CN100443628C - TiNx film preparing process on the surface of cutter for machining gear in automobile gear box - Google Patents
TiNx film preparing process on the surface of cutter for machining gear in automobile gear box Download PDFInfo
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- CN100443628C CN100443628C CNB2006100428128A CN200610042812A CN100443628C CN 100443628 C CN100443628 C CN 100443628C CN B2006100428128 A CNB2006100428128 A CN B2006100428128A CN 200610042812 A CN200610042812 A CN 200610042812A CN 100443628 C CN100443628 C CN 100443628C
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Abstract
The present invention discloses a process for preparing a TiNx film on the surface of a gear cutter for an automobile gearbox, which prepares the TiNx film on the surface of the gear cutter for an automobile gearbox by using hoare source forcing magnetron sputtering enhancement type magnetic filtration multiple-arc ion plating equipment. By detection, the TiNx film which is formed on the surface of the gear cutter for an automobile gearbox by using the process of the present invention has the film thickness of 2 microns, compact films, the fiber hardness of 30 to 40 GPa and good bonding force of film bases, and the TiNx film can greatly improve the service life of the gear cutter for an automobile gearbox. The present invention has the advantages of high efficiency, obvious strengthening effect and low cost.
Description
Technical field
The invention belongs to the hard thin film material Application Areas, further relate to the industrial PVD of a kind of employing (material surface physical vapor deposition) equipment, promptly Hall ion source actuated magnetron sputtering enhancing type magnetic filters the multi-arc ion coating film device prepares the TiNx rete at the automobile gearbox gear tool surface technology.
Background technology
Material surface physical gas phase deposition technology (PVD technology) has become one of important symbol of material revolution, world developed country industrial applications on the tool surface modification is handled.The PVD technology has advantages such as depositing temperature low (200-300 ℃), processing cycle short (4-8h), film appearance quality are good, the speedy steel cutting-tool surface film prepare aspect the acquisition widespread use.The PVD method 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.Thereafter, European and American countries has also obtained success, 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.At present, but the domestic tool surface surface ceramic deposition technology of suitability for industrialized production preferably that also is not applicable to, this makes that the internally coated cutter of state can't export on the one hand, and the cutter that uses on domestic on the other hand numerical control and the finish turning lathe is captured by import potteryization cutter substantially.
In the face of the cutter market of domestic tens billion of units, domestic cutter production and use producer have carried out exploitation widely one after another to cutter surface ceramic deposition technology.But the tool surface ceramic technology of present domestic industrial applications is mainly based on the TiN rete cheap, that technology content is lower, but the performance of general T iN rete can not satisfy more and more higher market demand.In the case, domestic manufacturer buys external filming equipment again one after another, the domestic market of seizing is also taken advantage of a favourable situation to enter one after another by external producer, but its coating cost high (the average plated film price of hobcutter being existed as Shanghai, Suzhou one), domestic most cutters use the producer can't industrial applications.It is generally acknowledged that factors such as Ti/N ratio reduces, grain-size reduces, crystalline is decrystallized, crystal prolongs the growth of solid matter direction can effectively improve the physicals of rete.Therefore, but developing has the TiNx Processes and apparatus of the big area industrial applications of significant advantage to become than general T iN to solve the major issue that China's cutter production improves the cutter quality, reduces cost, dominates the market, and the high-performance, the low-cost problem that solve the surface ceramic deposition rete of the higher automobile gearbox gear cutter of added value have more outstanding market position.
Summary of the invention
Defective or deficiency at above-mentioned prior art exists the objective of the invention is to, and propose a kind of technology for preparing the TiNx rete at the automobile gearbox gear tool surface.Adopt the TiNx rete of this prepared, have ultrahigh hardness, strong bonding force, anti-oxidant, corrosion resistant performance.
The technical solution that realizes above-mentioned task is as follows:
A kind of automobile gearbox gear tool surface prepares the technology of TiNx rete, this process using Hall ion source actuated magnetron sputtering enhancing type magnetic filters the multi-arc ion coating film device, prepare the TiNx rete at the automobile gearbox gear tool surface, it is characterized in that, comprise the following steps:
1) slightly takes out: will insert Hall ion source actuated magnetron sputtering enhancing type magnetic through the cutter of clean and filter in the body of heater reaction chamber of multi-arc ion coating film device, and open vacuum system body of heater is evacuated to 6.0 * 10
0Pa;
2) heating reaches and carefully takes out: slightly take out and finish back unlatching heating system, be heated to 100-500 ℃, opening carefully simultaneously, the system of taking out is evacuated to 5.0 * 10
-3Pa;
3) ion bombardment: carefully exhaust the Ar that opens after finishing in the gas supply system, keeping the Ar flow is 100-150ml/min, and bias voltage increases gradually and is stabilized in 900V, and dutycycle is 30-90%.High-energy ion bombardment tool surface in the plasma field that produces by the grid bias power supply system in equipment 20-50 minute makes pending tool surface obtain cleaning and activation treatment;
4) pressure regulation: opening carefully after argon ion bombardment finishes again, the system of taking out is evacuated to 5.0 * 10
-3Pa;
5) preplating: after pressure regulation finishes, open the magnetic controlling target deposition pure Ti of 5min and impose bias voltage 900V, dutycycle 50%～80% and bombard continuously, preplating finishes;
6) formal plating: after preplating finishes, close magnetic controlling target, open multiple arc target internal linear adjustment in 25 minutes: make nitrogen amount from 0ml/min to 400ml/min, dutycycle from 50% to 90%, bias voltage is reduced to 100V from 900V, arc stream 50-80A, and provide 24V voltage for the multi sphere target by the direct supply of equipment, provide 200V voltage by the midfrequent AC power supply for magnetic control spattering target, drop by the generation of magnetic filtration system filters arc target, the reactant gases ion of high ionization level is provided by the Hall source in the equipment, this moment, high-energy electron and gas molecule collision ionization produced glow discharge, formation has chemically active ion and free radical, and these ions and free radical react at tool surface and be deposited as film, depositing time 1h;
7) cooling: after the thin film deposition for the treatment of tool surface forms, closing device power-supply system, heating system and gas supply system successively, and stop vacuum system work, 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 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
The TiNx film that obtains at the automobile gearbox gear tool surface under the above-mentioned processing condition, after testing, 2 microns of film thicknesses, the rete densification, it shows dimension hardness Hv between 30-40GPa, and film-substrate cohesion is better.
Technology of the present invention is logical to realize that by Hall source forcing magnetron sputtering enhancing magnetic filtration multi-arc ion coating film device preparation and general T iN rete have the very automobile gearbox gear cutter TiNx rete of big-difference, very high hardness, high compactness, good film substrate bond strength.Therefore, this technology has high-level efficiency, strengthening effect technical superiority remarkable, with low cost.This technology is not appeared in the newspapers in existing film coating method.
Description of drawings
Fig. 1 is that the Hall source forcing magnetron sputtering that adopts of the present invention strengthens the three-dimensional arrangement that magnetic filters the multi-arc ion coating film device and always schemes;
Fig. 2 is the top cross-sectional view that the present invention adopts equipment;
Fig. 3 is the cross section pattern contrast photo of TiNx film and general T iN film, and wherein (a) is TiNx film of the present invention, (b) is general T iN film;
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and contriver provide.
Embodiment
Referring to accompanying drawing, Fig. 1 is that the Hall source forcing magnetron sputtering that adopts of the present invention strengthens the three-dimensional arrangement that magnetic filters the multi-arc ion coating film device 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 that the present invention adopts equipment.Be evenly equipped with eight cover multiple arc targets 9 on the body of heater, target adopts φ 80 circle targets (alloys target or metallic target), interior water-cooling structure, and link to each other with direct supply 4-1, relying on the starting the arc of electronics arc initiation device, target flows 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 two 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.Pending workpiece 12 is placed on the capstan head 10 by can revolving round the sun of driving of transmission system 5 and rotation, capstan head 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 detect the reaction in furnace situation by viewing window 7.
Adopt above-mentioned Hall ion source actuated magnetron sputtering enhancing type magnetic to filter the multi-arc ion coating film device and prepare the technology of TiNx rete at the automobile gearbox gear tool surface, at first the cutter that needs plated film is carried out pre-treatment, its processing step is:
1) oil removing: be to remove the tool surface greasy dirt, earlier cutter to be plated is put into cleaner for metal and boiled and boil 5-10 minute.
2) scavenging solution is ultrasonic: the cleaner for metal ultrasonic cleaning that will put into except that japanned cutter to be plated 5-10 minute.
3) pickling: the dilute hydrochloric acid solution of the cutter to be plated of the ultrasonic mistake of scavenging solution being put into proper concn soaked 2-5 minute.
4) pure water is ultrasonic: the cutter to be plated of pickling is put into distilled water ultrasonic 10 second～60 seconds.
5) dehydration: the cutter to be plated of the ultrasonic mistake of pure water is put into spirituous solution dewater.
6) oven dry: the cutter to be plated after will dewatering is dried.
To insert Hall ion source actuated magnetron sputtering enhancing type magnetic through the cutter to be plated 12 of above-mentioned clean and filter in the body of heater reaction chamber 1 of multi-arc ion coating film device, the slightly system of taking out that opens in the vacuum system 2 is evacuated to 6.0 * 10
0Pa opens heating system 6, is heated to 300 ℃ and also keeps stable to the plated film end always, and the carefully system of taking out that opens simultaneously in the vacuum system 2 is evacuated to 5.0 * 10
-3Pa; Carefully exhaust the Ar that opens after finishing in the gas supply system 3, keeping the Ar flow is 150ml/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 is further cleaned and activation treatment pending tool surface 12; The carefully system of taking out of opening again after argon ion bombardment finishes in the vacuum system 2 is evacuated to 5.0 * 10
-3Pa; After pressure regulation finishes, regulate and be biased into 900V, dutycycle 70% is opened midfrequent AC power supply 4-2 and is regulated power, and keeping carefully, the system of taking out is working order and opened the pure titanium of magnetic controlling target 8 platings 5 minutes; After preplating finished, linear adjustment in 25 minutes: nitrogen amount was from 0ml/min to 400ml/min, dutycycle from 50% to 90%, and bias voltage is from 900V to 100V, and arc stream keeps 50-80A.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 cutter 12 surfaces and are deposited as the TiNx film.Behind the deposition certain hour (1h), 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 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
Obtain the TiNx film at the automobile gearbox gear tool surface under the above-mentioned processing condition, detect through National Key Laboratory of Xi'an Communications University, detected result is as follows:
| Rete | Deposition attitude hardness (GPa) | Hardness (GPa) after 600 ℃ of annealing | Grain-size (nm) | Ti/N ratio | Crystal type |
| TiNx | 35～40 | 25～30 | About 13 | 0.75∶1 | Non-column crystal |
| TiN | 18～22 | 10～12 | About 16 | 0.88∶1 | Column crystal |
Laboratory through authorized by state is detected, and detection architecture is as follows:
| Rete | Microhardness (GPa) | Thicknesses of layers (μ m) | Rete cross section pattern | Bonding force |
| TiNx | 35～37 | 1.5-2 | Evenly, densification | Well |
Use producer's feedback opinion as follows:
| Cutter uses producer | The cutter model | Tool type | The cutter and the former rete place of production | Result of use behind the recoat TiNx rete behind the sharpening |
| Xi'an Fa Shite | SX22-2036 | Pinion cutter | Abroad | Be equal to the new cutter of import coating |
| Xi'an Fa Shite | SX21-2132 | Hobcutter | Abroad | Be equal to the new cutter of import coating |
This shows that the TiNx rete of purchasing out by this Technology can increase substantially the work-ing life of automobile gearbox gear cutter, the work-ing life that reaches external import coated cutting tool work-ing life after making it be applied to Fa Shite automobile gear cutter.
Claims (2)
1. an automobile gearbox gear tool surface prepares the technology of TiNx rete, this process using Hall ion source actuated magnetron sputtering enhancing type magnetic filters the multi-arc ion coating film device, prepare the TiNx rete at the automobile gearbox gear tool surface, it is characterized in that, comprise the following steps:
1) slightly takes out: will insert Hall ion source actuated magnetron sputtering enhancing type magnetic through the cutter of clean and filter in the body of heater reaction chamber of multi-arc ion coating film device, and open vacuum system body of heater is evacuated to 6.0 * 10
0Pa;
2) heating reaches and carefully takes out: slightly take out and finish back unlatching heating system, be heated to 100-500 ℃, opening carefully simultaneously, the system of taking out is evacuated to 5.0 * 10
-3Pa;
3) ion bombardment: carefully exhaust the Ar that opens after finishing in the gas supply system, keeping the Ar flow is 100-150ml/min, and bias voltage increases gradually and is stabilized in 900V, and dutycycle is 30-90%; High-energy ion bombardment tool surface in the plasma field that produces by the grid bias power supply system in the equipment 20 minutes～50 minutes makes pending tool surface obtain cleaning and activation treatment;
4) pressure regulation: opening carefully after argon ion bombardment finishes again, the system of taking out is evacuated to 5.0 * 10
-3Pa;
5) preplating: after pressure regulation finishes, open the magnetic controlling target deposition pure Ti of 5min and impose bias voltage 900V, dutycycle 50%～80% and bombard continuously, preplating finishes;
6) formal plating: after preplating finishes, close magnetic controlling target, open multiple arc target internal linear adjustment in 25 minutes: make nitrogen amount from 0ml/min to 400ml/min, dutycycle from 50% to 90%, bias voltage is reduced to 100V from 900V, arc stream 50-80A, and provide 24V voltage for the multi sphere target by the direct supply of equipment, provide 200V voltage by the midfrequent AC power supply for magnetic control spattering target, drop by the generation of magnetic filtration system filters arc target, the reactant gases ion of high ionization level is provided by the Hall source in the equipment, this moment, high-energy electron and gas molecule collision ionization produced glow discharge, formation has chemically active ion and free radical, and these ions and free radical react at tool surface and be deposited as film, depositing time 1h;
7) cooling: after the thin film deposition for the treatment of tool surface forms, closing device power-supply system, heating system and gas supply system successively, and stop vacuum system work, 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 10
2Pa is cooled to gradually below 100 ℃ and comes out of the stove.
2. technology as claimed in claim 1 is characterized in that, the method for described clean is, earlier cutter is put into cleaner for metal and is boiled and boil 5～10 minutes, removes the tool surface greasy dirt; Put into the cleaner for metal ultrasonic cleaning then 5～10 minutes; The dilute hydrochloric acid solution of putting into proper concn again soaked 2～5 minutes; Put into distilled water after ultrasonic 10～60 seconds through the cutter to be plated of pickling, put into spirituous solution and dewater, dehydration back oven dry can be carried out plated film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100428128A CN100443628C (en) | 2006-05-15 | 2006-05-15 | TiNx film preparing process on the surface of cutter for machining gear in automobile gear box |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100428128A CN100443628C (en) | 2006-05-15 | 2006-05-15 | TiNx film preparing process on the surface of cutter for machining gear in automobile gear box |
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| CN100443628C true CN100443628C (en) | 2008-12-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101831606B (en) * | 2010-04-27 | 2012-05-30 | 苏州鼎利涂层有限公司 | Ball valve surface treatment method |
| CN101988182A (en) * | 2010-12-08 | 2011-03-23 | 沈阳工业大学 | Surface modification method for wear-resisting orthodontic arch wire and obtained wear-resisting arch wire |
| CN102433536A (en) * | 2011-12-05 | 2012-05-02 | 沈阳理工大学 | Preparation method of high-bonding-strength titanium nitride (TIN) ceramic membrane on surface of low-carbon steel |
| CN105671504A (en) * | 2016-02-04 | 2016-06-15 | 东莞沙头朝日五金电子制品有限公司 | Method for plating PVD composite antimicrobial film |
| CN110468379A (en) * | 2019-08-27 | 2019-11-19 | 中国科学院金属研究所 | A kind of electric arc ion plating device configuring heated filament |
| CN112813390A (en) * | 2019-11-18 | 2021-05-18 | 河北召飞科技服务有限公司 | Argon ion passivation method for hard alloy cutter |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156598C (en) * | 2002-03-25 | 2004-07-07 | 西安交通大学 | PCVO plasma impregnation composite reinforced method for precise vane hot forging die |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156598C (en) * | 2002-03-25 | 2004-07-07 | 西安交通大学 | PCVO plasma impregnation composite reinforced method for precise vane hot forging die |
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