CN104018124A - Process for preparing semiconductor material SiC film - Google Patents
Process for preparing semiconductor material SiC film Download PDFInfo
- Publication number
- CN104018124A CN104018124A CN201410273829.9A CN201410273829A CN104018124A CN 104018124 A CN104018124 A CN 104018124A CN 201410273829 A CN201410273829 A CN 201410273829A CN 104018124 A CN104018124 A CN 104018124A
- Authority
- CN
- China
- Prior art keywords
- evaporation
- sputtering
- semiconductor material
- annealing
- thin film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 25
- 239000004065 semiconductor Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 36
- 238000000137 annealing Methods 0.000 claims abstract description 33
- 230000008020 evaporation Effects 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000010408 film Substances 0.000 claims abstract description 25
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 20
- 239000010439 graphite Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
- 239000010409 thin film Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000011856 silicon-based particle Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 29
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 26
- 238000000034 method Methods 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种半导体材料SiC薄膜的制备工艺，它包括下述步骤：步骤1、选取石墨片为衬底材料，并将石墨片打磨清洗干燥；步骤2、将石墨片固定在蒸镀室上方的样品架上，Si颗粒放置在蒸发坩埚内；步骤3、蒸镀；步骤4、蒸镀后冷却；步骤5、将蒸镀冷却后的石墨片固定在磁控溅射溅射室的转盘上，C靶材放置在射频靶上，溅射气体为Ar气；步骤6、溅射；步骤7、溅射后冷却，再取出置于高真空退火炉中退火，形成半导体SiC多晶薄膜；解决了传统采用单晶硅衬底作为基片制备碳化硅薄膜存在的成本高、工艺繁琐以及硅衬底与碳化硅之间存在较大的晶格失配和热膨胀失配，严重限制了其器件的性能和使用寿命等问题。
The invention discloses a preparation process of a semiconductor material SiC thin film, which comprises the following steps: step 1, selecting a graphite sheet as a substrate material, polishing, cleaning and drying the graphite sheet; step 2, fixing the graphite sheet in an evaporation chamber On the upper sample rack, Si particles are placed in the evaporation crucible; step 3, evaporation; step 4, cooling after evaporation; step 5, fixing the cooled graphite sheet after evaporation on the turntable of the magnetron sputtering chamber On the above, the C target is placed on the radio frequency target, and the sputtering gas is Ar gas; step 6, sputtering; step 7, cooling after sputtering, and then taking it out and annealing in a high vacuum annealing furnace to form a semiconductor SiC polycrystalline film; It solves the high cost and cumbersome process of preparing silicon carbide films traditionally using single crystal silicon substrates as substrates, as well as the large lattice mismatch and thermal expansion mismatch between silicon substrates and silicon carbide, which severely limits its devices performance and service life issues.
Description
Technical field
The invention belongs to carborundum films technology of preparing, relate in particular to a kind of preparation technology of semiconductor material SiC film.
Background technology
Silicon carbide (SiC) film has unique characteristics such as the chemical stability that energy gap is large, breakdown electric field is high, thermal conductivity is large, electronics saturation drift velocity is high, specific inductivity is little, capability of resistance to radiation is strong, good, it is gained great popularity at aspects such as high frequency, superpower, high-temperature electronic device and photoelectric devices, be described as one of third generation semiconductor material most with prospects.
In silicon carbide-based device application, the quality of high-power component heat dispersion directly affects its performance and life-span, and the quality problems of the film preparation and property of direct vivid device again.Therefore,, in actually operating, of paramount importance is exactly the selection of substrate material.By various preparation methods, in monocrystalline substrate, successfully prepared now carborundum films material both at home and abroad.But owing to there is the problems such as larger lattice mismatch and thermal expansion mismatch between silicon substrate and silicon carbide, seriously limited the performance and used life of its device.
Summary of the invention
The technical problem to be solved in the present invention: a kind of preparation technology of semiconductor material SiC film, using solve tradition adopt monocrystalline substrate as substrate, prepare that the cost that carborundum films exists is high, technique is loaded down with trivial details and silicon substrate and silicon carbide between there is larger lattice mismatch and thermal expansion mismatch, seriously limited the problems such as performance and used life of its device.
Technical solution of the present invention:
A preparation technology for semiconductor material SiC film, it comprises the steps:
Step 1, to choose graphite flake be substrate material, and by the graphite flake cleaning-drying of polishing;
Step 2, graphite flake is fixed on the specimen holder of deposited chamber top, Si particle is placed in evaporator crucible;
Step 3, evaporation;
Cooling after step 4, evaporation;
Step 5, the cooled graphite flake of evaporation is fixed on the rotating disk of magnetron sputtering sputtering chamber, C target is placed on radio frequency target, and sputter gas is Ar gas;
Step 6, sputter;
Cooling after step 7, sputter, then take out and to be placed in high vacuum annealing furnace and to anneal, semi-conductor SiC polycrystal film formed.
The preparation technology of a kind of semiconductor material SiC film according to claim 1, first vacuumizes deposited chamber before evaporation, when vacuum tightness is less than or equal to 3.0 * 10-4Pa, starts evaporation; Evaporation current is progressively added to 110A, starts evaporation; The power of resistance-type thermal evaporation during evaporation is 16～19KW, and vaporator rate remains on 28～30nm/min, and evaporation time is 8 minutes.
Before sputter, first sputtering chamber is vacuumized, when vacuum tightness is less than or equal to 2.0 * 10-5Pa, start sputter, sputtering pressure 2.0Pa, argon Ar flow 15sccm, power during sputter is 110W, sputtering time is 20 minutes.
In high vacuum annealing furnace described in step 7, annealing furnace back end vacuum tightness is less than or equal to 4.0 * 10-4Pa.
In high vacuum annealing furnace described in step 7, anneal, annealing time 1-5 hour, 950 ℃ of annealing temperatures
Beneficial effect of the present invention:
The present invention adopts resistance-type thermal evaporation and magnetron sputtering technique, has prepared environment-friendly semiconductor SiC thin-film material.The ultimate principle of resistance-type thermal evaporation heating is, evaporating materials is put into suitable resistance heating body, and energising makes the evaporation of evaporating materials direct heating, thereby makes evaporating materials deposit to and on substrate, form film with gaseous form.The ultimate principle of magnetron sputtering is, with high energy particle (Ar), clashes into target material surface, after the atom with target material surface or molecule carry out energy exchange, from fly out atom or molecule deposition of target material surface, at substrate, forms film; The present invention adopts resistance-type thermal evaporation and magnetron sputtering technique in graphite substrate, to deposit Si/C film, with being placed in vacuum annealing furnace, anneals.Annealing furnace vacuum tightness is less than or equal to 4.0 * 10
-4pa, annealing time 1-5 hour, 950 ℃ of annealing temperatures, obtain semiconductor material SiC film.At present domestic there is not yet in graphite substrate this evaporation of material resistance formula and the preparation technology of magnetron sputtering combined techniques and the report that associated hot treatment condition are studied; Adopt that graphite substrate is low with respect to traditional substrate cost compare, satisfactory mechanical property and chemical stability good, and conduction and heat dispersion are considerably beyond metallic copper; In addition, because graphite substrate has laminate structure, between each layer, with weak Van der Waals Wurz power combination, than being easier to separate silicon carbide from graphite substrate, transfer on other substrates, realize the preparation of silicon carbide device; Compared with prior art, it is lower that the present invention has production cost, the simple advantage of processing sequence; The invention solves tradition adopt monocrystalline substrate as substrate, prepare that the cost that carborundum films exists is high, technique is loaded down with trivial details and silicon substrate and silicon carbide between there is larger lattice mismatch and thermal expansion mismatch, seriously limited the problems such as performance and used life of its device.
accompanying drawing explanation:
Fig. 1 is sample X-ray diffractogram prepared by the present invention, in annealing temperature, is 950 ℃, and annealing time is respectively the X-ray diffractogram of 1～5h;
Fig. 2-Fig. 5 is Sample Scan Electronic Speculum figure prepared by the present invention, at 950 ℃ of annealing times, is respectively the scanning electron microscope (SEM) photograph of 1h, 2h, 3h, 5h.
embodiment:
Embodiments of the invention 1:
Step 1, graphite flake is smooth with #0-#6 sand papering, uses respectively 30% nitric acid, dehydrated alcohol, and acetone cleans 15 minutes successively, and object is to remove surperficial organism etc., then uses washed with de-ionized water 5 times, each 10 minutes.Finally the sample cleaning up is placed under 80 ℃ of conditions of loft drier and toasts, till surperficial complete drying.
Step 2, due to test with graphite substrate because area is less, use shell fragment to be fixed on the specimen holder of deposited chamber top, Si particle is directly placed in evaporator crucible.
Step 3, deposited chamber is vacuumized, when vacuum tightness is less than or equal to 3.0 * 10
-4during Pa, and keep for some time, then start evaporation, evaporation current is progressively added to 110A, formally starts evaporation; The power of resistance-type thermal evaporation during evaporation is 16～19KW, and vaporator rate remains on 28～30nm/min, and evaporation time is 8 minutes.
After completing, step 4, evaporation naturally cool to room temperature;
Step 5, take out the sputtering chamber that cooled sample is placed in magnetron sputtering, C target is placed on radio frequency target.
Step 6, first sputtering chamber is vacuumized, when vacuum tightness is less than or equal to 2.0 * 10
-5during Pa, and keep for some time; Then start sputter, sputtering pressure 2.0Pa, argon flow amount 15sccm, power during sputter is 110W, sputtering time is 20 minutes.
After step 7, sputter finish, naturally cool to room temperature, take out sample and be placed in high-temperature annealing furnace, in high vacuum annealing furnace, annealing furnace back end vacuum tightness is less than or equal to 4.0 * 10
-4pa.Annealing time 1-5 hour, 950 ℃ of annealing temperatures, form SiC polycrystal film.
Si particle purity is that 99.99%, C target purity is 99.99%.
The semiconductor material silicon carbide polycrystal film forming refer on graphite substrate, deposited 8 minutes (min) Si films, (min) C film after annealing reaction in 20 minutes generates.
Fig. 1 is the X-ray diffractogram of the sample prepared of 950 ℃ of different annealing times, visible in figure, except substrate C diffraction peak, there is SiC diffraction peak, and with PDF standard spectrum (card number: 73-2085), the crystal face (0075) (0141) (1175) of SiC diffraction peak is corresponding one by one, illustrate under preparation condition of the present invention, prepared the good SiC film of crystalline condition.
Fig. 2-Fig. 5 is the scanning electron microscope (SEM) photograph of the sample surface morphology prepared of 950 ℃ of different annealing times, and after result shows annealing 2h, SiC crystal grain is good to sample surfaces coverage, and grain-size is larger, and surface is comparatively smooth.Under the annealing conditions adopting in experiment, all there is the good SiC film of crystalline state to occur.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410273829.9A CN104018124B (en) | 2014-06-19 | 2014-06-19 | Process for preparing semiconductor material SiC film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410273829.9A CN104018124B (en) | 2014-06-19 | 2014-06-19 | Process for preparing semiconductor material SiC film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104018124A true CN104018124A (en) | 2014-09-03 |
| CN104018124B CN104018124B (en) | 2017-04-19 |
Family
ID=51435110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410273829.9A Expired - Fee Related CN104018124B (en) | 2014-06-19 | 2014-06-19 | Process for preparing semiconductor material SiC film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104018124B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543795A (en) * | 2015-12-18 | 2016-05-04 | 厦门大学 | Growing method for polycrystalline silicon carbide thin film |
| CN109166790A (en) * | 2018-07-28 | 2019-01-08 | 西安交通大学 | A method of utilizing perovskite oxide piezoelectric membrane on metal stresses layer removing graphene |
| CN111809149A (en) * | 2020-06-08 | 2020-10-23 | 贵州民族大学 | A kind of preparation method of 3C-SiC thin film |
| CN112548359A (en) * | 2020-11-30 | 2021-03-26 | 贵州大学 | Preparation method of surface functional composite structured monocrystalline silicon carbide |
| CN117051359A (en) * | 2023-09-22 | 2023-11-14 | 苏州市职业大学（苏州开放大学） | Device and method for preparing silicon carbide film on surface of graphite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594648A (en) * | 2003-09-10 | 2005-03-16 | 中国科学院半导体研究所 | Process for preparing silicon carbide film by magnetron sputtering method |
| CN101798680A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Magnetron sputtering preparation process for Mg2Si thin film made of environment-friendly semiconductor material |
| CN102373417A (en) * | 2011-11-08 | 2012-03-14 | 陕西科技大学 | Method for preparing antioxidant SiC coating on surface of graphite material |
-
2014
- 2014-06-19 CN CN201410273829.9A patent/CN104018124B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594648A (en) * | 2003-09-10 | 2005-03-16 | 中国科学院半导体研究所 | Process for preparing silicon carbide film by magnetron sputtering method |
| CN101798680A (en) * | 2010-04-15 | 2010-08-11 | 贵州大学 | Magnetron sputtering preparation process for Mg2Si thin film made of environment-friendly semiconductor material |
| CN102373417A (en) * | 2011-11-08 | 2012-03-14 | 陕西科技大学 | Method for preparing antioxidant SiC coating on surface of graphite material |
Non-Patent Citations (1)
| Title |
|---|
| SEUNG-HYUN MOON ET.AL: "THE EFFECTS ON HEAT TREATMENT OF SIC COATED / GRAPHITE PLATE BY RF SPUTTERING SYSTEM", 《ADVANCED MATERIALS DEVELOPMENT AND PERFORMANCE (AMDP2011) INTERNATIONAL JOURNAL OF MODERN PHYSICS: CONFERENCE SERIES》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543795A (en) * | 2015-12-18 | 2016-05-04 | 厦门大学 | Growing method for polycrystalline silicon carbide thin film |
| CN109166790A (en) * | 2018-07-28 | 2019-01-08 | 西安交通大学 | A method of utilizing perovskite oxide piezoelectric membrane on metal stresses layer removing graphene |
| CN111809149A (en) * | 2020-06-08 | 2020-10-23 | 贵州民族大学 | A kind of preparation method of 3C-SiC thin film |
| CN111809149B (en) * | 2020-06-08 | 2023-01-03 | 贵州民族大学 | Preparation method of 3C-SiC film |
| CN112548359A (en) * | 2020-11-30 | 2021-03-26 | 贵州大学 | Preparation method of surface functional composite structured monocrystalline silicon carbide |
| CN112548359B (en) * | 2020-11-30 | 2023-03-21 | 贵州大学 | Preparation method of surface functional composite structured monocrystalline silicon carbide |
| CN117051359A (en) * | 2023-09-22 | 2023-11-14 | 苏州市职业大学（苏州开放大学） | Device and method for preparing silicon carbide film on surface of graphite material |
| CN117051359B (en) * | 2023-09-22 | 2024-08-23 | 苏州市职业大学（苏州开放大学） | A device and method for preparing silicon carbide film on the surface of graphite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104018124B (en) | 2017-04-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102020263B (en) | Method for synthesizing graphene film material | |
| CN104018124A (en) | Process for preparing semiconductor material SiC film | |
| CN105018881B (en) | One kind contains V6O13The amorphous oxide vanadium thin-film material and preparation method of crystal | |
| CN100558933C (en) | A kind of preparation method of cubic boron nitride film | |
| CN105714382A (en) | Preparation method of large-size Cu(100) single-crystal copper foil | |
| CN106868469B (en) | A kind of method for preparing graphene without metal catalyst on silicon base | |
| CN104157744A (en) | Method realizing diamond base GaN base on epitaxial layer transferring | |
| CN106283052B (en) | A two-dimensional material regulating silicon-carbon composite structure hydrogen barrier coating and preparation method thereof | |
| CN111017920A (en) | High-thermal-conductivity graphite film and preparation method and application thereof | |
| CN110273176B (en) | Method for preparing large-area copper Cu (111) single crystal | |
| CN104805405A (en) | Aluminium nitride piezoelectric film and preparation method thereof | |
| CN104909359A (en) | A Direct and Rapid Preparation of Single-layer Graphene on SiO2/Si Substrate | |
| CN101339906A (en) | Preparation process of novel environmental semi-conductor photoelectronic material beta-FeSi2 film | |
| CN104209524A (en) | Preparation method of flexible pyroelectric film | |
| CN106399937B (en) | A method of preparing preferred orientation bismuth telluride thermal electric film | |
| CN102925866B (en) | Preparation technology for single-phase Mg2Si semiconductor film | |
| CN113264774A (en) | SiC crystal synthesized by seed induced microwave and preparation method thereof | |
| CN105441877B (en) | The technique that resistance-type thermal evaporation prepares ferrimagnet Fe3Si films | |
| CN106884141A (en) | A kind of Ti2The preparation method of AlC MAX phase films | |
| CN109988998A (en) | A kind of preparation method of multi-element high-entropy alloy thin film | |
| CN105274483A (en) | A kind of preparation method of negative thermal expansion material Sc2W3O12 thin film | |
| CN106653569A (en) | Preparation method of semiconductor material beta-SiC film | |
| CN105088160A (en) | Method for preparing SrRuO3 thin film with high (110) preferred orientation | |
| CN110453175A (en) | A kind of preparation method of vanadium oxide film | |
| CN104505462A (en) | Organic metal halide film and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170419 Termination date: 20210619 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |