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Method of producing heteroepitaxial silicon carbide films on silicon substrate. RU patent 2521142.

IPC classes for russian patent Method of producing heteroepitaxial silicon carbide films on silicon substrate. RU patent 2521142. (RU 2521142):

H01L21/205 -
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FIELD: physics.

SUBSTANCE: invention relates to the technology of producing semiconductor materials and can be used in making semiconductor devices. The method of producing heteroepitaxial silicon carbide films on a silicon substrate involves obtaining a film on the surface of a substrate by ion-plasma magnetron sputtering of one polycrystalline silicon carbide target while heating the substrate to temperature of 950-1400°C in an Ar atmosphere.

EFFECT: invention simplifies the technology by using one polycrystalline target and improves the quality of films owing to high adhesion.

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The invention relates to the technology of semiconducting materials and can be used for creation of semiconductor devices. More precisely the invention relates to the technology of production of heteroepitaxial structures of silicon carbide (SiC) on silicon (Si), which can be used as substrates in the manufacture of elements of semiconductor electronics, obtained on the basis of wide-gap material SiC.

There is a method of chemical vapor deposition, which in the foreign literature referred to as CVD (Chemical Vapor Deposition). There are different designs reaction chamber and the methods of synthesis of single-crystal films described in the publications of US 4123571 (31.10.1978), WO 9623912 (08.08.1996), US 5670414 (23.09.1997), US 6299683 (09.10.2001), JP 2005109408 (21.04.2005), EN 2394117 (24.03.2008), which allow the CVD method to implement the deposition of silicon carbide in the temperature range of substrates from 800 C to 2500°N

The method EN 2394117 (24.03.2008) is that as a result of chemical reactions in gas phase and on the surface of the substrate with the participation of the sources of the components of the film and of intermediate compounds, synthesis of the film material. As sources of the components of the film silicon carbide usually use silane and propane, dissolved hydrogen. In addition, the sources used and other substances: SiCl 4 , SiCl 2 H 2 , CH 3 SiH 3 , CH 3 SiCl 3 , (CH 3 ) 2 SiH 2 , (CH 3 ) 2 SiCl 2 , CH 4 , C 2 H 2 , C 2 H 6 . The rate of deposition of silicon carbide depends on the synthesis temperature and on the concentration of the sources of the components in the gas mixture.

The disadvantages of this method are the complexity of the technology of production, namely the need for the use of hydrides and silicon halides (complex from the point of view of ecology and safety of reagents). The disadvantage is the need to maintain the optimal composition of the gas components in the mixture and the complexity of implementation of the required process conditions in large reactors, where the uneven impact of reagent concentration by volume due to production of reagents and allocation of the reaction products.

There is a method for patent RU 2363067 (22.01.2008), which is manufacturing of products containing silicon wafer with the film silicon carbide on its surface, which includes heating of the substrate and synthesis of film on the surface of the substrate in the gas medium containing compounds of carbon, as a gas environment using oxide or carbon dioxide or a mixture of oxide or carbon dioxide with inert gas and/or nitrogen at a pressure of 20-600 PA, and heating of the silicon substrate is carried out until the temperature 950-1400°N Only carbon monoxide or carbon dioxide FROM 2 . You can use as a gas environment mixture of gases consisting of 45% by weight carbon oxide CO, 50 wt.% argon and 5 wt.% nitrogen.

This method is ineffective, that is, the difficulty lies in the multitude of the preliminary stages of preparation of the substrate. The disadvantage is the use of oxide compounds that can be formed in chemical reactions in the composition of obtained films residual oxygen in a kind of impurity. Another drawback is the small thickness of the coatings (50 nm).

Also known methods that use a combined approach. In these ways, components involved in chemical reactions at the surface of the substrate, are delivered from the solid and gaseous compounds.

The authors Joung et. al. (SiC formation for a solar cell passivation layer using an RF magnetron co-sputtering system. Nanoscale Research Letters 2012, 7:22) on the surface of 4 inch silicon substrate of p-type (100), using high frequency (HF) (100, 150, 170, 200 W) magnetron sputtering joint system from two sources-targets of silicon and graphite with additional overlap C 2 H 2 and Ar received film silicon carbide.

The disadvantage of this method of cultivation is two magnetron systems for independent spraying two targets - from the solid silicon and graphite, which complicates the design process plants, increases energy costs. Furthermore, the method does not allow you to obtain a uniform film thickness and density because of the impossibility of control of diffusion of hydrocarbon in the formed layers of silicon carbide. As a result of realization of the way it turns out, the film is relatively low quality, with amorphous structure.

The way the authors Qamar A. et al. (Synthesis and characterization of porous crystalline SiC thin films prepared by radio frequency reactive magnetron sputtering technique, Applied Surface Science 257, 2011, 6923-6927) system was used reactive magnetron sputtering silicon target diameter 4 inches (99,999% purity) in an RF discharge (13.56 MHz), 200 watt, in the atmosphere of gases Ar (99,999% purity) and CH 4 (99,999% purity) in the ratio Ar/CH 4 =80/20 (at.%). As substrates were used polished wafers of Si (100). The temperature of the substrate was 850-950 C. Previously, the substrate was cleaned with acetone and alcohol and were washed in an ultrasonic bath for 15 minutes each. The chamber was pumped to 9.3 x 10 -6 PA. The process was carried out for 30 minutes. The distance between the target and the substrate was 5 see

The disadvantages of this method are:

1. Time-consuming equipment for the coordination of high frequency signal with the load and instability discharge occurring in the near-cathode region, the difficulty in regulating relations in the resulting film of carbon from the gaseous component and silicon from the solid.

2. Spray rates on alternating current to less than half that of a direct current, as the sputtering of target atoms occurs in one half-period.

3. Use from the point of view of security of gas CH 4 as a source of carbon to obtain films of silicon carbide.

In the way WO 2009/011816 A1 (22.01.2009) get film heteroepitaxial SiC / Si by heating up to 1,000 degrees Celsius in the atmosphere of argon ion-plasma magnetron sputtering on direct current. Used target for magnetron sputtering on a direct current in a way not described, although it is the defining technological level of magnetron sputtering. In the body of the method is a reminder of the process with two targets Si and C, the target of monocrystalline wafers SiC (p - and n-type) with HF-magnetron sputtering and direct current priority is given to the process of reactive magnetron sputtering in an environment of methane (CH 4 ). This method is most close declared and therefore taken as a prototype.

The disadvantages of this method are obvious from the disadvantages of above-mentioned methods of obtaining films of silicon carbide silicon potoke. These weaknesses affect the perfection of the received epitaxial film.

The present invention is development of a new method of production of single-crystal film heteroepitaxial silicon carbide silicon substrate, which will provide safety and facilitation of technology, and to reduce production costs while maintaining the quality, sufficient for their subsequent use in the manufacture of elements of electronic engineering.

The technical result consists in the simplification of the production method, in improving the perfection of the coatings, silicon carbide silicon substrate.

The technical result is achieved plasma ion magnetron sputtering polycrystalline target SiC in argon atmosphere at direct current. The formation on a substrate of silicon epitaxial films of silicon carbide cubic polytype is on the surface preheated from 950 to 1400°C silicon wafer. The temperature of 950 C to this crystallization film silicon carbide in cubic politep on si substrate. The temperature of 1400 C to this melting point of silicon, which is the maximum value that have been obtained qualitative film silicon carbide silicon substrate.

Summary of the invention

The method of obtaining the film heteroepitaxial silicon carbide silicon substrate, which includes heating of the substrate temperatures of 950-1400°C in the atmosphere of Ar and obtaining of films on the substrate surface ion-plasma magnetron sputtering, differs in that the spraying carried out at direct current of one polycrystalline target silicon carbide.

A specific example

The method of obtaining the film heteroepitaxial silicon carbide silicon substrate consists of the following operations performed sequentially:

1. Download the working chamber:

a) preparation of the substrate the substrate using the monocrystal silicon plate brand KDB-3 (silicon semiconductor qualifications, doped with boron), area of 25 mm 2 300 microns thick with the orientation of the surface, rejected from the plane (111) (etching in HF within 2 hours, boiled in distilled water for 2 times, rinsing in alcohol);

b) installation of the substrate (13) at a distance of 5 cm from the magnetron in tungsten heater (11);

b) setting target (12) disc of polycrystalline silicon carbide with a diameter of 6 cm and a thickness of 0.5 cm, made from a powder of silicon carbide by pressing and subsequent sintering in argon at temperature 2400°C, on cooled by flowing water of the magnetron.

2. Pumping air from the working chamber with a vacuum system to 10 -6 mm Hg

3. The power of the heater surfaces (11), establishing a substrate temperature of 950 C.

4. Turning the system dosed overlap argon and bringing pressure from 0,6·10 -3 to 1·10 -3 mm Hg

5. The inclusion of cooling and power of the magnetron and receiving the discharge current density of 2-5 mA/cm 2 at a voltage between anode and cathode ~400 Century

6. 10 minutes after the beginning of the process of sputtering open the valve (10) and is deposition on a substrate for 30-60 minutes.

7. Upon reaching the required width of the epitaxial layer discharge current magnetron off, and the substrate cooled down to room temperature for 20 minutes.

On the figure 1 the block diagram of the magnetron sputtering system for thin SiC films on Si substrates, where 1 - stove installation, 2 - magnetic circuit, 3 - ring NdFeB magnets, 4 - brass cover, 5 - sealing fluoroplastic, 6 - insulating washer, 7 - metal washer, 8 - nut, 9 - tube input and output of the cooling water magnetron, 10 - flap, 11 - heater for the substrate, 12 - target, 13 - substrate, 14 - magnetic lines of force, 15 - stream of the sprayed substance.

Thus, the developed technology for formation on silicon substrates single-crystal films of silicon carbide with the necessary thickness and valid mechanical stresses. The proposed method allows to simplify the technology of production, to improve quality films and reduce energy costs.

The method of obtaining the film heteroepitaxial silicon carbide silicon substrate, which includes heating of the substrate temperatures of 950-1400°C in the atmosphere of Ar and obtaining of films on the substrate surface ion-plasma magnetron sputtering, wherein spraying is carried out on one of polycrystalline target silicon carbide.

 

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