CN104018124A - Process for preparing semiconductor material SiC film - Google Patents
Process for preparing semiconductor material SiC film Download PDFInfo
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- 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
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- evaporation
- sputtering
- graphite flake
- semiconductor material
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Abstract
The invention discloses a process for preparing a semiconductor material SiC film. The process comprises the following steps: 1, selecting a graphite flake as a substrate material, and polishing, cleaning and drying the graphite flake; 2, fixing the graphite flake on a sample rack above an evaporation chamber, and placing Si particles into an evaporation crucible; 3, evaporating; 4, cooling after evaporating; 5, fixing the evaporated and cooled graphite flake on a turntable of a magnetron sputtering chamber, and placing a C target on a radio frequency target, wherein the sputtering gas is Ar gas; 6, sputtering; 7, cooling after sputtering, and then taking out to place in a high-vacuum annealing furnace to anneal, so as to form a semiconductor SiC polycrystalline film. The problems of high cost and fussy process, and the problem that large lattice mismatch and thermal expansion mismatch existing between the silicon substrate and silicon carbide seriously limit the performance and the service life of an apparatus in the traditional preparation method of the silicon carbide film by adopting a single crystal silicon substrate as a substrate are solved.
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)
1. a preparation technology for semiconductor material SiC film, it comprises the steps:
Step 1, to choose graphite flake be substrate material, by the graphite flake cleaning-drying of polishing;
Step 2, the graphite flake after step 1 is processed are fixed on the specimen holder of deposited chamber top, and 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.
2. the preparation technology of a kind of semiconductor material SiC film according to claim 1, is characterized in that: before evaporation, first deposited chamber is vacuumized, when vacuum tightness is less than or equal to 3.0 * 10-4Pa, start 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.
3. the preparation technology of a kind of semiconductor material SiC film according to claim 1, is characterized in that: before sputter, first sputtering chamber is vacuumized, vacuum tightness is less than or equal to 2.0 * 10
-5during Pa, start sputter, sputtering pressure 2.0Pa, argon flow amount 15sccm, power during sputter is 110W, sputtering time is 20 minutes.
4. the preparation technology of a kind of semiconductor material SiC film according to claim 1, is characterized in that: in the high vacuum annealing furnace described in step 7, annealing furnace back end vacuum tightness is less than or equal to 4.0 * 10-4Pa.
5. the preparation technology of a kind of semiconductor material SiC film according to claim 1, is characterized in that: in the high vacuum annealing furnace described in step 7, anneals, and annealing time 1-5 hour, 950 ℃ of annealing temperatures.
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| CN201410273829.9A CN104018124B (en) | 2014-06-19 | 2014-06-19 | Process for preparing semiconductor material SiC film |
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| CN201410273829.9A CN104018124B (en) | 2014-06-19 | 2014-06-19 | Process for preparing semiconductor material SiC film |
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Cited By (4)
| 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 | 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 |
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 (6)
| 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 | Preparation method of 3C-SiC 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 |
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| CN104018124B (en) | 2017-04-19 |
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