CN101928933A - Method for preparing silicon carbide film - Google Patents
Method for preparing silicon carbide film Download PDFInfo
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- CN101928933A CN101928933A CN2009100878871A CN200910087887A CN101928933A CN 101928933 A CN101928933 A CN 101928933A CN 2009100878871 A CN2009100878871 A CN 2009100878871A CN 200910087887 A CN200910087887 A CN 200910087887A CN 101928933 A CN101928933 A CN 101928933A
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Abstract
The invention discloses a method for preparing a silicon carbide film, which comprises the following steps of: 1) preparing a substrate; 2) cleaning the substrate; 3) vacuumizing a chamber, and heating after achieving a preset value; 4) heating to a preset temperature, and entering into reaction gas; 5) adjusting work gas pressure, switching on a radio frequency power supply, and starting to react; and 6) continuously vacuumizing the chamber after reacting till that the temperature is less than the preset temperature. By adopting a plasma-assisting low-temperature preparation method, the method guarantees that the chamber has high-cost low vacuum, improves the crystallization degree of the film, reduces the generation of the impurity and the defect of the film, greatly improves the mechanical property of the film, and solves the problems of the small area, the high temperature, the large defect density, the multiple impurity, the bad adhering performance and the difficult manufacture of the silicon carbide film.
Description
Technical field
The present invention relates to the carborundum films preparing technical field, relate in particular to a kind of method for preparing carborundum films.
Background technology
Over nearly 20 years, along with the high speed development of film preparing technology, carborundum films has been widely used in the window material of supercoat, photoluminescence, field-effect transistor, thin-film light emitting diode and non-crystal silicon solar cell etc.
Silicon carbide is a kind of optimal X-ray diffraction optical element substrate film, and its performance is better than materials such as boron-doped silicon film, silicon nitride film far away.Even suffer 100kJ/cm
2The x optical radiation, the bearing accuracy of carborundum films still is better than 5nm, the X-ray diffraction optical element that go up to use of the U.S. " national portfire NIF " all is based on the silicon carbide substrates film for this reason.
But, carborundum films delays in industrial large-scale application, its major cause is that on the one hand film growth apparatus is backward, technology is immature, the preparation difficulty of carborundum films material etc., and film quality does not reach requirement on devices all the time, at present achieving no breakthrough property progress.Sophisticated silicon device manufacture craft is incompatible on element manufacturing Yu now on the other hand.
At present existing many methods comprise that ion implantation, physical vapor transport (PVT), rheotaxial growth (LPE), molecular beam epitaxy (MBE), magnetron sputtering (RMS) and laser pulse (PLD) etc. and be used to prepare carborundum films.
The present invention is based on existing P ECVD system, develop high performance amorphous silicon carbide film technology.By adjustment to processing parameter, make have big area, quality is good, can be applied to the amorphous silicon carbide film on MEMS (micro electro mechanical system) (MEMS) or the opto-electronic device.
Summary of the invention
(1) technical problem that will solve
Main purpose of the present invention is to provide a kind of method for preparing carborundum films, the problem little with the area that solves present preparation carborundum films, that temperature is high, defect concentration is big, impurity is many, adhesion is poor, making is difficult.
(2) technical scheme
For achieving the above object, the invention provides a kind of method for preparing carborundum films, comprising:
1) substrate preparation;
2) substrate cleans;
3) cavity vacuumizes, and reaches vacuum preset value post-heating;
4) be heated to preset temperature, feed reactant gases;
5) adjust operating air pressure, open radio-frequency power supply, begin reaction;
6) reaction finishes, and continues in the cavity to vacuumize, and is lower than preset temperature until temperature.
In the such scheme, substrate described in the step 1) comprises any in silicon, silica glass, sapphire and the stainless steel.
In the such scheme, the method of cleaning substrate step 2) is for being heated to the certain temperature immersion with substrate with the mixing solutions of the vitriol oil and hydrogen peroxide, with after the washed with de-ionized water, cleaned several minutes with toluene, acetone, each excusing from death of alcohol more then, at last substrate is dried.
In the such scheme, the preset value of vacuum tightness described in the step 3) is at least 3.5 * 10
-4Pa.
In the such scheme, preset temperature described in the step 4) is 180～300 ℃.
In the such scheme, the reactant gases that feeds described in the step 4) is the mixed gas of silane and methane.
In the such scheme, operating air pressure described in the step 5) is 20～120Pa.
In the such scheme, preset temperature described in the step 6) is 180 ℃.
(3) beneficial effect
From technique scheme as can be seen, the present invention has following beneficial effect:
1, utilizes the present invention, method by the preparation of using plasma assisted cryogenic, guarantee that cavity has high base vacuum degree, the degree of crystallization of film is improved, reduce film impurities and generation of defects simultaneously, improved mechanical properties in films greatly, the area that has solved the preparation carborundum films is little, temperature is high, defect concentration is big, impurity is many, adhesion is poor, make difficult problem.
2, utilize the present invention, but the depositing large-area amorphous silicon carbide film, and effectively reduce preparation temperature, and can be grown on the less substrate of heat budget, realize using widely.
Description of drawings
Fig. 1 is the method flow diagram of preparation carborundum films provided by the invention;
Fig. 2 is the total collection of illustrative plates of x-ray photoelectron spectroscopy element for preparing carborundum films according to the embodiment of the invention;
Fig. 3 is the x-ray photoelectron spectroscopy element silicon analysis collection of illustrative plates for preparing carborundum films according to the embodiment of the invention;
Fig. 4 is the x-ray photoelectron spectroscopy carbon analysis collection of illustrative plates for preparing carborundum films according to the embodiment of the invention;
Fig. 5 is the Fourier's infrared transmission spectrum for preparing carborundum films according to the embodiment of the invention.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
As shown in Figure 1, Fig. 1 is the method flow diagram of preparation carborundum films provided by the invention, and this method comprises:
Step 1: substrate preparation; Described substrate can adopt any in silicon, silica glass, sapphire and the stainless steel.
Step 2: substrate cleans; The method of cleaning substrate is soaked for substrate is heated to certain temperature with the mixing solutions of the vitriol oil and hydrogen peroxide, then with after the washed with de-ionized water, with toluene, acetone, each excusing from death cleaning of alcohol several minutes, at last substrate is dried again.
Step 3: cavity vacuumizes, and reaches vacuum preset value post-heating; The vacuum tightness preset value is at least 3.5 * 10
-4Pa.
Step 4: be heated to preset temperature, feed reactant gases; Preset temperature is 180～300 ℃, and the reactant gases of feeding is the mixed gas of silane and methane.
Step 5: adjust operating air pressure, open radio-frequency power supply, begin reaction; Operating air pressure is 20～120Pa.
Step 6: reaction finishes, and continues in the cavity to vacuumize, and is lower than preset temperature until temperature, and preset temperature is 180 ℃.
The present invention is 10 with substrate with the vitriol oil and hydrogen peroxide ratio at first: the mixing solutions of (1～3) soaked 15～30 minutes down at 120 ℃～130 ℃; After the taking-up, use washed with de-ionized water, cleaned 2～10 minutes with each excusing from death between 25 ℃～80 ℃ of toluene, acetone and ethanol; Have children outside the state plan between 25 ℃～80 ℃ with deionized water again and cleaned 2～10 minutes.After the oven dry, substrate can be used to deposit.
Deposition adopts 13.56MHz radio-frequency induction coupled plasma to strengthen chemical gas-phase deposition system, and the sample levels that cleaning, drying is crossed is placed on the sample table, and preliminary vacuum is evacuated to 10
-4More than the Pa, use helium to be diluted to 5% silane and high-purity methane as reactant gases, gas ratio is 4: (1～3) operating air pressure is 20～120Pa, and radio frequency power is that 50W～2500 underlayer temperatures are 180 ℃～300 ℃, and the reaction times is 15min～60min.
Embodiment
Present embodiment is selected 4 inches single crystalline Si sheets (100) crystal orientation for use, cleaning silicon chip before deposition, and step is as follows:
1) the Si sheet is put into dense H
2SO
4With the hydrogen peroxide ratio is to soak 30 minutes in 10: 3 the mixing liquid, and purpose is to remove to sink to the bottom greasy dirt;
2) use the washed with de-ionized water substrate;
3) in toluene, acetone and ethanol, have children outside the state plan cleaning 5 minutes respectively;
4) with deionized water excusing from death cleaning oven dry after 5 minutes.
5) silicon chip behind the cleaning, drying is put into reaction chamber, sample table is heated to 300 ℃, and vacuum tightness is evacuated to 2.5 * 10 in the reaction chamber
-4Pa, radio frequency power are 2500 operating air pressure 70Pa, SiH
4Flow is 40sccm, CH
4Flow is 0.5 hour for the 40sccm reaction times.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a method for preparing carborundum films is characterized in that, comprising:
1) substrate preparation;
2) substrate cleans;
3) cavity vacuumizes, and reaches vacuum preset value post-heating;
4) be heated to preset temperature, feed reactant gases;
5) adjust operating air pressure, open radio-frequency power supply, begin reaction;
6) reaction finishes, and continues in the cavity to vacuumize, and is lower than preset temperature until temperature.
2. the method for preparing carborundum films according to claim 1 is characterized in that: substrate described in the step 1) comprises any in silicon, silica glass, sapphire and the stainless steel.
3. the method for preparing carborundum films according to claim 1, it is characterized in that: step 2) described in clean substrate method for substrate is heated to the certain temperature immersion with the mixing solutions of the vitriol oil and hydrogen peroxide, then with after the washed with de-ionized water, cleaned several minutes with toluene, acetone, each excusing from death of alcohol again, at last substrate is dried.
4. the method for preparing carborundum films according to claim 1 is characterized in that: the preset value of vacuum tightness described in the step 3) is at least 3.5 * 10
-4Pa.
5. the method for preparing carborundum films according to claim 1 is characterized in that: preset temperature described in the step 4) is 180～300 ℃.
6. the method for preparing carborundum films according to claim 1 is characterized in that: the reactant gases that feeds described in the step 4) is the mixed gas of silane and methane.
7. the method for preparing carborundum films according to claim 1 is characterized in that: operating air pressure described in the step 5) is 20～120Pa.
8. the method for preparing carborundum films according to claim 1 is characterized in that: preset temperature described in the step 6) is 180 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100878871A CN101928933A (en) | 2009-06-24 | 2009-06-24 | Method for preparing silicon carbide film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100878871A CN101928933A (en) | 2009-06-24 | 2009-06-24 | Method for preparing silicon carbide film |
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| CN101928933A true CN101928933A (en) | 2010-12-29 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747325A (en) * | 2012-07-04 | 2012-10-24 | 华中科技大学 | Preparation method for vanadium dioxide thin film and product thereof, and application of product |
| CN102891073A (en) * | 2012-09-28 | 2013-01-23 | 南京航空航天大学 | Preparation method of low-temperature plasma auxiliary aluminum induced polycrystalline silicon carbide film |
| CN105386002A (en) * | 2015-11-16 | 2016-03-09 | 三峡大学 | Low-temperature preparation method for amorphous carbon thin film material |
| CN106498364A (en) * | 2016-10-24 | 2017-03-15 | 三峡大学 | A kind of preparation method of silicon carbide-containing nanoparticulate thin films material |
| CN113219513A (en) * | 2021-03-25 | 2021-08-06 | 重庆邮电大学 | Preparation method of irreversible X-ray counter |
-
2009
- 2009-06-24 CN CN2009100878871A patent/CN101928933A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747325A (en) * | 2012-07-04 | 2012-10-24 | 华中科技大学 | Preparation method for vanadium dioxide thin film and product thereof, and application of product |
| CN102747325B (en) * | 2012-07-04 | 2014-07-09 | 华中科技大学 | Preparation method for vanadium dioxide thin film and product thereof, and application of product |
| CN102891073A (en) * | 2012-09-28 | 2013-01-23 | 南京航空航天大学 | Preparation method of low-temperature plasma auxiliary aluminum induced polycrystalline silicon carbide film |
| CN102891073B (en) * | 2012-09-28 | 2015-01-14 | 南京航空航天大学 | Preparation method of low-temperature plasma auxiliary aluminum induced polycrystalline silicon carbide film |
| CN105386002A (en) * | 2015-11-16 | 2016-03-09 | 三峡大学 | Low-temperature preparation method for amorphous carbon thin film material |
| CN105386002B (en) * | 2015-11-16 | 2017-12-05 | 三峡大学 | A kind of low temperature preparation method of amorphous carbon film material |
| CN106498364A (en) * | 2016-10-24 | 2017-03-15 | 三峡大学 | A kind of preparation method of silicon carbide-containing nanoparticulate thin films material |
| CN113219513A (en) * | 2021-03-25 | 2021-08-06 | 重庆邮电大学 | Preparation method of irreversible X-ray counter |
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Open date: 20101229 |