CN100487158C - Hall Ion Source excitation magnetron sputtering enhancement magnetism filtration multi-arc ion composite coating method - Google Patents
Hall Ion Source excitation magnetron sputtering enhancement magnetism filtration multi-arc ion composite coating method Download PDFInfo
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- CN100487158C CN100487158C CNB200610042978XA CN200610042978A CN100487158C CN 100487158 C CN100487158 C CN 100487158C CN B200610042978X A CNB200610042978X A CN B200610042978XA CN 200610042978 A CN200610042978 A CN 200610042978A CN 100487158 C CN100487158 C CN 100487158C
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Abstract
The invention discloses a making method of magnetic control sputtering reinforced typed magnetic filter multihead ion composite coater excited by Hall source, which comprises the following steps: extracting into vacuum; heating; exciting ion; plating; improving the connecting strength; obtaining the entire and compact film system for industrial need.
Description
Technical field
The present invention relates to a kind of method and apparatus at tool and mould surface deposition hard thin film material, is that a kind of Hall ion source actuated magnetron sputtering enhancing type magnetic filters multi sphere ion composite film coating method specifically.
Background technology
Compare with PCVD (plasma auxiliary chemical vapor phase deposition method) with CVD (chemical meteorology deposition method), PVD (physics vapor phase deposition method) has advantages such as depositing temperature low (100-500 ℃), processing cycle short (4-8h), film appearance quality are good, the speedy steel cutting-tool surface film prepare aspect the acquisition widespread use.PVD comprises magnetron sputtering and ion plating, and Mattox had at first proposed ion plating technique in 1963, and has obtained patent in 1967, and thereafter, various ion platings and sputter coating technology occur in succession.What at first the PVD technology is applied on the high speed steel substrate preparation hard coating is Japanese vacuum technique company (U.L.VAC), they adopted in 1978 cathode ion plating (HCD) at the hobber coating surface TiN, the life-span is improved three times.Thereafter, European and American countries has also obtained success in succession, comes into the market in succession as the magnetron sputtering of German Legbold-Heraeus company, the heated filament cathode ion plating of Switzerland Balzers company, the multi-arc ion coating of U.S. Mualti-Arc company etc.In recent years, for further improving ionization level, increase the bonding force of film and matrix, Britain Teer company adopts the non-balance magnetically controlled sputter technology, has obtained unusual effect.
But still there are some technical problems in the PVD method of present various simple functions, and is low as magnetron sputtering deposition speed and film substrate bond strength; The drop that the multi-arc ion coating deposition process forms makes that film is loose, quality reduces.Therefore, to the various tool and mould surface treatments under the harsh Service Environment, suddenly wait to seek more efficiently composite strengthening method.
Summary of the invention
The technical problem to be solved in the present invention is at the defective of prior art or deficiency, proposes a kind of Hall ion source actuated magnetron sputtering enhancing type magnetic that obtains the complete high quality plated film of density and filters multi sphere ion composite film coating method.
The technical solution that realizes above-mentioned task is:
---obtain vacuum environment: pending workpiece is inserted Hall ion source actuated magnetron sputtering enhancing type magnetic filter in the body of heater reaction chamber of multi sphere ion composite coating equipment, to being evacuated to 1.0 * 10 in the reaction chamber
-2Pa-5.0 * 10
-'Pa, temperature remains on 50-100 ℃;
_ _ ion activation cleans: feeding flow to reaction chamber is the argon gas of 50-100ml/min, and the unbalanced pulse bias voltage also keeps bias voltage to increase gradually and is stabilized in 900-1000V, and the control dutycycle is 30-90%;
---transition rete preplating: open the magnetic controlling target deposition pure Ti of 5-30min and impose bias voltage 500-1000V;
---the plating of work rete: open multiple arc target, the control nitrogen amount is 100-500ml/min, dutycycle 30-90%, and bias voltage is from 100-900V, and arc current 50-100A, depositing time are 0.5-2h.
Further technical solution of the present invention is:
Vacuumize and heating steps in Heating temperature remain on 300 ℃.
Argon flow amount is 120ml/min in the argon ion bombardment step, and dutycycle is 70%.
Arc current is 75A in the plated film step, and depositing time is 1.5h.
Method of the present invention significantly improves the ionization level of reaction process by Hall source forcing technology, realize the adjustable mechanical filter of bias voltage by the magnetic filtering system, break through the drop technical barrier that forms in traditional multi-arc ion deposition thin-film process and solve time this difficult problem and the sedimentation rate that causes is crossed industrial production difficult problems such as low, by the control of arc stream size, the appropriate design of target and high rigidity, high tenacity, high compactness and the good binding intensity of the compound realization rete of multiple technology.The magnetron sputtering technique that phase introduces before and after thin film deposition can be the acquisition high-quality thin film supplemental support is provided, and particularly can satisfy some special tool and mould surface-treated industrialization needs under the harsh Service Environment.This inventive method has high-level efficiency, the significant technical superiority of strengthening effect.This compounding technology does not appear in the newspapers in existing film coating method.
Description of drawings
Accompanying drawing 1 is that the Hall source forcing magnetron sputtering that adopts of the present invention strengthens the three-dimensional arrangement that magnetic filters multi sphere ion composite coating equipment and always schemes.
Wherein label is represented respectively: 1, body of heater reaction chamber; 2, vacuum system; 3, airing system; 4, power-supply system; 5, workpiece transmission system; 6, heating system;
Accompanying drawing 2 is top cross-sectional view of present device.
Wherein label is represented respectively: 7, viewing window; 8, sputtering target; 9, multiple arc target; 10, workpiece plate; 11, hall ion source; 12, workpiece; 13, magnetic filtering system.
Embodiment
Fig. 1 is that the Hall source forcing magnetron sputtering that adopts of the present invention strengthens the three-dimensional arrangement that magnetic filters multi sphere ion composite coating equipment and always schemes.This equipment is the vertical structure of a button fly front, mainly is made up of body of heater vacuum system 2, airing system 3, power-supply system 4, heating system 6.Vacuum system 2 is connected by the rear end of pipeline with body of heater reaction chamber 1, and it is vacuumized.The highest attainable vacuum of this equipment is 5 * 10
-4Pa, system's step-up ratio are equipped with the pumping speed setter that pumping speed is regulated less than 0.5Pa/h.
Accompanying drawing 2 is top cross-sectional view of present device.Be evenly equipped with eight cover multiple arc targets 9 on the body of heater, target surface front-end configuration magnetic filtering system 13, target adopts the interior water-cooling structure of φ 80 circle targets (alloys target or metallic target), and links to each other with direct supply 4-1, relies on the starting the arc of electronics arc initiation device, target stream variable range 40-100A.The Qianmen inwall is equipped with two rectangle magnetron sputtering targets 8, and links to each other with the midfrequent AC power supply 4-2 of a cover 40KW.For the ionization level of raising reactant gases and the bonding strength of deposit film, improve film quality, this device is gone up and is equipped with the circular hall ion source 11 of three covers.By body of heater define for reaction chamber 1, body of heater is anode and ground connection, and equally distributed heater air flow pressure switch rod 6 is arranged in the body of heater, is pending workpiece 12 heating.Workpiece 12 is placed on the workpiece plate 10 by can revolving round the sun of driving of transmission system 5 and rotation, workpiece plate links to each other with the power supply 4-3 of bias system, between negative and positive the two poles of the earth by 40kW, bias voltage unipolar pulse bias voltage greater than 1200V, excite glow discharge, set up plasma field, and the discharge physics parameter is regulated and controlled.Can monitor the reaction in furnace situation by viewing window 7.
Airing system 3 is made up of three road mass flowmeters, mixed gas tank and high vacuum stopping valve.Respectively control, N
2, Ar, CH
4Flow, all flow valvees are by solenoid control in the system.Before gas entered reaction chamber 1, it is even that all gas is introduced into mixed gas tank thorough mixing.Working gas is entered in the reaction chamber 1 by special-purpose ventpipe, ventpipe is arranged in the center of reaction chamber according to the big I of reaction chamber and workpiece, also can be arranged in the periphery place of reaction chamber, or the two haves both at the same time, and be communicated with gas supply system 3, carry out the weight feed of gas.
Utilize above-mentioned Hall source forcing magnetron sputtering to strengthen magnetic filtration multi sphere ion composite coating equipment and can prepare TiN, TiC, (Ti, Si) N, (Ti, Si) C, (Ti, Si) CN, Ti (CN), (Ti, Al) hard thin film material such as N, its sedimentation rate per hour 2.0 μ m to 4.0 μ m, the densification of film microtexture, crystal grain are tiny, the surface is even, tool metalluster, and film-substrate cohesion is strong, and has good erosion resistance.
Be example mainly below, further set forth principle of work of the present invention with preparation TiN ganoine thin film.Here need to prove; this embodiment is the specific embodiment that the contriver provides; but be not limited to these examples; those skilled in the art are according to the principle of this embodiment; need not to spend creative work; be easy to realize to be used to prepare other the hard thin film material beyond this specification sheets, also ought belong to protection scope of the present invention.
Embodiment 1: preparation TiN ganoine thin film
1, pending workpiece 12 is inserted Hall ion source actuated magnetron sputtering enhancing type magnetic and filter in the body of heater reaction chamber 1 of multi-arc ion coating film device, open vacuum system 2 and be evacuated to 6.0 * 10
-3Pa opens heating system 6, is heated to 250 ℃ and keep stable always and finish to plated film
2, behind the heat tracing 30min, open the Ar in the gas supply system 3, keeping the Ar flow is 100ml/min, and bias voltage increases gradually and is stabilized in 900V, dutycycle 50%.High-energy ion bombardment workpiece surface in the plasma field that produces by the 4-3 of grid bias power supply system in the equipment 30 minutes makes pending workpiece surface 12 obtain cleaning and activation treatment;
3, open the system of carefully taking out pressure regulation to 6.0 * 10 in the vacuum system 2 after argon ion bombardment finishes again
-3Pa; After pressure regulation finishes, regulate and be biased into 900V, dutycycle 50% is opened arc power 4-1 and is regulated arc current to 75A, and the maintenance carefully system of taking out is working order and opens magnetic filtering system 13, opens the pure titanium of magnetic controlling target 8 platings then 15 minutes;
4, close magnetic controlling target, open multiple arc target, N
2Amount 300ml/min, dutycycle 80%, bias voltage 250V, arc stream 75A.In this process, be respectively the sparking voltage that multiple arc target 9 and sputtering target 8 provide 24V and 200V by multi sphere direct supply 4-1 and magnetron sputtering midfrequent AC power supply 4-2, filter the drop that multiple arc target produces by magnetic filtering system 13, the reactant gases ion of high ionization level is provided by Hall source 11, this moment, high-energy electron and gas molecule collision ionization produced glow discharge, formed to have chemically active Ti
+, N
-Ion and free radical, these ions and free radical react on workpiece 12 surfaces and are deposited as the TiN film.
5, behind the deposition certain hour, at first powered-down system 4 and heating system 6 are then closed gas supply system 3, stop vacuum system 2 work at last, finish coating film treatment, and to charging into an amount of N in the body of heater
2Protective atmosphere makes body of heater air pressure reach 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
Embodiment 2: preparation TiC ganoine thin film
1, pending workpiece 12 is inserted Hall ion source actuated magnetron sputtering enhancing type magnetic and filter in the body of heater reaction chamber 1 of multi-arc ion coating film device, open vacuum system 2 and be evacuated to 6.0 * 10
-3Pa opens heating system 6, is heated to 350 ℃ and keep stable always and finish to plated film;
2, behind the heat tracing 30min, open the Ar in the gas supply system 3, keeping the Ar flow is 80ml/min, and bias voltage increases gradually and is stabilized in 1200V, dutycycle 30%.High-energy ion bombardment workpiece surface in the plasma field that produces by the 4-3 of grid bias power supply system in the equipment 50 minutes makes pending workpiece surface 12 obtain cleaning and activation treatment;
3, open the system of carefully taking out pressure regulation to 6.0 * 10 in the vacuum system 2 after argon ion bombardment finishes again
-3Pa; After pressure regulation finishes, regulate and be biased into 800V, dutycycle 60% is opened arc power 4-1 and is regulated arc current to 70A, and the maintenance carefully system of taking out is working order and opens magnetic filtering system 13, opens the pure titanium of magnetic controlling target 8 platings then 15 minutes;
4, close magnetic controlling target, open multiple arc target, CH
4Amount 250ml/min, duty 70%, bias voltage 200V, arc stream 70A.In this process, be respectively the sparking voltage that multiple arc target 9 and sputtering target 8 provide 24V and 200V by multi sphere direct supply 4-1 and magnetron sputtering midfrequent AC power supply 4-2, filter the drop that multiple arc target produces by magnetic filtering system 13, the reactant gases ion of high ionization level is provided by Hall source 11, this moment, high-energy electron and gas molecule collision ionization produced glow discharge, formed to have chemically active Ti
+, C
-Ion and free radical, these ions and free radical react on workpiece 12 surfaces and are deposited as the TiN film.
5, behind the deposition certain hour, at first powered-down system 4 and heating system 6 are then closed gas supply system 3, stop vacuum system 2 work at last, finish coating film treatment, and to charging into an amount of N in the body of heater
2Protective atmosphere makes body of heater air pressure reach 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
Embodiment 3: preparation Ti (CN) ganoine thin film
1, pending workpiece 12 is inserted Hall ion source actuated magnetron sputtering enhancing type magnetic and filter in the body of heater reaction chamber 1 of multi-arc ion coating film device, open vacuum system 2 and be evacuated to 6.0 * 10
-3Pa opens heating system 6, is heated to 300 ℃ and keep stable always and finish to plated film
2, behind the heat tracing 30min, open the Ar in the gas supply system 3, keeping the Ar flow is 50ml/min, and bias voltage increases gradually and is stabilized in 1100V, dutycycle 35%.High-energy ion bombardment workpiece surface in the plasma field that produces by the 4-3 of grid bias power supply system in the equipment 40 minutes makes pending workpiece surface 12 obtain cleaning and activation treatment;
3, open the system of carefully taking out pressure regulation to 6.0 * 10 in the vacuum system 2 after argon ion bombardment finishes again
-3Pa; After pressure regulation finishes, regulate and be biased into 700V, dutycycle 70% is opened arc power 4-1 and is regulated arc current to 65A, and the maintenance carefully system of taking out is working order and opens magnetic filtering system 13, opens the pure titanium of magnetic controlling target 8 platings then 15 minutes;
4, close magnetic controlling target, open multiple arc target, N
2Amount 100ml/min, CH
4Amount 100ml/min, duty 75%, bias voltage 100V, arc stream 65A.In this process, be respectively the sparking voltage that multiple arc target 9 and sputtering target 8 provide 24V and 200V by multi sphere direct supply 4-1 and magnetron sputtering midfrequent AC power supply 4-2, filter the drop that multiple arc target produces by magnetic filtering system 13, the reactant gases ion of high ionization level is provided by Hall source 11, this moment, high-energy electron and gas molecule collision ionization produced glow discharge, formed to have chemically active Ti
+, N
-, C
-Ion and free radical, these ions and free radical react on workpiece 12 surfaces and are deposited as the TiN film.
5, behind the deposition certain hour, at first powered-down system 4 and heating system 6 are then closed gas supply system 3, stop vacuum system 2 work at last, finish coating film treatment, and to charging into an amount of N in the body of heater
2Protective atmosphere makes body of heater air pressure reach 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
Claims (2)
1, a kind of Hall ion source actuated magnetron sputtering enhancing type magnetic filters multi sphere ion composite film coating method, comprises vacuumizing in the reaction chamber and the workpiece surface plated film, it is characterized in that present method may further comprise the steps:
---obtain vacuum environment: pending workpiece is inserted Hall ion source actuated magnetron sputtering enhancing type magnetic filter in the body of heater reaction chamber of multi sphere ion composite coating equipment, to being evacuated to 1.0 * 10 in the reaction chamber
-2Pa-5.0 * 10
-4Pa, temperature remains on 50-100 ℃;
_ _ ion activation cleans: feeding flow to reaction chamber is the argon gas of 50-100ml/min, and the unbalanced pulse bias voltage also keeps bias voltage to increase gradually and is stabilized in 900-1000V, and the control dutycycle is 30-90%;
---transition rete preplating: open the magnetic controlling target deposition pure Ti of 5-30min and impose bias voltage 500-1000V;
---the plating of work rete: open multiple arc target, the control nitrogen amount is 100-500ml/min, dutycycle 30-90%, and bias voltage is 100-900V, arc current 50-100A, depositing time are 0.5-2h.
2, Hall ion source actuated magnetron sputtering enhancing type magnetic according to claim 1 filters multi sphere ion composite film coating method, it is characterized in that arc current is 75A in the work rete plating step, and depositing time is 1.5h.
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| US8021768B2 (en) * | 2009-04-07 | 2011-09-20 | National Material, L.P. | Plain copper foodware and metal articles with durable and tarnish free multiplayer ceramic coating and method of making |
| CN104947046B (en) * | 2015-07-28 | 2017-10-27 | 魏永强 | Multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method |
| CN104975263A (en) * | 2015-07-28 | 2015-10-14 | 魏永强 | Multi-stage magnetic field arc ion plating and radio-frequency magnetron sputtering composite deposition method |
| CN105734501A (en) * | 2016-05-06 | 2016-07-06 | 魏永强 | Method for multi-level magnetic field arc ion plating and twin-target medium-frequency magnetron sputtering composite deposition |
| CN105908135A (en) * | 2016-05-09 | 2016-08-31 | 魏永强 | Multistage magnetic field ion plating and twin-target high-power pulse magnetron sputtering composite method |
| CN105908147B (en) * | 2016-07-07 | 2017-07-21 | 重庆科技学院 | Non-balance magnetically controlled sputter electrode and system |
| CN109811316B (en) * | 2019-04-04 | 2021-05-28 | 中国核动力研究设计院 | Zirconium alloy coating with high burnup and long service life and preparation method thereof |
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| CN1664161A (en) * | 2005-03-21 | 2005-09-07 | 西安交通大学 | Hall ion source actuated magnetron sputtering enhancing type multi-arc ion plating film method |
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| CN1664161A (en) * | 2005-03-21 | 2005-09-07 | 西安交通大学 | Hall ion source actuated magnetron sputtering enhancing type multi-arc ion plating film method |
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