CN106783553B - III-nitride micro-column structure with graphene/dielectric material as composite substrate and preparation method thereof - Google Patents
III-nitride micro-column structure with graphene/dielectric material as composite substrate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a III-nitride micro-column structure with graphene/dielectric material as a composite substrate and a preparation method thereof. The method comprises the steps of directly preparing graphene on a non-sapphire dielectric material by a low-temperature solid carbon source method to obtain a composite substrate, and growing a III-nitride micro-column on the graphene of the composite substrate to obtain a III-nitride micro-column structure with the graphene/dielectric material as the composite substrate. The technical scheme of the invention solves the problem that the III-nitride cannot nucleate and grow on certain dielectric materials, and widens the range of the III-nitride epitaxial dielectric substrate. Particularly, the epitaxial III-nitride is epitaxial by using the graphene/quartz composite substrate, so that the epitaxial cost can be effectively reduced. The method has simple and easy flow, cheap and easily obtained raw materials, and is suitable for large-scale production.
Description
Technical Field
The invention relates to a III-nitride micron column structure taking graphene/dielectric material as a composite substrate and a preparation method thereof, in particular to a method for growing a III-nitride micron column on a dielectric material by utilizing a low-temperature solid carbon source method, epitaxially growing the III-nitride micron column on the graphene/dielectric material composite substrate and taking the graphene as an insertion layer, and belongs to the technical field of semiconductor materials.
Background
The III-nitride as a third-generation semiconductor material has the advantages of direct band gap, large forbidden band width and the like, and is widely applied to the photoelectronic fields of illumination, display, ultraviolet detection and the like. At present, the III-nitride material is mostly prepared by epitaxial growth from a sapphire substrate, and the III-nitride epitaxy on other dielectric materials such as silicon dioxide is relatively difficult.
Before the present invention was made, chinese invention patent (CN 102593294 a) "composite gallium nitride based semiconductor growth substrate and method for making the same" proposes a composite gallium nitride based semiconductor growth substrate, which comprises: a substrate and a lattice buffer layer made of Diamond-like carbon (DLC), which is formed by DLC and nitrideThe combination of the silicon nitride and the silicon nitride overcomes the problems of lattice mismatch, thermal mismatch and the like when common substrates such as quartz glass or metal substrates and the like are used for growing the gallium nitride semiconductor material; the chinese utility model patent (CN 203697610U) "indium nitride/gallium nitride/glass structure" proposes a structure of depositing a gallium nitride buffer layer film on glass, and depositing indium nitride on the gallium nitride buffer layer film. Chinese invention patent (CN 101320686)' HVPE method for growing SiO in gallium nitride film 2 The nanometer mask and method' proposes that a layer of metal Al is evaporated on a GaN template by an electron beam, then porous Anodic Aluminum Oxide (AAO) is generated by adopting an electrochemical method, and then a layer of dielectric SiO is deposited 2 Layer, then using acid or alkali solution to remove AAO and obtain SiO on the GaN template 2 And (3) carrying out lattice distribution on the nano particles, cleaning, and then placing the template serving as a substrate in an HVPE reaction chamber to grow a GaN thick film. The material prepared by the method has relatively complex process flow.
Because group iii nitride is difficult to nucleate on certain dielectric materials, the prior art has not been able to directly grow group iii nitride semiconductors on substrates to achieve higher quality.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the III-nitride micro-column structure which has low production cost and simple operation and can directly grow and obtain high-quality III-nitride semiconductor on the substrate and takes the graphene/dielectric material as the composite substrate, and the preparation method thereof.
In order to achieve the above object, the present invention provides a method for preparing a iii-nitride micro-pillar structure with graphene/dielectric material as a composite substrate, wherein a low-temperature solid carbon source method is adopted to directly grow graphene on the dielectric material, and the method comprises the following steps:
1. plating a nickel film layer on the surface of the dielectric material substrate by adopting an ion beam sputtering or electron beam evaporation process, wherein the thickness of the nickel layer is 50-500 nm;
2. ultrasonically dispersing graphite powder with the purity of more than 99.9% in ethanol, and coating the graphite powder on the surface of a nickel film;
3. placing the dielectric material substrate coated with graphite powder in a reaction chamber, heating for 3-10 minutes under the conditions of argon atmosphere and temperature of 300-600 ℃, and growing between the nickel layer and the interface of the dielectric material after natural cooling to obtain a graphene layer;
4. placing the substrate in FeCl 3 In the solution, the nickel layer is corroded;
5. after the nickel layer is completely corroded, cleaning the nickel layer by using deionized water to obtain a graphene/dielectric material composite substrate taking graphene as an insertion layer;
6. growing a III-group nitride micro-column on a graphene insertion layer of the graphene/dielectric material composite substrate by adopting a hydride vapor phase epitaxy method or a metal organic chemical vapor deposition method to obtain the III-group nitride micro-column structure taking the graphene/dielectric material as the composite substrate.
The dielectric material comprises one of silicon dioxide, tantalum pentoxide, hafnium dioxide, zinc sulfide and zinc selenide.
The group III nitride is one of GaN, alN, inN and ternary or quaternary alloy thereof.
The technical scheme of the invention also comprises a III-nitride micro-column structure which is prepared by the preparation method and takes the graphene/dielectric material as a composite substrate: growing a graphene insertion layer on a dielectric material; growing a III-nitride micron column on the graphene insertion layer, wherein the height of the micron column is 10-300 um, and the diameter of the micron column is 10-300 um.
In the technical scheme of the invention, a hydride vapor phase epitaxy method or a metal organic chemical vapor deposition method is adopted to grow the III-group nitride micron column on the graphene, and the following technical scheme can be adopted: placing the obtained graphene/dielectric material composite substrate into a cavity of a hydride vapor phase epitaxy system or a metal organic chemical vapor deposition system, and treating for 10-20 minutes under the conditions of hydrogen atmosphere and 900-1000 ℃; introducing XCl in hydride vapor phase epitaxy system 3 And NH 3 Respectively used as a three-family source and a nitrogen source, X is a three-family metal Al, ga, in, XCl 3 Formed by reaction of HCl upstream of a hydride vapor phase epitaxy system with group III metals Al, ga, in, NH 3 And XCl 3 The group III nitride XN is reacted downstream of the hydride vapor phase epitaxy system and deposited on the surface of the composite substrate. Introducing X (CH) into a metal organic chemical vapor deposition system 3 ） 3 And NH 3 Respectively used as a three-family source and a nitrogen source, and after reaction, three-family nitride is generated and deposited on the surface of the composite substrate.
Group iii nitride semiconductors of higher quality are not readily epitaxially grown on dielectric materials due to the difficulty of nucleation and growth of group iii nitrides on certain dielectric materials. According to the invention, high defect state graphene grows on a dielectric material by a low-temperature solid carbon source method, a III-group nitride micron column grows on a composite substrate formed by the graphene/the dielectric material in an epitaxial manner, and a III-group nitride semiconductor with higher quality is obtained by directly growing on the substrate by taking the graphene as an insertion layer, so that the problems are successfully solved.
Compared with the prior art, the invention has the following advantages:
1. by using a low-temperature solid carbon source method, high-defect-state graphene which is beneficial to nucleation of III-nitride directly grows on a medium substrate, and the graphene does not need to be transferred; high-quality III-nitride micro-columns can be directly epitaxially grown on graphene; the growth of the group III nitride semiconductor on the dielectric material is successfully realized.
2. Compared with the prior art, the technology for growing the III-nitride micron column on the graphene/dielectric material composite substrate has the characteristics of low cost, simplicity in operation, capability of large-scale production and the like.
Drawings
Fig. 1 is a schematic structural diagram of a iii-nitride micro-pillar grown on a composite substrate according to an embodiment of the present invention, where: 1. a dielectric material; 2. a graphene insertion layer; 3. a group III nitride micro-pillar;
fig. 2 is an optical microscope image of graphene grown by a low-temperature solid carbon source method according to an embodiment of the present invention;
fig. 3 is a raman spectrum of graphene grown by a low-temperature solid-state carbon source method according to an embodiment of the present invention;
fig. 4 is a scanning electron microscope image of a gallium nitride micro-column grown on a graphene/quartz composite substrate by a hydride vapor phase epitaxy method according to an embodiment of the present invention;
fig. 5 is a scanning electron microscope image of a gan microcolumn and a corresponding crt fluorescence test image according to an embodiment of the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining the drawings and the specific embodiment.
Example 1
Referring to fig. 1, which is a schematic diagram of a group iii nitride micro-pillar structure grown on a composite substrate provided in this embodiment, a graphene insertion layer 2 is grown on a dielectric material 1 to obtain a composite substrate; growing a III-nitride micron column 3 on the graphene insertion layer 2 of the composite substrate, and preparing the III-nitride micron column by adopting the following steps:
step one, preparing a graphene/dielectric material composite substrate, wherein the dielectric material provided by the embodiment is quartz, and growing high-defect-state graphene which is beneficial to nitride nucleation on the dielectric material by using a low-temperature solid carbon source method, specifically comprising the following steps:
1. ultrasonically cleaning a quartz substrate in acetone for 3 minutes, taking out the quartz substrate, ultrasonically cleaning the quartz substrate in ethanol for 3 minutes, and ultrasonically cleaning the quartz substrate in deionized water for 3 minutes;
2. plating a nickel layer with the thickness of 200nm on the surface of the quartz substrate by adopting an ion beam sputtering or electron beam evaporation method;
3. ultrasonically dispersing 2g of graphite powder with the purity of 99.9 percent into 50ml of ethanol, and coating the graphite powder on the surface of the obtained nickel layer;
4. putting the quartz substrate coated with the graphite powder into a reaction chamber, vacuumizing, injecting argon, and heating at 500 ℃ for 5 minutes to enable carbon to permeate into the metal nickel layer; and after heating is stopped, naturally cooling the chamber to room temperature, precipitating carbon from the nickel layer, and growing high-defect graphene between the nickel layer and the quartz interface. Referring to the attached drawing, fig. 2 is an optical microscope image of the morphology of high defect state graphene obtained in this embodiment, in which the graphene shown at 1 is thicker and the graphene at 2 is thinner; referring to fig. 3, which is a raman spectrum of the obtained graphene, corresponding to positions 1 and 2 (corresponding to curves 1 and 2, respectively) in fig. 2, characteristic signals of the graphene, namely a D peak, a G peak and a 2D peak, can be measured, wherein the D peak of the raman spectrum is very strong, which indicates that the obtained graphene has high defects.
5. Placing the substrate prepared in the step 4 into FeCl with the concentration of 0.4mol/l 3 And etching to remove the nickel layer in the solution, and repeatedly cleaning with deionized water until the deionized water is colorless, thereby obtaining the graphene/quartz composite substrate.
And step two, taking graphene/quartz as a composite substrate, and epitaxially growing a gallium nitride micron column on the composite substrate by using a hydride vapor phase epitaxy method, wherein the method comprises the following specific steps:
1. placing the composite substrate into a cavity of a hydride vapor phase epitaxy system, and processing for 15 minutes at 960 ℃ in a hydrogen atmosphere;
2. NH is introduced after the hydrogen treatment is finished 3 And GaCl 3 Respectively used as a nitrogen source and a gallium source, the molar weight ratio V/III of the gallium source is 50, the growth pressure is 0.7Pa, and the nucleation process of the gallium nitride is about 20 minutes at the temperature of 950 ℃;
3. raising the temperature to 1050 ℃, and epitaxially growing the gallium nitride micron column structure for 2 hours; after the growth is finished, the temperature is reduced to 300 ℃ at the speed of 5 ℃ per minute, and then the mixture is naturally cooled to the room temperature.
Referring to fig. 4, it is a scanning electron microscope image of a gallium nitride micro-column grown on a graphene/quartz composite substrate by using a hydride vapor phase epitaxy method according to this embodiment; in the figure, a is a scanning electron microscope image of high defect state low temperature solid carbon source graphene, wherein natural steps can be seen, which indicates that the nucleation growth of gallium nitride can be realized without further processing the graphene; b and c are the top view and 30 degree elevation side view of the gallium nitride micro-column, respectively, and it can be seen that the surface of the micro-column is very smooth; the d-picture is a scanning electron micrograph of gallium nitride grown on a quartz substrate without a graphene insertion layer, and the results show that, except for some scattered polycrystalline grains, no gallium nitride micropillars can be obtained, because gallium nitride is difficult to nucleate directly on quartz. Fig. 4 shows that the graphene/quartz composite substrate provided by the invention can smoothly realize epitaxial growth of gallium nitride.
The gallium nitride microcolumn obtained in this example was subjected to a cathode ray fluorescence test, and the cathode ray was generated at a voltage of 5KV to 30 KV. Areas of good quality emit brighter light under excitation by the cathode rays than areas of poor quality. Referring to fig. 5, a scanning electron microscope (a) of one of the gan micropillars provided in this example and a corresponding crt fluorescence test (b) are shown, except that the central small area is dark, and the other areas are very bright. The prepared gallium nitride micro-column dislocation density is lower, and the quality of the gallium nitride crystal is higher.
Claims (4)
1. A preparation method of a III-nitride micro-column structure with graphene/dielectric material as a composite substrate is characterized in that a low-temperature solid carbon source method is adopted to directly grow graphene on the dielectric material, and comprises the following steps:
(1) Plating a nickel film layer on the surface of the dielectric material substrate by adopting an ion beam sputtering or electron beam evaporation process, wherein the thickness of the nickel layer is 50-500 nm;
(2) Ultrasonically dispersing graphite powder with the purity of more than 99.9% in ethanol, and coating the graphite powder on the surface of a nickel film;
(3) Placing the dielectric material substrate coated with graphite powder in a reaction chamber, heating for 3-10 minutes under the conditions of argon atmosphere and temperature of 300-600 ℃, and growing between the nickel layer and the interface of the dielectric material after natural cooling to obtain a graphene layer;
(4) Placing the substrate in FeCl 3 In the solution, the nickel layer is corroded;
(5) After the nickel layer is completely corroded, cleaning the nickel layer by using deionized water to obtain a graphene/dielectric material composite substrate taking graphene as an insertion layer;
(6) Growing a III-group nitride micro-column on a graphene insertion layer of the graphene/dielectric material composite substrate by adopting a hydride vapor phase epitaxy method or a metal organic chemical vapor deposition method to obtain the III-group nitride micro-column structure taking the graphene/dielectric material as the composite substrate.
2. The method for preparing the III-nitride micro-column structure with the graphene/dielectric material as the composite substrate according to claim 1, is characterized in that: the dielectric material comprises one of silicon dioxide, tantalum pentoxide, hafnium dioxide, zinc sulfide and zinc selenide.
3. The method for preparing the III-nitride micro-column structure with the graphene/dielectric material as the composite substrate according to claim 1, is characterized in that: the III-nitride is one of GaN, alN, inN and ternary or quaternary alloy thereof.
4. A III-nitride micro-column structure taking graphene/dielectric material as a composite substrate, which is obtained by the preparation method of claim 1, is characterized in that: growing a graphene insertion layer on a dielectric material; growing a III-nitride micron column on the graphene insertion layer, wherein the height of the micron column is 10-300 um, and the diameter of the micron column is 10-300 um.
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| CN103258926A (en) * | 2013-04-28 | 2013-08-21 | 西安交通大学 | LED vertical chip structure and manufacturing method |
| WO2013157014A1 (en) * | 2012-04-20 | 2013-10-24 | Tata Institute Of Fundamental Research | Group iii-nitride semiconducting material and a method of manufacturing the same |
| CN104045079A (en) * | 2014-06-25 | 2014-09-17 | 无锡格菲电子薄膜科技有限公司 | Method for epitaxially growing graphene on sapphire/epitaxial metal interface |
| CN105633225A (en) * | 2016-03-08 | 2016-06-01 | 西安电子科技大学 | Gallium nitride growth method based on graphene and magnetron sputtering aluminum nitride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013157014A1 (en) * | 2012-04-20 | 2013-10-24 | Tata Institute Of Fundamental Research | Group iii-nitride semiconducting material and a method of manufacturing the same |
| CN103258926A (en) * | 2013-04-28 | 2013-08-21 | 西安交通大学 | LED vertical chip structure and manufacturing method |
| CN104045079A (en) * | 2014-06-25 | 2014-09-17 | 无锡格菲电子薄膜科技有限公司 | Method for epitaxially growing graphene on sapphire/epitaxial metal interface |
| CN105633225A (en) * | 2016-03-08 | 2016-06-01 | 西安电子科技大学 | Gallium nitride growth method based on graphene and magnetron sputtering aluminum nitride |
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