CN107895685A - The preparation method of highly crystalline quality graphene - Google Patents

The preparation method of highly crystalline quality graphene Download PDF

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CN107895685A
CN107895685A CN201710877794.3A CN201710877794A CN107895685A CN 107895685 A CN107895685 A CN 107895685A CN 201710877794 A CN201710877794 A CN 201710877794A CN 107895685 A CN107895685 A CN 107895685A
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sic
etching
substrate
materials
graphene
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辛斌
尹巍
杨文耀
刘文波
夏继宏
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/02373—Group 14 semiconducting materials
    • H01L21/02378—Silicon carbide
    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02524—Group 14 semiconducting materials
    • H01L21/02527—Carbon, e.g. diamond-like carbon
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02524—Group 14 semiconducting materials
    • H01L21/02529—Silicon carbide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02634—Homoepitaxy
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
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Abstract

The present invention relates to a kind of preparation method of highly crystalline quality graphene, this method includes：Choose SiC substrate；Etching SiC substrate forms the pre-etching substrate of mesa structure；In the pre-etching Grown 3C SiC materials；3C SiC materials are pyrolyzed, to complete the preparation of highly crystalline graphene.The present invention is effectively isolated influencing each other between defect, perfect crystalline membrane is realized on etching table top by pre-etching SiC substrate；In addition, the 3C SiC directions that atomic layer arranges on [111] direction are constant, the generation of step beam can be avoided, so as to prepare higher-quality graphene.

Description

The preparation method of highly crystalline quality graphene
Technical field
The present invention relates to field of semiconductor devices, more particularly to a kind of preparation method of highly crystalline quality graphene.
Background technology
The unique physicochemical properties of graphene, are expected in semiconductor, photovoltaic, lithium battery, biology, medical treatment, display etc. Tradition and new industry bring revolutionary advancement.Scientific circles and industrial quarters explore the extensive side for preparing high-quality graphene always Method.
The method for preparing graphene at present has two major classes, and the first kind is exactly from top to bottom, by the model for destroying graphite layers Moral wals force is peeled off graphite layer by layer, and the final acquisition number of plies is less or the graphene of individual layer, this kind of method mainly include Mechanical stripping method, liquid phase stripping method are with oxidation-reduction method；Another major class is from bottom to top, composition to be reconstructed by the aggregation of C atoms Graphene film, this kind of method mainly include chemical vapor infiltration and carborundum pyrolysismethod.Because first kind preparation method has The reasons such as large area and the large-scale production that preparation technology is unstable, poor repeatability, yield and efficiency are low, is difficult to graphene It is difficult in terms of being applied to semiconductor devices preparation.The preparation method of wafer level graphene has CVD epitaxial growth methods at present With SiC high temperature pyrolytic cracking (HTP)s.CVD epitaxial growth method shortcomings are that energy resource consumption is big, and graphene sheet layer and the substrate of acquisition interact By force, the graphene in Many times metal substrate needs to carry out being transferred on dielectric (such as SiO2Deng substrate), recycle it Electrology characteristic carries out device preparation.Therefore whole process complexity is higher, and material property loss is serious, and material is easily contaminated, Thus a series of problems, such as bringing process repeatability.
SiC high temperature pyrolytic cracking (HTP)s are under UHV condition, and monocrystalline 4H/ is removed by means such as electron bombardment, acid cleanings Oxide on 6H-SiC substrates, then (1250-1450 DEG C) heating under vacuum or protective gas environment by substrate, make surface of SiC Si atoms distil, and the C atoms left reconstruct to form graphene.For preparing device, the advantage of this method includes：1), SiC is served as a contrast The graphene grown on basal surface need not carry out cumbersome transfer step and can be applied to device manufacture, avoid material transfer The pollution problem that process is brought.2), SiC sheets as semiconductor even semi-insulator, its energy gap is big, breakdown electric field is high, The each side performances such as thermal conductivity, heat resistance, radioresistance and chemical property stabilization are good.It is very suitable as substrate.3)、SiC Substrate can make graphene produce energy gap, be advantageous to improve the switching characteristic of device.
SiC substrate growth graphene can utilize the technological means such as conventional lithography or electron printing directly on whole chip Carry out the etching of device or circuit.Whole preparation technology can be incorporated into traditional device preparation technology to realize large-scale production. But at present there is the problems such as graphene domain size is small, discontinuous, crystallization is in uneven thickness in SiC pyrolysismethods, limit the party Formula prepares the application prospect of graphene.
The content of the invention
Therefore, to solve technological deficiency and deficiency existing for prior art, the present invention proposes a kind of highly crystalline quality graphite The preparation method of alkene.
Specifically, the preparation method for a kind of highly crystalline quality graphene that one embodiment of the invention proposes, including：
Choose SiC substrate；
Etch the pre-etching substrate that the SiC substrate forms mesa structure；
In the pre-etching Grown 3C-SiC materials；
The 3C-SiC materials are pyrolyzed, to complete the preparation of the highly crystalline graphene.
In one embodiment of the invention, the SiC substrate is 4H-SiC substrates or 6H-SiC substrates.
In one embodiment of the invention, SiC substrate described in pre-etching forms the pre-etching substrate of mesa structure, bag Include：
Pre-etching figure is formed in the SiC substrate；
Using ICP techniques or RIE techniques, the pre-etching substrate of mesa structure is formed in SiC substrate etching table top.
In one embodiment of the invention, pre-etching figure is formed in the SiC substrate, including：
Metal and photoresist are deposited in the SiC substrate；
Using standard development technique, using mask plate, the photoresist is etched, forms the pre-etching figure.
In one embodiment of the invention, the length of side for the polygon that the mesa structure is formed along cross section is 500 μm ~5mm, the depth formed along longitudinal section are 2~4 μm.
In one embodiment of the invention, the SiC substrate is 4H-SiC substrates, correspondingly, is served as a contrast in the pre-etching Before 3C-SiC materials being grown on bottom, in addition to：
The homoepitaxy 4H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 4H-SiC layers.
In one embodiment of the invention, in the pre-etching Grown 3C-SiC materials, including：
In the 3C-SiC materials that the 4H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
In one embodiment of the invention, the SiC substrate is 6H-SiC substrates, correspondingly, is served as a contrast in the pre-etching Before 3C-SiC materials being grown on bottom, in addition to：
The homoepitaxy 6H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 6H-SiC layers.
In one embodiment of the invention, in the pre-etching Grown 3C-SiC materials, including：
In the 3C-SiC materials that the 6H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
In one embodiment of the invention, the 3C-SiC materials are pyrolyzed, including：
At a temperature of 1300 DEG C -1500 DEG C, using SiC epitaxial furnaces, the 3C-SiC materials are pyrolyzed.
The present invention realizes large area by pre-etching SiC substrate, uniformly connected on the basis of traditional Si C pyrolytic graphite alkene The preparation of continuous, highly crystalline quality graphene；It is simultaneously optimization graphene preparation technology, it is surface optimization to introduce 3C-SiC epitaxial layers Cushion.
The crystalline quality that the present invention improves graphene improves the surface smoothness of SiC substrate and reduces surface defect first. The flatness selection 3C-SiC for improving substrate surface carries out graphene extension.Because 4H/6H-SiC crystal exists in the z-axis direction Turnover phenomenon, therefore there is step Shu Xianxiang in the plane of crystal being easy in nearly (0001) face.And 3C-SiC is on [111] direction The direction of atomic layer arrangement is constant, the generation of step beam can be avoided, so as to prepare higher-quality graphene.Reduce surface Defect effective manner is by pre-etching SiC, is effectively isolated influencing each other between defect, and perfect knot is realized on etching table top Brilliant film.
By the detailed description below with reference to accompanying drawing, other side of the invention and feature become obvious.But it should know Road, the accompanying drawing is only the purpose design explained, not as the restriction of the scope of the present invention, because it should refer to Appended claims.It should also be noted that unless otherwise noted, it is not necessary to which scale accompanying drawing, they only try hard to concept Ground illustrates structure and flow described herein.
Brief description of the drawings
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in detail.
Fig. 1 is a kind of flow chart of the preparation method of highly crystalline quality graphene provided in an embodiment of the present invention；
Fig. 2 is a kind of conventional mask；
Fig. 3 is a kind of mask plate of etching SiC substrate provided in an embodiment of the present invention；
Fig. 4 a- Fig. 4 i are that a kind of technique of preparation method of highly crystalline quality graphene provided in an embodiment of the present invention is illustrated Figure.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in conjunction with the accompanying drawings to the present invention Embodiment be described in detail.
Embodiment one
Fig. 1 is a kind of flow chart of the preparation method of highly crystalline quality graphene provided in an embodiment of the present invention.This method Comprise the following steps：
Step a, SiC substrate is chosen；
Step b, the pre-etching substrate that the SiC substrate forms mesa structure is etched；
Step c, in the pre-etching Grown 3C-SiC materials；
Step d, the 3C-SiC materials are pyrolyzed, to complete the preparation of the highly crystalline graphene
Wherein, SiC substrate described in step a is 4H-SiC substrates or 6H-SiC substrates.
Wherein, step b can include：
Step b1, pre-etching figure is formed in the SiC substrate；
Step b2, using ICP techniques or RIE techniques, the pre-etching of mesa structure is formed in SiC substrate etching table top Substrate.
Further, step b1 can include：
Step b11, metal and photoresist are deposited in the SiC substrate；
Step b12, using standard development technique, using mask plate, the photoresist is etched, forms the pre-embossed corrosion figure Shape.
Further, the length of side for the polygon that the mesa structure in step b2 is formed along cross section be 500 μm~ 5mm, the depth formed along longitudinal section are 2~4 μm.
Wherein, the SiC substrate is 4H-SiC substrates, before step c, can also be included：
The homoepitaxy 4H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 4H-SiC layers.
Further, for step c, can include：
In the 3C-SiC materials that the 4H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
Wherein, the SiC substrate is 6H-SiC substrates, before step c, can also be included：
The homoepitaxy 6H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 6H-SiC layers.
Further, for step c, can include：
In the 3C-SiC materials that the 6H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
Wherein, for step d, can include：
At a temperature of 1300 DEG C -1500 DEG C, using SiC epitaxial furnaces, the 3C-SiC materials are pyrolyzed.
Beneficial effects of the present invention are specially：
1st, because 4H/6H-SiC crystal has turnover phenomenon in the z-axis direction, therefore it is easy to the crystalline substance in nearly (0001) face There is step Shu Xianxiang in body surface face, by pre-etching SiC, is effectively isolated influencing each other between defect, is realized on etching table top Perfect crystalline membrane；
2nd, the 3C-SiC directions that atomic layer arranges on [111] direction are constant, the generation of step beam can be avoided, so as to make It is standby go out higher-quality graphene.
Embodiment two
The present embodiment (6H-SiC substrates are similarly) by taking 4H-SiC substrates as an example, the preparation of the highly crystalline quality graphene of large area Method comprises the following steps：
Step 21, pre-etching table top
As shown in Fig. 2 Fig. 2 is a kind of conventional mask, carry out ICP, RIE etching and subsequent epitaxial process show as it is each to The opposite sex, etch rate and growth rate may be caused in the inconsistent situation of different directions.As shown in figure 3, Fig. 3 is real for the present invention A kind of mask plate of etching SiC substrate of example offer is provided.From [0001] direction, observation has triple axially symmetric structures to hexagonal crystal system, Carry out ICP, RIE etching and follow-up epitaxial process is presented with more preferable isotropism feature.From commercial, positive axis 4H- SiC substrate, mask is done using metal, using the mask prepared along crystal face (1-100) face,；By ICP (inductively wait from Daughter) etching or RIE reaction and plasmas etching, SiC polishing Si faces substrate on 500 μ m of dry etching, 500 μm of -5mm × 5mm Etc. table top not of uniform size, i.e. the length of side is 500 μm of -5mm table top, all table tops by raceway groove that etching depth is 2~4 μm every From, it is preferable that the channel isolation that can be about 3 μm with selective etching depth.Specially：
Step 211, the Al for precipitating in 4H-SiC substrate surfaces using PVD or technique for vacuum coating 0.5-1 μm；
Step 212, using standard development technique and mask pre-etching figure is formed on 4H-SiC substrates, including：
Photoresist is deposited in Al layer surfaces, using standard development technique and mask, photoresist is etched, forms pre-embossed corrosion figure Shape.
Step 213, using wet-etching technology the Al of exposure is removed；(according to acetic acid：Phosphoric acid：Nitric acid：Water=4：4：1： 1 ratio performs etching)
Step 214, utilize solvent and plasma removal photoresist；
Step 215, utilize ICP or RIE techniques etching 4H-SiC substrates；ICP or RIE techniques use STS MP- 0566 instrument, 50sccm SF are used in etching process6And 5sccm oxygen, 5mTorr etching cavity pressure.
Step 216, utilize wet-etching technology removal Al masks.
Step 22, homoepitaxy, growing surface are (0001) face 4H-SiC；
Step 221, the 4H-SiC substrates after etching are cleaned by standard technology, are dried up；
Step 222,4H-SiC substrates are put into epitaxial furnace；1550-1700 DEG C is heated in Silicon-rich environment；Then it is warm Degree keeps constant closing silicon source 3min, removes the element silicon in epitaxial furnace, introduces carbon source successively and silicon source carries out homoepitaxy 3- 5min, form the 4H-SiC substrates that mesa surfaces are (0001) face.
Step 23, hetero-epitaxy surface are (111) face 3C-SiC
By the means that cool, it is nucleated 3C-SiC.After 4H-SiC substrate table tops surface nucleation grows 3C-SiC films, rise High-temperature is to 1600 DEG C, and to form the 3C-SiC in (111) face, 3C-SiC is generally non-impurity-doped, to realize 3C-SiC as insulation Layer.
Step 24, pyrolysismethod prepare graphene
Hydrogen, Sources gas and impurity gas are closed, only retains argon gas composition, reduces temperature to 1300 DEG C -1500 DEG C, while auxiliary Gases Chlorine is introduced, pyrolytic graphite alkene is carried out in epitaxial furnace.
Beneficial effects of the present invention are specially：
1st, in the present embodiment, step 22,23,24 can under the gaseous environment in CVD equipment in-situ (original position) it is complete Into, and cleaning process is introduced after step 21, the pollution that removable dry etching is brought, therefore, the program can be effectively Prevent pollution problem；
2nd, the step 23 of the present embodiment, except the appearance that can avoid transferring in 4H/6H-SiC substrates, can also be mixed using original position Miscellaneous mode adjusts the doping concentration on SiC top layers, and the requirement for advantageously reducing SiC substrate (such as can be in N-type by adulterating means The SiC layer of I types or p-type is inserted between SiC substrate and the graphene ultimately formed), simultaneously because the doping concentration of graphene with The doping concentration of SiC layer is relevant, therefore the doping concentration of final graphene layer can also be adjusted by 3C-SiC layers doping concentration.
Embodiment three
It is a kind of system of highly crystalline quality graphene provided in an embodiment of the present invention to refer to Fig. 4 a- Fig. 4 g, Fig. 4 a- Fig. 4 g The process schematic representation of Preparation Method.On the basis of above-described embodiment, the present embodiment is by more detail to the technique stream of the present invention Journey is introduced.This method includes：
Step 31, using PVD or technique for vacuum coating, 0.5-1 μm of gold is deposited on positive axis 4H-SiC substrates 31 Belong to Al 32, as shown in fig. 4 a.
Step 32, the photoresist 33 isolated is prepared on Al32 films surface using standard development technology, as shown in Figure 4 b.
Step 33, using wet-etching technology by the films of Al 32 etch, as illustrated in fig. 4 c.
Step 34, using solvent, plasma etc. remove photoresist 33, as shown in figure 4d.
Step 35, using ICP or RIE techniques 4H-SiC substrates 31 are etched, as shown in fig 4e.
Step 36, remove Al32 films using wet-etching technology, obtain table top pre-etching substrate 34, as shown in fig. 4f.
Step 37, cleaning table top pre-etching substrate 34, the homoepitaxy 4H-SiC on the table top of table top pre-etching substrate 34, The table top pre-etching substrate 35 that mesa surfaces are (0001) face is generated, as shown in figure 4g；
Step 38, table top pre-etching substrate 35 is put into SiC epitaxial furnaces VP508, in the platform of table top pre-etching substrate 35 One layer of 3C-SiC 36 is grown on rank, as shown in figure 4h.
Step 39, in SiC epitaxial furnaces, by 3C-SiC 36 pyrolysis form graphene 37, as shown in figure 4i.
In summary, system of the specific case to highly crystalline quality graphene provided in an embodiment of the present invention used herein The principle and embodiment of Preparation Method are set forth, and the explanation of above example is only intended to help the method for understanding the present invention And its core concept；Meanwhile for those of ordinary skill in the art, according to the thought of the present invention, in embodiment and There will be changes in application, in summary, this specification content should not be construed as limiting the invention, the present invention Protection domain should be defined by appended claim.

Claims (10)

  1. A kind of 1. preparation method of highly crystalline quality graphene, it is characterised in that including：
    Choose SiC substrate；
    Etch the pre-etching substrate that the SiC substrate forms mesa structure；
    In the pre-etching Grown 3C-SiC materials；
    The 3C-SiC materials are pyrolyzed, to complete the preparation of the highly crystalline graphene.
  2. 2. according to the method for claim 1, it is characterised in that the SiC substrate is that 4H-SiC substrates or 6H-SiC are served as a contrast Bottom.
  3. 3. according to the method for claim 1, it is characterised in that SiC substrate described in pre-etching forms the pre-embossed of mesa structure Substrate is lost, including：
    Pre-etching figure is formed in the SiC substrate；
    Using ICP techniques or RIE techniques, the pre-etching substrate of mesa structure is formed in SiC substrate etching table top.
  4. 4. according to the method for claim 3, it is characterised in that pre-etching figure is formed in the SiC substrate, including：
    Metal and photoresist are deposited in the SiC substrate；
    Using standard development technique, using mask plate, the photoresist is etched, forms the pre-etching figure.
  5. 5. according to the method for claim 3, it is characterised in that the side for the polygon that the mesa structure is formed along cross section A length of 500 μm~5mm, the depth formed along longitudinal section are 2~4 μm.
  6. 6. according to the method for claim 2, it is characterised in that the SiC substrate is 4H-SiC substrates, correspondingly, in institute Before stating pre-etching Grown 3C-SiC materials, in addition to：
    The homoepitaxy 4H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 4H-SiC layers.
  7. 7. according to the method for claim 6, it is characterised in that in the pre-etching Grown 3C-SiC materials, bag Include：
    In the 3C-SiC materials that the 4H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
  8. 8. according to the method for claim 2, it is characterised in that the SiC substrate is 6H-SiC substrates, correspondingly, in institute Before stating pre-etching Grown 3C-SiC materials, in addition to：
    The homoepitaxy 6H-SiC materials on the pre-etching substrate, using the pre-etching substrate surface formed crystal face as (0001) 6H-SiC layers.
  9. 9. according to the method for claim 8, it is characterised in that in the pre-etching Grown 3C-SiC materials, bag Include：
    In the 3C-SiC materials that the 6H-SiC layer surfaces growth crystal face that crystal face is (0001) is (111).
  10. 10. according to the method for claim 1, it is characterised in that the 3C-SiC materials are pyrolyzed, including：
    At a temperature of 1300 DEG C~1500 DEG C, the 3C-SiC materials are pyrolyzed using SiC epitaxial furnaces.
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Publication number Priority date Publication date Assignee Title
CN116514112A (en) * 2023-06-09 2023-08-01 中电科先进材料技术创新有限公司 Preparation method of large-area graphene on silicon surface
CN116514112B (en) * 2023-06-09 2023-12-19 中电科先进材料技术创新有限公司 Preparation method of large-area graphene on silicon surface

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Application publication date: 20180410