CN103981496B - A kind of apparatus and method preparing TiAlCrN multi-element coating - Google Patents
A kind of apparatus and method preparing TiAlCrN multi-element coating Download PDFInfo
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Abstract
Patent of the present invention relates to TiAlCrN multi-element coating, refer in particular to the device that a kind of containing field Nonequilibrium magnetic sputtering method prepares TiAlCrN multi-element coating and the method utilizing device to prepare coating, being unique in that of its device comprises four magnetrons, make the magnetic line of force can extend directly into another magnetron from a magnetron, form the magnetic well closed, electron escape be can effectively stop, thus sputtering yield and ionization level improved.
Description
Technical field
Patent of the present invention relates to TiAlCrN multi-element coating, refer in particular to a kind of containing field Nonequilibrium magnetic sputtering method and prepare the apparatus and method of TiAlCrN multi-element coating, the containing field Nonequilibrium magnetic sputtering method devising a kind of advanced person prepares the device of TiAlCrN multi-element coating, its coating is good with substrate combinating strength, when being applied to cut by force, on cutter and high extruding force mould, coating is difficult to peel off, it is also possible to make compound and laminated coating.
Background technology
Along with progress and the development of metal cutting of modern industry, especially high-speed cutting, hard machining and the appearance of dry cutting technique, metal cutting tool is proposed the highest requirement；Cutting tool surface-coating technology is the material surface modifying technology that recent decades answers that the market development of demand is got up；Superhard nitride coatings both can effectively extend the service life of cutting tool, can play again its superhard, tough, wear-resisting, advantage of self-lubricating, thus improve metal cutting tool durability and adaptability in the modern course of processing.
Adding Al element in TiN coating, the TiAlN coating of deposition can significantly improve its corrosion resistance and operating temperature range, and TiAlN coating is after middle addition Cr element, and coating shows more preferable high-temperature oxidation resistance and wearability；Therefore, carbide tool deposit compared with TiN, TiAlN coating that novel TiAlCrN coating is traditional with deposition, there is the feature of higher wearability, hardness, high temperature oxidation resistance and high thermal stability, it is particularly suitable for high-speed dry cutting, the present invention devises a kind of containing field Nonequilibrium magnetic sputtering method and prepares the device of TiAlCrN multi-element coating, is effectively improved TiAlCrN multi-element coating film and substrate combinating strength.
Summary of the invention
Patent of the present invention is to use containing field unbalanced magnetron sputter ion plating technique method to prepare TiAlCrN multi-element coating at cutter substrate surface, being unique in that of its device comprises four magnetrons, make the magnetic line of force can extend directly into another magnetron from a magnetron, form the magnetic well closed, can effectively stop electron escape, thus improving sputtering yield and ionization level, apparatus of the present invention are as it is shown in figure 1, be mainly made up of vacuum system, power-supply system, control system, cooling system four part.
Vacuum system includes: vacuum chamber, target, specimen holder, Nonequilibrium magnetic keyholed back plate, iodine-tungsten lamp heater, mechanical pump and diffusion pump, mechanical pump and diffusion pump are connected with vacuum chamber respectively；It is positioned at vacuum chamber central authorities for installing the specimen holder of sample；In coating deposition process, sample rotates with work rest, makes coating be evenly distributed；4 targets are installed: Ti target, Cr target, Al target, Cr target on vacuum chamber furnace wall；4 targets are symmetrical；Nonequilibrium magnetic keyholed back plate is installed so that Nonequilibrium magnetic keyholed back plate is the most symmetrical on each target；Iodine-tungsten lamp heater is built in bottom vacuum chamber.
First order vacuum uses mechanical pump slightly to take out, second level vacuum uses diffusion pump essence to take out, vacuum chamber built-in iodine-tungsten lamp heater, sample is arranged on the specimen holder of vacuum chamber central authorities, coating deposition process rotates with specimen holder, coating is made to be evenly distributed, 4 targets are installed: Ti target on vacuum chamber furnace wall, Cr target, Al target, Cr target, equipped with Nonequilibrium magnetic keyholed back plate on target, magnetron is symmetrical, this makes the magnetic line of force can extend directly into another magnetron from a magnetron, so as generation closed magnetic field, effectively stop electron escape, improve sputtering yield and ionization level.
Power-supply system is divided into two parts: a part provides 4 shielding power supplies of DC voltage respectively for 4 Nonequilibrium magnetic keyholed back plates, and shielding power supply is connected with target；Another part provides pulsed bias for sample, is connected with sample.
Control system includes: reacting gas N2Introducing vacuum chamber with protective gas Ar by flow control meter, regulation flow controls sputtering pressure, and the operation of whole system uses computer software to be controlled；
Cooling system: too high for preventing from sputtering the target temperature caused, target is hollow bore, is similar to water pipe structure, and such as Fig. 5, hollow bore, therefore can be with direct water-cooling as bosh.
Accompanying drawing explanation
Fig. 1 containing field Nonequilibrium magnetic sputtering method prepares the installation drawing of TiAlCrN multi-element coating.
1-iodine-tungsten lamp heater；2-magnetron；3-Ti target；4-shielding power supply；5-specimen holder；6-Cr target；7-vacuum chamber；8-Al target；9-grid bias power supply；10-Cr target；11-mechanical pump；12-diffusion pump；13-flow control meter；14-N2；15-Ar；16-cooling water pipe.
Fig. 2 TiAlCrN multi-element coating surface topography；(a) low power pattern；(b) high power pattern.
Fig. 3 TiAlCrN multi-element coating EDS analyzes.
Fig. 4 TiAlCrN multi-element coating bond strength.
Fig. 5 target material structure schematic diagram.
Detailed description of the invention
(1) strong magnet and soft iron composition unbalanced magnetic field are utilized, selecting purity is that Ti target, Al target and the Cr target of 99.99% are as sputtering target material, specification is 100 × 100mm, sample is through No. 80～No. 1200 sand paper and abrasive paper for metallograph polishing, granularity be 2.5 diamond polishing agent be polished to minute surface, successively put into acetone and alcoholic solution ultrasonic waves for cleaning 10min again, remove matrix surface impurity and oils and fats；Cr target and Cr target, Ti target and Al are each mounted opposite on vacuum chamber furnace wall, and sample is placed on specimen holder, and in coating deposition process, sample rotates with work rest, set work rest rotary speed as 20 r/ min, so that coating is uniform.
(2) utilizing two-stage vacuum system: prime uses mechanical pump slightly to take out, rear class uses diffusion pump essence to take out the final vacuum of system as being evacuated to 5 × 10-3Pa；Vacuum chamber built-in iodine-tungsten lamp device is used to heat, underlayer temperature controls at 200 DEG C, and purity 99.99%Ar gas introduces sputtering chamber by effusion meter simultaneously, and sputtering pressure can be controlled by regulation flow, keep sputtering pressure 0.5Pa, sample is carried out glow discharge 10min；The pulse power of each sputtering target selects the adjustable power supply of 25kHz, 0 ~ 3A, and sputtering target material applies the voltage (shielding power supply offer) of 50-500V, and in sputtering body of heater, rated voltage is 100V ~ 600V, and rated power provides for 50kW(pulsed bias).
(3) magnetron is symmetrical, and this makes the magnetic line of force can extend directly into another magnetron from a magnetron, in order to produce closed magnetic field, effectively stops electron escape, improves sputtering yield and ionization level.
(4) atom of target material surface out (is sputtered) the most exactly by Ar ion bom bardment.Atom is electric neutrality, can directly go out magnetic potential trap, not retrained by magnetic field, these atom bombardments and be deposited on surface of the work formed densification coating.
(5) target material surface sputters electronics, electronics is the subatomic particle in electronegativity, can be captured by magnetic potential trap, accelerated by convolution in magnetic potential trap, then bombard the Ar atom in this region, make ionization go out increasing Ar ion, sputter procedure starts, will produce increasing Ar ion, make glow discharge be controlled oneself, sputter procedure is constant.
(6) bombardment of a large amount of high energy particles can cause the temperature of target and magnetron to raise, and adds bosh, can obtain circulating cooling when making target cool down in target.
null(7) TiAlCrN coating morphology is prepared as shown in Figure 2 by containing field Nonequilibrium magnetic sputtering method device，Surface chemistry element mass fraction (mass，%): Ti 7.41、Al 18.57、Cr 20.54、N 34.32、C 9.74、O 7.09、Fe 0.15、Co 0.37、W 1.81，Atomic fraction (at，%): Ti 3.12、Al 13.87、Cr 7.96、N 49.39、C 16.35、O 8.94、Fe 0.05、Co 0.13、W 0.20，As shown in Figure 3，Wherein Ca、K、The elements such as Cl are impurity，Its content does not shows，C、O、Fe、Co、Elements such as w is tool matrix diffraction maximum.
(8) TiAlCrN coating has higher interface bond strength, and recording its bond strength by scarification is 87.6N, as shown in Figure 4.
Claims (5)
1. the device utilizing a kind of TiAlCrN of preparation multi-element coating prepare TiAlCrN multi-element coating method, it is characterised in that bag
Include following steps:
(1) utilizing strong magnet and soft iron composition unbalanced magnetic field, selecting purity is that Ti target, Al target and the Cr target of 99.99% are as spattering
Shooting at the target material, specification is 100 × 100mm, and sample is through No. 80～No. 1200 sand paper and abrasive paper for metallograph polishing, and granularity is 2.5
Diamond polishing agent is polished to minute surface, more successively puts into acetone and alcoholic solution ultrasonic waves for cleaning 10min, removes matrix surface miscellaneous
Matter and oils and fats；Cr target and Cr target, Ti target and Al are each mounted opposite on vacuum chamber furnace wall, and sample is placed on specimen holder,
In coating deposition process, sample rotates with work rest, sets work rest rotary speed as 20r/min, so that coating is uniform；
(2) utilizing two-stage vacuum system: prime uses mechanical pump slightly to take out, rear class uses diffusion pump essence to take out the final vacuum of system
For being evacuated to 5 × 10-3Pa；Using vacuum chamber built-in iodine-tungsten lamp device to heat, underlayer temperature controls at 200 DEG C, purity simultaneously
99.99%Ar gas introduces sputtering chamber by effusion meter, and sputtering pressure can be controlled by regulation flow, keeps sputtering pressure
0.5Pa, carries out glow discharge 10min to sample；The pulse power selection 25kHz of each sputtering target, 0～3A adjustable power supply,
Sputtering target material applies the voltage of 50-500V, and shielding power supply provides；In sputtering body of heater, rated voltage is 100V～600V, specified
Power is 50kW, and pulsed bias provides；
(3) magnetron is symmetrical, and this makes the magnetic line of force extend directly into another magnetron from a magnetron, in order to produce Guan Bi
Magnetic field, effectively stops electron escape, improves sputtering yield and ionization level；
(4) atom of target material surface is out formed sputtering by Ar ion bom bardment, and atom is electric neutrality, directly goes out magnetic potential trap, is not subject to
The constraint in magnetic field, these atom bombardments and be deposited on surface of the work formed densification coating；
(5) target material surface sputters electronics, and electronics is the subatomic particle in electronegativity, can be captured by magnetic potential trap, in magnetic potential trap
Being accelerated by convolution, then bombard the Ar atom in this region, make ionization go out increasing Ar ion, sputter procedure starts,
Will produce increasing Ar ion, make glow discharge be controlled oneself, sputter procedure is constant；
(6) bombardment of a large amount of high energy particles can cause the temperature of target and magnetron to raise, and adds bosh, make target in target
Circulating cooling is obtained during material cooling.
2. prepare as claimed in claim 1 TiAlCrN multi-element coating method, it is characterised in that: prepared by described one
The device of TiAlCrN multi-element coating, is mainly made up of vacuum system, power-supply system, control system, cooling system four part,
Vacuum system includes: vacuum chamber, target, specimen holder, Nonequilibrium magnetic keyholed back plate, iodine-tungsten lamp heater, mechanical pump and diffusion pump；
Mechanical pump and diffusion pump are connected with vacuum chamber respectively, are positioned at vacuum chamber central authorities for installing the specimen holder of sample, deposit at coating
In journey, sample rotates with work rest, makes coating be evenly distributed, and iodine-tungsten lamp heater is built in bottom vacuum chamber；Vacuum chamber furnace wall
On 4 targets are installed: Ti target, Cr target, Al target, Cr target；4 targets are symmetrical；It is provided with non-on each target
Unbalanced magnetron pipe is so that Nonequilibrium magnetic keyholed back plate is the most symmetrical；The magnetic line of force is made to extend directly into another magnetic from a magnetron
Keyholed back plate, in order to produce closed magnetic field, effectively stops electron escape, improves sputtering yield and ionization level.
3. prepare as claimed in claim 2 TiAlCrN multi-element coating method, it is characterised in that: power-supply system is divided into two
Point: a part provides 4 shielding power supplies of DC voltage respectively for 4 Nonequilibrium magnetic keyholed back plates, and shielding power supply is connected with target；
Another part provides pulsed bias for sample, is connected with sample.
4. prepare as claimed in claim 2 TiAlCrN multi-element coating method, it is characterised in that: control system includes reacting
Gas N2, protective gas Ar and flow control meter, reacting gas N2Introduced very by flow control meter with protective gas Ar
Empty room, regulation flow controls sputtering pressure, and the operation of whole system uses computer software to be controlled.
5. prepare as claimed in claim 2 TiAlCrN multi-element coating method, it is characterised in that: cooling system comprises target,
Too high for preventing from sputtering the target temperature caused, target is hollow bore, hollow bore as bosh, therefore direct water-cooling.
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| CN117778969B (en) * | 2023-12-28 | 2024-05-24 | 江苏富乐华功率半导体研究院有限公司 | Auxiliary processing device and method for ultrathin light-transmitting material thermal diffusivity test sample |
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Effective date of registration: 20200319 Address after: No. 99 Dacui Road, Lugou Town, Jianhu County, Yancheng City, Jiangsu Province Patentee after: YANCHENG CHONGDA PETROCHEMICAL MACHINERY Co.,Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Changzhou University Patentee before: CHANGZHOU UNIVERSITY |