed into H.Now in environment, mainly there is the atomic group forming between CH3, NH2, H, TMG, DMG, MMG, NH3, CH4 and other C-H.According to bond energy size, after the two bond fissions of C=C under hot conditions in Graphene, be first combined with NH2 and/or MMG, thereby at Graphene Surface Creation gallium nitride film layer.
Prepare the initial stage of graphene film layer at high temperature, at the local graphene film layer that forms island chain architectural feature of the surface of Si substrate meeting, this graphene film layer can be used as resilient coating, when after growth certain thickness, the insulation of annealing is again processed, and forms desirable graphene film layer.The temperature of annealing is different and different according to the temperature of the characteristic of backing material and growing graphene thin layer, for example can be at N
2in atmosphere, at 700 ℃ of temperature, anneal, in order to reduce the stress of gallium nitride film layer.
The preparation method of the gallium nitride film layer that the present embodiment provides, first forms graphene film layer on the surface of indirect substrate, then forms gallium nitride film layer on the surface of graphene film layer.Because the part difference in graphene film layer exists island or chain structure, and between carbon atom, connect fairly regular, pliable and tough, lattice mismatch is little, therefore can effectively reduce the dislocation density in gallium nitride film layer growth process, thereby improves the performance of gallium nitride film layer.
In addition, graphene film layer thermal conductivity is good, and high temperature resistant, can improve the radiating efficiency of device in later stage encapsulation, and then improves device useful life.
Gallium nitride film layer after the superficial growth of graphene film layer completes can be in cleavage under mechanicals efforts along lattice direction, and smooth surface, can directly contact with glass, plastics and metal material, therefore can carry out the preparation of multiple device.As, the gallium nitride after graphene film superficial growth completes can directly carry out the vertical encapsulation of LED after luminous extension cleavage.
Utilize substrate that this preparation method obtains compared with Sapphire Substrate, the surface that not be used in substrate is prepared electrode and can be realized vertical encapsulation, thereby makes the service efficiency of gallium nitride film layer at least improve 20%; Compared with silicon carbide substrates, can effectively reduce the cost of manufacture of gallium nitride film layer; Compared with silicon materials substrate, no longer make highly difficult Si-GaN resilient coating, and can effectively reduce the impact of stress on device.
The present embodiment also provides a kind of substrate, and as shown in Figure 4, substrate comprises indirect substrate 41 and is arranged on the gallium nitride layer 43 on indirect substrate 41 surfaces, indirectly between substrate 41 and gallium nitride layer 43, is also being provided with graphene film layer 42.
In the present embodiment, substrate 41 can be Sapphire Substrate, SiC substrate, Si substrate, LiAlO indirectly
3substrate or ZnO substrate.The substrate that the present embodiment provides can be for making LED, blue laser and solar cell.
The substrate that the present embodiment provides, being indirectly provided with graphene film layer between substrate and gallium nitride layer, can reduce the lattice mismatch between indirect substrate and gallium nitride layer by graphene film layer, thereby can improve the performance of gallium nitride layer, and reduce stress; And graphene film has good thermal conductivity, can improve device useful life; This substrate conduction, the surface that not be used in substrate is prepared electrode and can be realized vertical encapsulation, thereby makes the service efficiency of gallium nitride film layer at least improve 20%.
Be understandable that, above execution mode is only used to principle of the present invention is described and the illustrative embodiments that adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (15)
1. a preparation method for gallium nitride film layer, is characterized in that, comprises the following steps:
Obtain indirect substrate, and described indirect substrate is cleaned;
Surface at described indirect substrate forms graphene film layer;
Surface at described graphene film layer forms gallium nitride film layer.
2. the preparation method of gallium nitride film layer according to claim 1, is characterized in that, comprises in the step that described indirect substrate is cleaned:
Toluene, carbon tetrachloride, acetone, ethanol, deionized water are mixed to obtain and mix cleaning fluid;
Utilize described mixing cleaning fluid to carry out ultrasonic cleaning to described indirect substrate;
At the concentrated sulfuric acid and H
2o
2mixed liquor in soak described indirect substrate;
Utilize described in HF solution removal the native oxide of substrate surface indirectly;
Utilize described in deionized water rinsing substrate indirectly;
Remove the moisture of described indirect substrate surface.
3. the preparation method of gallium nitride film layer according to claim 2, is characterized in that, described indirect substrate ultrasonic cleaning 5～10min, and described indirect substrate is at the concentrated sulfuric acid and H
2o
2mixed liquor in soak 3～6min, utilize described in deionized water rinsing indirectly substrate 3～8 times.
4. the preparation method of gallium nitride film layer according to claim 2, is characterized in that, utilizing mass concentration is the native oxide that 2.5～4.5% HF solution etches away described indirect substrate surface.
5. the preparation method of gallium nitride film layer according to claim 2, is characterized in that, utilizes high pure nitrogen to dry up described indirect substrate, to remove the moisture of described indirect substrate surface.
6. the preparation method of gallium nitride film layer according to claim 1, is characterized in that, the step of making graphene film layer on the surface of described indirect substrate comprises:
Surface at described indirect substrate forms SiC thin layer;
Make the thermal decomposition of described SiC thin layer, thereby form graphene film layer on the surface of described indirect substrate.
7. the preparation method of gallium nitride film layer according to claim 6, it is characterized in that, form SiC thin layer by high temperature distillation, liquid phase epitaxy, magnetron sputtering, pulsed laser deposition, chemical vapour deposition (CVD) or molecular beam epitaxial process on the surface of described indirect substrate.
8. the preparation method of gallium nitride film layer according to claim 6, is characterized in that, the step that forms SiC thin layer on the surface of described indirect substrate comprises:
At described indirect substrate surface uniform spreading Polycarbosilane;
At the temperature of 1050～1300 ℃, make described Polycarbosilane cracking form SiC thin layer.
9. the preparation method of gallium nitride film layer according to claim 6, is characterized in that, before the surface of described indirect substrate forms graphene film layer, also needs:
The described indirect substrate of original position baking 1～3 hour at the temperature of 500～900 ℃.
10. the preparation method of gallium nitride film layer according to claim 6, it is characterized in that, it is in 1100 ℃ of above environment that the described indirect substrate that surface is formed with to described SiC thin layer is placed on temperature, make the thermal decomposition of described SiC thin layer, thereby form graphene film layer on the surface of described graphene film layer.
The preparation method of 11. gallium nitride film layers according to claim 6, it is characterized in that, form in the step of gallium nitride film layer on the surface of described indirect substrate, the described indirect substrate that surface is formed with to graphene film layer is placed in 900 ℃ of above environment, and passes into TMGa gas and NH
3gas, gas carrier is H
2gas, makes the two bond fissions of C=C in described graphene film layer, and is combined with NH2 and/or MMG and forms gallium nitride film layer.
The preparation method of 12. gallium nitride film layers according to claim 11, is characterized in that, forming after gallium nitride film layer, also comprises annealing in process, in order to reduce the stress of described gallium nitride film layer.
13. according to the preparation method of the gallium nitride film layer described in claim 1-12 any one, it is characterized in that, described indirect substrate is Sapphire Substrate, SiC substrate or Si substrate, LiAlO
3substrate or ZnO substrate.
14. 1 kinds of substrates, comprise indirect substrate and the gallium nitride layer that is arranged on described indirect substrate surface, it is characterized in that, between described indirect substrate and described gallium nitride layer, are also provided with graphene film layer.
15. substrates according to claim 14, is characterized in that, for making LED, blue laser and solar cell.
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| CN105731825A (en) * | 2016-03-04 | 2016-07-06 | 北京大学 | Method for preparing aluminum nitride thin film by utilizing graphene glass at low cost and large area |
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| CN106835268A (en) * | 2017-01-17 | 2017-06-13 | 苏州瑞而美光电科技有限公司 | A kind of preparation method of group III-nitride substrate |
| CN106960781A (en) * | 2017-03-28 | 2017-07-18 | 刘志斌 | A kind of gallium nitride film and preparation method thereof and graphene film and preparation method thereof |
| CN108428618A (en) * | 2018-03-16 | 2018-08-21 | 西安电子科技大学 | Growing method of gallium nitride based on graphene insert layer structure |
| CN108428618B (en) * | 2018-03-16 | 2020-06-16 | 西安电子科技大学 | Gallium nitride growth method based on graphene insertion layer structure |
| CN108511322A (en) * | 2018-03-29 | 2018-09-07 | 太原理工大学 | A method of preparing GaN film in two-dimentional graphite substrate |
| CN109285758A (en) * | 2018-08-30 | 2019-01-29 | 中国科学院半导体研究所 | The method of growing nitride film in graph substrate |
| CN109411552A (en) * | 2018-10-11 | 2019-03-01 | 苏州大学 | A kind of miniature flexible ultraviolet detector and preparation method thereof based on gallium nitride film |
| CN113394306A (en) * | 2021-05-18 | 2021-09-14 | 浙江大学 | Reusable ZnO single crystal substrate based on graphene and method for preparing ZnO film |
| CN115832137A (en) * | 2023-02-16 | 2023-03-21 | 江西乾照光电有限公司 | LED epitaxial wafer, epitaxial growth method and LED chip |
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