CN104278234B - Preparation technology for self-lubricating coating with wide temperature range of room temperature to 800 DEG C - Google Patents

Preparation technology for self-lubricating coating with wide temperature range of room temperature to 800 DEG C Download PDF

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Publication number
CN104278234B
CN104278234B CN201310274061.2A CN201310274061A CN104278234B CN 104278234 B CN104278234 B CN 104278234B CN 201310274061 A CN201310274061 A CN 201310274061A CN 104278234 B CN104278234 B CN 104278234B
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coating
room temperature
temperature range
chromium
wide temperature
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CN104278234A (en
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李红轩
卢小伟
吉利
刘晓红
周惠娣
陈建敏
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • 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

Abstract

The invention discloses a preparation technology for a self-lubricating coating with a wide temperature range of room temperature to 800 DEG C. An arc ion plating method is employed for preparing a chrome oxide coating, and the prepared chrome oxide coating has relatively small friction coefficient (0.15-0.4) and relatively low wear rate at the wide temperature range of room temperature to 800 DEG C, especially at 800 DEG C, the friction coefficient is about 0.15 and the wear rate is about 10-7 mm＜3＞/Nm. Because of the good mechanical properties and tribology performances, the chrome oxide coating is applied to sealing of foil sheets of aero-engines, gas bearings and other friction moving parts working at the wide temperature range of room temperature to 800 DEG C.

Description

A kind of technology of preparing of the wide temperature range self-lubricating coat in use of room temperature to 800 DEG C
Technical field
The present invention relates to a kind of room temperature is respectively provided with the preparation skill of the chromium oxide coating of self-lubricating property in 800 DEG C of wide temperature ranges Art.
Background technology
In view of the demand to wide temperature range solid lubricant coating for the high-tech industries such as Aero-Space, smelting chemical, thermonuclear, grind Study carefully personnel its exploration is gradually increased, but up to the present also do not find that a kind of single coating disclosure satisfy that and arrive in room temperature All there is in high temperature width temperature range relatively low wear rate and less coefficient of friction, therefore it is carried out research and development have important Scientific value and application prospect.The deposition technique of coating mainly includes gas phase deposition technology, plasma spray technology, laser melting coating skill Art etc. is especially more ripe with the application of gas phase deposition technology and plasma spray technology.
Arc ion plating is the technology that a kind of typical physical gas-phase deposite method prepares film.Its principle is in vacuum chamber Interior, substrate applies an electric field with evaporation source, when chamber pressure is suitable, can produce glow discharge or arc between evaporation source and substrate Light discharge, with electron collision during, the ion of gas ion and target can be formed, these ions in the electric field be accelerated fly Basad, then occur to condense under the influence of Ions Bombardment and form film.Compared with magnetron sputtering, it has advantages below： (1) film is preferable with the combination of substrate；（2）Film deposition rate is very fast；（3）Film is preferable around plating property；（4）Film consistency carries High；(5) metal ionization level is high, is conducive to the uniformity of film；(6) one arcs are multiplex, be heating source and pre- bombardment purifies Source and ionization source,（7）Target utilization is higher etc..
Chromium oxide is considered as one of oxide the hardest for a long time always, simultaneously its have good corrosion resistance and Distinctive optical property, is widely used in sun light absorbing material and photocopy mould etc..But adopt non-magnetron sputtering at present more Method prepares chromium oxide coating, and it is poor around plating property for complicated shape part, and its oxygen content is relatively low simultaneously, thus have impact on The tribological property of coating, limits application in wide temperature range for the chromium oxide coating.
Content of the invention
Present invention is primarily targeted at providing a kind of room temperature to be respectively provided with the coating of self-lubricating property in 800 DEG C of wide temperature ranges The technology of preparing of material.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of technology of preparing of the wide temperature range self-lubricating coat in use of room temperature to 800 DEG C, using the method preparation of arc ion plating, its The deposition process being characterised by the method coating is to complete in the vacuum cavity of coating machine being furnished with electric arc, concretely comprises the following steps：
A, activation cleaning surface：Smooth, clean metallic substrates are placed within cavity, vacuumize 1.5 × 10-2Pa with Under, it is passed through argon gas as ionization of gas, opens pulsed bias power supply, glow discharge produces plasma, and substrate surface is carried out Activation cleaning；
B, transition zone preparation：After cleaning finishes, using the method deposition chromium transition zone first of arc ion plating, from chromium post Target as arc ion plating target, using argon gas as ionization of gas, the additional back bias voltage of matrix, after deposition chromium transition zone close；
C, deposited oxide chrome coating：Arc ion plating target selects to be still chromium post target, then is passed through oxygen, by controlling nitrogen The size that the flow-rate ratio of gas and oxygen and electric current and substrate are biased controls the structure of coating；
D, coating post processing：Made annealing treatment, then naturally cooled to room temperature.
In step, metallic substrates are selected from M2 high-speed steel, Nickel-Based Steel, stainless steel or aluminium alloy, plasma-activated Process parameters range is：Cavity air pressure 0.4～2.0Pa, biases -100V～-1000V.
In stepb, chromium transition zone process parameters range is：Cavity air pressure 0.2～1.0Pa, sputtering current 1～200 A, Pulsed bias -50～-500V, transition region thickness 30～500 nm.
In step C, chromium oxide layer process parameters range is：Cavity air pressure 0.2～1.0Pa, O2/Ar flow-rate ratio is 1:5 ～5:1, sputtering current 1～200 A, pulsed bias -50～-500V, coating layer thickness 0.5～5um.
In step D, parameter and annealing scope is：200～1000 DEG C of annealing temperature, 1～20 DEG C/min of programming rate, Temperature retention time is 0.5～5h.
The main component of this film is Cr and Cr2O3, its section structure is as shown in Figure 1.Cr transition zone is primarily to increase Film and adhesion in the range of wide temperature range for the matrix, Cr2O3 is the wear-resisting phase of its anti-attrition.
The main performance index of product of the present invention is as shown in the table：
The present invention prepares chromium oxide coating using the method for arc ion plating.The method and the oxygen using magnetron sputtering preparation Change chrome coating compare, arc ions electroplating method preparation chromium oxide coating, increased for complex sample around plating property, coating with The adhesion of substrate is higher, and the oxygen content of coating also increases, thus improve the mechanical performance of coating, antioxygenic property and Tribological property etc..Through investigating, the chromium oxide coating prepared using arc ions electroplating method is in the wide temperature range scope of room temperature to 800 DEG C Inside it is respectively provided with less coefficient of friction（0.15-0.4）With relatively low wear rate, especially left 0.15 in 800 DEG C of coefficient of frictions The right side, wear rate is also 10-7mm3/ Nm about.In view of its good mechanical performance and tribological property, chromium oxide coating can be applied In the foil seal of aero-engine, gas bearing etc. is operated in the fricting movement part in the range of 800 DEG C of wide temperature ranges for the room temperature.
Brief description
Fig. 1 is Cr2O3The ESEM shape appearance figure of the section of film.
Fig. 2 is Cr2O3The coefficient of friction of coating room temperature to 800 DEG C.
Specific embodiment
Embodiment 1：
A. sample pretreatment：The stainless steel being polished to minute surface is carried out being cleaned by ultrasonic 10 with distilled water, acetone respectively Min, is dried up with nitrogen immediately, is placed in settling chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10-2Below Pa, is passed through high-purity argon gas It is 1.5 Pa to air pressure.Open pulsed bias power supply, regulation voltage level is -500 V, carries out argon plasma Bombardment and cleaning 20min.
B. deposition chromium transition zone：Adjust argon flow amount, make cavity air pressure maintain 0.45Pa, open post arc power, Regulation electric current is 90A, biases as -200V, closing when transition zone deposition about 200nm.
C. deposited oxide layers of chrome：It is passed through the mixed gas of high-purity argon gas and oxygen, make chamber pressure maintain 0.45Pa left The right side, the flow-rate ratio of control argon gas and oxygen is 1:2, open post arc power, regulation electric current is 90A, bias as -200V, deposition is about Cool down after 2h, when temperature is down to below 50 DEG C, release vacuum begins to speak to sample.
D. sample post processing：It is incubated 2h at 400 DEG C in Muffle furnace of sample.
Embodiment 2：
A. sample pretreatment：The aluminium alloy being polished to minute surface is carried out being cleaned by ultrasonic 10 with distilled water, acetone respectively Min, is dried up with nitrogen immediately, is placed in settling chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10-2Below Pa, is passed through high-purity argon gas It is 1.0 Pa to air pressure.Open pulsed bias power supply, regulation voltage level is -400 V, carries out argon plasma Bombardment and cleaning 15min.
B. deposition chromium transition zone：Adjust argon flow amount, make cavity air pressure maintain 0.45Pa, open post arc power, Regulation electric current is 100A, biases as -300V, closing when transition zone deposition about 200nm.
C. deposited oxide layers of chrome：It is passed through the mixed gas of high-purity argon gas and oxygen, make chamber pressure maintain 0.45Pa left The right side, the flow-rate ratio of control argon gas and oxygen is 1:1, open post arc power, regulation electric current is 100A, bias as -300V, deposition is about Cool down after 2h, when temperature is down to below 50 DEG C, release vacuum begins to speak to sample.
D. sample post processing：It is incubated 3h at 500 DEG C in Muffle furnace of sample.
Embodiment 3：
A. sample pretreatment：The high-temperature steel being polished to minute surface is carried out being cleaned by ultrasonic 10 with distilled water, acetone respectively Min, is dried up with nitrogen immediately, is placed in settling chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10-2Below Pa, is passed through high-purity argon gas It is 2.0 Pa to air pressure.Open pulsed bias power supply, regulation voltage level is -700 V, carries out argon plasma Bombardment and cleaning 50min.
B. deposition chromium transition zone：Adjust argon flow amount, make cavity air pressure maintain 0.45Pa, open post arc power, Regulation electric current is 80A, biases as -400V, closing when transition zone deposition about 200nm.
C. deposited oxide layers of chrome：It is passed through the mixed gas of high-purity argon gas and oxygen, make chamber pressure maintain 0.45Pa left The right side, the flow-rate ratio of control argon gas and oxygen is 2:1, open post arc power, regulation electric current is 50A, bias as -400V, deposition is about Cool down after 2h, when temperature is down to below 50 DEG C, release vacuum begins to speak to sample.
D. sample post processing：It is incubated 1h at 800 DEG C in Muffle furnace of sample.

Claims (3)

1. the technology of preparing of the wide temperature range self-lubricating coat in use of a kind of room temperature to 800 DEG C, using the method preparation of arc ion plating, it is special Levy and be that the deposition process of the method coating is to complete in the vacuum cavity of coating machine being furnished with electric arc, concretely comprises the following steps：
A, activation cleaning surface：Smooth, clean metallic substrates are placed within cavity, vacuumize 1.5 × 10-2Below Pa, leads to Enter argon gas as ionization of gas, open pulsed bias power supply, glow discharge produces plasma, substrate surface is carried out with activation clear Wash；
B, transition zone preparation：After cleaning finishes, using the method deposition chromium transition zone first of arc ion plating, made from chromium post target For arc ion plating target, using argon gas as ionization of gas, the additional back bias voltage of matrix, close after deposition chromium transition zone；Described chromium Transition zone process parameters range is：Cavity air pressure 0.2～1.0Pa, sputtering current 1～200 A, pulsed bias -50～-500V, Transition region thickness 30～500 nm；
C, deposited oxide chrome coating：Arc ion plating target selects to be still chromium post target, then is passed through oxygen, by control argon gas and The size that the flow-rate ratio of oxygen and electric current and substrate are biased controls the structure of coating；Described chromium oxide layer technological parameter model Enclose for：Cavity air pressure 0.2～1.0Pa, O2/ Ar flow-rate ratio is 1:2～2:1, sputtering current 1～200 A, pulsed bias -50～- 500V, 0.5～5 μm of coating layer thickness；
D, coating post processing：Made annealing treatment, then naturally cooled to room temperature.
2. the technology of preparing of the wide temperature range self-lubricating coat in use of room temperature as claimed in claim 1 to 800 DEG C is it is characterised in that in step In rapid A, metallic substrates are selected from M2 high-speed steel, Nickel-Based Steel, stainless steel or aluminium alloy, plasma-activated process parameters range For：Cavity air pressure 0.4～2.0Pa, biases -100V～-1000V.
3. the technology of preparing of the wide temperature range self-lubricating coat in use of room temperature as claimed in claim 1 to 800 DEG C is it is characterised in that in step In rapid D, parameter and annealing scope is：200～1000 DEG C of annealing temperature, 1～20 DEG C/min of programming rate, temperature retention time is 0.5～5h.
CN201310274061.2A 2013-07-02 2013-07-02 Preparation technology for self-lubricating coating with wide temperature range of room temperature to 800 DEG C Active CN104278234B (en)

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CN106811725B (en) * 2015-11-27 2019-02-15 中国科学院宁波材料技术与工程研究所 Wide adaptive lubricant coating of temperature range and the preparation method and application thereof
CN106282942A (en) * 2016-08-08 2017-01-04 苏州极地实业有限公司 A kind of method at metal material surface deposited oxide nickel thin film
CN110983275B (en) * 2019-12-25 2022-02-01 南京华塑增材制造有限公司 Low-temperature preparation method of silver-doped titanium dioxide nano antibacterial composite coating on surface of PETG appliance
CN111334769B (en) * 2020-04-02 2021-11-02 中国科学院宁波材料技术与工程研究所 PbO-Cr2O3Co-doped film and preparation method and application thereof
CN111534799B (en) * 2020-05-29 2021-11-12 四川大学 Oxidation-resistant and heat-insulating ceramic coating and preparation method thereof
CN112610608B (en) * 2020-11-26 2022-07-15 东南大学 Wide-temperature-range self-lubricating bearing and preparation method thereof
CN112962066A (en) * 2021-02-04 2021-06-15 中国科学院兰州化学物理研究所 Preparation method of chromium oxide wide-temperature-range self-lubricating self-repairing coating

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