CN1654701A - Nano super-lattice structured superhard composite film cutting tool and deposition method therefor - Google Patents
Nano super-lattice structured superhard composite film cutting tool and deposition method therefor Download PDFInfo
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- CN1654701A CN1654701A CN 200510018266 CN200510018266A CN1654701A CN 1654701 A CN1654701 A CN 1654701A CN 200510018266 CN200510018266 CN 200510018266 CN 200510018266 A CN200510018266 A CN 200510018266A CN 1654701 A CN1654701 A CN 1654701A
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Abstract
The present invention is super hard composite film in nanometer superlattice structure for cutter and its depositing process, and especially relates to the setting and components of the work targets. Inside the vacuum chamber, there are inner target, middle target and outer target. The depositing process includes the steps of depositing the transition layer, depositing the super hard film TiAlN/TiAlYN/TiAlN/CrN in nanometer superlattice structure, and depositing the surface self-lubricating film. The super hard film in nanometer superlattice structure has high microscopic hardness and high antioxidant performance, greatly higher that of conventional cutter coating. The complete high quality coating forming process combines the adhering transition layer, main antiwear layer and surface self-lubricating layer perfectly and makes the high grade cutter possess long service life.
Description
Technical field
The present invention relates to a kind of superhard composite film cutting tool and deposition method thereof in the new material technology field, specifically, relate to the setting and the target composition of target.
Background technology
One deck hard films is plated with the method for vacuum ion plating in surface at metal cutting tool, in the work-ing life that can significantly improve cutter, has become high-grade cutter and has made indispensable operation.Along with the develop rapidly of modern manufacturing industry, cutter coat has been proposed more and more higher requirement, normally used titanium nitride (TiN), titanium carbide (TiC) and TiAlN (TiAlN) etc. can not be satisfied the demand.
At present, continue to bring out new superhard film in the world and be applied to the metal cutting tool coating.The method that employing magnetron sputterings such as the P.Eh.Hovsepian of Britain and cathodic arc ion plating combine, depositing nano superstructure TiAlN/TiAlYN/ and TiAlN/CrN superhard film, [J] .P.Eh.Hovsepian, D.B.Lewis, W.D.munz, Surf.coat.Technol.133-134 (2000) 166-175; P.Eh.Hovsepian, W.D.munz, Vacuum69-(2003) 27-36).The highest microhardness of this film is up to 55-60GPa, and oxidation resistance temperature is above 900 ℃.
Realize industrialization for this high-quality superhard film being applied to cutting tool, also need to improve the film system design of cutter coat, could guarantee of the technical requirements of modern processing industry cutter coat.Above-mentioned technology distance production practicality also has sizable gap.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect that prior art exists, a kind of nano super-lattice structured superhard composite film cutting tool and deposition method thereof of suitable suitability for industrialized production is provided.Require composite membrane except having higher microhardness and scale resistance, also should have the surface self-lubricating performance of firm sticking power and low-friction coefficient, production low cost and high efficiency; This requirement is that industrial production type equipment is indispensable.
The object of the present invention is achieved like this:
1, the film of composite membrane system design
The superhard composite 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.Obviously, any single-material all can not satisfy above-mentioned technical requirements comprehensively.The deposition superhard composite film should develop towards the direction of diversification, multilayer film.
As shown in Figure 1, the first layer on cutter 8 has been the transition layer A of adhesive attraction, the second layer is main wearing layer---nano super-lattice structured superhard film (TiAlN/TiAlYN/TiAlN/CrN, be called for short superhard film) B, the 3rd layer is the self-lubricating film C of low-friction coefficient, and all rete is once finished on a coating equipment;
Described transition layer A is titanium nitride (TiN) or titanium carbide (TiC) composite membrane of mixing yttrium;
Described superhard film B is n layer TiAlN (TiAlN) B1, mix TiAlN (TiAlYN) B2, the TiAlN TiAlN B1 of yttrium (Y), chromium nitride (CrN) B3; 1000≤n≤9000.
Described self-lubricating layer C is a kind of diamond-film-like (DLC-Cr) of mixing chromium (Cr).
2, the setting of working target
The present invention deposits the superhard composite film of superstructure on many target position vaccum ion coater, this coating equipment is made up of vacuum chamber 4, fire door 5, work rest 6, bleeding point 7, power supply and Controlling System etc.
As shown in Figure 2, target 1, external target 2 hit 3 in the present invention was provided with in vacuum chamber 4 altogether;
Specifically, outer wall place in vacuum chamber 4, counter-clockwise direction is disposed with an interior target 1.1, interior two targets 1.2, interior three targets 1.3, interior four targets 1.4, and 90 degree are symmetrical distribution each other;
A target 3.1 during counter-clockwise direction is disposed with on the circle of center φ 45cm in vacuum chamber 4, in two targets 3.2, in three targets 3.3, in four targets 3.4, respectively with an interior target 1.1, interior two targets 1.2, interior three targets 1.3, interior four targets 1.4, relatively; 3 is relative with interior target 1 owing to hit, and constitutes target magnetic field is coupled, and promptly the outer ring magnet polarity of target is opposite.Consequently place workpiece 8 on the work rest 6 to be immersed in to hit 3 with interior target 1 coupled magnetic field, improved the density of plasma body, thereby can improve the sedimentation rate of film and the density of film.
On the outer wall of vacuum chamber 4, an outer target 2.1 is arranged in the middle of an interior target 1.1 and interior two targets 1.2; Outer two targets 2.2 are arranged in the middle of interior three targets 1.3 and interior four targets 1.4.
The target of an interior target 1.1 is pure chromium, and the target of interior two targets 1.2 is titanium aluminium (TiAl) alloy, and the target of interior three targets 1.3 is titanium aluminium (TiAlY) alloy of mixing yttrium, and the target of interior four targets 1.4 is titanium aluminium (TiAl) alloy;
The target of external target 2 is titanium yttrium (TiY) alloy;
3 the target of hitting is a high purity graphite.
3, the step of deposition composite membrane
(1) deposition transition layer A
According to the material classification of workpiece, select the material of desire plating transition layer, for example, rapid steel metalloid cutting tool adopts titanium nitride (TiN) as transition layer usually; And Wimet class cutter should adopt titanium carbide (TiC) as transition layer.Can improve the matching of sticking power and deposited film and body material like this.No matter depositing titanium nitride (TiN) still is a titanium carbide (TiC) in the present invention, and all adopting titanium alloy is target.In the titanium target, add the rare earth element yttrium (Y) of 7at.%, can make the titanium nitride (TiN) or titanium carbide (TiC) grain refining of generation, thereby improve titanium and the wetting property of body material and the sticking power of deposited film and matrix.
Utilize the external target 2 of two cover rectangle planes to finish, the target of external target 2 is titanium yttrium (TiY) alloy;
Argon nitrogen (Ar-N
2) gas mixture is working gas, deposition is mixed the titanium nitride (TiN) or titanium carbide (TiC) transition layer of yttrium, controls its thickness 0.3-0.5 μ m.
(2) deposition superhard film B
Utilize target 1 deposition superhard film B in the quadruplet; The target of two targets 1.2, interior four targets 1.4 is titanium aluminium (TiAl) alloy wherein, and its chemical constitution is 35Ti-65Al at.%; The target of three targets 1.3 is for mixing titanium aluminium (TiAlY) alloy of yttrium (Y) wherein, and its chemical constitution is 48Ti-48Al-4Y at.%; A target 1.1 adopts pure chromium target wherein.During the deposition superhard film, target 1 starts argon nitrogen (Ar-N simultaneously in the quadruplet
2) gas mixture is working gas.When workpiece 8 when the vacuum chamber inward turning circles, on workpiece 8, plated four tunics successively, they are TiAlN/TiAlYN/TiAlN/CrN successively.Difference different because of its chemical ingredients and lattice parameter has formed tangible interface.Regulate and control the speed of rotation of workpiece 8, just can modulate the thickness of each layer deposited film in certain limit.Along with the continuous rotary plating of workpiece, periodicity is repeated to deposit above-mentioned rete.If the plated film time is 2-3 hour, deposited film is with superimposed several thousand layers of above-mentioned film, the film of this structure is exactly superstructure superhard film B, it the super model amount that is referred to as and exceptional hardness effect on the physics will occur, and superhard film B will obtain to form its conventional microhardness 2-5 of rete ultrahigh hardness doubly.The thickness that superhard film B must control its modulation period is the nanoscale magnitude, is 3-8nm if control each deposition cycle film thickness of this film, and maximum value will appear in the hardness of superhard film B.The total thickness of control superhard film B is 3-5 μ m.The microhardness of the sedimentary this superhard film B of the present invention reaches as high as 58GPa generally greater than 40GPa, and the resistance to oxidation temperature is higher than 950 ℃.
(3) deposition self-lubricating film C
Deposit the self-lubricating film of one deck low-friction coefficient on the surface of superhard film again, can reduce the cutting force of metal cutting tool, reduce the abrasion in the mould use, for being significant the work-ing life of improving cutter and mould.
Utilization of the present invention hit 3 and an interior target 1.1 finish.
Self-lubricating film is a kind of diamond-film-like (DLC-Cr) of mixing chromium (Cr).3 the target of hitting is a high purity graphite, and the target of an interior target 1.1 is a pure metal chromium.During operation, above-mentioned target starts simultaneously, and argon (Ar) is a working gas.The working current of regulation and control graphite target and chromium target, making the ratio that contains chromium (Cr) in the diamond-film-like (DLC-Cr) of mixing chromium (Cr) is 4-8at.%.The self-lubricating film of this moment has minimum frictional coefficient and wear rate, and they are respectively: μ=0.05-0.09, Kc=1.0 * 10
-17m
3/ mN; The microhardness of diamond-film-like (DLC-Cr) is in the 20-25GPa scope.
The present invention has the following advantages and positively effect:
1. the nano super-lattice structured superhard film B that deposits by the present invention has higher microhardness and scale resistance, has substantially exceeded the performance of conventional cutter coat.
2. the present invention is the complete cutter high-quality coating coating technique of a cover, excessive layer A, main wearing layer B and surface self-lubricating layer C that it will play adhesive attraction very ideally combine, make this cutter high-quality coating 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.
3. actual film coating method is produced in suitable industrialization provided by the invention, 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;
The nano super-lattice structured superhard film of B-(TiAlN/TiAlYN/TiAlN/CrN) is called for short superhard film, comprising:
B1-TiAlN (TiAlN);
B2-mixes yttrium TiAlN (TiAlYN);
B3-chromium nitride (CrN);
The C-self-lubricating film.
Dress magnetron sputtering target in the 1-, target in being called for short comprises:
1.1-dress magnetron sputtering target in first, a target in being called for short, target is pure chromium;
1.2-dress magnetron sputtering target in second, two targets in being called for short, target is the TiAl alloy;
1.3-dress magnetron sputtering target in the 3rd, three targets in being called for short, target is the TiAlY alloy;
1.4-dress magnetron sputtering target in the 4th, four targets in being called for short, target is the TiAl alloy.
The 2-electric arc target is called for short external target, comprises
2.1-first electric arc target is called for short an outer target, target is the TiY alloy;
2.2-second electric arc target is called for short outer two targets, target is the TiY alloy.
3-center magnetron sputtering target, abbreviation hits, and comprises
3.1-the first center magnetron sputtering target, a target in the abbreviation, target are high purity graphite;
3.2-the second center magnetron sputtering target, two targets in the abbreviation, target are high purity graphite;
3.3-the 3rd center magnetron sputtering target, three targets in the abbreviation, target are high purity graphite;
3.4-the 4th center magnetron sputtering target, four targets in the abbreviation, target are high purity graphite.
The 4-vacuum chamber.
The 5-fire door.
The 6-work rest.
The 7-bleeding point.
The 8-workpiece.
Embodiment
1, the depositing operation of superhard composite film
1. workpiece shove charge
Workpiece 8 matting are clean, after dewatered drying is handled, install on the work rest 6, all operation will keep the cleanliness factor of workpiece 8 and work rest 6.
2. vacuumize and the workpiece baking
After workpiece 8 is laid and finished, close the fire door 5 of vacuum chamber 4, by the use rules of vacuum unit, to vacuum chamber 4 pumping high vacuums to 3 * 10
-3Pa opens the baking heating power supply then, workpiece rotational frequency 4-6 circle/minute, storing temperature is controlled at 350-400 ℃ all the time, enters next-step operation after storing temperature is up to standard.
3. glow ion cleans
Feed argon (Ar) gas, control air pressure is 2Pa, the unbalanced pulse grid bias power supply, voltage is slowly increased to 1200V, and dutycycle is 80%, and workpiece rotational frequency is the same, this moment, workpiece was in the glow ion cleaning, further removed the pollutant of workpiece surface, scavenging period 20 minutes.
4. high energy titanium ion bombardment
Reducing argon (Ar) airshed makes air pressure reduce to 3 * 10
-2Pa, workpiece 8 rotating speeds and grid bias power supply keep the previous step working parameter.Open external target 2, the arc current 150-160A of control target.Ion (the Ti+ of the titanium of arc evaporation and yttrium, Y+), with very high energy bombardment workpiece surface, remove foreign gas and other pollutent of workpiece surface chemisorption, and make part Ti+ and Y+ ion mix the following 3-5nm of workpiece substrate upper layer, to improve the sticking power of deposited film.
5. depositing Ti YN transition layer A
Grid bias power supply is transferred to 200-250V, and dutycycle 40-50% feeds Ar-N
2Gas mixture, Ar: N
2=1: 8, regulation and control air pressure is 0.5Pa, workpiece 8 rotating speed 4-6 circle/minute, the working parameter of external target 2 keeps previous step technology, depositing Ti YN filtering layer, depositing time 30 minutes.
6. deposit superhard film B
Change N
2-Ar gas mixture ratio of mixture is Ar: N
2=3: 1, operating air pressure, workpiece rotational frequency and grid bias power supply working parameter are constant.Open the interior target 1 of quadruplet of vacuum chamber 4 perisporiums, except that the sputtering power of an interior target 1.1 is controlled to be the 10KW, the sputtering power of two targets 1.2, interior three targets 1.3, interior four targets 1.4 is controlled at about 18KW in all the other, deposition superhard film (TiAlN/TiAlYN/TiAlN/CrN) B reduces electric arc target 2 electric currents gradually until shutoff simultaneously.According to the actual requirement of different workpieces 8, depositing time is controlled to be 2-4 hour, thickness 3-5 μ m.
7. deposition surface self-lubricating film C
Reduce nitrogen flow gradually until shutoff, adjusting argon flow amount makes gas pressure in vacuum remain 0.5Pa, workpiece 8 rotating speeds and grid bias power supply working parameter are constant, unlatching hits 3, the regulation and control sputtering power is 15KW, the working current of a target 1.1 is 5-8A in adjusting, and the time of deposition DLC-Cr self-lubricating film is 1-2 hour, and the control thickness is 1-2 μ m.
8. blowing out
A target 1.1 in reducing, 3 the working current of hitting turn-off grid bias power supply until shutoff, turn-off the baking power supply, and Workpiece Rotating is closed high vacuum valve after continuing to keep 30 minutes, according to the regulation of working specification, stops the vacuum unit, last closing device power supply and water coolant.
2, experimental result
(1) on a vacuum plating unit, two cover magnetron sputtering targets are housed, adopt the 93Ti-7Y alloy target material, deposit the TiN film of mixing yttrium, test its microhardness Hv=21-23GPa, the sticking power of rete adopts scratch method for test, its critical load Lc＞70N.
(2) on a Hauzer HTC100-4 ABS type equipment, two cover cathode arc targets and two cover magnetron sputtering targets are set, the target of two cover electric arc target is TiAl alloy (35Ti-65Al at.%), it is 99.8% chromium target that the targets of two cover magnetron sputtering targets are respectively TiAlY alloy (48Ti-48Al-4Y at.%) and purity, the superlattice composite membrane that deposits is TiAlCrN/TiAlYN, test the microhardness Hv=36GPa of its print, wear rate Kc=2.5 * 10
-16m
3/ mN, deposit the DLC-Cr self-lubricating film in the above after, wear rate drops to Kc=1.0 * 10
-16m
3/ mN, resistance to oxidation temperature＞950 ℃.
(3) in the vacuum plating of a Teer UDP450 type, configuration quadruplet magnetically controlled DC sputtering target, the target of one cover target is the chromium target, its excess-three cover target dress high purity graphite target, deposition is mixed chromium diamond-film-like DLC-Cr, its microhardness Hv=20-40GPa, coefficientoffriction=0.06-0.18, wear rate Kc=1.0 * 10
-17-2.0 * 10
-16m
3/ mN.
(4) on a homemade CK-1250 type coating equipment, three cover unbalanced magnetic field magnetron sputtering targets are set, the target of one cover target is blunt chromium, all the other two suit TiAl alloy target materials (alloying constituent 50Ti-50Al at%), deposit superlattice composite membrane TiAlN/CrN, thickness 3-4 μ m, surperficial avy blue, smooth, its microhardness 48-55GPa.
Experimental result shows that superhard composite film of the present invention has fabulous performance.
Claims (4)
1, a kind of nano super-lattice structured superhard composite film cutting tool comprises cutter (8), it is characterized in that:
Composite membrane on cutter (8) has been followed successively by the transition layer (A) of adhesive attraction, the nano super-lattice structured superhard film (B) of main wearing layer, the self-lubricating layer of low frictional factor (C);
Described transition layer (A) is for mixing the titanium nitride TiN or the titanium carbide TiC composite membrane of yttrium;
Described superhard film (B) is the n layer, every layer of the TiAlN TiAlYN (B2) that is followed successively by TiAlN TiAlN (B1), mixes yttrium, TiAlN TiAlN (B1), chromium nitride CrN (B3); 1000≤n≤9000;
Described self-lubricating layer (C) is a kind of diamond-film-like DLC-Cr that mixes chromium Cr.
2, a kind of nano super-lattice structured superhard composite film cutting tool deposition method comprises many target position vaccum ion coater and deposition method, it is characterized in that:
(1) setting of working target
In vacuum chamber (4), be provided with interior target (1) altogether, hit (3), external target (2);
Outer wall place in vacuum chamber (4), counter-clockwise direction is disposed with an interior target (1.1), interior two targets (1.2), interior three targets (1.3), interior four targets (1.4);
A target (3.1) during counter-clockwise direction is disposed with on the circle of center in vacuum chamber (4), in two targets (3.2), in three targets (3.3), in four targets (3.4), respectively with an interior target (1.1), interior two targets (1.2), interior three targets (1.3), interior four targets (1.4), relatively;
On the outer wall of vacuum chamber (4), an outer target (2.1) is arranged in the middle of an interior target (1.1) and interior two targets (1.2); Outer two targets (2.2) are arranged in the middle of interior three targets (1.3) and interior four targets (1.4);
The target of an interior target (1.1) is pure chromium, and the target of interior two targets (1.2) is a titanium aluminium TiAl alloy, and the target of interior three targets (1.3) is a titanium aluminium TiAlY alloy of mixing yttrium, and the target of interior four targets (1.4) is a titanium aluminium TiAl alloy;
The target of external target (2) is a titanium yttrium TiY alloy;
The target of (3) of hitting is a high purity graphite.
(2) step of deposition composite membrane
1. deposit transition layer (A)
Utilize external target (2) to finish, the target of external target (2) is a titanium yttrium TiY alloy;
Argon nitrogen Ar-N
2Gas mixture is a working gas, and deposition is mixed the titanium nitride TiN or the titanium carbide TiC transition layer of yttrium, controls its thickness 0.3-0.5 μ m;
2. deposit superhard film (B)
Utilize target (1) deposition superhard film (B) in the quadruplet; The target of two targets (1.2), interior four targets (1.4) is a titanium aluminium TiAl alloy wherein, and its chemical constitution is 35Ti-65Al at.%; The target of three targets (1.3) is a titanium aluminium TiAlY alloy of mixing yttrium Y wherein, and its chemical constitution is 48Ti-48Al-4Y at.%; A target (1.1) adopts pure chromium target wherein.During the deposition superhard film, target (1) starts argon nitrogen Ar-N simultaneously in the quadruplet
2Gas mixture is a working gas;
Each deposition cycle film thickness is 3-8nm, and the total thickness of control superhard film (B) is 3-5 μ m;
3. deposit self-lubricating film (C)
Utilization hits (3) and an interior target (1.1) is finished;
3 the target of hitting is a high purity graphite, and the target of an interior target 1.1 is a pure metal chromium.
3, by the deposition method of the described a kind of nano super-lattice structured cutter superhard film coating of claim 2, it is characterized in that: an interior target (1.1), interior two targets (1.2), interior three targets (1.3), interior four targets (1.4), 90 degree are symmetrical distribution each other.
4, by the deposition method of the described a kind of nano super-lattice structured cutter superhard film coating of claim 2, it is characterized in that: a target (3.1) during counter-clockwise direction is disposed with on the circle of center φ 45cm in vacuum chamber (4), in two targets (3.2), in three targets (3.3), in four targets (3.4).
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| CN104271792B (en) * | 2012-05-02 | 2016-06-01 | 韩国冶金株式会社 | Cutting tool hard coat |
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| CN103938157B (en) * | 2014-05-12 | 2016-05-25 | 重庆科技学院 | A kind of ZrNbAlN superlattice coating and preparation method |
| CN105538348A (en) * | 2016-02-25 | 2016-05-04 | 武汉苏泊尔炊具有限公司 | Cutter and manufacturing method thereof |
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| CN108330453A (en) * | 2018-01-31 | 2018-07-27 | 广东工业大学 | A kind of AlTiN/AlTiYN nanometer multilayers cutter coat and preparation method thereof |
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| CN112359321A (en) * | 2020-10-27 | 2021-02-12 | 蚌埠市利锋五金制品有限公司 | Kitchen cutter and forming method of hard film of cutter |
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