CN102409289A - Preparation method of B-C-N ternary film - Google Patents
Preparation method of B-C-N ternary film Download PDFInfo
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- CN102409289A CN102409289A CN2011103073316A CN201110307331A CN102409289A CN 102409289 A CN102409289 A CN 102409289A CN 2011103073316 A CN2011103073316 A CN 2011103073316A CN 201110307331 A CN201110307331 A CN 201110307331A CN 102409289 A CN102409289 A CN 102409289A
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- film
- body material
- graphite
- target
- boron
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052796 boron Inorganic materials 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 29
- 239000010439 graphite Substances 0.000 claims abstract description 29
- 238000004544 sputter deposition Methods 0.000 claims abstract description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910011208 Ti—N Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 2
- 239000010408 film Substances 0.000 description 35
- 238000000034 method Methods 0.000 description 6
- 238000000151 deposition Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
A preparation method of a B-C-N ternary film by radio frequency (13.56 MHz) magnetron sputtering forms a multilayer transition film of Ti, TiN, Ti-B-C-N on a metal substrate surface so as to improve the binding performance of the B-C-N ternary film and the metal substrate; meanwhile, an appropriate graphite/boron composite target and corresponding sputtering technological parameters are selected so as to obtain a high-performance film with a stoichiometric ratio close to BC2N; the B-C-N thickness in the film is about 150 nm; the atom percents of elements on the film surface is 23.4B-52.2C-24.4N; and the hardness of the surface is about 15 GPa.
Description
Technical field
The present invention relates to a kind of preparation method of material surface coating, especially a kind of preparation method of B-C-N ternary film.
Background technology
According to mechanism's similarity of diamond and cube BN (c-BN), people's expected in theory can be synthesized the B-C-N ternary film, and expects that it can have adamantine ultrahigh hardness and c-BN high-temperature stability, oxidation-resistance etc. concurrently.And confirm through extensive experimental; Synthetic B-C-N ternary film is truly feasible; And also certain the same with cube BN the hardness of B-C-N ternary film with superelevation with diamond; In addition, compare with hard coats such as diamond, carbonitrides, it also has unrivaled use advantages such as the internal stress of stability at elevated temperature excellence, film is low.Therefore, the B-C-N ternary film not only becomes the hard coat hot research fields, and its practical application in corresponding field is also increasingly extensive, has immeasurable huge performance potential and wide application prospect.
And the method that is used to prepare the B-C-N ternary film is also very general, and for example the film synthesis preparation method of routine such as chemical Vapor deposition process and physical vaporous deposition can be used for preparing the B-C-N ternary film.But when being to use chemical gaseous phase depositing process, often its boron source gas etc. all has toxicity, all causes very big pressure for environment and production safety; Moreover, research shows the result of chemical gaseous phase depositing process preparation, all trends towards obtaining hexangle type B-C-N ternary film but not cube B-C-N ternary film.Comparatively speaking, to be sputtered to the physical gas-phase deposite method of characteristic, because of it uses solid phase target source usually, then safer convenience the particularly important is it and trends towards making a cube B-C-N ternary film.
Yet, for the control of the composition of B-C-N ternary film, with the problems such as elimination of the close attachment of matrix, film internal stress on, still have various deficiencies, become the obstacle of restriction B-C-N ternary film widespread use.
Summary of the invention
To the problems referred to above, the object of the invention promptly is to rf magnetron sputtering B-C-N ternary film preparation method selects suitable processing parameter, thereby obtains a kind of and the matrix bond preparation method of high-performance rigid B-C-N ternary film closely.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is following:
At first, with the metal matrix material surface finish, and after each cleans about 10min in ultrasonic cleaner with acetone, alcohol and deionized water etc. respectively, dry up subsequent use with nitrogen.
Subsequently; Body material is placed on the sample table in the Vakuumkammer; And the Ti target placed different target position respectively with graphite/boron composition target, wherein said graphite/boron composition target is that cyclic boron is enclosed within outside the flaky graphite of circle, and the area of graphite and boron is than 2.5: 1-2: between 1; The purity of graphite is 99.999%, the purity of boron is 99.9%, and graphite/boron composition target and body material distance are 7-8cm.
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10
-4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and preparatory sputter 2-3min, the power of sputter is 50-70W in advance, with the film formation surface of further cleaning body material.
The flow of keeping Ar subsequently is 8-10sccm; Control body material temperature is 40-50 ℃, when gas pressure in vacuum is 1-1.5Pa, applies the negative bias of 100-150V to body material; Remove the baffle plate of Ti target simultaneously; Power with 50-70W carries out sputter, and sputtering time is 5-10min, to form the pure Ti film of one deck.
Begin to feed the N that flow is 0.3-0.6sccm subsequently
2And the flow of keeping Ar is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 40-50 ℃; Continuation is carried out sputter with the power of 50-70W, and sputtering time is 15-25min, to form one deck Ti-N binary film.
The flow of keeping Ar subsequently is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is 100-150V, and the temperature of rising body material is 250-300 ℃, N
2Flow be 0.8-1sccm, remove the baffle plate of graphite/boron composition target, the power that the Ti target is kept with 50-70W carries out sputter, and graphite/boron composition target carries out sputter with 100-110W power, sputtering time is 15-25min, to form Ti-B-C-N quaternary film.
The flow of keeping Ar subsequently is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 250-300 ℃, closes Ti target baffle plate and keeps graphite/boron Film by Sputtering of Composite Target, N
2Flow raise and to be 3.5-4.5sccm, sputtering power is increased to 130-140W, sputtering time is 80-100min, to form the B-C-N ternary film.
Advantage of the present invention is: formed Ti, TiN, Ti-B-C-N multilayer transition film at metal base surface, to improve B-C-N film and metallic matrix good binding performance; Simultaneously, select suitable graphite/boron composition target and corresponding splash-proofing sputtering process parameter for use, obtained to approach BC
2The high performance thin film of N stoichiometric ratio.
Embodiment
Below, through concrete embodiment the present invention is elaborated.
A kind of radio frequency of B-C-N ternary film (13.56MHz) magnetron sputtering preparation method, it comprises following preparation process:
At first, select for use the W6Mo5Cr4V2 rapid steel,, and after each cleans about 10min in ultrasonic cleaner with acetone, alcohol and deionized water etc. respectively, dry up subsequent use with nitrogen its surface finish as body material.
Subsequently; Body material is placed on the sample table in the Vakuumkammer; And the Ti target placed different target position respectively with graphite/boron composition target, wherein said graphite/boron composition target is that cyclic boron is enclosed within outside the flaky graphite of circle, and the area of graphite and boron is than at 2.2: 1; The purity of graphite is 99.999%, the purity of boron is 99.9%, and graphite/boron composition target and body material distance are 8cm.
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10
-4Pa feeds the Ar that flow is 9sccm simultaneously, when gas pressure in vacuum is 3Pa, and preparatory sputter 2min, the power of sputter is 60W in advance, with the film formation surface of further cleaning body material.
The flow of keeping Ar subsequently is 9sccm, and control body material temperature is 40 ℃, when gas pressure in vacuum is 1.5Pa; Apply the negative bias of 130V to body material, remove the baffle plate of Ti target simultaneously, carry out sputter with the power of 60W; Sputtering time is 7min, to form the pure Ti film of one deck.
Begin to feed the N that flow is 0.4sccm subsequently
2, and the flow of keeping Ar is that 9sccm, gas pressure in vacuum are that the negative bias of 1.5Pa, body material is that the temperature of 130V, body material is 40 ℃, continues to carry out sputter with the power of 60W, sputtering time is 20min, to form one deck Ti-N binary film.
The flow of keeping Ar subsequently is that 9sccm, gas pressure in vacuum are that the negative bias of 1.5Pa, body material is 130V, and the temperature of rising body material is 270 ℃, N
2Flow be 0.9sccm, remove the baffle plate of graphite/boron composition target, the power that the Ti target is kept with 60W carries out sputter, and graphite/boron composition target carries out sputter with 110W power, sputtering time is 20min, to form Ti-B-C-N quaternary film.
The flow of keeping Ar subsequently is that 9sccm, gas pressure in vacuum are that the negative bias of 1.5Pa, body material is that the temperature of 130V, body material is 270 ℃, closes Ti target baffle plate and keeps graphite/boron Film by Sputtering of Composite Target, N
2Flow raise and to be 4sccm, sputtering power is increased to 140W, sputtering time is 90min, to form the B-C-N ternary film.
Through test, the thickness of surperficial B-C-N film is about 150nm, and the atoms of elements percentage composition of film surface is 23.4B-52.2C-24.4N, and the hardness on surface is about 15GPa.Appearance is smooth smooth, and frictional coefficient is about 0.11 during 5mN.The placement a few days does not have the problem of obvious cracking, projection to occur in air.
Claims (2)
1. the radio frequency of a B-C-N ternary film (13.56MHz) magnetron sputtering preparation method is characterized in that:
At first, with the metal matrix material surface finish, and after each cleans about 10min in ultrasonic cleaner with acetone, alcohol and deionized water etc. respectively, dry up subsequent use with nitrogen.
Subsequently; Body material is placed on the sample table in the Vakuumkammer; And the Ti target placed different target position respectively with graphite/boron composition target, wherein said graphite/boron composition target is that cyclic boron is enclosed within outside the flaky graphite of circle, and the area of graphite and boron is than 2.5: 1-2: between 1; The purity of graphite is 99.999%, the purity of boron is 99.9%, and graphite/boron composition target and body material distance are 7-8cm.
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10
-4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and preparatory sputter 2-3min, the power of sputter is 50-70W in advance, with the film formation surface of further cleaning body material.
The flow of keeping Ar subsequently is 8-10sccm; Control body material temperature is 40-50 ℃, when gas pressure in vacuum is 1-1.5Pa, applies the negative bias of 100-150V to body material; Remove the baffle plate of Ti target simultaneously; Power with 50-70W carries out sputter, and sputtering time is 5-10min, to form the pure Ti film of one deck.
Begin to feed the N that flow is 0.3-0.6sccm subsequently
2And the flow of keeping Ar is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 40-50 ℃; Continuation is carried out sputter with the power of 50-70W, and sputtering time is 15-25min, to form one deck Ti-N binary film.
The flow of keeping Ar subsequently is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is 100-150V, and the temperature of rising body material is 250-300 ℃, N
2Flow be 0.8-1sccm, remove the baffle plate of graphite/boron composition target, the power that the Ti target is kept with 50-70W carries out sputter, and graphite/boron composition target carries out sputter with 100-110W power, sputtering time is 15-25min, to form Ti-B-C-N quaternary film.
The flow of keeping Ar subsequently is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 250-300 ℃, closes Ti target baffle plate and keeps graphite/boron Film by Sputtering of Composite Target, N
2Flow raise and to be 3.5-4.5sccm, sputtering power is increased to 130-140W, sputtering time is 80-100min, to form the B-C-N ternary film.
2. the radio frequency of a kind of B-C-N ternary film according to claim 1 (13.56MHz) magnetron sputtering preparation method; It is characterized in that: the thickness of said B-C-N film is about 150nm; Hardness is about 15GPa, and the atoms of elements percentage composition is 23.4B-52.2C-24.4N.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110307331 CN102409289B (en) | 2011-10-11 | 2011-10-11 | Preparation method of B-C-N ternary film |
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| CN 201110307331 CN102409289B (en) | 2011-10-11 | 2011-10-11 | Preparation method of B-C-N ternary film |
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| CN102409289B CN102409289B (en) | 2013-09-18 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525734A (en) * | 2009-03-31 | 2009-09-09 | 西安交通大学 | Method for preparing boron, carbon and nitrogen hard coating |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525734A (en) * | 2009-03-31 | 2009-09-09 | 西安交通大学 | Method for preparing boron, carbon and nitrogen hard coating |
Non-Patent Citations (2)
| Title |
|---|
| 《Surface and Coatings Technology》 20060630 Z.F.Zhou,et al. "Synthesis and characterization of boron carbon nitride films by radio frequency magnetron sputtering" 第334-340页 1-2 第128-129卷, * |
| Z.F.ZHOU,ET AL.: ""Synthesis and characterization of boron carbon nitride films by radio frequency magnetron sputtering"", 《SURFACE AND COATINGS TECHNOLOGY》 * |
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