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 PDFInfo
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- 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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- ion plating
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- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 26
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 14
- 238000007733 ion plating Methods 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 25
- 229910052786 argon Inorganic materials 0.000 claims description 19
- 239000011651 chromium Substances 0.000 claims description 18
- 230000007704 transition Effects 0.000 claims description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052804 chromium Inorganic materials 0.000 claims description 15
- 238000000151 deposition Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910001256 stainless steel alloy Inorganic materials 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- 229910001311 M2 high speed steel Inorganic materials 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 238000000678 plasma activation Methods 0.000 claims 1
- 239000013077 target material Substances 0.000 claims 1
- 239000011888 foil Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- 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
本发明公开了一种室温到800℃宽温域自润滑涂层的制备技术。本发明采用电弧离子镀的方法制备氧化铬涂层，制备的氧化铬涂层在室温到800℃宽温域范围内均具有较小的摩擦系数（0.15-0.4）和较低的磨损率，尤其是在800℃摩擦系数在0.15左右，磨损率也在10-7mm3/Nm左右。鉴于其良好的机械性能和摩擦学性能，氧化铬涂层可应用于航空发动机的箔片密封，气体轴承等工作在室温到800℃宽温域范围内的摩擦运动部件。The invention discloses a preparation technology of a self-lubricating coating in a wide temperature range from room temperature to 800°C. The present invention adopts the method of arc ion plating to prepare chromium oxide coating, and the prepared chromium oxide coating has a small friction coefficient (0.15-0.4) and a low wear rate in a wide temperature range from room temperature to 800°C, especially The friction coefficient is about 0.15 at 800°C, and the wear rate is about 10 -7 mm 3 /Nm. In view of its good mechanical properties and tribological properties, chromium oxide coatings can be applied to foil seals of aeroengines, gas bearings and other frictional moving parts that work in a wide temperature range from room temperature to 800 °C.
Description
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)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310274061.2A CN104278234B (en) | 2013-07-02 | 2013-07-02 | Preparation technology for self-lubricating coating with wide temperature range of room temperature to 800 DEG C |
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|---|---|---|---|
| CN201310274061.2A CN104278234B (en) | 2013-07-02 | 2013-07-02 | Preparation technology for self-lubricating coating with wide temperature range of room temperature to 800 DEG C |
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| CN104278234A true CN104278234A (en) | 2015-01-14 |
| CN104278234B CN104278234B (en) | 2017-02-22 |
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Cited By (8)
| 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 | A kind of PbO-Cr2O3 co-doped thin film and its preparation method and application |
| CN111534799A (en) * | 2020-05-29 | 2020-08-14 | 四川大学 | A kind of anti-oxidation and thermal insulation 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 |
| CN118497675A (en) * | 2024-07-22 | 2024-08-16 | 苏州芯合半导体材料有限公司 | Riving knife coating and preparation method thereof |
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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 | A kind of chromium oxide coating preparation technology |
-
2013
- 2013-07-02 CN CN201310274061.2A patent/CN104278234B/en active Active
Patent Citations (2)
| 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 | A kind of chromium oxide coating preparation technology |
Cited By (11)
| 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 temperature range adaptive lubricating coating and its preparation method and application |
| 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 | A kind of PbO-Cr2O3 co-doped thin film and its preparation method and application |
| CN111534799A (en) * | 2020-05-29 | 2020-08-14 | 四川大学 | A kind of anti-oxidation and thermal insulation 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 | A kind of 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 |
| CN118497675A (en) * | 2024-07-22 | 2024-08-16 | 苏州芯合半导体材料有限公司 | Riving knife coating and preparation method thereof |
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| CN104278234B (en) | 2017-02-22 |
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