CN104087909A - Preparation method of cubic silicon carbide film - Google Patents
Preparation method of cubic silicon carbide film Download PDFInfo
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- CN104087909A CN104087909A CN201410317559.7A CN201410317559A CN104087909A CN 104087909 A CN104087909 A CN 104087909A CN 201410317559 A CN201410317559 A CN 201410317559A CN 104087909 A CN104087909 A CN 104087909A
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Abstract
The invention discloses a preparation method of a cubic silicon carbide film, which comprises the following steps: (1) placing a monocrystalline silicon substrate on a substrate seat of a cold-wall type laser chemical vapor deposition device, vacuumizing, and raising the temperature of the substrate seat to 100-900 ℃; (2) introducing carrier gas containing HMDS into the reactor, wherein the flow rate of the HMDS is 1-20 sccm, and adjusting the vacuum degree to 10-10 kPa; (3) loading continuous laser to irradiate the surface of the silicon substrate, wherein the wavelength is 750-1150 nanometers, the power is 10-150W, and the time is 1-10 minutes; (4) and stopping introducing the current-carrying gas containing HMDS, closing the laser, stopping heating, vacuumizing and naturally cooling to room temperature to obtain the cubic silicon carbide film. The surface defects of the cubic silicon carbide film prepared by the method grow obliquely to the growth direction of the film, and the phenomenon of self-extinction can occur when adjacent defects meet, so that the crystal defects in the material are effectively reduced.
Description
Technical field
The present invention relates to a kind of preparation method who reduces the cubic silicon carbide film of lattice defect, belong to inorganic materials structure control field.
Background technology
Silicon carbide has that energy gap is large, voltage breakdown is high, accommodate in high temperature, superpower, high frequency and extreme radiation environment and apply, being the ideal material of development high frequency, high temperature resistant, radiation-resistance semiconductor microelectronic device and circuit, is important third generation semiconductor material.
Silicon carbide has multiple polymorphism, different according to atom stacking order on perpendicular to c-axis direction, silicon carbide can be divided into the polytype that kind more than 200 is different.Because cubic silicon carbide (3C-SiC) fusing point is lower than silicon (fusing point of silicon is 1420 ℃), so 3C-SiC is unique can growth on monocrystalline silicon substrate and the carbofrax material of excellent performance.This means that only 3C-SiC is the crystal formation that is hopeful to obtain large size material.In addition, fabulous thermal expansion and lattice match between (111) crystal face in 3C-SiC and III-V compound (as gan) and Graphene, make to take the device that semiconducter device that SiC epitaxial film or wafer are substrate is substrate than traditional silicon or sapphire, working life improves that 10 times above and energy consumption lowers approximately 2/3rds, and the semiconducter device being derived by it has more wide application prospect.
But (defect in 3C-SiC film crystal grain (111) face prepared by CVD, perpendicular to the direction of growth of film, cannot be eliminated, and has affected the popularization of carborundum films and related device application thereof in general chemical vapour deposition.Therefore, the technology of preparing of improving cubic silicon carbide material seems particularly important, and the technology after improvement can also be controlled the microstructure of material when preparing material, and produces lattice defect in certain defect elimination mechanism minimizing material.
Summary of the invention
Technical problem to be solved by this invention is that a kind of preparation method of cubic silicon carbide film is provided for the deficiency of above-mentioned prior art existence, sedimentation velocity is fast, the lattice defect of gained carborundum films is few, and the lattice defect of silicon carbide is with deposit thickness increase and the minimizing fast of film.
A preparation method for cubic silicon carbide film, comprises the steps:
(1) monocrystalline silicon substrate is put in the substrate holder of cold wall type laser chemical vapor deposition reactor, and vacuum tightness is adjusted to below 10Pa, and the heating system in reactor is set, make substrate holder temperature rise to 100～900 ℃;
(2) will be containing hexamethyldisilane ((CH
3)
3-Si-Si-(CH
3)
3, be abbreviated as HMDS) current-carrying gas pass in reactor, the flow of HMDS is 1～20sccm, regulates vacuum tightness to the 10～10kPa in reactor;
(3) load continuous laser and irradiate silicon substrate surface, wavelength 750～1150 nanometers, adjusting laser power is 10～150W, it loads Laser Time is 1～10 minute;
(4) stop passing into the current-carrying gas that contains HMDS, close the heating system in laser and reactor, vacuumize, the vacuum tightness in reactor is adjusted to below 10Pa, and naturally cools to room temperature, obtain being deposited on the cubic silicon carbide film on monocrystalline silicon substrate.
Press such scheme, described monocrystalline silicon substrate can make its surface clean through pre-treatment, and silicon single crystal is fully exposed.Described pretreated method is: first substrate is placed in to ethanol supersound process 15 minutes, then be placed in the mixing solutions heating in water bath 10 minutes of ammoniacal liquor, hydrogen peroxide and water, then the mixing solutions that is placed in hydrofluoric acid and water soaks 1 minute, finally by deionized water washes clean.Wherein, the volume ratio of ammoniacal liquor, hydrogen peroxide and water is 1:1:5, and the bath temperature of this mixing solutions is set to 80 ℃; The volume ratio of hydrofluoric acid and water is 1:50.In this technique, ammoniacal liquor used is analytical pure ammoniacal liquor, NH
3massfraction is 28%; Hydrogen peroxide is analytical pure hydrogen peroxide, H
2o
2> 30%; Hydrofluoric acid is analytical pure hydrofluoric acid, and HF is greater than 40%.
Press such scheme, described current-carrying gas is argon gas, hydrogen etc.
The present invention by adjusting transport the current-carrying airshed of hexamethyldisilane, the temperature of substrate surface, the laser power of loading and time, is controlled thickness and the structure of the cubic silicon carbide film of deposition while passing into after hexamethyldisilane depositing silicon carbide.
Compared with prior art, the invention has the beneficial effects as follows:
First, the plane defect of cubic silicon carbide film prepared by the present invention favours the growth of film growth direction, when meeting, adjacent defect can there is " certainly withering away " phenomenon, thereby effectively reduce the lattice defect in material, and the lattice defect of silicon carbide is with deposit thickness increase and the minimizing fast of film;
The second, when the present invention prepares cubic silicon carbide film, the sedimentation rate of cubic silicon carbide film is fast, and sedimentation velocity can reach 50 μ m/min;
The 3rd, the method for the invention is very energy-conservation, and laser direct irradiation silicon substrate mainly gives substrate surface local heat energy, and other positions of reactor are heated less, have reduced energy consumption.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the XRD figure spectrum of the cubic silicon carbide film of the embodiment of the present invention 1 preparation.
Fig. 3 be the embodiment of the present invention 1 preparation cubic silicon carbide film cross section transmission electron microscope (TEM) as.
Fig. 4 (a) is that the transmission electron microscope (TEM) of cubic silicon carbide film cross section of the embodiment of the present invention 1 preparation is as, the TEM picture of the carborundum films of (b) preparing for traditional C VD method.
In Fig. 5 (b) and (d) when preparing cubic silicon carbide film, the carborundum films direction of growth angled (111) plane defect disappearance schematic diagram.(b) and (d) representing respectively has antiphase domain boundary (APB) and the twin boundary (TB) that favours film growth direction in carborundum films in the present invention.In figure five (a) and (c) be illustrated respectively in carborundum films prepared by general CVD method, antiphase domain boundary (APB) and twin boundary (TB) are perpendicular to the direction of growth of film;
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but the present invention is not only confined to the following examples.
Monocrystalline silicon substrate described in following embodiment can make its surface clean through pre-treatment, described pretreated method is: monocrystalline silicon substrate is cut into size for 1cm * 2cm, first ultrasonic cleaning 15 minutes in ethanol, in temperature, be the ammoniacal liquor of 80 ℃ again, in the mixing solutions of hydrogen peroxide and water, clean 10 minutes, then in hydrofluoric acid aqueous solution, clean 1 minute, finally with deionized water, rinse well.Wherein in the mixing solutions of ammoniacal liquor, hydrogen peroxide and water, the specific volume of ammoniacal liquor, hydrogen peroxide and water is than being 1:1:5, and in hydrofluoric acid aqueous solution, the volume ratio of hydrofluoric acid and water is 1:50.The ammoniacal liquor using is analytical pure ammoniacal liquor, NH
3massfraction is 28%; Hydrogen peroxide is analytical pure hydrogen peroxide, H
2o
2> 30%; Hydrofluoric acid is analytical pure hydrofluoric acid, and HF is greater than 40%.
Embodiment 1
A preparation method for cubic silicon carbide film, comprises the steps:
(1) monocrystalline silicon substrate is put in the substrate holder of cold wall type laser chemical vapor deposition reactor, and vacuum tightness is adjusted to below 10Pa, and the heating system in reactor is set, make substrate holder temperature rise to 300 ℃;
(2) the current-carrying gas Ar gas containing hexamethyldisilane (HMDS) is passed in reactor, the flow of HMDS is 3sccm, by regulating vacuum pump extraction valve to make the vacuum tightness in reactor, is 10000Pa;
(3) load continuous laser and irradiate silicon substrate surface, wavelength 808 nanometers, adjusting laser power is 80W, loading Laser Time is 10 minutes;
(4) stop passing into the Ar gas that contains HMDS, close the heating system in laser and reactor, vacuumize, the vacuum tightness in reactor is adjusted to below 10Pa, and naturally cools to room temperature, obtain being deposited on the cubic silicon carbide film on monocrystalline silicon substrate.
As shown in Figure 2, the cubic silicon carbide film that prepared by the present embodiment carries out XRD test.From scheming, can find out to only have the diffraction peak of cubic silicon carbide (111) and (222), and there is no the diffraction peak of other crystal face of silicon carbide, result shows that thin film composition is 3C-SiC, and its (111) crystal face is parallel to substrate.
Fig. 3 be the present embodiment transmission electron microscope (TEM) of being deposited on the cubic silicon carbide film on monocrystalline silicon substrate as.Known according to Fig. 3, be parallel on the in-plane of substrate surface, the average cross section diameter d of carborundum grain and its distance h apart from silicon substrate surface, meet formula d=h
v, v is 0.7, much larger than the standby cubic silicon carbide film of traditional C VD legal system (v value is about 0.517).This shows that the present invention prepares gained silicon carbide lattice defect in the process of growth and disappearing fast along with the increase of thickness.
Fig. 4 (a) is deposited on the TEM picture of the cubic silicon carbide film on monocrystalline silicon substrate for the present embodiment, wherein, silicon carbide surface defect favours the direction of growth of film, the TEM picture of the carborundum films of (b) preparing for traditional C VD method, and its silicon carbide surface defect is parallel to substrate surface.
In the carborundum films of preparing in traditional C VD method, antiphase domain boundary (APB) and twin boundary (TB) are perpendicular to the direction of growth of film, and as Fig. 5 (a) with (c), the APB that it is parallel to each other or TB are difficult to meet and disappear.On the contrary, in the present invention, have the APB that favours film growth direction in film, as shown in Fig. 5 (b), this APB can meet with adjacent APB along with the growth of film, finally mutually buries in oblivion; TB also has similar situation, as shown in Fig. 5 (d).
Embodiment 2
A preparation method for cubic silicon carbide film, comprises the steps:
(1) monocrystalline silicon substrate is put in the substrate holder of cold wall type laser chemical vapor deposition reactor, and vacuum tightness is adjusted to below 10Pa, and the heating system in reactor is set, make substrate holder temperature rise to 600 ℃;
(2) the current-carrying gas Ar gas containing hexamethyldisilane (HMDS) is passed in reactor, the flow of HMDS is 10sccm, and regulating the vacuum tightness in reactor is 1000Pa;
(3) load continuous laser and irradiate silicon substrate surface, wavelength 1080 nanometers, adjusting laser power is 20W, loading Laser Time is 3 minutes;
(4) stop passing into the H that contains HMDS
2, close the heating system in laser and reactor, vacuumize, the vacuum tightness in reactor is adjusted to below 10Pa, and naturally cools to room temperature, obtain being deposited on the cubic silicon carbide film on monocrystalline silicon substrate.
Cubic silicon carbide thin film composition prepared by the present embodiment is 3C-SiC, and its (111) crystal face is parallel to substrate.
Embodiment 3
A preparation method for cubic silicon carbide film, comprises the steps:
(1) monocrystalline silicon substrate is put in the substrate holder of cold wall type laser chemical vapor deposition reactor, and vacuum tightness is adjusted to below 10Pa, and the heating system in reactor is set, make substrate holder temperature rise to 900 ℃;
(2) will be containing the current-carrying gas H of hexamethyldisilane (HMDS)
2pass in reactor, the flow of HMDS is 18sccm, and regulating the vacuum tightness in reactor is 100Pa;
(3) load continuous laser and irradiate silicon substrate surface, optical maser wavelength is 1080 nanometers, and adjusting laser power is 150W, and loading Laser Time is 1 minute;
(4) stop passing into the current-carrying gas H that contains HMDS
2, close the heating system in laser and reactor, vacuumize, the vacuum tightness in reactor is adjusted to below 10Pa, and naturally cools to room temperature, obtain being deposited on the cubic silicon carbide film on monocrystalline silicon substrate.
Cubic silicon carbide thin film composition prepared by the present embodiment is 3C-SiC, and its (111) crystal face is parallel to substrate.
Above-described specific embodiment, has carried out further detailed description to object of the present invention, technical scheme and beneficial effect.For a person skilled in the art, the present invention can have various modifications and variations, and all any modifications of making in the spirit and principles in the present invention, are equal to replacement, improvement etc., all should be in protection scope of the present invention.
Claims (4)
1. a preparation method for cubic silicon carbide film, is characterized in that comprising the steps:
(1) monocrystalline silicon substrate is put in the substrate holder of cold wall type laser chemical vapor deposition reactor, and vacuum tightness is adjusted to below 10Pa, and the heating system in reactor is set, make substrate holder temperature rise to 100～900 ℃;
(2) the current-carrying gas containing hexamethyldisilane is passed in reactor, the flow of hexamethyldisilane is 1～20sccm, regulates vacuum tightness to the 10～10kPa in reactor;
(3) load continuous laser and irradiate silicon substrate surface, wavelength 750～1150 nanometers, adjusting laser power is 10～150W, it loads Laser Time is 1～10 minute;
(4) stop passing into the current-carrying gas that contains hexamethyldisilane, close the heating system in laser and reactor, the vacuum tightness in reactor is adjusted to below 10Pa, and is cooled to room temperature, obtain being deposited on the cubic silicon carbide film on monocrystalline silicon substrate.
2. the preparation method of a kind of cubic silicon carbide film according to claim 1, is characterized in that described monocrystalline silicon substrate makes its surface clean through pre-treatment.
3. the preparation method of a kind of cubic silicon carbide film according to claim 2, it is characterized in that described pretreated method is: first substrate is placed in to ethanol supersound process, then the mixing solutions that is placed in ammoniacal liquor and hydrogen peroxide cleans, then be placed in after hydrofluoric acid aqueous solution cleaning, by deionized water washes clean.
4. the preparation method of a kind of cubic silicon carbide film according to claim 1, is characterized in that the current-carrying solid/liquid/gas reactions device of described hexamethyldisilane is argon gas or hydrogen.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498897A (en) * | 2014-12-12 | 2015-04-08 | 武汉理工大学 | Preparation method of silicon carbide film |
| CN105671628A (en) * | 2016-02-01 | 2016-06-15 | 昝育德 | Device and method for growing sliced or special-shaped warped single crystal through melting in laser heating area |
| CN105803422A (en) * | 2016-05-27 | 2016-07-27 | 洛阳理工学院 | SiC film preparation device and method for preparing SiC film at low vacuum degree |
| CN106044774A (en) * | 2016-05-31 | 2016-10-26 | 上海纳晶科技有限公司 | Preparation method of low-temperature, low-cost and high-purity ultra-fine silicon carbide particles |
| WO2017070877A1 (en) * | 2015-10-29 | 2017-05-04 | Ibiden Co., Ltd. | METHOD FOR FORMING CVD-SiC LAYER AND CVD-SiC LAYER FORMED BY THE METHOD |
| CN106835071A (en) * | 2017-01-23 | 2017-06-13 | 武汉理工大学 | A kind of preparation method of CVD silicon carbide material |
| CN107513698A (en) * | 2017-09-08 | 2017-12-26 | 武汉理工大学 | A kind of preparation method of cubic silicon carbide silicon coating |
| CN107881489A (en) * | 2017-10-31 | 2018-04-06 | 浙江大学 | A kind of laser auxiliary heating chemical vapor deposition coating apparatus and method |
| CN110323126A (en) * | 2019-04-15 | 2019-10-11 | 武汉理工大学 | A kind of preparation method of Si/SiC/ grapheme material |
| CN110534348A (en) * | 2019-07-31 | 2019-12-03 | 气相科技(武汉)有限公司 | A kind of electrode material and preparation method thereof based on 3C-SiC film |
| WO2019227395A1 (en) * | 2018-05-31 | 2019-12-05 | Ibiden Co., Ltd. | Fine grained 3C-SiC thick films and a process for preparing the same |
| CN114150292A (en) * | 2021-12-14 | 2022-03-08 | 武汉理工大学 | Thermal shock resistant silicon carbide nano porous coating material and preparation method and application thereof |
| CN115959669A (en) * | 2023-01-30 | 2023-04-14 | 武汉理工大学 | Preparation method of SiC nano powder |
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| CN104498897A (en) * | 2014-12-12 | 2015-04-08 | 武汉理工大学 | Preparation method of silicon carbide film |
| WO2017070877A1 (en) * | 2015-10-29 | 2017-05-04 | Ibiden Co., Ltd. | METHOD FOR FORMING CVD-SiC LAYER AND CVD-SiC LAYER FORMED BY THE METHOD |
| CN105671628A (en) * | 2016-02-01 | 2016-06-15 | 昝育德 | Device and method for growing sliced or special-shaped warped single crystal through melting in laser heating area |
| CN105671628B (en) * | 2016-02-01 | 2018-04-20 | 昝涵今 | A kind of laser heats the device and its growing method of the big thin slice of growing by zone melting or Special-shaped warp monocrystalline |
| CN105803422A (en) * | 2016-05-27 | 2016-07-27 | 洛阳理工学院 | SiC film preparation device and method for preparing SiC film at low vacuum degree |
| CN106044774A (en) * | 2016-05-31 | 2016-10-26 | 上海纳晶科技有限公司 | Preparation method of low-temperature, low-cost and high-purity ultra-fine silicon carbide particles |
| CN106044774B (en) * | 2016-05-31 | 2018-02-27 | 上海纳晶科技有限公司 | A kind of preparation method of low temperature low cost high-purity silicon carbide ultrafine dust |
| CN106835071A (en) * | 2017-01-23 | 2017-06-13 | 武汉理工大学 | A kind of preparation method of CVD silicon carbide material |
| CN107513698B (en) * | 2017-09-08 | 2019-03-08 | 武汉理工大学 | A kind of preparation method of cubic silicon carbide silicon coating |
| CN107513698A (en) * | 2017-09-08 | 2017-12-26 | 武汉理工大学 | A kind of preparation method of cubic silicon carbide silicon coating |
| CN107881489A (en) * | 2017-10-31 | 2018-04-06 | 浙江大学 | A kind of laser auxiliary heating chemical vapor deposition coating apparatus and method |
| CN107881489B (en) * | 2017-10-31 | 2019-12-24 | 浙江大学 | Laser-assisted heating chemical vapor deposition coating device and method |
| WO2019227395A1 (en) * | 2018-05-31 | 2019-12-05 | Ibiden Co., Ltd. | Fine grained 3C-SiC thick films and a process for preparing the same |
| CN110323126A (en) * | 2019-04-15 | 2019-10-11 | 武汉理工大学 | A kind of preparation method of Si/SiC/ grapheme material |
| CN110534348A (en) * | 2019-07-31 | 2019-12-03 | 气相科技(武汉)有限公司 | A kind of electrode material and preparation method thereof based on 3C-SiC film |
| CN114150292A (en) * | 2021-12-14 | 2022-03-08 | 武汉理工大学 | Thermal shock resistant silicon carbide nano porous coating material and preparation method and application thereof |
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| CN115959669A (en) * | 2023-01-30 | 2023-04-14 | 武汉理工大学 | Preparation method of SiC nano powder |
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