CN1059935C - Isometric nanometer boron nitride film and its preparation - Google Patents
Isometric nanometer boron nitride film and its preparation Download PDFInfo
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- CN1059935C CN1059935C CN98104978A CN98104978A CN1059935C CN 1059935 C CN1059935 C CN 1059935C CN 98104978 A CN98104978 A CN 98104978A CN 98104978 A CN98104978 A CN 98104978A CN 1059935 C CN1059935 C CN 1059935C
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Abstract
The present invention relates to an isometric nanometer boron nitride film and a preparation method thereof. The isometric nanometer boron nitride film belongs to a thin-film material and the preparation method belongs to a method of physical vapor deposition. An isometric boron nitride film (3) is deposited on a silicon chip backing (1) directly with a transition layer arranged in the middle of the backing. Scales of crystal grains are 4 to 10 nm on average. The preparation method adopts a film plating machine and a radio frequency magnetron sputtering technology to strictly control the volume ratio of argon and nitrogen, and also control total pressure. Bias voltage of the backing (1) is gradually increased in a range of-(400 to 200) V, and temperature is controlled in a range of 400 to 500 DEG C. The device and the technology of the present invention have the advantages of easy process, low cost, small crystal grain scales of the prepared thin film, good crystallization, high integral purity and no burst; besides, the present invention is suitable for practical application.
Description
The invention belongs to a kind of thin-film material that the method for physical vapor deposition is prepared, particularly use the method for rf magnetron sputtering to prepare a kind of isometric nanometer boron nitride film material.
Cubic boron nitride (C-BN) has many excellent properties, as high rigidity, high resistivity, high heat conductance, good high temperature oxidation resistance and excellent chemical stability, sizable energy gap (6.2ev) and radioresistance.As thin-film material, it can give full play to these performances, utilizes these mechanics, electricity and semiconducting behavior can be used as the superhard coating of machine tools, can do high-power p type or n N-type semiconductorN device, can be used for aerospace radioprotective electronics device.Particularly it and some metal and isolator reasonable combination constitute storage element, and its storage capacity improves 28 times.
Recent two decades comes, and the various countries scientist adopts various chemical vapor deposition (CVD)s and physical vapor deposition (PVD) method to prepare cubic boron nitride film.The method of following the immediate a kind of vapour deposition of the present invention is that the technological process of the lonely light discharge ion film plating of magnetic control prepares cubic boron nitride film.Utilizing the lonely light discharge apparatus for ionically plating of magnetic control, is substrate with the silicon chip, at argon gas (Ar) and nitrogen (N
2) atmosphere in, be solid vaporizer with solid-state boron (B), under lonely light discharge and the action of a magnetic field, produce plasma body and on substrate deposition generate the C-BN film.In preparation process, add earlier on the silicon chip substrate-the 100v bias voltage, on silicon chip substrate, form the unordered hexagonal boron nitride film of one deck, reduce being biased into-200V again, cubic boron nitride is deposited on the hexagonal boron nitride.The structure of the cubic boron nitride film that this prepared goes out can be referring to Fig. 1.Fig. 1 is the cross-sectional view of prior art, and wherein 1 is silicon chip substrate, and 2 is the hexagonal boron nitride layer, and on hexagonal boron nitride layer 2 is cubic boron nitride film 3.Promptly between substrate 1 and cubic boron nitride film 3, hexagonal boron nitride layer 2 is arranged as transition layer.Because the existence of this transition layer is arranged, can alleviate the internal stress of thin-film material, keep cubic boron nitride film 3 not explosions.Simultaneously because the existence of this transition layer, and reduced the whole purity of cubic boron nitride film, the use of thin-film material is restricted, particularly given and make electronics element and bring difficulty.
The present invention adopts processing condition combination preferably and adopts the method for the bias voltage that raises piecemeal, direct growth cubic boron nitride film on substrate, but reach prepare whole purity height, not explosion, advantages of good crystallization, granularity is little, cost is low and the purpose of the cubic boron nitride film material of widespread use.
Isometric nanometer boron nitride film material of the present invention is a substrate with silicon chip or nickel sheet, directly deposits cubic boron nitride film on substrate, does not promptly have transition layer between substrate and cubic boron nitride film; The crystal particle scale of cubic boron nitride film is 4～10nm.
Fig. 2 provides the schematic cross-sectional view of cubic boron nitride film material of the present invention.Wherein 1 is substrate, and 3 is cubic boron nitride film.One side at the deposition cubic boron nitride film 3 of the substrate 1 of silicon chip or nickel sheet by the negative bias on the control substrate 1 among the preparation technology, was impregnated with the nitrogen ion before deposition cubic boron nitride film 3.Such structure can guarantee the high and not explosion of cubic boron nitride film 3 purity.
Description of drawings:
Fig. 1 is the schematic cross-sectional view of the cubic boron nitride film material of prior art.
Fig. 2 is the schematic cross-sectional view of cubic boron nitride film material of the present invention.
Isometric nanometer boron nitride film of the present invention is to use magnetic control sputtering film plating device, adopts the technological process of rf magnetron sputtering, direct deposition growing cubic boron nitride film 3 on the substrate 1 of silicon chip or nickel sheet.Key is to carry out nitriding to handle before the deposition cubic boron nitride film, makes film begin growth in the substrate top layer, increases the sticking power of film, overcomes the big problem of internal stress, makes not explosion of film.
Concrete processing condition are, are rake thin with the hexagonal boron nitride, charge into argon gas (Ar) and nitrogen (N after vacuumizing in the vacuum chamber of magnetic control sputtering film plating device
2), the volume ratio of the two is 100: (1～3), and the gas total pressure is controlled at 1.0～1.3Pa; The temperature of substrate 1 is controlled at 400～500 ℃; Substrate 1 connects with direct supply, makes substrate 1 produce self-bias, and the bias voltage size raises piecemeal in-(400～200) V scope, and nitriding is 1～2 hour under low bias voltage, and the sputter growing film is 0.5～2 hour under high bias voltage.
The cubic boron nitride film of processing condition preparations thus, through infrared spectra high-resolution electron microscope diffraction spectra analytical proof, this film is pure polycrystal cubic boron nitride film, the average crystal grain yardstick is 4～10nm.
Embodiment: with the hexagonal boron nitride is rake thin, is substrate 1 with the silicon chip, places in the vacuum chamber, and the sealed vacuum chamber charges into Ar and N again to vacuumize
2Gas, the two volume ratio is 100: 1.9, the gas total pressure is 1.2Pa, the temperature that makes substrate 1 of heating remains on (400 ± 2) ℃, the bias voltage that silicon chip substrate 1 is applied raises piecemeal, promptly add earlier-400V, again bias voltage was risen to through 1～2 hour-(200 ± 2) V, finish through 0.5～1.0 hour time deposition.
Why will the bias voltage of substrate 1 being raise piecemeal, is because substrate 1 under-400V bias voltage, can not deposit cubic boron nitride, but nitriding handles, and makes thereafter the cubic boron nitride film 3 of growth not add transition layer and directly deposits not explosion of film.After process-400V bias voltage for some time, bias voltage is risen to-(200 ± 2) V.Begin the cubic boron nitride of growing in the substrate top layer of nitriding, and form the structure of isometric nanometer boron nitride film material of the present invention, the crystal particle scale of this film is 5nm.
Isometric nanometer cubic boron nitride film material of the present invention has characteristics such as granularity is little, advantages of good crystallization, whole purity height, not explosion of strong adhesion.The technology of preparation isometric nanometer cubic boron nitride film material of the present invention, raw material sources are extensive, and cost is low; Equipment is fairly simple, and the condition ratio is easier to control, and is very favourable to carrying out large-scale production.Of the present invention cube of cubic boron nitride film material can be as the machine tools superhard coating, can mix becomes p type or n N-type semiconductorN material, can become novel multimode holder with some metal and isolator reasonable combination, also can be as the single-electron device material in field widespread uses such as large-scale integrated circuits.
Claims (3)
1. isometric nanometer boron nitride film material is to be substrate (1) with silicon chip or nickel sheet, it is characterized in that substrate (1) is gone up direct growth cubic boron nitride film (3), and the crystal particle scale of cubic boron nitride film (3) is 4～10nm.
2. an isometric nanometer boron nitride film preparation methods is used magnetic control sputtering film plating device, adopts the technological process of rf magnetron sputtering, charge into argon gas and nitrogen in the vacuum chamber, it is characterized in that, be rake thin with the hexagonal boron nitride, and the temperature of substrate (1) is controlled at 400～500 ℃; Argon gas is 100 with the volume ratio of nitrogen: (1～3), total pressure are 1.0～1.3Pa; What add on the substrate (1) of silicon chip or nickel sheet is biased in-raises piecemeal in (400～200) V scope, and nitriding is 1～2 hour under low bias voltage, and the sputter growing film is 0.5～2 hour under high bias voltage.
3. according to the making method of the described isometric nanometer boron nitride film material of claim 2, it is characterized in that it is to add earlier-400V that the bias voltage that adds on the said substrate (1) raises piecemeal, through 1.0～2.0 hours, again bias voltage is risen to-(200 ± 2) V, finish through 0.5～1.0 hour deposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98104978A CN1059935C (en) | 1998-01-21 | 1998-01-21 | Isometric nanometer boron nitride film and its preparation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN98104978A CN1059935C (en) | 1998-01-21 | 1998-01-21 | Isometric nanometer boron nitride film and its preparation |
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| CN1197847A CN1197847A (en) | 1998-11-04 |
| CN1059935C true CN1059935C (en) | 2000-12-27 |
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| CN98104978A Expired - Fee Related CN1059935C (en) | 1998-01-21 | 1998-01-21 | Isometric nanometer boron nitride film and its preparation |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100460560C (en) * | 2006-07-03 | 2009-02-11 | 吉林大学 | Process for the preparation of cubic boron nitride material |
| CN101798678B (en) * | 2010-03-29 | 2012-04-25 | 天津师范大学 | Novel super-hard TiB2/c-BN nano multi-layer film prepared by magnetron sputtering technique |
| CN102167612B (en) * | 2011-01-14 | 2012-09-26 | 中国人民解放军国防科学技术大学 | Preparation method of boron nitride coating on fiber surface |
| CN103668106B (en) * | 2012-09-01 | 2016-01-20 | 董国材 | A kind of method preparing monolayer hexagonal boron nitride |
| CN104948653A (en) * | 2015-04-27 | 2015-09-30 | 陈曦 | Production method of buffering and energy-absorbing nano fluid |
| CH713453A1 (en) * | 2017-02-13 | 2018-08-15 | Evatec Ag | Process for producing a substrate with a boron-doped surface. |
| CN110791805A (en) * | 2019-10-31 | 2020-02-14 | 中国电子科技集团公司第十三研究所 | Substrate, epitaxial wafer and growth method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5483920A (en) * | 1993-08-05 | 1996-01-16 | Board Of Governors Of Wayne State University | Method of forming cubic boron nitride films |
| JPH08144049A (en) * | 1994-09-21 | 1996-06-04 | Masaji Miyake | Production of thin cubic crystal boron nitride film |
| JPH08144045A (en) * | 1994-11-22 | 1996-06-04 | Toshiba Tungaloy Co Ltd | Cubic boron nitride coated member |
| JPH09202966A (en) * | 1996-01-23 | 1997-08-05 | Nippon Seimitsu Kk | Formation of thin film |
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1998
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5483920A (en) * | 1993-08-05 | 1996-01-16 | Board Of Governors Of Wayne State University | Method of forming cubic boron nitride films |
| JPH08144049A (en) * | 1994-09-21 | 1996-06-04 | Masaji Miyake | Production of thin cubic crystal boron nitride film |
| JPH08144045A (en) * | 1994-11-22 | 1996-06-04 | Toshiba Tungaloy Co Ltd | Cubic boron nitride coated member |
| JPH09202966A (en) * | 1996-01-23 | 1997-08-05 | Nippon Seimitsu Kk | Formation of thin film |
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| CN1197847A (en) | 1998-11-04 |
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