CN107365963A - PVD oxide coating preparation methods - Google Patents

PVD oxide coating preparation methods Download PDF

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Publication number
CN107365963A
CN107365963A CN201710305307.6A CN201710305307A CN107365963A CN 107365963 A CN107365963 A CN 107365963A CN 201710305307 A CN201710305307 A CN 201710305307A CN 107365963 A CN107365963 A CN 107365963A
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coating
arc
cae
pvd
preparation
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赵海波
梁红樱
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Sichuan University
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Sichuan University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a kind of PVD oxide coatings preparation method, especially a kind of oxide coating preparation method for being related to oxide coating preparation field.The present invention provides a kind of deposition height, the good oxide coating preparation method of obtained coating insulation effect.The oxide coating preparation method of the present invention, amplitude is moved radially using resultant field CAE increase arc spots density, raising arc spot translational speed, increase arc spot while ion deposition is carried out using cathodic arc ion plating；Electric field caused by insulator positive charge build-up is eliminated using resultant field CAE pulse control techniques or bipolar pulse bias techniques；The ion propulsion of Coating Materials is nearby reacted to band film-coating workpiece using resultant field CAE；Insulation oxide coatings growth is controlled by the depositing temperature of the output energy sum of resultant field CAE control ions, deposition height, the sull of excellent insulation performance can be made using the present processes.

Description

PVD oxide coating preparation methods
Technical field
The present invention relates to a kind of PVD oxide coatings preparation method, especially one kind to be related to oxide coating preparation field Oxide coating preparation method.
Background technology
During High-speed machining or DRY CUTTING, cutting temperature turns into the main original for influenceing coated cutting tool service life Cause, therefore improve the high-temperature behavior of film, ensure that the red hardness of coated cutting tool turns into PVD (Physical Vapor in recent years Deposition) the exploitation focus of technology.Technology the most frequently used PVD can be divided into three major types：Vacuum evaporation coating (Vacuum Evaporating), magnetron sputtering (Magnetron Sputtering), cathodic arc ion plating (Arc Ion Plating).
The coating of high rigidity, current research can be obtained by PVD methods, its hardness reaches more than 3500HV not May.But PVD depositing temperature is usually located at less than 600 DEG C, in hot environment, the decomposition of coating, the decline of hardness can not Avoid.On the premise of PVD entirety technology of preparing routes are not influenceed, temperature is formed to PVD hard coats, thermal diffusion protection is one The effective method of kind.One layer of other film layer of ad eundem (micron) is established on hard coat, completely cuts off conducting, being first for temperature The diffusion of element, forms the protection to hard coat, extends the military service cycle of coated cutting tool.
Theoretical research shows that alumina type coating has good a heat blocking and chemical wear resistance, thus from 2000 with Come, the research of PVD oxide coatings progressively deploys.PVD is operated under a relatively low temperature conditionss, to be formed good Good oxide coating, some that can be run into are difficult.Such as low deposition, low ionization, the compactness of oxide coating, The problems such as solid solubility, associativity, electric conductivity.
Research for PVD alumina type coatings mainly has SwedenUniversity, Germany Institute of Materials Research, University of Hannover, the Vienna of Australia University of Technology, Switzerland Institut de Physique de la Matiere Condens é e, Nagaoka University of Technology, the Kobe Steel of Japan, LTD, the Shanghai Communications University of China, method Nancy-University of state etc..
It is a great technological break-through to prepare oxide coating using PVD methods.Relative to nitride coatings, oxide The characteristics of coating maximum is with thermal insulation and chemical inertness.Thermal insulation can completely cut off to formation such as nitride coatings to be protected, and Chemical inertness can then separate phase counterdiffusion and chemical abrasion of the cutter with workpiece.According to Wei Deman --- Fu Laici laws (wiede Mann-Franz Law), at less low temperature, the ratio between the thermal conductivity factor of metal and electrical conductivity are proportional to temperature.Therefore can With inference, good thermal insulation and chemical inertness, the insulating properties depending on oxide coating.
For PVD ion plating techniques, its most basic principle is the ionization by evaporation atom, in electric field Under effect, cation is promoted to accelerate to drive towards workpiece surface to be coated, so as to obtain preferable coating structure and performance.This process bag Containing 2 concepts, first, evaporation atom answers more ionizations；Second, workpiece to be coated should be conductor, so as to the application of electric field.
The preparation method of PVD oxides is more in disorder at present, mostly in a manner of sputtering based on, including DC, MS, RF etc., splash It is strong that the source of penetrating can suppress " poisoning " phenomenon of material target surface, multi-component sputtering ability.But because ionization level, ion energy are relative It is relatively low, it is unfavorable for the generation of high quality oxide coating.The main crux of oxide coating is prepared using sputtering method to be, oxygen Compound is not good enough with nitride bonded, and sedimentation rate is too low, is unfavorable for practical application.
AIP contributes to the generation of ionization, for O2It is no exception, but in O2When excessive or original electric field changes, O2 It is easier to react on cathode target surface, oxide is generated, so as to cause the failure of cathodic discharge, it is impossible to needed for normal output The element wanted, as " it is poisoned ".PVD oxide is using aluminum oxide master as Al, AlTi material are more easy to relatively and O at present2Occur anti- Should, therefore conventional way is that the Cr of certain content is added in Al materials, to prevent the oxidation of target surface.But chromium oxide stability It is relatively poor, the change of oxide coating performance can be caused.
In summary, insulation oxide coating is formed using the method for prior art and following problem is present：
First, O2It is easier to react on cathode target surface, generates oxide, so as to cause the failure of cathodic discharge, no Required element can be normally exported, produces " poisoning " phenomenon of evaporation source material target surface；
2nd, electric field caused by the accumulation of insulator positive charge hinders the progress of deposition；
3rd, ion energy is low, is not enough to realize transition of the metal nitride to insulation oxide coating, and obtain well Adhesion；
4th, under relatively low temperature conditions, α-Al how are regulated and controled2O3Growth the problem of.
Due to above reason, under conditions of prior art, common ion plating technique is not appropriate for insulation oxide painting The preparation of layer.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of deposition height, and obtained coating insulation effect is good PVD oxide coating preparation methods.
The present invention solves PVD oxide coating preparation methods used by its technical problem, using cathode arc ion Increase arc spot density using resultant field CAE while plating carries out ion deposition, improve arc spot translational speed, increase arc spot radially Mobile range；The production of insulator positive charge build-up is eliminated using resultant field CAE pulse control techniques or bipolar pulse bias techniques Raw electric field；The ion propulsion of Coating Materials is reacted near workpieces to be coated using resultant field CAE；By compound The output energy and depositing temperature of magnetic field CAE control ions control insulation oxide coatings growth.
It is further, including following steps：
A, workpiece to be coated is positioned in vacuum chamber, then to vacuum chamber；
B, 40~60sccm Ar gas is sent into, and vacuum chamber is preheated；
C, electron beam heats；
D, treat film-coating workpiece surface and carry out gas plasma etching；
E, plated film is carried out to workpiece surface；
F, cooling treatment is carried out to film-coating workpiece.
It is further that the wherein preheating time is 39 minutes to 41 minutes.
It is further vacuum intraventricular pressure is less than 5 × 10 by force after being vacuumized in the step A-2Pa。
It is further that pressure in vacuum tank is adjusted to (2.0~3.0) × 10 in step C-1Pa, Ar throughput are adjusted to 90 ~120sccm；And filament supply is driven, the electric current of filament supply is stepped up to 170~230A；Field supply is opened, and by magnetic Field current is adjusted to 12~20A；Arc power is opened, the electric current of arc power is gradually added to 180A.
It is further in D steps, heater current is maintained 170~230A；Arc current reduces to 100~120A；Magnetic Field current reduces to 6~8A；Pressure in vacuum tank is adjusted to (2.0~2.4) × 10-1Pa, Ar throughput 50~60sccm, H2Throughput 15 ~20, breakdown grid bias power supply, gradually power-up is depressed into 0~200V of direct current, 300~500V of pulse.
It is further to carry out plated film using 8 cathode arc sources in E steps.
It is further that controlled sputtering source implantation simple substance element is utilized in E steps.
The beneficial effects of the invention are as follows：The application makes arc spot closeer using resultant field CAE, translational speed faster, radially Mobile range is bigger, avoids oxygen and is reacted on cathode target surface, and skill is biased using pulse control technique or bipolar pulse Art solves positive charge build-up and caused harmful effect is formed to oxide coating, using resultant field CAE axial directions Push Technology, The energy of deposited particles is improved, while controls output energy and the depositing temperature of ion to be insulated to control by resultant field CAE Oxide coating grows.The application solves cathode arc by cathodic arc ion plating technology combination resultant field CAE technologies Ion plating prepares the problem of oxide coating, and deposition height, the sull of excellent insulation performance can be made.
Brief description of the drawings
Fig. 1 is the target source distribution figure that triple oxide film is made using the present processes；
Fig. 2 is the AlTiN/AlTiON coating morphology figures prepared using the present processes；
Fig. 3 is the AlTiN/AlCrON coating morphology figures prepared using the present processes；
Fig. 4 is the thickness measured drawing of the oxide prepared using the present processes；
Fig. 5 is AlTiN and AlTiN/Al2O3XRD spectrum comparison diagram；
Fig. 6 is microscopic appearance comparison diagram of the coating after high-temperature process；
Fig. 7 is the hardness measured drawing using the aluminum oxide coating layer obtained by the present processes；
Fig. 8 is the scratch test figure using the coating obtained by the present processes；
Fig. 9 is the shape appearance figure of the coating obtained by the method for prior art；
Figure 10 is containing Al67Ti33Blade wear of the tool flank figure after the Tool in Cutting of N coatings；
Figure 11 is containing Al67Ti33Blade wear of the tool flank figure after the Tool in Cutting of N/AlTiON coatings；
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
The PVD oxide coating preparation methods of the present invention, while ion deposition is carried out using cathodic arc ion plating Amplitude is moved radially using resultant field CAE increase arc spots density, raising arc spot translational speed, increase arc spot；Utilize compound magnetic Field CAE pulse control techniques or bipolar pulse bias techniques eliminate electric field caused by insulator positive charge build-up；Utilize compound magnetic Field CAE is nearby reacted the ion propulsion of Coating Materials to band film-coating workpiece；The defeated of ion is controlled by resultant field CAE Go out the depositing temperature of energy sum to control insulation oxide coatings growth.Because in deposition process, CAE sources can provide higher Energy and ionization level, be more conducive to the formation of oxide.Simultaneous oxidation nitride layer is affected by temperature, and change is obvious.It is actually warm Degree determines the performance of oxide coating, and the CAE technologies of cathodic arc ion plating are in the deposition process of oxide, it is possible to provide Higher energy and ionization level, contributes to the formation of oxide.From the point of view of coating composition, using the insulation oxygen obtained by the application Compound coating, the content of its oxygen element are higher.Make arc spot closeer using resultant field CAE, translational speed faster, moves radially width Degree is bigger, and such oxygen element is reacted by arc spot driving guiding to workpiece surface, and away from cathode target surface, thus effectively keep away Oxygen is exempted to react on cathode target surface, oxide has been generated, so as to cause the failure of cathodic discharge, it is impossible to normally export institute The element needed.Caused electric field can prevent ion in the deposition of workpiece surface after positive charge build-up in coating process, and this Application eliminates caused electricity after positive charge build-up using electric field caused by pulse control technique or bipolar pulse bias techniques Field solves positive charge build-up and caused harmful effect is formed to oxide coating.Utilize resultant field CAE axial directions Push Technology The ion propulsion of Coating Materials is nearby reacted to band film-coating workpiece, the energy of deposited particles is improved, with can be with work The reaction of part surface and strong bonded.Improving the output energy of ion and depositing temperature by resultant field CAE simultaneously makes to grow Insulation oxide coating there is more preferable insulating properties.Wherein CAE pulse control techniques and resultant field CAE axial directions Push Technology For prior art.Wherein CAE refers to cathodic arc technique.The application passes through cathodic arc ion plating technology combination resultant field CAE technologies solve the problems, such as that cathodic arc ion plating prepares oxide coating, and deposition height, excellent insulation performance can be made Sull.Through experimental tests, 1~2 μm/h can be reached using the present processes its sedimentation rates, and prior art Sedimentation rate be less than 0.5 μm/h, therefore the application substantially increases the sedimentation rate in sull preparation process.Such as figure Shown in 4,1.69 μm are reached using thickness of the present processes through deposited oxide layer after an hour.
Using the XRD spectrum of film made of the present processes and single AlTiN films as shown in figure 5, can by Fig. 5 Obvious to observe, there is the preferred orientation in (113) face in PVD oxides, this compared with single AlTiN after the application It is orientated further strong, this orientation and O2Flow it is relevant, diffracted intensity is with O2Increase and increase, embody Al2O3Phase is deposited .
Fig. 6 is microscopic appearance comparison diagram of the coating after 2 two hours high-temperature process, and wherein Fig. 6 left-half is Al67Ti33Microscopic appearance comparison diagrams of the N after 900 DEG C of high-temperature process 2h, Fig. 6 right half part is Al67Ti33N/AlTiON Microscopic appearance comparison diagram after 1100 DEG C of high-temperature process 2h.The characteristics of PVD, is the coating that can obtain extreme hardness, But under the conditions of high-temperature machining, diffusion of the oxygen element to coat inside, diffusion of Ti, Al element to outside, it can all cause coating Oxidation, decomposition and the reduction of hardness (see shown in Fig. 6 left-halfs).In hot environment, certain isolation barrier, resistance are established The only diffusion of heat and coherent element, delays the decay of coating performance, is a kind of effective technical scheme.Fig. 6 right-hand component by In features such as the insulating of oxide coating, thermal insulation, inertia, form good isolation barrier, its structure after high-temperature process still Original structure is so maintained well, has effectively delayed the decay of coating performance.
As shown in fig. 7, by actual measurement, the aluminum oxide coating layer hardness about 2600HK made using the present processes.
As shown in figure 8, to carrying out scratch test using oxide coating made from the present processes, when the external force of experiment Coating surface is just destroyed when reaching 96N, therefore the adhesion of coating is up to 96N made from the application method.
Carry out cutting contrast experiment to the cutter containing different coating, experimental result as shown in Figure 10 and Figure 11, wherein scheming 10 be containing Al67Ti33Blade wear of the tool flank figure after the Tool in Cutting of N coatings, as can be seen from the figure Al67Ti33N coatings Blade abrasion is it is obvious that and have obvious glue to consider phenomenon to be worth doing；Figure 11 is containing Al67Ti33After the Tool in Cutting of N/AlTiON coatings Blade wear of the tool flank figure, as can be seen from the figure Al67Ti33The abrasion of N coated chips is less than normal, and substantially existing without viscous bits As.
The oxide coating of the application is made using multicomponent alloy laminated film Preparation equipment, and the equipment possesses 8 negative electrodes Arc source, 2 controlled sputtering sources, resultant field, heated filament ion gun, can complete PVD ion platings.
The oxide coating preparation method of the present invention includes following steps：
A, will be positioned over film-coating workpiece in vacuum chamber, then to vacuum chamber；B, it is sent into 40~60sccm Ar Gas, and vacuum chamber is preheated；C, electron beam heats；D, treat film-coating workpiece surface and carry out gas plasma etching；E、 Plated film is carried out to workpiece surface；F, cooling treatment is carried out to film-coating workpiece.Preheating time was advisable with 40 minutes, preheating 40 After minute, composite heating is carried out, composite heating time range is 70~100min.Make vacuum intraventricular pressure after being vacuumized in step A It is strong to be less than 5 × 10-2Pa。
Pressure in vacuum tank is adjusted to (2.0~3.0) × 10 in step C-1Pa, Ar throughput are adjusted to 90~120sccm；And Filament supply is driven, is stepped up the electric current of filament supply to 170~230A；Field supply is opened, and field supply is adjusted to 12 ~20A；Arc power is opened, the electric current of arc power is gradually added to 180A.Using aforementioned parameters, using heated filament ion source heating, Ionization level can be increased, dramatically increase the amount of ions of participation plated film, be advantageous to the formation of coating.
In D steps, heater current is set to maintain 170~230A；Arc current reduces to 100~120A；Field supply reduces to 6 ~8A；Pressure in vacuum tank is adjusted to (2.0~2.4) × 10-1Pa, Ar throughput 50~60sccm, H2Throughput 15~20, breakdown is inclined Voltage source, gradually power-up are depressed into 0~200V of direct current, 300~500V of pulse.Film-coating workpiece surface is treated using aforementioned parameters to carry out Ion etching, improves workpiece surface activity, and film is formed beneficial in workpiece surface.
As shown in figure 1, carry out plated film using 8 cathode arc sources in E steps.The design in 8CAE sources, can be more favourable In the matching of multicomponent material, such as AlTi and AlCr combination；2 controlled sputtering sources are introduced on the basis of 8 cathode arc sources then It is easy to the implantation of other elements, such as Mo, W, V, Nb, Y, Ce.
As shown in Figures 2 and 3, the insulation oxide coating prepared using the present processes shows noncrystalline state, when O2When increasing to certain dose, resulting coating is Al-Ti-O systems, is shown in Table 1, and is a kind of membrane system of insulation, resistance More than 10M Ω, from the point of view of coating composition, the insulation oxide coating obtained by us, the content of its oxygen element is higher.And Fig. 9 It is then to use coating made from prior art, its tissue still shows column crystal, belongs to a kind of typical nitride structure Form.
Table 1Al-Ti-O coating compositions
Element Weight Atom
Percentage Percentage
C K 12.92 23.28
Al K 23.79 19.09
Ti K 18.08 8.17
W M 9.49 1.12
O 35.72 48.33
Total amount 100.00
Here is to prepare triple oxide film, Ti/AlTiMoN/AlTiON preparation technology using the present processes Process
(1) pre-treatment：
Before plated film, cutter is dried after conventional alkalescent cleaning agent and the cleaning of absolute alcohol ultrasonic wave, is placed in coating chamber；
(2) preparation before coating：
1. vacuum chamber is inflated, fire door is opened；
2. changing electric arc, sputter target material as needed, sight glass is changed；
3. clean each position of body of heater, pressure 0.6MPa with high pressure air rifle；
4. selecting appropriate fixture, load workpiece (cutter), confirm that clamp movement is reliably errorless；
5. confirming electron gun, arc source, sputtering source, impressed current anode, the insulation status of work piece holder, its resistance should be greater than 100KΩ；
6. close deposited chamber, close vent valve.
(3) vacuumize (to 5 × 10-2Pa) and preheat
1. start handpiece Water Chilling Units；
2. pump, fore pump are maintained, opens and takes out valve in advance；
3. starting compound vacuum gauge, thermocouple rule 1 are opened, test fore line vacuum, vacuum is less than 5Pa
4. start molecular pump；
5. after molecular pump enters normal operating conditions, and vacuum degree in vacuum chamber satisfaction is less than 5Pa, closing takes out valve, opened in advance Open preceding step valve, high vacuum valve；
6. when vacuum values are less than 5 × 10-2During Pa, the Ar gas for the 40~60sccm that makes a gift to someone, and open auxiliary heating (5KW)；
7. open workpiece to rotate, frequency modulation 15Hz；
8. the composite heating stage is prepared to enter into after 40min.
(4) electron beam heats
1. pressure in vacuum tank is adjusted to (2.0~3.0) × 10-190~120sccm of Pa, Ar throughput；
2. driving filament supply, electric current is slowly risen to 170~230A；
3. opening field supply is adjusted to 12~20A；
4. open arc power supply, switch goes to heating gear；
5. causing electric arc, electric current is gradually added in 180A；
6. 70~100min of composite heating period.
(5) gas plasma etches
1. heater current maintains 170~230A；
2. arc current reduces to 100~120A；
3. field supply reduces to 6~8A；
4. pressure in vacuum tank is adjusted to (2.0~2.4) × 10-1Pa, Ar throughput 50~60sccm, H2Throughput 15~ 20sccm；
5. breakdown grid bias power supply, gradually power-up is depressed into 0~200V of direct current, 300~500V of pulse；
6. the ion etching period is about 80~150min.
(6) coating
1. TiN transition zones：480~680sccm of nitrogen flow, bias are adjusted to 150V, open 2 CAE sources (Ti), arc target electricity Flow 100~120A, 180~600sec of cycle；
2. Ti/AlTi layers：540~900sccm of nitrogen flow, bias are adjusted to 100~120V, open 4 CAE sources (Al67Ti33), arc 80~120A of target current, 3600~7200sec of cycle；
3. open 2 MS sources (Mo), 1~3A of sputtering current, 3600~7200sec of cycle：Nitrogen flow 540~ 900sccm, bias are adjusted to 80~100V；
4. close 4 CAE sources (Al67Ti33), open 2 CAE sources (Al70~80Ti20~30), arc 100~120A of target current, 1800~3600sec of cycle, it is sent into O230~150sccm of gas；
5. close electric arc, sputtering target source, grid bias power supply；
6. close heating source, N2、O2Source, close molecular pump power source；Send nitrogen 80~120sccm；
7. argon gas is sent to 30Pa；
(7) cool down：60~120min of process time.

Claims (8)

1.PVD oxide coating preparation methods, it is characterised in that：While ion deposition is carried out using cathodic arc ion plating Amplitude is moved radially using resultant field CAE increase arc spots density, raising arc spot translational speed, increase arc spot, utilizes compound magnetic Electric field caused by field CAE pulse control techniques or bipolar pulse bias techniques elimination insulator positive charge build-up, utilizes compound magnetic Field CAE axial direction Push Technologies are reacted the ion propulsion of Coating Materials near workpieces to be coated, pass through resultant field CAE The output energy and depositing temperature for controlling ion control insulation oxide coatings growth.
2. PVD oxide coatings preparation method as claimed in claim 1, it is characterised in that：Including following steps：
A, workpiece to be coated is positioned in vacuum chamber, then to vacuum chamber；
B, 40~60sccm Ar gas is sent into, and vacuum chamber is preheated；
C, electron beam heats；
D, treat film-coating workpiece surface and carry out gas plasma etching；
E, plated film is carried out to workpiece surface；
F, cooling treatment is carried out to film-coating workpiece.
3. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：The preheating time is 39 points Clock was to 41 minutes.
4. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：Make after being vacuumized in the step A Vacuum intraventricular pressure is less than by force 5 × 10-2Pa。
5. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：Pressure in vacuum tank is adjusted in step C To (2.0~3.0) × 10-1Pa, Ar throughput are adjusted to 90~120sccm；Open filament power supply, is stepped up filament supply Electric current is to 170~230A；Field supply is opened, and field supply is adjusted to 12~20A；Arc power is opened, by the electricity of arc power Stream is gradually added to 180A.
6. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：In D steps, make heater current Maintain 170~230A；Arc current reduces to 100~120A；Field supply reduces to 6~8A；Pressure in vacuum tank be adjusted to (2.0~ 2.4)×10-1Pa, Ar throughput 50~60sccm, H2Throughput 15~20, breakdown grid bias power supply, gradually power-up are depressed into direct current 0 ~200V, 300~500V of pulse.
7. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：8 negative electrodes are used in E steps Arc source carries out plated film.
8. PVD oxide coatings preparation method as claimed in claim 2, it is characterised in that：Magnetron sputtering is utilized in E steps Source is implanted into simple substance element.
CN201710305307.6A 2017-05-03 2017-05-03 PVD oxide coating preparation methods Pending CN107365963A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114164405A (en) * 2021-12-07 2022-03-11 四川真锐晶甲科技有限公司 Cutter thick film nitride coating and preparation method thereof

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US5827580A (en) * 1996-03-27 1998-10-27 Regents Of The University Of California Low temperature formation of electrode having electrically conductive metal oxide surface
CN101768727A (en) * 2009-12-31 2010-07-07 中国地质大学（北京） Complex vacuum deposition device
CN102943240A (en) * 2012-11-12 2013-02-27 广东世创金属科技有限公司 Multifunctional plasma enhanced coating system
CN103540900B (en) * 2013-10-22 2016-01-13 中国科学院金属研究所 A kind of magnetron arc ion plating composite deposition technique and deposition apparatus

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Publication number Priority date Publication date Assignee Title
CN1046356A (en) * 1990-03-22 1990-10-24 四川大学 The preparation method of film of multicomponent metal oxide
US5827580A (en) * 1996-03-27 1998-10-27 Regents Of The University Of California Low temperature formation of electrode having electrically conductive metal oxide surface
CN101768727A (en) * 2009-12-31 2010-07-07 中国地质大学（北京） Complex vacuum deposition device
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