CN102304701A - Preparation method of silicon carbide film - Google Patents
Preparation method of silicon carbide film Download PDFInfo
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- CN102304701A CN102304701A CN201110287216A CN201110287216A CN102304701A CN 102304701 A CN102304701 A CN 102304701A CN 201110287216 A CN201110287216 A CN 201110287216A CN 201110287216 A CN201110287216 A CN 201110287216A CN 102304701 A CN102304701 A CN 102304701A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 52
- 239000010703 silicon Substances 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 15
- 239000003575 carbonaceous material Substances 0.000 claims description 11
- 229910000077 silane Inorganic materials 0.000 claims description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 150000001721 carbon Chemical group 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 230000002140 halogenating effect Effects 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 125000004432 carbon atom Chemical group C* 0.000 abstract 2
- 238000005658 halogenation reaction Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of silicon carbide film preparation, in particular to a method for preparing a silicon carbide film by using atomic layer deposition equipment. The preparation method comprises the following steps: placing a silicon substrate in a reaction cavity of the atomic layer deposition equipment; introducing a carbon-containing substance into the reaction cavity of the atomic layer deposition equipment, and carrying out carbon chemical adsorption on the carbon-containing substance and the surface of the silicon substrate to ensure that carbon atoms in the carbon-containing substance are adsorbed on the surface of the silicon substrate; and introducing a silicon-containing substance into the reaction cavity of the atomic layer deposition equipment, carrying out halogenation reaction on the silicon-containing substance and the surface of the silicon substrate, forming a carbon-silicon bond by silicon atoms in the silicon-containing substance and carbon atoms on the surface of the silicon substrate, and generating a silicon carbide film structure on the surface of the silicon substrate after the reaction is completed. The invention uses the atomic layer deposition equipment, and utilizes the influence of the lattice structure of the substrate on the growth, so that the grown silicon carbide film structure has complete lattices, and meanwhile, the structural performance of the film grown on the silicon substrate is improved.
Description
Technical field
The present invention relates to the carborundum films preparing technical field, be specifically related to a kind of method for preparing carborundum films with atomic layer deposition apparatus.
Background technology
Archie is inferior since finding the SiC material in 1891, and SiC has become the non-oxide ceramic material that people widely utilize.It has numerous characteristics; As hardness highly, wear-resisting cut, high temperature resistant, resistance to oxidation, corrosion-resistant, high heat conductance, high chemical stability, broad-band gap and high electron mobility etc., be used as the raw material that abrasive material, refractory materials, electrical heating element, black non-ferrous metal metallurgy etc. are used.Its common crystalline structure has six sides and two kinds of structures of cubes, and it is used as the heat dissipation problem that substrate can solve device preferably, therefore is seized of consequence in technical field of semiconductor illumination.Secondly, in the popular Graphene of recent research, thermal treatment SiC substrate is a kind of method for preparing Graphene, and this discovery has impelled the utilization of carbofrax material again.The method for preparing at present silicon carbide mainly is reduction SiO
2Method, muriatic synthetic can the obtaining of hydrocarbon polymer and silicon than high purity material, epitaxy SiC also is the method in research on Sapphire Substrate.But present method all is faced with the higher difficult problem of production cost, and the price of SiC substrate all remains high.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of carborundum films, the carborundum films film that said method is prepared has complete lattice.
In order to achieve the above object, the technical scheme of the present invention's employing is:
A kind of preparation method of carborundum films comprises the steps:
Silicon substrate is positioned in the atomic layer deposition apparatus reaction chamber;
In said atomic layer deposition apparatus reaction chamber, feed carbonaceous material, said carbonaceous material and the absorption of said surface of silicon generation carbon geochemistry make that the carbon atom in the said carbonaceous material is adsorbed on said surface of silicon;
In said atomic layer deposition apparatus reaction chamber, feed silicon-containing material; Said silicon-containing material and said surface of silicon generation halogenating reaction; The Siliciumatom in the said silicon-containing material and the carbon atom of said surface of silicon form carbon silicon key; After question response was complete, said surface of silicon promptly generated the carborundum films structure.
In the such scheme, the said step that silicon substrate is positioned in the atomic layer deposition apparatus reaction chamber also comprises before: said surface of silicon substrate is through reference liquid and hydrofluoric acid treatment, and si-h bond is contained on the surface after said silicon substrate is handled.
In the such scheme, said carbonaceous material is a tetracol phenixin.
In the such scheme, the flow velocity of said tetracol phenixin is 10sccm-400sccm, and inlet period is 0.5s-1s.
In the such scheme, said silicon-containing material is a silane.
In the such scheme, the flow velocity of said silane is 10sccm-100sccm, and the time is 0.5s-1s.
In the such scheme, said step at feeding carbonaceous material or silicon-containing material in said atomic layer deposition apparatus reaction chamber also comprises before: feed argon gas or nitrogen to the atomic layer deposition apparatus reaction chamber.
Compare with the prior art scheme, the beneficial effect that the technical scheme that the present invention adopts produces is following:
The present invention uses atomic layer deposition apparatus, and the crystalline network of utilizing substrate makes the carborundum films structure that grows have complete lattice to the influence of growth, also makes that the structure properties of the film of growth is improved on silica-based simultaneously.
Description of drawings
Fig. 1 is the synoptic diagram of the treated formation of surface of silicon Si-H key in the embodiment of the invention;
The synoptic diagram of Fig. 2 for feeding tetracol phenixin and react to the ald reaction chamber in the embodiment of the invention with silicon substrate;
Fig. 3 is the synoptic diagram after surface of silicon is adsorbed by carbon fully in the embodiment of the invention;
The synoptic diagram of Fig. 4 for feeding silane and react to the ald reaction chamber in the embodiment of the invention in the surface of silicon carbon atom;
Fig. 5 is the synoptic diagram after the surface of silicon carbon atom reacts completely in the embodiment of the invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment technical scheme of the present invention is described in detail.
Present embodiment provides a kind of preparation method of carborundum films, specifically comprises the steps:
Step 101 through the surface of reference liquid and hydrofluoric acid treatment silicon single crystal (111) substrate, forms si-h bond in surface of silicon, and as shown in Figure 1, wherein, reference liquid is meant: No. 1 liquid, the vitriol oil: ydrogen peroxide 50=4:1; No. 2 liquid, ammoniacal liquor: pure water: ydrogen peroxide 50=1:5:1; No. 3 liquid, hydrochloric acid: ydrogen peroxide 50: pure water=1:1:6;
Step 102 fed nitrogen 30 seconds in the atomic layer deposition apparatus reaction chamber, reaction chamber is cleaned;
Step 103, opening device, the adjustment working parameter reaches the required Working environment of experiment; In the atomic layer deposition apparatus reaction chamber, feed tetracol phenixin CCl
4, tetracol phenixin is that the mode with saturated evaporation enters into reaction chamber through carrier gas, carrier gas flux is 30sccm; Time is 0.5s, carbon atom in the tetracol phenixin and surface of silicon generation chemical reaction, and carbon atom is adsorbed on surface of silicon; As shown in Figure 2, reaction formula is:
Reaction times is 5s, and the result after reacting completely as shown in Figure 3;
Step 104 fed nitrogen 30 seconds in the atomic layer deposition apparatus reaction chamber, reaction chamber is cleaned;
Step 105 feeds silane SiH in the atomic layer deposition apparatus reaction chamber
4Silane is that the mode with saturated evaporation enters into reaction chamber through carrier gas; The flow velocity of carrier gas is 30sccm; Inlet period is 0.5s; Silane and surface of silicon generation halogenating reaction, the chlorine atom of hydrogen atom in the silane and surface of silicon generates by product HCl and is rejected to outside the reaction chamber, and Siliciumatom in the silane and carbon atom form the C-Si key; As shown in Figure 4, reaction formula is:
After the surface of silicon carbon atom reacted completely, as shown in Figure 5, surface of silicon formed the carborundum films structure;
Step 106 according to required thickness, repeats above step 102 and step 105, can on silicon substrate, successively bear the carborundum films structure.
In the present embodiment, can also use argon gas that the ald reaction chamber is cleaned in step 102 and the step 104.
The present invention through chemical action, makes carbon atom be adsorbed on the substrate through in ALD equipment reaction cavity, feeding carbonaceous material.In cavity, feed silicon-containing material on this basis again, the unreacted functional group of functional group in the silicon-containing material and surface of silicon interacts the formation by product and is rejected to outside the cavity.Remaining carbon, Siliciumatom then form cuboidal carborundum films under the effect of substrate crystal structure.
The present invention generates carborundum films through mutual replacement that alternately feed of two provenances, utilizes the influence of the crystalline network of substrate to growth, makes that the carborundum films structure that grows has complete lattice; The invention enables the growth of carborundum films to be not limited to Sapphire Substrate, make the structure properties of the carborundum films of on silicon substrate, growing be improved simultaneously.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. the preparation method of a carborundum films is characterized in that, comprises the steps:
Silicon substrate is positioned in the atomic layer deposition apparatus reaction chamber;
In said atomic layer deposition apparatus reaction chamber, feed carbonaceous material, said carbonaceous material and the absorption of said surface of silicon generation carbon geochemistry make that the carbon atom in the said carbonaceous material is adsorbed on said surface of silicon;
In said atomic layer deposition apparatus reaction chamber, feed silicon-containing material; Said silicon-containing material and said surface of silicon generation halogenating reaction; The Siliciumatom in the said silicon-containing material and the carbon atom of said surface of silicon form carbon silicon key; After question response was complete, said surface of silicon promptly generated the carborundum films structure.
2. the preparation method of carborundum films according to claim 1; It is characterized in that; The said step that silicon substrate is positioned in the atomic layer deposition apparatus reaction chamber also comprises before: said surface of silicon substrate is through reference liquid and hydrofluoric acid treatment, and si-h bond is contained on the surface after said silicon substrate is handled.
3. the preparation method of carborundum films according to claim 1 is characterized in that said carbonaceous material is a tetracol phenixin.
4. like the preparation method of carborundum films as described in the claim 3, it is characterized in that the flow velocity of said tetracol phenixin is 10sccm-400sccm, inlet period is 0.5s-1s.
5. the preparation method of carborundum films according to claim 1 is characterized in that said silicon-containing material is a silane.
6. like the preparation method of carborundum films as described in the claim 5, it is characterized in that the flow velocity of said silane is 10sccm-100sccm, the time is 0.5s-1s.
7. the preparation method of carborundum films according to claim 1; It is characterized in that said step at feeding carbonaceous material or silicon-containing material in said atomic layer deposition apparatus reaction chamber also comprises before: feed argon gas or nitrogen to the atomic layer deposition apparatus reaction chamber.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103205806A (en) * | 2012-01-11 | 2013-07-17 | 中国科学院微电子研究所 | Preparation method of single crystal cubic carbon nitride film |
CN104392929A (en) * | 2014-11-26 | 2015-03-04 | 上海华力微电子有限公司 | Preparation method of intercalated silicon carbide |
US20150329965A1 (en) * | 2012-12-21 | 2015-11-19 | Prasad Narhar Gadgil | Methods of low temperature deposition of ceramic thin films |
CN105529247A (en) * | 2014-10-21 | 2016-04-27 | 上海华力微电子有限公司 | Preparation method of embedded silicon-germanium |
CN106835067A (en) * | 2017-01-14 | 2017-06-13 | 太原理工大学 | A kind of method of Zr alloy surface Graphene Passivation Treatment corrosion-inhibiting coating |
CN112825299A (en) * | 2019-11-20 | 2021-05-21 | 中国科学院微电子研究所 | Method for depositing silicon carbide film |
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US5281274A (en) * | 1990-06-22 | 1994-01-25 | The United States Of America As Represented By The Secretary Of The Navy | Atomic layer epitaxy (ALE) apparatus for growing thin films of elemental semiconductors |
US20020096104A1 (en) * | 2001-01-19 | 2002-07-25 | Hoya Corporation | Single crystal SiCand method of producing the same as well as SiC semiconductor device and SiC composite material |
US20070062441A1 (en) * | 2005-09-16 | 2007-03-22 | Yaroslav Koshka | Method for epitaxial growth of silicon carbide |
CN101631894A (en) * | 2006-12-08 | 2010-01-20 | 瓦里安半导体设备公司 | Technique for atomic layer deposition |
-
2011
- 2011-09-26 CN CN201110287216A patent/CN102304701A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US5281274A (en) * | 1990-06-22 | 1994-01-25 | The United States Of America As Represented By The Secretary Of The Navy | Atomic layer epitaxy (ALE) apparatus for growing thin films of elemental semiconductors |
US20020096104A1 (en) * | 2001-01-19 | 2002-07-25 | Hoya Corporation | Single crystal SiCand method of producing the same as well as SiC semiconductor device and SiC composite material |
US20070062441A1 (en) * | 2005-09-16 | 2007-03-22 | Yaroslav Koshka | Method for epitaxial growth of silicon carbide |
CN101631894A (en) * | 2006-12-08 | 2010-01-20 | 瓦里安半导体设备公司 | Technique for atomic layer deposition |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103205806A (en) * | 2012-01-11 | 2013-07-17 | 中国科学院微电子研究所 | Preparation method of single crystal cubic carbon nitride film |
CN103205806B (en) * | 2012-01-11 | 2015-10-28 | 中国科学院微电子研究所 | Preparation method of single crystal cubic carbon nitride film |
US20150329965A1 (en) * | 2012-12-21 | 2015-11-19 | Prasad Narhar Gadgil | Methods of low temperature deposition of ceramic thin films |
CN105143503A (en) * | 2012-12-21 | 2015-12-09 | 普拉萨德·纳哈·加吉尔 | Methods of low temperature deposition of ceramic thin films |
CN105529247A (en) * | 2014-10-21 | 2016-04-27 | 上海华力微电子有限公司 | Preparation method of embedded silicon-germanium |
CN104392929A (en) * | 2014-11-26 | 2015-03-04 | 上海华力微电子有限公司 | Preparation method of intercalated silicon carbide |
CN106835067A (en) * | 2017-01-14 | 2017-06-13 | 太原理工大学 | A kind of method of Zr alloy surface Graphene Passivation Treatment corrosion-inhibiting coating |
CN112825299A (en) * | 2019-11-20 | 2021-05-21 | 中国科学院微电子研究所 | Method for depositing silicon carbide film |
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