CN104278234A - 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
CN104278234A
CN104278234A CN201310274061.2A CN201310274061A CN104278234A CN 104278234 A CN104278234 A CN 104278234A CN 201310274061 A CN201310274061 A CN 201310274061A CN 104278234 A CN104278234 A CN 104278234A
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coating
room temperature
chromium
ion plating
transition layer
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CN104278234B (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 room temperature is to the technology of preparing of 800 DEG C wide temperature range self-lubricating coat in use
Technical field
The present invention relates to the technology of preparing all in a kind of room temperature to 800 DEG C of wide temperature ranges with the chromium oxide coating of self-lubricating property.
Background technology
Consider that the hi-tech industries such as aerospace, smelting chemical, thermonuclear are to the demand of wide temperature range solid lubricant coating, the exploration of researchist to it increases gradually, but up to the present also do not find that a kind of single coating can meet all have lower wear rate and less frictional coefficient in room temperature to the wide temperature range of high temperature, therefore carries out research and development to it and has important scientific value and application prospect.The deposition technique of coating mainly comprises gas phase deposition technology, hot-spraying techniques, laser melting and coating technique etc., especially comparatively ripe with the application of gas phase deposition technology and hot-spraying techniques.
Arc ion plating is the technology that a kind of typical physical gas-phase deposite method prepares film.Its principle is in vacuum chamber, substrate and evaporation source apply an electric field, when chamber pressure is suitable, glow discharge or arc discharge can be produced between evaporation source and substrate, with in electronic impact process, can form the ion of gaseous ion and target, these ions are accelerated in the electric field flies to substrate, so condensation occur under ion bombardment impact and form film.Compared with magnetron sputtering, it has the following advantages: (1) film and substrate in conjunction with better; (2) film deposition rate is very fast; (3) film is better around plating property; (4) film density improves; (5) metal ionization level is high, is conducive to the homogeneity of film; (6) one arcs are multiplex, are heating source and bombard purification source and ionization source in advance, and (7) target utilization is more high.
Chromic oxide is considered to one of the hardest oxide compound for a long time always, and it has good erosion resistance and distinctive optical property simultaneously, is widely used in sunlight absorbing material and photocopy mould etc.But at present adopt non-magnetically controlled sputter method to prepare chromium oxide coating, its poor around plating property for complicated shape part, its oxygen level is lower, thus have impact on the tribological property of coating, limits the application of chromium oxide coating in wide temperature range more simultaneously.
Summary of the invention
Main purpose of the present invention is to provide the technology of preparing all in a kind of room temperature to 800 DEG C of wide temperature ranges with the coated material of self-lubricating property.
Object of the present invention realizes by following technical scheme:
Room temperature is to a technology of preparing for 800 DEG C wide temperature range self-lubricating coat in use, and adopt the method preparation of arc ion plating, it is characterized in that the deposition process of the method coating completes in the vacuum cavity of the coating equipment being furnished with electric arc, concrete steps are:
A, activation clean surface: smooth, clean metal base is placed within cavity, vacuumizes 1.5 × 10 -2below Pa, passes into argon gas as ionization of gas, opens pulsed bias power supply, and glow discharge produces plasma body, carries out activation cleaning to substrate surface;
Prepared by B, transition layer: after cleaning, utilize the method first deposition chromium transition layer of arc ion plating, select chromium post target as arc ion plating target, using argon gas as ionization of gas, matrix adds negative bias, closes after deposition chromium transition layer;
C, deposited oxide chromiumcoating: it is still chromium post target that arc ion plating target is selected, then passes into oxygen, execute by controlling the throughput ratio of nitrogen and oxygen and electric current and substrate the structure that biased size controls coating;
D, coating aftertreatment: carry out anneal, then naturally cool to room temperature.
In step, metal base is selected from M2 rapid steel, Nickel-Based Steel, stainless steel or aluminium alloy, and plasma-activated process parameters range is: cavity air pressure 0.4 ~ 2.0Pa, bias voltage-100V ~-1000V.
In stepb, chromium transition layer 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, and O2/Ar throughput ratio is 1:5 ~ 5:1, sputtering current 1 ~ 200 A, pulsed bias-50 ~-500V, coat-thickness 0.5 ~ 5um.
In step D, parameter and annealing scope is: annealing temperature 200 ~ 1000 DEG C, heat-up rate 1 ~ 20 DEG C/min, and soaking time is 0.5 ~ 5h.
The main component of this film is Cr and Cr 2o 3, its section structure as shown in Figure 1.Cr transition layer is mainly in order to increase film and the bonding force of matrix within the scope of wide temperature range, and 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 adopts the method for arc ion plating to prepare chromium oxide coating.The method is compared with the chromium oxide coating adopting magnetron sputtering to prepare, chromium oxide coating prepared by arc ions electroplating method, add for complex sample around plating property, the bonding force of coating and substrate is stronger, the oxygen level of coating also increases, thus improves mechanical property, the antioxidant property and tribological property etc. of coating.Through investigating, the chromium oxide coating adopting arc ions electroplating method to prepare all has less frictional coefficient (0.15-0.4) and lower wear rate within the scope of room temperature to 800 DEG C of wide temperature ranges, especially at 800 DEG C of frictional coefficient about 0.15, wear rate is also 10 -7mm 3about/Nm.The mechanical property good in view of it and tribological property, chromium oxide coating can be applicable to the foil seal of aircraft engine, and gas bearing etc. are operated in room temperature to the fricting movement parts within the scope of 800 DEG C of wide temperature ranges.
Accompanying drawing explanation
Fig. 1 is Cr 2o 3the scanning electron microscope shape appearance figure of the section of film.
Fig. 2 is Cr 2o 3coating room temperature is to the frictional coefficient of 800 DEG C.
Embodiment
Embodiment 1:
A. sample pretreatment: the stainless steel distilled water, the acetone that are polished to minute surface are carried out ultrasonic cleaning 10 min respectively, dries up with nitrogen immediately, be placed in sediment chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10 -2below Pa, passing into high-purity argon gas to air pressure is 1.5 Pa.Open pulsed bias power supply, regulation voltage level is-500 V, carries out argon plasma Bombardment and cleaning 20min.
B. deposition chromium transition layer: regulate argon flow amount, make cavity air pressure maintain about 0.45Pa, open post arc power, adjustment electric current is 90A, and bias voltage is-200V, closes when transition layer deposits about 200nm.
C. deposited oxide layers of chrome: the mixed gas passing into high-purity argon gas and oxygen, chamber pressure is made to maintain about 0.45Pa, the throughput ratio controlling argon gas and oxygen is 1:2, open post arc power, adjustment electric current is 90A, bias voltage is-200V, cools after depositing about 2h, discharges vacuum begin to speak to sample when temperature is down to below 50 DEG C.
D. sample aftertreatment: sample is incubated 2h at 400 DEG C in retort furnace.
Embodiment 2:
A. sample pretreatment: the aluminium alloy distilled water, the acetone that are polished to minute surface are carried out ultrasonic cleaning 10 min respectively, dries up with nitrogen immediately, be placed in sediment chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10 -2below Pa, passing into high-purity argon gas to air pressure is 1.0 Pa.Open pulsed bias power supply, regulation voltage level is-400 V, carries out argon plasma Bombardment and cleaning 15min.
B. deposition chromium transition layer: regulate argon flow amount, make cavity air pressure maintain about 0.45Pa, open post arc power, adjustment electric current is 100A, and bias voltage is-300V, closes when transition layer deposits about 200nm.
C. deposited oxide layers of chrome: the mixed gas passing into high-purity argon gas and oxygen, chamber pressure is made to maintain about 0.45Pa, the throughput ratio controlling argon gas and oxygen is 1:1, open post arc power, adjustment electric current is 100A, bias voltage is-300V, cools after depositing about 2h, discharges vacuum begin to speak to sample when temperature is down to below 50 DEG C.
D. sample aftertreatment: sample is incubated 3h at 500 DEG C in retort furnace.
Embodiment 3:
A. sample pretreatment: the high-temperature steel distilled water, the acetone that are polished to minute surface are carried out ultrasonic cleaning 10 min respectively, dries up with nitrogen immediately, be placed in sediment chamber.Vacuum chamber internal gas pressure is evacuated to 1.5 × 10 -2below Pa, passing into high-purity argon gas to air pressure is 2.0 Pa.Open pulsed bias power supply, regulation voltage level is-700 V, carries out argon plasma Bombardment and cleaning 50min.
B. deposition chromium transition layer: regulate argon flow amount, make cavity air pressure maintain about 0.45Pa, open post arc power, adjustment electric current is 80A, and bias voltage is-400V, closes when transition layer deposits about 200nm.
C. deposited oxide layers of chrome: the mixed gas passing into high-purity argon gas and oxygen, chamber pressure is made to maintain about 0.45Pa, the throughput ratio controlling argon gas and oxygen is 2:1, open post arc power, adjustment electric current is 50A, bias voltage is-400V, cools after depositing about 2h, discharges vacuum begin to speak to sample when temperature is down to below 50 DEG C.
D. sample aftertreatment: sample is incubated 1h at 800 DEG C in retort furnace.

Claims (5)

1. room temperature is to a technology of preparing for 800 DEG C wide temperature range self-lubricating coat in use, and adopt the method preparation of arc ion plating, it is characterized in that the deposition process of the method coating completes in the vacuum cavity of the coating equipment being furnished with electric arc, concrete steps are:
A, activation clean surface: smooth, clean metal base is placed within cavity, vacuumizes 1.5 × 10 -2below Pa, passes into argon gas as ionization of gas, opens pulsed bias power supply, and glow discharge produces plasma body, carries out activation cleaning to substrate surface;
Prepared by B, transition layer: after cleaning, utilize the method first deposition chromium transition layer of arc ion plating, select chromium post target as arc ion plating target, using argon gas as ionization of gas, matrix adds negative bias, closes after deposition chromium transition layer;
C, deposited oxide chromiumcoating: it is still chromium post target that arc ion plating target is selected, then passes into oxygen, execute by controlling the throughput ratio of nitrogen and oxygen and electric current and substrate the structure that biased size controls coating;
D, coating aftertreatment: carry out anneal, then naturally cool to room temperature.
2. the method for claim 1, it is characterized in that, in step, metal base is selected from M2 rapid steel, Nickel-Based Steel, stainless steel or aluminium alloy, plasma-activated process parameters range is: cavity air pressure 0.4 ~ 2.0Pa, bias voltage-100V ~-1000V.
3. the method for claim 1, is characterized in that, in stepb, chromium transition layer 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.
4. the method for claim 1, is characterized in that, in step C, chromium oxide layer process parameters range is: cavity air pressure 0.2 ~ 1.0Pa, and O2/Ar throughput ratio is 1:5 ~ 5:1, sputtering current 1 ~ 200 A, pulsed bias-50 ~-500V, coat-thickness 0.5 ~ 5um.
5. the method for claim 1, is characterized in that, in step D, parameter and annealing scope is: annealing temperature 200 ~ 1000 DEG C, heat-up rate 1 ~ 20 DEG C/min, and soaking 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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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106811725A (en) * 2015-11-27 2017-06-09 中国科学院宁波材料技术与工程研究所 Temperature range self adaptation lubricant coating wide and preparation method and application
CN110983275A (en) * 2019-12-25 2020-04-10 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
CN111334769A (en) * 2020-04-02 2020-06-26 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
CN111534799A (en) * 2020-05-29 2020-08-14 四川大学 Oxidation-resistant and heat-insulating ceramic coating and preparation method thereof
CN112610608A (en) * 2020-11-26 2021-04-06 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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US3535006A (en) * 1969-01-29 1970-10-20 Kaman Aerospace Corp Bearing construction
CN1506492A (en) * 2002-12-06 2004-06-23 中国科学院金属研究所 Chromium oxide coating preparing process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3535006A (en) * 1969-01-29 1970-10-20 Kaman Aerospace Corp Bearing construction
CN1506492A (en) * 2002-12-06 2004-06-23 中国科学院金属研究所 Chromium oxide coating preparing process

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106811725A (en) * 2015-11-27 2017-06-09 中国科学院宁波材料技术与工程研究所 Temperature range self adaptation lubricant coating wide and preparation method and application
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
CN110983275A (en) * 2019-12-25 2020-04-10 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
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
CN111334769A (en) * 2020-04-02 2020-06-26 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
CN111534799A (en) * 2020-05-29 2020-08-14 四川大学 Oxidation-resistant and heat-insulating ceramic coating and preparation method thereof
CN112610608A (en) * 2020-11-26 2021-04-06 东南大学 Wide-temperature-range self-lubricating bearing 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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