CN100360705C - High oxidation resistance nanocrystalline-amorphous structured superhard composite film cutting tool and deposition method therefor - Google Patents
High oxidation resistance nanocrystalline-amorphous structured superhard composite film cutting tool and deposition method therefor Download PDFInfo
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- CN100360705C CN100360705C CNB2005100182674A CN200510018267A CN100360705C CN 100360705 C CN100360705 C CN 100360705C CN B2005100182674 A CNB2005100182674 A CN B2005100182674A CN 200510018267 A CN200510018267 A CN 200510018267A CN 100360705 C CN100360705 C CN 100360705C
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Abstract
The present invention discloses a cutter coated with a superhard high-oxidation-resistant nanocrystalline-amorphous structured composite film and a deposition method thereof, which relates to a cutter coated with a superhard composite film and a deposition method thereof in the technical field of new materials, particularly to a cutter coated with a superhard nanocrystalline-amorphous structured film and a composite oxide film. The cutter is characterized in that a cutter 8 is orderly coated with a transition layer A with the adhesive action, a superhard nanocrystalline-amorphous structured nc-TiAlN/a-Si3N4 film B, a composite oxide film C for increasing the oxidation resistance and a self-lubrication film D with low friction coefficient. The deposition method comprises: an external target 1, an internal target 2 and an ion source 3 are arranged in a vacuum chamber 4. The present invention provides a film coating method which is suitable for practical industrial production; the deposition method has the characteristics of high production efficiency, good coating quality and low production cost, and has wide application value for various high-speed steel cutters, hard alloy cutters, ceramic cutters and various moulds.
Description
Technical field
The present invention relates to superhard composite film cutting tool and deposition method thereof in the new material technology field, particularly relate to a kind of nanocrystalline and amorphous structure superhard film and complex oxide film.
Background technology
The metal cutter plates hard coat, is considered to the revolution of cutting-tool engineering, and the cost that its increases is not many, but can increase substantially the work-ing life of cutter.Along with developing by leaps and bounds of modern manufacturing industry, difficult-to-machine material is more and more.Common cutter coat titanium nitride (TiN), titanium carbide (TiC) and TiAlN (TiAlN) etc. clearly can not adapt to harsh processing environment.External industrially developed country studies successfully many novel super-hard film materials one after another, and the H.D.Mammling of wherein Portuguese S.Carvalho and Germany etc. adopts magnetron sputtering and cathodic arc method deposition (Ti, Si, Al) N nano composite membrane and TiAlN/a-Si respectively
3N
4Nano composite membrane [S.Carvalho, E.Ribeiro, L, Rebouta etal.Surf, Soat, Technol.172 (2003) 109-116; H.D.Mannling, D.S.Patil, K.Motoet al.Surf.Coat Technol 146-147 (2001) 263-267].Its microhardness is up to 57GPa up to 40-50GPa; The resistance to oxidation temperature is above 1000 ℃.
Adopting physical vapor deposition (PVD) method plating hardening oxidation thing film on metal cutting tool, improve its stock-removing efficiency, is many pursuits of being engaged in the scientific worker of cutter coat research and design.As far back as 1996, the W.D.Sproul of the U.S. just proposed depositing Al
2O
3/ ZrO
2The imagination of oxide compound superlattice film, [S.D.Sproul, Science, 273 (1996) 889], but do not see the report of success so far.The development of vacuum coating technology provides twin target midfrequent AC magnetron sputtering technique, ion beam assisted deposition, and modern techniquies such as bidirectional pulse bias voltage deposition, the oxide film PVD method that this difficulty is bigger just might realize.
The film of above-mentioned super-hard film material and composite oxides is used it as metal cutting tool, also have no small gap.Adopt TiSi alloys target and TiAl alloys target to carry out reaction magnetocontrol sputtering, its result generates nanocrystalline nc-TiN/a-Si
3N
4Composite membrane, but can't generate nc-AlN/a-Si
3N
4, when this film directly was plated on the metal cutting tool, sticking power was difficult for guaranteeing, and its skin friction coefficient is big, is unfavorable for improving the abrasion resistance properties of cutter coat.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect that prior art exists, a kind of high oxidation resistance nanocrystalline and amorphous structure superhard composite film cutting tool and deposition method thereof are provided.
The object of the present invention is achieved like this.
1, the film of composite membrane system design
The superhard thin film that metal cutting tool and mould use requires to have " superhard, tough, heatproof, low wearing and tearing, self-lubricating " and very high sticking power, and obviously, any list-material all can not satisfy above-mentioned technical requirements comprehensively.The deposition superhard thin film develops towards the direction of diversification, multilayer film.
As shown in Figure 1, the composite membrane on cutter 8 has been followed successively by transition layer A, the nanocrystalline and amorphous structure (nc-TiAlN/a-Si of adhesive attraction
3N
4) superhard film (abbreviation superhard film) B, improve complex oxide film C, the self-lubricating film D of low frictional factor of oxidation resistent susceptibility, all retes are once finished on a coating equipment;
Described transition layer A, or be the zirconium nitride (ZrN) of doped rare earth element yttrium (Y), or be the zirconium carbide (ZrC) of doped rare earth element yttrium (Y);
TiAlN (TiAlN) uniform crystal particles that described superhard film B is a nanoscale intersperses among amorphous phase silicon nitride (Si
3N
4) among;
Described complex oxide film C is the aluminium sesquioxide (Al that mixes silicon of nanoscale
2O
3) and mix the zirconium dioxide (ZrO of yttrium
2) the superstructure complex oxide film formed.
Described self-lubricating film D is for mixing the diamond-film-like of titanium (Ti) and silicon (Si).
2, the setting that hits of vacuum chamber 4
The present invention adopts the physical vapor deposition (PVD) method to plate each layer function film on many target position vaccum ion coater.Coating equipment is made up of vacuum chamber 4, fire door 5, bleeding point 6, work rest 7, power supply and Controlling System etc.
At vacuum chamber 4 10 cover magnetron sputtering targets are set altogether: at vacuum chamber 4 outer walls, being provided with the cylindrical twin magnetic controlled sputtering target of 6 covers is external target; The promptly interior target of other 4 cover Rectangular Planar Magnetron Sputtering Target is contained on the circle of center Φ 45cm in the vacuum chamber 4, constitutes with corresponding external target respectively target magnetic field is coupled, and pole polarity is opposite.2 cover diameter low energy broad beam ion source, one is sleeved on the fire door 5 relative with bleeding point 6, on the another set of circle that is contained in center Φ 45cm in the vacuum chamber; Work rest 7 connects the bidirectional pulse grid bias power supply.
Specifically, as shown in Figure 2, the present invention is provided with external target, interior target, ion source altogether in vacuum chamber 4;
External target is included in outer wall place in the vacuum chamber 4, the outer target 1.1 that counter-clockwise direction sets gradually, outer two targets 1.2, outer three targets 1.3, outer four targets 1.4, outer five targets 1.5, outer six targets 1.6; The line of centres with fire door 5 and bleeding point 6 is an axle, a then outer target 1.1, outer two targets 1.2, outer three targets 1.3 and outer four targets 1.4, outer five targets 1.5, and outer six targets 1.6 are distribution symmetrically and evenly;
Interior target is included in an interior target 2.1, interior two targets 2.2, interior three targets 2.3, interior four targets 2.4 that counter-clockwise direction sets gradually on the circle of center φ 45cm in the vacuum chamber 4; In a target 2.1, interior two targets 2.2, interior 3 targets 2.3, interior four targets 2.4 respectively with an outer target 1.1, outer two targets 1.2, outer five targets 1.5, outer six targets 1.6 are relative;
Ion source is included on the fire door 5 second ion source 3.2 relative with bleeding point 6 that is provided with on the circle of first ion source 3.1 that is provided with and center φ 45cm in vacuum chamber 4;
An outer target 1.1, outer two targets 1.2, outer three targets 1.3, outer four targets 1.4, outer five targets 1.5, the target of outer six targets 1.6 is respectively aluminum silicon alloy, zirconium yittrium alloy, titanium silicon, aluminum silicon alloy, zirconium yittrium alloy, titanium silicon;
The target of interior target is a high purity graphite.
3, the deposition step of composite membrane
(1) deposition of transition layer A
The deposition of this transition layer A utilizes outer two targets 1.2, outer five targets 1.5 to finish.
With zirconium yttrium (Zr-Y) alloys target deposition transition layer, should select the material of transition layer according to the material classification of cutter 8.For example: rapid steel class cutter, adopt zirconium nitride (ZrN) as transition layer usually; And Wimet class cutter adopts zirconium carbide (ZrC) as transition layer usually, can improve the matching of sticking power and the deposited film and the body material of deposited film like this.
The present invention adopts zirconium yttrium (Zr-Y) alloys target deposition to mix the transition layer of yttrium, and in alloy, rare earth element yttrium accounts for 5-9 at.%; The adding of rare earth element yttrium can make the grain refining of zirconium nitride (ZrN) or zirconium carbide (ZrC), and improves the wetting property of zirconium (Zr) and body material, thereby can increase the sticking power of deposited film and matrix.
The zirconium nitride transition layer of mixing yttrium with deposition is an example below, the method for deposition transition layer is described: cutter 8 usefulness chemical processes are cleaned up; Cleaned 20 minutes through ionic fluid earlier in vacuum chamber 4, make the surface reach the atom level cleanliness factor, the control ion beam energy is 1000eV, and vacuum chamber feeds argon (Ar) gas, and keep-uping pressure is 2 * 10
-2Pa; After finishing, cleaning changes logical argon nitrogen (Ar-N
2) gas mixture, ratio of mixture Ar: N
2=3: 1, keeping vacuum chamber pressure is 5 * 10
-1Pa, unidirectional pulse bias voltage-800-1000V, duty 75-85%; Open outer two targets 1.2, outer five targets 1.5, control sputtering current 38-42A, the ion energy that improves ionic fluid carries out Ion Mixing to 2000eV, makes sedimentary zirconium (Zr) and yttrium (Y) atom, can infiltrate the degree of depth of workpiece substrate surface 3-5nm; After 5-8 minute, ion beam energy is reduced to 150-200eV, enter the ion beam assisted depositing stage, pulsed bias-150 200V, dutycycle 40-50%, maintenance workpiece revolution speed 4-6 circle/minute, make sedimentary zirconium nitride (ZrYN) transition layer of mixing yttrium have higher sticking power and rete density, keep cutter 8 storing temperature 350-400 ℃, the thickness 0.3-0.5 μ m of control transition layer.
(2) nanocrystalline and amorphous (nc-TiAlN/a-Si
3N
4) deposition of superhard film
Utilize an outer target 1.1, outer three targets 1.3, outer four targets 1.4, outer six targets, 1.6 depositions.
Wherein two overlap titanium silicon targets, silicon content 4-8at.%, the aluminum silicon alloy target of a separate set of, silicon content 4-8at.%; During the deposition superhard film, open this quadruplet target simultaneously, working gas argon nitrogen (Ar-N
2) gas mixture.Because the result of reactive sputtering, the metal titanium atom is easy to generate the titanium nitride (TiN) of centroid cubic crystal system, the metallic aluminium atom also generates the aluminium nitride (AlN) of hexagonal system easily, and the speed of rotation of regulation and control workpiece just can be controlled at the grain-size of above-mentioned nitride below the 10nm.When generating above-mentioned nitride, the element silicon in two kinds of alloys target is also sputtered out, and it but generates amorphous phase Si
3N
4, clad crystal grain outside surface simultaneously at above-mentioned metal nitride, stop crystal grain further to be grown up.This film meets the rule that the Hall-Patch relational expression is described, and its yielding stress or hardness are directly proportional with its Young's modulus, and is subjected to the restriction of tiny crack growth in the technology.The grain-size of metal nitride hard phase is the principal element that influences the composite membrane microhardness in the composite membrane, the ratio of amorphous phase also has a significant impact the microhardness of film, metal nitride nanocrystal and amorphous phase nitride form firm interface, and avoiding the crystal boundary slippage is the gordian technique that improves the composite membrane microhardness.
Concrete deposition method is as follows: after the thickness of transition layer reaches predetermined number, open above-mentioned quadruplet target, reduce the electric current of outer two targets 1.2, outer five targets 1.5 then gradually until 0, the sputtering current 28-32A of outer three targets 1.3 of control, outer six targets 1.6, the sputtering current 38-42A of the outer target 1.1 of control, outer four targets 1.4 keeps (Ar-N
2) gaseous tension 5 * 10 of ratio of mixture 3: 1 and vacuum chamber
-1Pa, the adjustment grid bias power supply is a bidirectional pulse, pulsed voltage 200-250V, dutycycle 40-50%, 4-6 rev/min of control workpiece revolution speed, ion source leads to Ar-N
2Gas mixture, flow 20sccm, ion beam energy 150-200eV keeps workpiece temperature 350-400 ℃, after control superhard film thickness reaches 3-5 μ m, enters next step technology.
(3) deposition of complex oxide film C
In vacuum plating unit, utilize an outer target 1.1, outer two targets 1.2, outer four targets 1.4, outer five targets, 1.5 depositions to mix the aluminium sesquioxide (Al of silicon
2O
3) and mix the zirconium dioxide (ZrO of yttrium
2) the superstructure complex oxide film formed.
Open above-mentioned quadruplet external target, working gas is argon oxygen (Ar-O
2) gas mixture; Because the result of reactive sputtering has generated aluminium sesquioxide (Al
2O
3) and zirconium dioxide (ZrO
2), silicon and yttrium mix respectively in the oxide film, and these two kinds of oxide compounds all have the chemical property of stabilizer pole, and are the highest two kinds of microhardness in all oxides film, the hardness of oxide compound is more much lower than metal nitride and carbide after all, will mix the aluminium sesquioxide (Al of silicon
2O
3) and mix the zirconium dioxide (ZrO of yttrium
2) form the superlattice composite membrane, will improve its microhardness greatly.
Concrete deposition method is as follows:
Deposition finishes after the superhard film B, and the electric current that reduces outer three targets 1.3, outer six targets 1.6 gradually is until O, and opens outer two targets 1.2, outer five targets 1.5, reduces nitrogen flow gradually until 0; Open oxygen simultaneously, flow increases to Ar: O gradually
2=5: 1-4: 1, keeping deposition pressure is (5-8) * 10
-1Pa, workpiece revolution speed be 4-6 circle/minute, bidirectional pulse bias voltage 200-250V, dutycycle 40-50%, the sputtering current 38-42A of two targets 1.2, outer five targets 1.5 outside keeping, the sputtering current 38-42A of an outer target 1.1, outer four targets 1.4, keep ion source gas flow 20sccm, Ar, O
2Ratio of mixture is identical with reactive sputtering gas, the ion energy 150-200eV of ionic fluid, and the thickness of control composite oxides is 2-3 μ m.
(4) deposition of self-lubricating film D
Needs according to reality is used on the outermost top layer of workpiece, deposit the self-lubricating film of one deck low-friction coefficient, can reduce the cutting force of cutter, reduce the abrasion in the mould use, for being significant the work-ing life of improving cutter and mould.
The present invention adopts outer three targets 1.3, interior target totally five cover target deposition self-lubricating film D.
The target of outer three targets 1.3 is titanium silicon (TiSi) alloy, and the target of interior target is high purity graphite;
During deposition, above-mentioned five cover targets start simultaneously, and argon (Ar) is a workpiece gas, keeps vacuum chamber pressure (5-8) * 10
-1Pa, the sputtering current of interior target is controlled at 28-32A, and the sputtering current of outer three targets 1.3 is 5-8A, Workpiece Rotating speed, workpiece temperature is all consistent with the depositing operation of complex oxide film C with ionogenic working parameter.
The self-lubricating film D that deposits is a diamond-film-like of mixing titanium and silicon, and it is by SP
3Amorphous diamond phase and the SP of hybrid electron track Cheng Jian
2The kish phase composite of hybrid electron track Cheng Jian, the microhardness HK=20-25GPa of this film, wear rate Kc=1.0 * 10
-17m
3/ mN, coefficientoffriction<0.1 in the DLC-Ti film, must control titaniferous ratio be 4-8%, the thickness of self-lubricating film is 1-2 μ m.
Above-mentioned four class functional membranes are deposited on the various metal cutting tools successively, can be used for the cutting of heavy lift high speed cutting, dried cutting and various difficult-to-machine materials.
The present invention has the following advantages and positively effect:
1, the nanocrystalline and amorphous structure superhard film that deposits by the present invention is a kind of novel super-hard thin-film material, and it not only has higher microhardness, and the resistance to oxidation temperature is above 1000 ℃, than the cutter coat excellent performance of routine.
2, one deck complex oxide film C of the present invention promptly mixes the aluminium sesquioxide (AL of silicon
2O
3) and mix the zirconium dioxide (ZrO of yttrium
2) the superstructure complex oxide film formed, it is the highest two kinds of microhardness in all oxides material, also has highly stable chemical property simultaneously.It is introduced cutter coat, can improve greatly coated cutting tool in the heavy lift high speed cutting, do the work-ing life in cutting and the difficult-to-machine material.
3, the present invention is the complete cutter high-quality coating film coating method of a cover, transition layer A, superhard film B, complex oxide film C and surface self-lubricating film D that it will play adhesive attraction very ideally combine, make the high-quality coating of this cutter can adapt to the modern manufacturing industry technical requirements very harsh, the work-ing life of having improved high-grade cutter to metal cutting tool.
4, the invention provides a kind of suitable industrialization and produce actual film coating method, have production efficiency height, coating quality is good, production cost is low characteristics, for various types of speedy steel cutting-tools, inserted tool and sintex, and various mould all has a wide range of applications.
Description of drawings
The film of Fig. 1-composite membrane is a design diagram;
Fig. 2-vaccum ion coater vacuum chamber cross sectional representation.Wherein:
The A-transition layer;
B-nanocrystalline and amorphous structure (nc-TiAlN/a-Si
3N
4) superhard film, be called for short superhard film;
The C-complex oxide film;
The D-self-lubricating film.
Cylindrical twin magnetic controlled sputtering target is called for short external target, comprising:
1.1-the first cylindrical twin magnetic controlled sputtering target is called for short an outer target, target is an aluminum silicon alloy;
1.2-the second cylindrical twin magnetic controlled sputtering target is called for short outer two targets, target is the zirconium yittrium alloy;
1.3-three cylinders shape twin magnetic controlled sputtering target is called for short outer three targets, target is a titanium silicon;
1.4-the 4th cylindrical twin magnetic controlled sputtering target is called for short outer four targets, target is an aluminum silicon alloy;
1.5-the 5th cylindrical twin magnetic controlled sputtering target is called for short outer five targets, target is the zirconium yittrium alloy;
1.6-the 6th cylindrical twin magnetic controlled sputtering target is called for short outer six targets, target titanium silicon is alloy.
The rectangle magnetron sputtering target, target in being called for short comprises:
2.1-the first rectangle magnetron sputtering target, a target in being called for short, target is the high purity graphite target;
2.2-the second rectangle magnetron sputtering target, two targets in being called for short, target is the high purity graphite target;
2.3-the 3rd rectangle magnetron sputtering target, three targets in being called for short, target is the high purity graphite target;
2.4-the 4th rectangle magnetron sputtering target, four targets in being called for short, target is the high purity graphite target.
Diameter low energy broad beam ion source is called for short ion source, comprising:
3.1-first diameter low energy broad beam ion source is called for short first ion source;
3.2-second diameter low energy broad beam ion source is called for short second ion source.
The 4-vacuum chamber.
The 5-fire door.
The 6-bleeding point.
The 7-work rest.The 8-cutter.
Embodiment
1, the explanation of several important technological problems
The application of 1. cylindrical magnetic control sputtering target
The two class film material with function nanocrystalline and amorphous structure (nc-TiAlN/a-Si that the present invention relates to
3N
4) superhard film (abbreviation superhard film) and mix the aluminium sesquioxide (Al of silicon
2O
3), mix the zirconium dioxide (ZrO of yttrium
2) the superstructure complex oxide film formed, all belong to the very high insulating film of resistivity, the sputter product is often attached to the non-sputter area of target surface during deposition, and be extended to sputter area gradually, cause target surface " poisoning " phenomenon, positive charge is enriched on the insulating film, to to a certain degree causing the target surface arc discharge, the lighter causes the target power supply job insecurity, severe patient even burn shielding power supply, the best approach that solves this technical problem is to adopt cylindrical twin magnetic controlled sputtering target, adapted midfrequent AC shielding power supply.Cylindrical target is compared with the rectangle plane target with power, higher sputter deposition rate is arranged, and its target utilization is much higher, and three kinds of alloy target materials that the present invention adopts are all made the pipe shape easily, do not have processing difficulties.
2. the use of bidirectional pulse grid bias power supply
Common vacuum ion membrane plating, workpiece connects negative bias, and is positively charged from the metal ion that target as sputter comes out, and obtains kinetic energy under the workpiece effect of electric field, with higher speed bombardment workpiece surface, improved the density and the sticking power of deposited film.Deposition process for insulating film, the poor electric conductivity of insulating film, positive charge constitute the structure of similar electrical condenser at the negative potential of its surface-area base and workpiece, when insulating film during at a certain thickness, when relative voltage surpassed a certain threshold value, it was breakdown insulating film to take place, and this is concerning film-coating workpiece, to be catastrophic, change the unidirectional pulse grid bias power supply that is connected on the workpiece into the bidirectional pulse grid bias power supply, can eliminate long-pending base of positive charge on insulating film surface, thereby avoided the electrical breakdown of depositional coating.
3. ionogenic use
The present invention adopts full magnetron sputtering deposition two class novel super-hard films, adapted diameter low energy broad beam ion source, ion source is workpiece further physics cleaning in vacuum chamber, make it to reach the atom level cleanliness factor, high efficiency purging method is provided, magnetron sputtering is compared with cathodic arc ion plating, because of its ionization level is low, thereby the rete of magnetically controlled sputter method rate of film build and the too late cathodic arc ion plating of film adhesion often occurs.Adopt ion beam assisted depositing, just can remedy the deficiency of magnetron sputtering plating, add cylindrical twin target midfrequent AC magnetron sputtering The application of new technique, the superlattice composite membrane and the nanocrystalline and amorphous superhard composite film that new magnetron sputtering technique can be deposited have neat interface are brought into play its irreplaceable advantage.
2, experimental result
Experiment 1: on an Alcatel SCM650 type equipment, configuration quadruplet magnetron sputtering target adopts TiAl alloy (Ti
0.5Al
0.5) target and TiSi alloys target (siliceous 3-8at.% in the Ti alloy), adopt magnetically controlled DC sputtering depositing Ti AlSiN film, its microhardness Hv=41-58GPa, Young's modulus 438-538GPa.
Experiment 2: on the two target magnetic control sputtering coating equipments of a DMS type, adopt DC pulse reactive sputter-deposition Al
2O
3, workpiece connects pulsed bias power supply, frequency 40KHz.Control sputtering power 11-17KW, obtains nanocrystalline Al by underlayer temperature 760-770 ℃
2O
3, grain-size 20-30nm, thickness 2 μ m, the highest microhardness Hv=22GPa.
Experiment 3: on a MRC-90ZM type magnetron sputtering coater, adopt DC pulse reactive sputter-deposition ZrO
2, pulsed bias power supply, frequency 20KHz, pulse shielding power supply frequency 30KHz, working gas Ar-O
2Gas mixture generates cubic phase m-ZrO
2, microhardness Hv=14-21GPa, sedimentation rate is 75% of a pure metal zirconium.
Experimental result shows that superhard composite film of the present invention has fabulous performance.
Claims (2)
1, a kind of superhard composite film cutting tool of high oxidation resistance nanocrystalline and amorphous structure comprises cutter (8), it is characterized in that:
Composite membrane on cutter (8) has been followed successively by transition layer (A), the nanocrystalline and amorphous structure nc-TiAlN/a-Si of adhesive attraction
3N
4Superhard film (B), the complex oxide film (C) that improves oxidation resistent susceptibility, the self-lubricating film (D) of low-friction coefficient;
Described transition layer (A), or be the zirconium nitride of doped rare earth element yttrium, or be the zirconium carbide of doped rare earth element yttrium;
Described superhard film (B) intersperses among composite membrane among the amorphous phase silicon nitride for the TiAlN uniform crystal particles of nanoscale;
Described complex oxide film (C) is the aluminium sesquioxide of mixing silicon of nanoscale and the superstructure complex oxide film of the zirconium dioxide composition of mixing yttrium;
Described self-lubricating film (D) is for mixing the diamond-film-like of titanium and silicon.
2, a kind of deposition method of superhard composite film cutting tool of high oxidation resistance nanocrystalline and amorphous structure, be included in the physical vapor deposition PVD method of each layer function film of deposition on many target position vaccum ion coater, this coating equipment is made up of vacuum chamber (4), fire door (5), bleeding point (6), work rest (7), power supply and Controlling System etc.;
It is characterized in that:
(1) setting that hits of vacuum chamber (4)
In vacuum chamber (4), be provided with external target, interior target, ion source altogether;
External target is included in outer wall place in the vacuum chamber (4), the outer target (1.1) that counter-clockwise direction sets gradually, outer two targets (1.2), outer three targets (1.3), outer four targets (1.4), outer five targets (1.5), outer six targets (1.6); The line of centres with fire door (5) and bleeding point (6) is an axle, a then outer target (1.1), outer two targets (1.2), outer three targets (1.3) and outer four targets (1.4), outer five targets (1.5), and outer six targets (1.6) are distribution symmetrically and evenly;
Interior target is included in an interior target (2.1), interior two targets (2.2), interior three targets (2.3), interior four targets (2.4) that counter-clockwise direction sets gradually on the circle of vacuum chamber (4) interior center φ 45cm; In a target (2.1), interior two targets (2.2), interior three targets (2.3), interior four targets (2.4) respectively with an outer target (1.1), outer two targets (1.2), outer five targets (1.5), outer six targets (1.6) are relative;
Ion source is included in second ion source (3.2) relative with bleeding point (6) that is provided with on the circle of last first ion source (3.1) that is provided with of fire door (5) and center φ 45cm in vacuum chamber (4);
An outer target (1.1), outer two targets (1.2), outer three targets (1.3), outer four targets (1.4), outer five targets (1.5), the target of outer six targets (1.6) is respectively aluminum silicon alloy, zirconium yittrium alloy, titanium silicon, aluminum silicon alloy, zirconium yittrium alloy, titanium silicon;
The target of interior target (2) is a high purity graphite;
(2) deposition step of composite membrane
1. the deposition of transition layer (A)
Utilize outer two targets (1.2), outer five targets (1.5) to finish;
The control thickness is 0.3-0.5 μ m;
2. nanocrystalline and amorphous nc-TiAlN/a-Si
3N
4The deposition of superhard film (B)
Utilize an outer target (1.1), outer three targets (1.3), outer four targets (1.4), outer six targets (1.6) to finish;
The control thickness is 3-5 μ m;
3. the deposition of complex oxide film (C)
Utilize an outer target (1.1), outer two targets (1.2), outer four targets (1.4), outer five targets (1.5) to finish;
The control thickness is 2-3 μ m;
4. the deposition of self-lubricating film (D)
Outer three targets (1.3) of utilization, interior target totally five cover targets are finished;
The control thickness is 1-2 μ m.
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CN101768724B (en) * | 2008-12-29 | 2011-08-03 | 中国科学院兰州化学物理研究所 | Method for preparing film on stainless steel |
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