CN106653569A - Preparation method of semiconductor material beta-SiC film - Google Patents
Preparation method of semiconductor material beta-SiC film Download PDFInfo
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- CN106653569A CN106653569A CN201611156214.3A CN201611156214A CN106653569A CN 106653569 A CN106653569 A CN 106653569A CN 201611156214 A CN201611156214 A CN 201611156214A CN 106653569 A CN106653569 A CN 106653569A
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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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02266—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by physical ablation of a target, e.g. sputtering, reactive sputtering, physical vapour deposition or pulsed laser deposition
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- 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
- H01L21/02107—Forming insulating materials on a substrate
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Abstract
The invention provides a preparation method of a semiconductor material beta-SiC film. The method comprises the following steps of firstly selecting a common graphite flake or pyrolytic graphite as a substrate and cleaning and drying the substrate; depositing a Si film on the substrate in a sputtering manner to form a Si/C structure; and finally putting the Si/C structure in a high-vacuum heat treatment furnace for annealing at 1,000 DEG C for 10-14 hours to obtain a wide band-gap semiconductor beta-SiC film. Compared with the prior art, the method has the advantages that the graphite flake is adopted as the substrate and Si is directly taken as a target material, so that technological parameters are easy to control by adopting a magnetron sputtering method, the prepared SiC film is uniform and good in repeatability, the problem of relatively large lattice mismatch and thermal expansion mismatch between the silicon substrate and silicon carbide is solved, and the disadvantages that the technological parameters are difficult to control, the cost is relatively high and massive production is difficult to implement in the prior art are overcome. The preparation method belongs to the technical field of semiconductor film preparation.
Description
Technical field
The present invention relates to a kind of preparation method of β-SiC thin film, belongs to semiconductor film field of membrane preparation.
Background technology
Carborundum (SiC) material has high thermal conductivity, electron saturation velocities height, breakdown voltage height, the low property of dielectric constant
Can, there is huge potential quality in fields such as the semiconductor photoelectronic devices for preparing high temperature resistant, high-power, high frequency and intense radiation, be
A kind of semiconductor material with wide forbidden band of new generation that can be used under extreme conditions.
At present, main magnetron sputtering including chemical vapour deposition technique and physical vapour deposition (PVD) of the preparation of SiC thin film etc.；Greatly
It is many that substrate is done using high purity single crystal silicon chip, but due to there is 20% lattice mismatch and larger heat between silicon substrate and carborundum
The problems such as expansion coefficient mismatch, seriously limit the performance and used life of its device.Chemical vapor deposition and for thin film life
Long gas source is (such as SiH4、C3H8Deng) major part belongs to combustible and explosive articles, poisonous, its tail gas pollution Environmental insults mostly
Health is unfavorable, and utilization rate is low, high cost.Simultaneously chemical vapor deposition growth thin film easily forms in the film impurity particle, breaks
The integrity of bad thin film.In SiC thin film prepared by magnetron sputtering, with high purity single crystal silicon chip as substrate, minority adopts glass to great majority
Glass piece, sapphire and base steel are substrate；And, majority is to be difficult to extensive life as target high cost with the sintering target of SiC
Produce.
The content of the invention
It is an object of the invention to：A kind of preparation method of semi-conducting material β-SiC thin film is provided, to solve existing SiC
The difficult control of technological parameter that the technology of preparing of thin film is present, it is relatively costly, it is difficult to the problems such as large-scale production.
To solve the above problems, intend using the preparation method of such a semi-conducting material β-SiC thin film, it includes following
Step：
First step, chooses graphite flake and makees substrate, and cleaning is dried up；
Second step, one layer of Si film of magnetron sputtering deposition on substrate forms Si/C structure samples；
Third step, the sample that above-mentioned steps are obtained is positioned in hypertonic solutions stove carries out heat treatment acquisition broadband
Gap semiconductor β-SiC thin film.
Preferably, graphite substrate is two kinds of common graphite and pyrolytic graphite in first step；
Preferably, sputtering sedimentation Si films in second step, sputtering chamber vacuum level requirements are less than or equal to 5.0 × 10-5Pa, room temperature
Or underlayer temperature is as follows for sputtering sedimentation parameter under the conditions of 350～500 DEG C two kinds：1.0～4.0Pa of sputtering pressure, argon flow amount
10～25sccm, 80～140W of sputtering power, deposition Si film thicknesses are about 420～840nm；
Preferably, in third step, back end vacuum reaches 8.0 × 10 in hypertonic solutions stove-4Heat up after Pa, annealing
900～1200 DEG C of temperature, annealing time is 10～14 hours.Whole annealing process vacuum is better than 2.0 × 10-3Pa。
Compared with prior art, the present invention adopts aboundresources, cheap and environmentally safe graphite flake to be lining
Bottom, directly does target with Si targets, and using magnetron sputtering method, the easily controllable Si thickness of sputter procedure is thin to prepare high-quality SiC
Film, so as to obtain a kind of efficient, environmentally friendly, cheap SiC thin film preparation method, exists larger between solution silicon substrate and carborundum
Lattice mismatch and thermal expansion mismatch, and overcome the difficult control of technological parameter that prior art is present, it is relatively costly, it is difficult to extensive
The shortcomings of production.
Description of the drawings
Fig. 1 is that the present invention deposits the thick Si films of 560nm on common graphite substrate, and annealing temperature is 1000 DEG C, during annealing
Between for 10～14h prepare sample X-ray diffractogram；
Fig. 2 is that the present invention deposits the thick Si films of 560nm on common graphite substrate, and annealing temperature is 1000 DEG C, during annealing
Between for 12h prepare Sample Scan electron microscope；
Fig. 3 is the present invention on pyrolytic graphite substrate, and room temperature and underlayer temperature are to deposit 560nm under the conditions of 300～500 DEG C
Thick Si films, annealing temperature is 1000 DEG C, and annealing time is sample X-ray diffractogram prepared by 12h；
Fig. 4 is the present invention on pyrolytic graphite substrate, and underlayer temperature is the Si films of deposition 560nm thickness under the conditions of 450 DEG C, is moved back
Fiery temperature is 1000 DEG C, and annealing time is Sample Scan electron microscope prepared by 12h；
Fig. 5 is on common graphite substrate, the thick Si films of 420～630nm to be deposited under room temperature condition, and annealing temperature is 1000
DEG C, annealing time is sample X-ray diffractogram prepared by 12h；
Fig. 6 is on common graphite substrate, the thick Si films of 630nm to be deposited under room temperature condition, and annealing temperature is 1000 DEG C, annealing
Time is the scanning electron microscope (SEM) photograph of sample surface morphology prepared by 12h.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, further will be made to invention by accompanying drawing below
Ground is described in detail.
Embodiment 1：
(1) the common graphite piece of single-sided polishing is cleaned 15 minutes successively in acetone, anhydrous alcohol, it is therefore an objective to remove surface
Organic substance etc., then deionized water clean 5 times, 10 minutes every time, after drying up, graphite flake is fixed on pallet, send into
The sputtering chamber of magnetic control sputtering system.
(2) when sputtering chamber vacuum is less than or equal to 5.0 × 10-5After Pa, before formal sputtering, sputter clean Si target surface
10min, the main oxide layer for removing target material surface.One layer of 560nm of the sputtering sedimentation thick Si films on graphite flake, form Si/C knots
Structure, intrinsic Si targets (purity is 99.99%) the diameter 60mm of sputtering, thickness are 5mm.Sputtering parameter is shown in Table 1.
(3) room temperature is naturally cooled to after the completion of sputtering, taking-up sample is positioned over adds a cover in molybdenum box, and molybdenum box is put into into fine vacuum
The uniform temperature zone of heat-treatment furnace, is evacuated to 8.0 × 10-41000 DEG C are warming up to after Pa, 10～14h of constant temperature, Temperature fall, experiment is joined
Number is shown in Table 1.Whole annealing process vacuum is better than 2.0 × 10-3Pa, forms β-SiC thin film after annealing.
Fig. 1 is that the thick Si films of 560nm are deposited on common graphite substrate, and annealing temperature is 1000 DEG C, annealing time is 10～
Sample X-ray diffractogram prepared by 14h, visible in figure, in addition to common graphite substrate diffraction peak, remaining peak is β-SiC diffraction
Peak, and with PDF standard spectrum (card numbers：The main peak of crystal face (111) (220) (311) three of β-SiC diffraction maximums is one by one in 73-1665)
Correspondence, under illustrating preparation condition described in the present embodiment, is prepared for the good β-SiC thin film of crystalline condition.
Fig. 2 is that the thick Si films of 560nm are deposited on common graphite substrate, and annealing temperature is 1000 DEG C, and annealing time is 12h systems
The scanning electron microscope (SEM) photograph of standby sample surface morphology, as a result shows and sputter under room temperature condition that Si thickness is 560nm, annealing temperature is
1000 DEG C, annealing time 12h, β-SiC crystal grain distribution is uniform, and crystallite dimension is larger, surfacing.Testing adopted annealing
Under the conditions of, there is the good β-SiC thin film of crystalline state to occur.
Table 1 is sputtered and annealing conditions
Embodiment 2：
(1) the pyrolytic graphite piece of single-sided polishing is cleaned 15 minutes successively in acetone, anhydrous alcohol, it is therefore an objective to remove surface
Organic substance etc., then deionized water clean 5 times, 10 minutes every time, after drying up, graphite flake is fixed on pallet, send into
The sputtering chamber of magnetic control sputtering system.
(2) when sputtering chamber vacuum is less than or equal to 5.0 × 10-5After Pa, 350～500 DEG C of underlayer temperature splashes on graphite flake
One layer of 560nm Si film of deposition is penetrated, Si/C structures are formed, sputtering parameter is shown in Table 2.(purity is the intrinsic Si targets of sputtering
99.99%) diameter 60mm, thickness are 5mm.Before formal sputtering, sputter clean Si target surface 10min is main to remove target table
The oxide layer in face.
(3) room temperature is naturally cooled to after the completion of sputtering, taking-up sample is positioned over adds a cover in molybdenum box, and molybdenum box is put into into fine vacuum
The uniform temperature zone of heat-treatment furnace, is evacuated to 8.0 × 10-41000 DEG C are warming up to after Pa, constant temperature 12 hours, Temperature fall, experiment is joined
Number is shown in Table 2.Whole annealing process vacuum is better than 2.0 × 10-3Pa, forms β-SiC thin film after annealing.
Fig. 3 is on pyrolytic graphite substrate, and room temperature and underlayer temperature are to deposit the thick Si of 560nm under the conditions of 300～500 DEG C
Film, annealing temperature is 1000 DEG C, and annealing time is sample X-ray diffractogram prepared by 12h, visible in figure, except pyrolytic graphite lining
Outside the diffraction maximum of bottom, remaining peak is β-SiC diffraction maximums, and with PDF standard spectrum (card numbers：β-SiC diffraction maximums in 73-1665)
The main peak of crystal face (111) (220) (311) three is corresponded, and under illustrating preparation condition of the present invention, is prepared for crystalline condition good
β-SiC thin film.
Fig. 4 is that on pyrolytic graphite substrate, underlayer temperature is the Si films of deposition 560nm thickness under the conditions of 450 DEG C, and annealing temperature is
1000 DEG C, annealing time is the scanning electron microscope (SEM) photograph of sample surface morphology prepared by 12h, as a result shows that underlayer temperature is 450 DEG C of bars
It is 560nm that Si thickness is sputtered under part, and annealing temperature is 1000 DEG C, and annealing time 12h, β-SiC crystal grain distribution is uniform, crystallite dimension
It is larger, surfacing.Under the conditions of adopted silicon is tested, there is the good β-SiC thin film of crystalline state to occur.
Table 2 is sputtered and annealing conditions
Embodiment 3：
(1) the common graphite piece of single-sided polishing is cleaned 15 minutes successively in acetone, anhydrous alcohol, it is therefore an objective to remove surface
Organic substance etc., then deionized water clean 5 times, 10 minutes every time, after drying up, graphite flake is fixed on pallet, send into
The sputtering chamber of magnetic control sputtering system.
(2) when sputtering chamber vacuum is less than or equal to 5.0 × 10-5After Pa, on graphite flake one layer 420 of sputtering sedimentation～
630nm Si films, form Si/C structures, and sputtering parameter is shown in Table 3.Intrinsic Si targets (purity the is 99.99%) diameter of sputtering
60mm, thickness are 5mm.Before formal sputtering, sputter clean Si target surface 10min, the main oxide layer for removing target material surface.
(3) room temperature is naturally cooled to after the completion of sputtering, taking-up sample is positioned over adds a cover in molybdenum box, and molybdenum box is put into into fine vacuum
The uniform temperature zone of heat-treatment furnace, is evacuated to 8.0 × 10-41000 DEG C are warming up to after Pa, constant temperature 12 hours, Temperature fall, experiment is joined
Number is shown in Table 3.Whole annealing process vacuum is better than 2.0 × 10-3Pa, forms β-SiC thin film after annealing.
Table 3 is sputtered and annealing conditions
Fig. 5 is on common graphite substrate, the thick Si films of 420～630nm to be deposited under room temperature condition, and annealing temperature is 1000
DEG C, annealing time is sample X-ray diffractogram prepared by 12h, visible in figure, in addition to pyrolysis graphite substrate diffraction maximum, remaining peak
Be β-SiC diffraction maximums, and with PDF standard spectrum (card numbers：The crystal face (111) (220) of β-SiC diffraction maximums in 73-1665)
(311) three main peaks are corresponded, and under illustrating preparation condition of the present invention, are prepared for the good β-SiC thin film of crystalline condition.
Fig. 6 is on common graphite substrate, the thick Si films of 630nm to be deposited under room temperature condition, and annealing temperature is 1000 DEG C, annealing
Time is the scanning electron microscope (SEM) photograph of sample surface morphology prepared by 12h, as a result shows and sputter under room temperature condition that Si thickness is 630nm,
Annealing temperature is 1000 DEG C, and annealing time 12h, β-SiC crystal grain distribution is uniform, and crystallite dimension is larger, surfacing.In experiment institute
Under the conditions of the Si thickness for adopting is for 630nm, there is the good β-SiC thin film of crystalline state to occur.
Claims (4)
1. a kind of preparation method of semi-conducting material β-SiC thin film, it is characterised in that comprise the steps：
First step, chooses graphite flake and makees substrate, and cleaning is dried up；
Second step, one layer of Si film of magnetron sputtering deposition on substrate forms Si/C structure samples；
Third step, the sample that above-mentioned steps are obtained is positioned in hypertonic solutions stove carries out heat treatment acquisition broad-band gap half
Conductor β-SiC thin film.
2. a kind of preparation method of semi-conducting material β-SiC thin film according to claim 1, it is characterised in that：First step
Middle graphite substrate is two kinds of common graphite and pyrolytic graphite.
3. a kind of preparation method of semi-conducting material β-SiC thin film according to claim 1, it is characterised in that：Second step
Middle sputtering sedimentation Si films, sputtering chamber vacuum level requirements are less than or equal to 5.0 × 10-5Pa, room temperature or underlayer temperature are 350～500 DEG C,
Sputtering sedimentation parameter is as follows under the conditions of two kinds：1.0～4.0Pa of sputtering pressure, 10～25sccm of argon flow amount, sputtering power 80～
140W, deposition Si film thickness is 420～840nm.
4. a kind of preparation method of semi-conducting material β-SiC thin film according to claim 1, it is characterised in that：Third step
In, back end vacuum reaches 8.0 × 10 in hypertonic solutions stove-4Heat up after Pa, 900～1200 DEG C of annealing temperature, during annealing
Between be 10～14 hours, whole annealing process vacuum be better than 2.0 × 10-3Pa。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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 |
| US20120270053A1 (en) * | 2011-04-21 | 2012-10-25 | Villalobos Guillermo R | SITU GROWN SiC COATINGS ON CARBON MATERIALS |
| CN105088174A (en) * | 2014-05-20 | 2015-11-25 | 鞠云 | Novel SiC film preparing process |
-
2016
- 2016-12-14 CN CN201611156214.3A patent/CN106653569A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120270053A1 (en) * | 2011-04-21 | 2012-10-25 | Villalobos Guillermo R | SITU GROWN SiC COATINGS ON CARBON MATERIALS |
| 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 |
| CN105088174A (en) * | 2014-05-20 | 2015-11-25 | 鞠云 | Novel SiC film preparing process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20170510 |