CN105483595A - Inorganic coating with lower thermal expansion coefficient and preparing method of inorganic coating - Google Patents
Inorganic coating with lower thermal expansion coefficient and preparing method of inorganic coating Download PDFInfo
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- CN105483595A CN105483595A CN201510783584.9A CN201510783584A CN105483595A CN 105483595 A CN105483595 A CN 105483595A CN 201510783584 A CN201510783584 A CN 201510783584A CN 105483595 A CN105483595 A CN 105483595A
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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Abstract
The invention relates to an inorganic coating with a lower thermal expansion coefficient and a preparing method of the inorganic coating. Polyacrylonitrile/carbon nanotube conductive fibers and Mo-ZrC composite powder are adopted in the coating to serve as raw materials, and are sprayed to a metal base body, so that the coating is obtained. According to the inorganic coating, the mechanical property of the coating can be improved, the lower thermal expansion coefficient is reduced, and the coating has the characteristic of being capable of keeping high friction coefficients; and meanwhile, the wear rate can be reduced, and therefore the service life of the coating is prolonged.
Description
Technical field
The present invention relates to field of material technology, particularly relate to a kind of inorganic coating with low thermal coefficient of expansion and preparation method thereof.
Background technology
Wear-resistant coating, as a kind of means of surface modification, can give the wear resisting property of body material excellence, extends its work-ing life.Therefore, the research of wear-resistant coating gets more and more people's extensive concerning always.Abrasion-resistant coating material requires low-friction coefficient usually, but some certain applications needs great friction coefficient coated material, as automobile synchronizer etc.Synchronizer is one of vitals of automobile gearbox, effectively can reduce the vibrations in automobile gear shift process, impact and noise, thus improves the stability of automobile operation and the security of traveling.The friction materials changing synchronizer structure and the synchronizer conical surface is the main means improving synchronizer performance.For guaranteeing the serviceability that wheel box is good, require that synchronizer friction lining material has the high and over-all properties such as stable frictional coefficient, good wear resistance, high temperature resistant, excellent resistance to shock loads ability.
Metal molybdenum (Mo) has the features such as the thermal shock resistance of anticorrosive, resistance to adhesive wear, high thermal conductivity, low-expansion coefficient and excellence, is often used to the tribological property improving speed reduction unit synchronous ring, internal-combustion engine piston ring.At present, the technique preparing molybdenum coating has detonation flame spraying, flame plating and plasma spraying etc.Explosive spray coating technique is more complicated, and this method prepares molybdenum coating rarely seen laboratory report.What industrial application was more is oxy-acetylene flame line-material coating method, and the method equipment is simple, but prepared molybdenum coating porosity is comparatively large, and coat inside, in conjunction with poor, causes that its wear resisting property reduces, work-ing life is partially short.Mo belongs to metallic substance, is easy to carry out mechanical workout, but simultaneously its hardness lower (1500MPa-1600MPa), cause its abrasion resistance properties to reduce, work-ing life is shorter.In molybdenum coating, add ceramic composition, be conducive to improving its wear resisting property.
Plasma spraying coating has the features such as porosity is low, bonding strength is high, spraying raw material is powder, spray material scope is wide.Existing research employing plasma spraying method has prepared the plasma spraying molybdenum alloy coat for automobile synchronizer at present, and have studied interpolation alloying element to the impact of its wear resisting property.
Zirconium carbide (ZrC), there is the features such as high rigidity (25.5GPa), high-melting-point (3420 DEG C) and good chemical stability, studiedly be applied to various severe rugged environment, as as abrasive material, for the processing of Wimet, corundum or glass, and the coating material etc. of fuel pellet in aerospace high temperature material and nuclear reaction.
CN104651770A discloses a kind ofly has inorganic coating of great friction coefficient and low wear rate and preparation method thereof, and described coating adopts Mo-ZrC composite granule to be raw material, and spraying obtains on metal base, and in described coating, ZrC content is 10 ~ 80vol.%.This coating can keep the feature of great friction coefficient, reduces its wear rate simultaneously, thus extends its work-ing life.But this coating still haves much room for improvement in mechanical property and hot expansibility.
Therefore, how to research and develop and a kind ofly there is great friction coefficient and low wear rate and there is excellent mechanical property, and the inorganic coating with lower thermal expansivity is current emphasis.
Summary of the invention
For solving deficiency of the prior art, the present invention, by each component in adjustment inorganic coating, improves each performance of coating, makes it while having great friction coefficient and low wear rate, also has excellent mechanical property, and has lower thermal expansivity.
For reaching this object, present invention employs following technical scheme:
First aspect, the invention provides a kind of inorganic coating, and described coating contains polyacrylonitrile/carbon nanotube conducting fiber and Mo-ZrC composite granule.
The present invention is by the basis of the coating containing Mo-ZrC composite granule, add polyacrylonitrile/carbon nanotube conducting fiber again, wherein Mo-ZrC composite granule and polyacrylonitrile/carbon nanotube conducting fiber two kinds component can play synergistic function, its coating has excellent mechanical property, and reduces thermal expansivity.
Preferably, in coating of the present invention, the massfraction of polyacrylonitrile/carbon nanotube conducting fiber is 60-80%, such as, can be 60%, 65%, 68%, 70%, 72%, 75%, 80%; The massfraction of described Mo-ZrC composite granule is 20-40%, such as, can be 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38%, 40%.Wherein, in described Mo-ZrC composite granule, the mass ratio of Mo powder and ZrC powder is 3-5:1-4, is preferably 3:1.
In the present invention, described coat-thickness is 200-1000 μm, such as, can be 200 μm, 400 μm, 600 μm, 800 μm, 1000 μm, is preferably 300-600 μm.
Second aspect, present invention also offers the preparation method of the inorganic coating described in first aspect, comprises the following steps:
(1) polyacrylonitrile/carbon nanotube conducting fiber is prepared;
(2) after polyacrylonitrile/carbon nanotube conducting fiber step (1) obtained and Mo powder and ZrC powder Homogeneous phase mixing, as raw material;
(3) adopt plasma spraying method, raw material is sprayed on base material, obtains described coating.
In the present invention, described metal base comprises stainless steel.
In the present invention, described Mo powder, ZrC powder realize Homogeneous phase mixing by mechanical attrition method; Preferably, the particle diameter of described Mo powder is 50-100 μm, and purity is greater than 95wt%; The particle diameter of ZrC powder is 10-100 μm, and purity is greater than 95wt%.
In the present invention, described polyacrylonitrile/carbon nanotube conducting fiber adopts following methods to obtain: after using the mixing solutions of the vitriol oil and concentrated nitric acid that multi-walled carbon nano-tubes is carried out functionalization, with polyacrylonitrile blended, adopt wet-formed method to prepare.
Particularly, described polyacrylonitrile/carbon nanotube conducting fiber adopts following methods to obtain:
(1) functionalization of carbon nanotube: the diameter of raw material multi-walled carbon nano-tubes used is 40-60nm, and length is 0.5-500 μm, and purity is greater than 95%; Take a certain amount of multi-walled carbon nano-tubes and put into reactor, the mixed solution of the vitriol oil of 98% and the concentrated nitric acid of 70% is added under vigorous stirring, put into constant temperature oil bath reflux 1-3h take out, repeatedly rinse with deionized water, finally gained black solid be placed in vacuum drying oven in 40-50 DEG C of drying.
(2) preparation of polyacrylonitrile/carbon nanotube spinning solution:
By through functionalization or immerse in DMF solvent without the carbon nanotube of functionalization and polyacrylonitrile, make it fully swelling, then heat up, stir, polyacrylonitrile is dissolved, maintenance total solid content is 10-20%, obtain the blend solution of content of carbon nanotubes, then by this solution ultrasonic irradiation 10-30min, make carbon nanotube dispersed under hyperacoustic effect, finally by filtration under diminished pressure, vacuum defoamation, obtained co-blended spinning stoste.
(3) preparation of polyacrylonitrile/carbon nanotube conducting fiber
On the wet-formed equipment of conventional lab scale, by co-blended spinning solution after filtering, measuring, the precipitation bath be made up of solvent DMF and water is clamp-oned by orifice, wherein the content of DMF solvent is 50%, wire drawing multiple is 7 times, then through washing, oiling, dry heat sizing and rolling step, make polyacrylonitrile/carbon nanofiber.
At present, carbon nano-tube fibre and/or polyacrylonitrile are all the conductivities for improving co-mixing system, but, the present invention is by adding in inorganic paint by polyacrylonitrile/carbon nano-tube fibre, by playing synergistic function with Mo-ZrC composite granule, its coating is but provided with excellent mechanical property, and reduces thermal expansivity.
In the present invention, the processing parameter of described plasma spraying comprises: plasma gas Ar:30-50slpm; Plasma gas H2:5-20slpm, preferred 8-18slpm; Powder carrier gas Ar:1.5-5slpm; Spray distance: 80-350mm, preferred 80-250mm; Spray power: 30-58KW; Powder feeding rate: 6-30r/ minute; Spray pressure: 100-800mbar.
Compared with prior art, the present invention at least has following beneficial effect:
(1) polyacrylonitrile/carbon nano-tube fibre adds in inorganic paint by the present invention, and by playing synergistic function with Mo-ZrC composite granule, its coating is but provided with excellent mechanical property, and reduces thermal expansivity.
(2) coating of the present invention can keep the feature of great friction coefficient, reduces beyond its wear rate simultaneously, also has excellent erosion resistance.
Embodiment
Following embodiment further illustrates the present invention, should be understood that following embodiment is only for illustration of the present invention, and unrestricted the present invention.
Enumerate embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
In the present embodiment, the massfraction of polyacrylonitrile/carbon nanotube conducting fiber is 65%; The massfraction of Mo-ZrC composite granule is 35%, and wherein, the mass ratio of Mo powder and ZrC powder is 3:1.
The concrete preparation method of coating is as follows:
(1) polyacrylonitrile/carbon nanotube conducting fiber is prepared:
The functionalization of (a) carbon nanotube: the diameter of raw material multi-walled carbon nano-tubes used is 40-60nm, and length is 0.5-500 μm, and purity is greater than 95%; Take a certain amount of multi-walled carbon nano-tubes and put into reactor, the mixed solution of the vitriol oil of 98% and the concentrated nitric acid of 70% is added under vigorous stirring, put into constant temperature oil bath reflux 1h take out, repeatedly rinse with deionized water, finally gained black solid be placed in vacuum drying oven in 50 DEG C of dryings.
The preparation of (b) polyacrylonitrile/carbon nanotube spinning solution:
By through functionalization or immerse in DMF solvent without the carbon nanotube of functionalization and polyacrylonitrile, make it fully swelling, then heat up, stir, polyacrylonitrile is dissolved, total solid content is kept to be 20%, obtain the blend solution of content of carbon nanotubes, then by this solution ultrasonic irradiation 30min, make carbon nanotube dispersed under hyperacoustic effect, finally by filtration under diminished pressure, vacuum defoamation, obtained co-blended spinning stoste.
The preparation of (c) polyacrylonitrile/carbon nanotube conducting fiber
On the wet-formed equipment of conventional lab scale, by co-blended spinning solution after filtering, measuring, the precipitation bath be made up of solvent DMF and water is clamp-oned by orifice, wherein the content of DMF solvent is 50%, wire drawing multiple is 7 times, then through washing, oiling, dry heat sizing and rolling step, make polyacrylonitrile/carbon nanofiber.
(2), after polyacrylonitrile/carbon nanotube conducting fiber step (1) obtained and Mo powder and ZrC powder Homogeneous phase mixing, as raw material, wherein the preparation method of Mo-ZrC composite granule is as follows:
Be that 40% to take particle diameter be respectively the Mo powder of 10-100 μm and particle diameter is the ZrC powder of 10 ~ 80 μm by ZrC volume content, mechanically mixing in whirling vibration ball mill, ball grinder speed of rotation is set as 150rpm (rpm), ratio of grinding media to material (mass ratio) is 2:1, ball milling is after 3 hours, take off ball grinder, composite granule sieves for subsequent use through 80 orders.
(3) pre-treatment is carried out to stainless steel substrate: the stainless steel disk base material (Ф 60mm × 8mm) after sandblasting (sandblasting pressure is about 0.2MPa) process is placed in ethanol solution ultrasonic 5 minutes, dry for standby; Using plasma spraying technology, equipment is the A-2000 plasma spray system of SulzerMetro company (Switzerland), the S3 type mechanical manipulator composition that this system is produced primarily of F4-MB type spray gun and ABB AB (U.S.), powder feeder is the two powder feed system of Twin-10 type.Coating prepared by stainless steel disk base material after treatment, and the plasma spray process parameter of employing is as follows: plasma gas Ar flow is 32slpm; Plasma gas H2 flow is 16slpm; Powder carrier gas Ar flow is 5slpm; Spray distance is 140mm; Rate of feed is 25r/min; Spray power is 32kW.
Embodiment 2
In the present embodiment, the massfraction of polyacrylonitrile/carbon nanotube conducting fiber is 80%; The massfraction of Mo-ZrC composite granule is 20%, and wherein, the mass ratio of Mo powder and ZrC powder is 3:1.
The concrete preparation method of coating is as follows:
(1) polyacrylonitrile/carbon nanotube conducting fiber is prepared:
The functionalization of (a) carbon nanotube: the diameter of raw material multi-walled carbon nano-tubes used is 40-60nm, and length is 0.5-500 μm, and purity is greater than 95%; Take a certain amount of multi-walled carbon nano-tubes and put into reactor, the mixed solution of the vitriol oil of 98% and the concentrated nitric acid of 70% is added under vigorous stirring, put into constant temperature oil bath reflux 1h take out, repeatedly rinse with deionized water, finally gained black solid be placed in vacuum drying oven in 50 DEG C of dryings.
The preparation of (b) polyacrylonitrile/carbon nanotube spinning solution:
By through functionalization or immerse in DMF solvent without the carbon nanotube of functionalization and polyacrylonitrile, make it fully swelling, then heat up, stir, polyacrylonitrile is dissolved, total solid content is kept to be 20%, obtain the blend solution of content of carbon nanotubes, then by this solution ultrasonic irradiation 30min, make carbon nanotube dispersed under hyperacoustic effect, finally by filtration under diminished pressure, vacuum defoamation, obtained co-blended spinning stoste.
The preparation of (c) polyacrylonitrile/carbon nanotube conducting fiber
On the wet-formed equipment of conventional lab scale, by co-blended spinning solution after filtering, measuring, the precipitation bath be made up of solvent DMF and water is clamp-oned by orifice, wherein the content of DMF solvent is 50%, wire drawing multiple is 7 times, then through washing, oiling, dry heat sizing and rolling step, make polyacrylonitrile/carbon nanofiber.
(2), after polyacrylonitrile/carbon nanotube conducting fiber step (1) obtained and Mo powder and ZrC powder Homogeneous phase mixing, as raw material, wherein the preparation method of Mo-ZrC composite granule is as follows:
Be that 40% to take particle diameter be respectively the Mo powder of 10-100 μm and particle diameter is the ZrC powder of 10 ~ 80 μm by ZrC volume content, mechanically mixing in whirling vibration ball mill, ball grinder speed of rotation is set as 150rpm (rpm), ratio of grinding media to material (mass ratio) is 2:1, ball milling is after 3 hours, take off ball grinder, composite granule sieves for subsequent use through 80 orders.
(3) pre-treatment is carried out to stainless steel substrate: the stainless steel disk base material (Ф 60mm × 8mm) after sandblasting (sandblasting pressure is about 0.2MPa) process is placed in ethanol solution ultrasonic 5 minutes, dry for standby; Using plasma spraying technology, equipment is the A-2000 plasma spray system of SulzerMetro company (Switzerland), the S3 type mechanical manipulator composition that this system is produced primarily of F4-MB type spray gun and ABB AB (U.S.), powder feeder is the two powder feed system of Twin-10 type.Coating prepared by stainless steel disk base material after treatment, and the plasma spray process parameter of employing is as follows: plasma gas Ar flow is 32slpm; Plasma gas H2 flow is 16slpm; Powder carrier gas Ar flow is 5slpm; Spray distance is 140mm; Rate of feed is 25r/min; Spray power is 32kW.
Comparative example 1
Preparation Mo-ZrC composite granule:
Be that 40% to take particle diameter be respectively the Mo powder of 10-100 μm and particle diameter is the ZrC powder of 10 ~ 80 μm by ZrC volume content, mechanically mixing in whirling vibration ball mill, ball grinder speed of rotation is set as 150rpm (rpm), and ratio of grinding media to material (mass ratio) is 2:1.Ball milling, after 3 hours, takes off ball grinder, and composite granule sieves for subsequent use through 80 orders.
Preparation coating:
1) pre-treatment is carried out to stainless steel substrate: the stainless steel disk base material (Ф 60mm × 8mm) after sandblasting (sandblasting pressure is about 0.2MPa) process is placed in ethanol solution ultrasonic 5 minutes, dry for standby;
2) using plasma spraying technology, equipment is the A-2000 plasma spray system of SulzerMetro company (Switzerland), the S3 type mechanical manipulator composition that this system is produced primarily of F4-MB type spray gun and ABB AB (U.S.), powder feeder is the two powder feed system of Twin-10 type.Coating prepared by stainless steel disk base material after treatment, and the plasma spray process parameter of employing is as follows: plasma gas Ar flow is 32slpm; Plasma gas H2 flow is 16slpm; Powder carrier gas Ar flow is 5slpm; Spray distance is 140mm; Rate of feed is 25r/min; Spray power is 32kW; The powder sprayed is obtained Mo-ZrC composite granule.
As shown in table 1 by embodiment 1-2 and comparative example 1 are obtained Volume erosion rate (W) respectively in low load 20N situation, and it has been carried out respectively to the mensuration of thermal expansion size changing rate and elongation at break.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative example 1 | |
| Volume erosion rate (10 -3mm/N·m) | 0.89±0.13 | 0.85±0.0.9 | 1.33±0.12 |
| Thermal expansion size changing rate (50-260 DEG C) | 1.8％ | 2.5％ | 3.0％ |
| Elongation at break/% | 180 | 158 | 139 |
Can be found out by the above results, the present invention is by the composition of adjustment inorganic coating, by increasing polyacrylonitrile/carbon nanotube conducting fiber, compare and adopt Mo-ZrC compound coating separately, except keeping the feature of great friction coefficient, reduce beyond its wear rate, it also has excellent mechanical property, and has lower thermal expansivity simultaneously.
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (7)
1. an inorganic coating, is characterized in that, described coating contains polyacrylonitrile/carbon nanotube conducting fiber and Mo-ZrC composite granule.
2. inorganic coating according to claim 1, is characterized in that, in described coating, the massfraction of polyacrylonitrile/carbon nanotube conducting fiber is the massfraction of 60-80%, Mo-ZrC composite granule is 20-40%.
3. inorganic coating according to claim 1 and 2, is characterized in that, described coat-thickness is 200-1000 μm, is preferably 300-600 μm.
4. the preparation method of the inorganic coating according to any one of claim 1-3, is characterized in that, comprises the following steps:
(1) polyacrylonitrile/carbon nanotube conducting fiber is prepared;
(2) after polyacrylonitrile/carbon nanotube conducting fiber step (1) obtained and Mo powder and ZrC powder Homogeneous phase mixing, as raw material;
(3) adopt plasma spraying method, raw material is sprayed on base material, obtains described coating.
5. method according to claim 4, is characterized in that, the particle diameter of described Mo powder is 50-100 μm, and purity is greater than 95wt%; The particle diameter of ZrC powder is 10-100 μm, and purity is greater than 95wt%.
6. method according to claim 4, it is characterized in that, described polyacrylonitrile/carbon nanotube conducting fiber adopts following methods to obtain: after using the mixing solutions of the vitriol oil and concentrated nitric acid that multi-walled carbon nano-tubes is carried out functionalization, with polyacrylonitrile blended, wet-formed method is adopted to prepare.
7. method according to claim 4, is characterized in that, the processing parameter of described plasma spraying comprises: plasma gas Ar:30-50slpm; Plasma gas H2:5-20slpm, preferred 8-18slpm; Powder carrier gas Ar:1.5-5slpm; Spray distance: 80-350mm, preferred 80-250mm; Spray power: 30-58KW; Powder feeding rate: 6-30r/ minute; Spray pressure: 100-800mbar.
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| CN106480397A (en) * | 2016-10-21 | 2017-03-08 | 过冬 | A kind of have inorganic coating of low thermal coefficient of expansion and preparation method thereof |
| CN107141975A (en) * | 2017-06-26 | 2017-09-08 | 俞秀英 | A kind of antibacterial is except methanal paint and preparation method thereof |
| CN107435129A (en) * | 2017-06-29 | 2017-12-05 | 顾渊 | A kind of inorganic coating and preparation method thereof |
| RU2756355C1 (en) * | 2020-11-05 | 2021-09-29 | Федеральное государственное унитарное предприятие «Всероссийский научно-исследовательский институт автоматики им.Н.Л.Духова» (ФГУП «ВНИИА») | Method for applying a thin-film polyacrylonitrile-based coating |
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Application publication date: 20160413 |