CN107034428B - A kind of ceramic coatings organic matter composite powder and its spraying method suitable for spraying - Google Patents

A kind of ceramic coatings organic matter composite powder and its spraying method suitable for spraying Download PDF

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CN107034428B
CN107034428B CN201710278049.7A CN201710278049A CN107034428B CN 107034428 B CN107034428 B CN 107034428B CN 201710278049 A CN201710278049 A CN 201710278049A CN 107034428 B CN107034428 B CN 107034428B
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powder
organic matter
spraying
ceramic
coating
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CN107034428A (en
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董艳春
路项媛
李延彬
关少康
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Hebei University of Technology
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Hebei University of Technology
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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
    • C23C4/06—Metallic material
    • C23C4/08—Metallic material containing only metal elements
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C09D127/18—Homopolymers or copolymers of tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
    • C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
    • C09D161/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Inorganic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Abstract

The present invention is a kind of ceramic coatings organic matter composite powder and its spraying method suitable for spraying.The composite powder is made by following methods：(1) ceramic slurry and organic slurry are mixed together, stirs 2~3 hours, obtains uniformly mixed composite powder slurry；Wherein, quality proportioning is ceramic powders：Organic matter powder=9:1~7:1；The particle size range of ceramic powders is 30nm~5 μm；Organic matter is PEEK or PTFE；The particle size range of organic matter powder is 20~40 μm；(2) the organic composite powder of ceramic coatings is prepared with the method for mist projection granulating；(3) dry solid ceramic cladding organic matter composite powder is screened, filters out the powder that size is -200~+300 purposes.Ceramics made from coated composite powder through the invention-organic matter composite coating has good wearability and corrosion resistance, meanwhile, realize the self-lubrication of coating.

Description

A kind of ceramic coatings organic matter composite powder and its spraying method suitable for spraying
Technical field
The present invention relates to a kind of methods that ceramic coated cladding organic matter composite powder prepares self-lubricating composite coating, especially relate to And a kind of ceramic coatings organic matter dusty spray suitable for spraying, and the preparation side with wear-resisting, corrosion resistance composite coating Method.The invention belongs to wear resistant corrosion resistant coatings arts.
Background technique
Ceramic material not only has high intensity, high rigidity, high-melting-point, high chemical stability, good thermal conductivity, low rubs The advantages that wiping coefficient, but also have many advantages, such as excellent wearability, corrosion resistance, heat resistance.The disadvantage is that brittleness is big, it is difficult to Prepare large-size ceramic structural member.Strength of Metallic Materials height, good toughness, wearability are good, but electrification easily occurs in saline-alkali environment It learns corrosion and fails；Organic resin material is corrosion-resistant, wear-resisting, good toughness, degradable, but intensity is low.Using single variety material Material is difficult to meet the use demand in this complex environment in ocean.Therefore, it prepares a kind of by the high-wearing feature of ceramics and organic Combined ceramics-the organic composite coating of the good toughness of object, corrosion resistance has greatly warp to protection metallic matrix Meaning of helping and scientific value.
Plasma spraying temperature is high, is particularly suitable for preparing the coating of materials with high melting point, is current oxide ceramics and nitridation A kind of the most frequently used and most effective method in the preparation of object ceramic coating and research.Plasma spraying has simple process, flexibly side Just, workpiece is without the characteristics of redesigning.Reaction and plasma spraying integrates plasma spraying and self- propagating technology, preparation It is high-efficient at low cost, it is suitable for various sizes piece surface.But since plasma arc temperature is very high, higher than point of organic matter Temperature is solved, plasma spraying machinery hybrid ceramic-organic matter powder is easy to cause the carbonization of the organic matter in spraying process.Therefore, The composite powder for studying a kind of ceramic coatings organic matter suitable for spraying, make its ceramics in spraying process can melt and The degradation that will cause organic matter is particularly important.
Summary of the invention
Technical purpose of the invention is that abrasion and Anticorrosion cannot be solved simultaneously for above-mentioned homogenous material, provides A kind of ceramic coatings organic matter composite powder and ceramics-organic matter composite coating suitable for spraying.The present invention passes through to ceramic powders Ceramic packet is prepared for spray granulation after mixing under the action of appropriate dispersing agent and binder with the selection of organic matter Organic matter composite powder is covered, is finally prepared for ceramics-organic matter composite coating on metallic matrix with the method for plasma spraying again, And then improve the wearability and corrosion resistance of matrix.
The technical scheme is that：
A kind of ceramic coatings organic matter composite powder suitable for spraying, which is made by following methods, including following step Suddenly：
(1) preparation of ceramic slurry：Deionized water is added in ceramic powders, stirs, dispersing agent is then added, is continued Stirring；Binder is added, obtains ceramic powder slurry after finally agitated；
Wherein, the quality of dispersing agent is the 0.9%~1.1% of ceramic powders quality, and the quality of deionized water is ceramic powder The 5/6~10/9 of last quality, binder quality are the 5/9~2/3 of ceramic powders quality；
(2) preparation of organic slurry：Dehydrated alcohol is poured into organic matter powder, stirring dissolves organic matter powder Afterwards, dispersing agent is added, continues to stir, binder is eventually adding, obtains organic slurry after stirring；
Wherein, the quality of the dispersing agent in this step is the 0.9%~1.1% of organic matter powder；The quality of dehydrated alcohol It is the 3/5~1 of organic matter quality, binder quality is the 1/4~1/5 of organic matter；
(3) two kinds of slurries are mixed together, is stirred for 2~3 hours, obtain uniformly mixed composite powder slurry；
Wherein, quality proportioning is ceramic powders：Organic matter powder=9:1~7:1；
The binder is stirred 40~45 minutes under the conditions of 95 DEG C by thickener and deionized water and is prepared, quality Than for thickener：Deionized water=1：100；The thickener is sodium cellulose glycolate；
Ceramics are preferably Al2O3、TiN、BN、ZrO2、Cr2O3Or Nb2O5, the particle size range of ceramic powders is 30nm~5 μm；
Organic matter is preferably PEEK (polyether-ether-ketone), PTFE (polytetrafluoroethylene (PTFE))；The particle size range of organic matter powder is 20 ~40 μm；
The dispersing agent is preferably sodium polyphosphate；
(4) the organic composite powder of ceramic coatings is prepared with the method for mist projection granulating；Using air-flowing type spray granulation plant, Mist projection granulating parameter is set as：260 DEG C~300 DEG C of inlet air temperature, 110 DEG C~130 DEG C of leaving air temp, atomizer frequency is 100 ~110Hz, nozzle air current amount pressure control between 0.08-0.1MPa, wriggling revolution speed 35-40r/min, and charging revolution speed is 30~40r/min, charging rate are controlled in 10~14ml/min；It introduces the slurry into, finally obtains dry solid ceramic cladding Organic matter composite powder；
(5) dry solid ceramic cladding organic matter composite powder is screened, filter out size be -200~+ The powder of 300 purposes；
The spraying method of the ceramic coatings organic matter composite powder for being suitable for spraying, includes the following steps：
(1) matrix specimen surface is pre-processed；
(2) Ni-10%wtAl self-melting alloy powder is sprayed in advance in matrix surface, obtain with a thickness of 80~120 μm Bond coating；The matrix is metal material；
(3) ceramic coatings organic matter composite powder is put into powder feeder, matrix is sprayed to using the method for plasma spraying Surface, obtains ceramics-organic matter composite coating, coating with a thickness of 300-500 μm；
Wherein, spray parameters are set as：400~500A of operating current；50~60V of arc voltage；Argon flow 40~ 60L/min, 0.6~0.8MPa of pressure；7~10L/min of nitrogen flow, 0.6~0.8MPa of pressure；2~5L/min of powder feeding rate； 80~110mm of spray distance；Spray angle is 90 °；Spray gun scanning speed is 0.005~0.007m/s；Wherein nitrogen is used as and send Powder gas, argon gas is as protection gas.
The metal material is specially 45# steel, Q235 or Q345.
The beneficial effects of the invention are as follows：The present invention provides a kind of ceramic coatings organic matter dusty sprays, utilize plasma The powder spray is formed ceramics-organic matter composite coating by spraying technology after metal base surface.It is embodied in：
(1) ceramics-organic matter composite coating does not limit certain specific ceramics and organic matter.
(2) the ceramic coatings organic matter composite powder is that have good sphericity, ceramic powder as made from spray granulation End is coated on organic matter surface, avoids the degradation under hot conditions of the organic matter in spraying process.
(3) composite coating of this method preparation avoids the degradation of organic matter and organic compared with mechanical mixture powder-feeding method The problem of object is unevenly distributed in ceramic coating.Organic matter is evenly distributed in ceramic coating, both shows ceramic coating Excellent wearability, corrosion resistance, and the advantage of the good toughness of organic matter has been played, realize the self-lubrication of composite coating. By taking embodiment 1 as an example, under the conditions of load is 20N, Al2O3The abrasion loss of-PEEK composite coating and single Al2O3The mill of coating Damage amount is compared, and reduces 37%.When load is 30N, 20% is reduced.It is compound from 0.68 to be reduced to 0.58. for coefficient of friction simultaneously The corrosion potential of coating is by single Al2O3- the 501.9mV of coating is increased to -592.6mV, and corrosion electric current density is by 13.92 μ A cm-2It is reduced to 7.31/ μ Acm-2。
(4) this method prepares composite coating and is made by reaction and plasma spraying method, in typical layer structure and some Coating is in nano-scale, and coating combines comparatively dense, and porosity is low (SEM photograph can illustrate).The presence of organic matter can releive The stress that molten state ceramics generate in cooling procedure reduces the generation of crackle.
In conclusion ceramics provided by the present invention-organic matter composite coating has good wearability and corrosion resistance. Meanwhile also achieving the self-lubrication of coating.The composite coating is suitable under abrasion, corrosion working conditions, such as various seas Means of transport, conveys under various types of naval ship waters and storage facilities, the fields such as coastal facility, before extremely wide application Scape.
Detailed description of the invention
Fig. 1 is Al in the embodiment of the present invention 12O3The SEM of/PEEK coated composite powder schemes；
Fig. 2 is Al in the embodiment of the present invention 12O3The SEM figure of/PEEK coated composite powder scratched；
Fig. 3 is plasma spraying Al in the embodiment of the present invention 12O3The SEM of-PEEK composite coating schemes；
Fig. 4 is plasma spraying Al in the embodiment of the present invention 12O3The XRD diffracting spectrum of-PEEK composite coating coating；
Fig. 5 is plasma spraying Al in the embodiment of the present invention 12O3- PEEK composite coating and single Al2O3The abrasion of coating Spirogram；
Fig. 6 is plasma spraying Al in the embodiment of the present invention 12O3- PEEK composite coating and single Al2O3The polarization of coating Curve；
Fig. 7 is TiH in the embodiment of the present invention 22The SEM of/PEEK coated composite powder schemes；
Fig. 8 is TiH in the embodiment of the present invention 22The SEM figure of/PEEK coated composite powder scratched；
Fig. 9 is the XRD diffracting spectrum of TiN/PEEK composite coating in the embodiment of the present invention 2；
Specific embodiment
Present invention is further described in detail for embodiment with reference to the accompanying drawing, it should be pointed out that implementation as described below Example is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Al of the present invention2O3The granularity of powder is 80nm~420nm, TiH2The granularity of powder is 1 μm~5 μm, BN powder Granularity is 30~500nm, ZrO2The granularity of powder is 40~500nm, and the granularity of PEEK powder is 20~30 μm, the granularity of Ni/Al powder For -200~+300 mesh.
Binder of the present invention stirred under the conditions of 95 DEG C by thickener and deionized water 40~45 minutes preparation and At mass ratio is thickener：Deionized water=1：100；The thickener is sodium cellulose glycolate.
Embodiment 1：
In the present embodiment, Al is prepared for the method for mist projection granulating2O3/ PEEK coated composite powder, in 45# steel matrix specimen surface Al is prepared using reaction and plasma spraying technique2O3- PEEK composite coating.
The preparation method of the coating is as follows：
1:Al2O3The preparation of/PEEK coated composite powder
(1)Al2O3The preparation of slurry：Weigh the Al that granularity is 80nm~400nm2O3Powder 180g is placed in beaker 1, is claimed It removes ionized water 200g to pour into beaker 1, stir 15 minutes.Then dispersing agent (sodium polyphosphate) 1.8g is added, stirs 20 points Clock.It is eventually adding binder 100g, is mixed 1 hour, prepares Al2O3Slurry.
(2) PEEK material by preparation：It weighs the PEEK20g that granularity is 20~40 μm to be placed in beaker 2, be added appropriate anhydrous Ethyl alcohol about 20ml, stirring are completely dissolved PEEK in 10 minutes.Then dispersing agent 0.2g is added, is stirred 10 minutes.It is eventually adding Binder 5g stirs 30 minutes, prepares PEEK slurry.
(3) PEEK slurry is poured into Al2O3Slurry mixes together, is stirred when pouring into glass bar, stirs again after pouring into completely It mixes 2~3 hours, is mixed into the slurry that solid content is 39%.
(4) Al is prepared with the method for mist projection granulating2O3/ PEEK coated composite powder；Using air-flowing type spray granulation plant, make by spraying Grain parameter is set as：280 DEG C of inlet air temperature, 120 DEG C of leaving air temp, atomizer frequency is 100Hz, the control of nozzle air current amount pressure Between 0.08-0.1MPa, wriggling revolution speed 35r/min, charging revolution speed is 40r/min, and charging rate is controlled in 12ml/ min.It introduces the slurry into, finally obtains dry solid Al2O3/ PEEK coated composite powder.
(5) the solid Al that will be obtained2O3/ PEEK coated composite powder feeding is screened, and filtering out size is -200~+300 Purpose is suitble to the powder of spraying.
2:Al2O3The preparation of-PEEK composite coating
(1) 45# steel matrix sample is put into TPS-1 type vapour-pressure type sand-blasting machine, surface is carried out at blasted rough Reason, abrasive grain are inhaled into nozzle, are accelerated in high pressure draught, are ejected into matrix surface, obtain clean, coarse surface, thus Increase the binding force between matrix and coating；
(2) before spray-on coating, in order to enhance the bond strength of coating and matrix, Ni- is sprayed on steel matrix surface in advance 10%wtAl self-melting alloy powder obtains the bond coating with a thickness of 100 μm.
(3) by the Al of preparation2O3/ PEEK composite granule is put into the powder feeder of GP-80 type plasma spraying equipment, is led to Powder feeding gas is crossed, is sent into the plasma flame flow of high temperature and high speed.Specially：Matrix is fixed on spraying working platform, work is adjusted Electric current 500A；Arc voltage 60V；Powder feeding rate is 3L/min, and spray gun scanning speed is 0.0064m/s, and adjustment spray distance is 100mm, spray angle are 90 °, argon flow 40L/min, argon pressure 0.8MPa, nitrogen flow 7L/min, nitrogen pressure 0.8MPa starts to spray, obtains Al2O3- PEEK composite coating, the thickness of coating are about 300 μm.Wherein, nitrogen is as powder feeding Gas, argon gas is as protection gas.
Fig. 1 is Al obtained above2O3The SEM of/PEEK coated composite powder schemes.As can be seen that the coated composite powder sphericity of preparation is very Height, nanometer Al2O3It is wrapped in the surface PEEK well.
Fig. 2 is Al obtained above2O3The SEM figure of/PEEK coated composite powder scratched.As can be seen that intermediate bulky grain is PEEK, the fine particle of outside are Al2O3。
Fig. 3 is the Al that plasma spraying obtains2O3- PEEK composite coating SEM figure, is found out by figure, which is in typical layer Shape structure, coating texture are comparatively dense.Black is mutually PEEK in coating, and grey form and aspect are Al2O3。
Fig. 4 is the XRD diffracting spectrum of above-mentioned coating.Wherein Fig. 4 a is the XRD diffracting spectrum of alumina powder, Al2O3Including γ-Al2O3With α-Al2O3.Fig. 4 b is the XRD diffracting spectrum of PEEK powder.Fig. 4 c is the XRD diffracting spectrum of composite coating, compound Coating is by γ-Al2O3With α-Al2O3And PEEK composition.
To above-mentioned obtained Al2O3- PEEK composite coating carries out hardness test with microhardness tester.The application load of this experiment Time is 15s, magnitude of load 100g.10 points are chosen on each sample, are then averaged, are obtained the hard of composite coating Angle value.The average hardness of composite coating is HV0.11151。
To Al obtained above2O3- PEEK composite coating carries out wear test.For the sake of comparing, with identical spray parameters The single Al of lower spraying2O3Coating is as a comparison.Using SFT-2M type pin disk-type friction abrasion tester comparative analysis pure alumina The friction-wear test of coating and composite coating under 20N and 30N load-up condition, experimental period 30min.Pass through frictional experiment After measure single Al2O3Coating coefficient of friction is 0.68, and composite coating coefficient of friction is 0.58.Abrasion loss is as shown in figure 5, therefrom As can be seen that with single Al2O3Coating is compared, the Al in the present embodiment2O3The wear rate of-PEEK composite coating is lower than single Al2O3Coating, under the conditions of load is 20N, Al2O3The abrasion loss of-PEEK composite coating and single Al2O3The abrasion loss phase of coating Than reducing 37%.When load is 30N, 20% is reduced.It follows that Al2O3- PEEK composite coating shows more excellent Wearability and antifriction quality.
To Al obtained above2O3- PEEK composite coating carries out electrochemistry experiment.For the sake of comparing, joined with identical spraying The single Al of several lower sprayings2O3Coating is as a comparison.Dynamic potential scanning, current potential have been carried out using Shanghai Chen Hua electrochemical workstation Range is；- 0.2V~+0.4V (relative to open circuit potential), scanning speed 0.2mV/s.Obtain polarization curve as shown in fig. 6, The corrosion potential and corrosion current of composite coating are respectively -501.9mV and 7.31/ μ Acm-2, single Al2O3The corrosion of coating Current potential and corrosion current are respectively -592.6mV and 13.92 μ Acm-2, composite coating shows superior corrosion resistance.
Embodiment 2：
In the present embodiment, TiH is prepared for the method for mist projection granulating2/ PEEK coated composite powder, in 45# steel matrix specimen surface TiN-PEEK composite coating is prepared using reaction and plasma spraying technique.
TiH2The preparation method of/PEEK coated composite powder and coating is as follows：
1:TiH2The preparation of/PEEK coated composite powder
(1)TiH2The preparation of slurry：Weighing granularity is 1 μm~5 μm TiH2Powder 180g is placed in beaker 1, weighs deionization Water 150g is poured into beaker 1, is stirred 20 minutes.Then dispersing agent (sodium polyphosphate) 1.8g is added, stirs 20 minutes.Finally plus Enter binder 120g, is mixed 1 hour, prepares TiH2Slurry.
(2) PEEK material by preparation：It weighs the PEEK20g that granularity is 20~40 μm to be placed in beaker 2, be added appropriate anhydrous Ethyl alcohol about 20ml, stirring are completely dissolved PEEK in 10 minutes.Then dispersing agent 0.2g is added, is stirred 10 minutes.It is eventually adding Binder 5g stirs 30 minutes, prepares PEEK slurry.
(3) PEEK slurry is poured into TiH2Slurry mixes together, is stirred when pouring into glass bar, stirs again after pouring into completely It mixes 2~3 hours, is mixed into the slurry that solid content is 41%.
(4) TiH is prepared with the method for mist projection granulating2/ PEEK coated composite powder；Using air-flowing type spray granulation plant, make by spraying Grain parameter is set as：270 DEG C of inlet air temperature, 120 DEG C of leaving air temp, atomizer frequency is 110Hz, the control of nozzle air current amount pressure Between 0.08-0.1MPa, wriggling revolution speed 30r/min, charging revolution speed is 40r/min, and charging rate is controlled in 10ml/ min.It introduces the slurry into, finally obtains dry solid TiH2/ PEEK coated composite powder.
(5) the solid TiH that will be obtained2/ PEEK coated composite powder feeding is screened, and filtering out size is -200~+300 Purpose is suitble to the powder of spraying.
2:The preparation of TiN-PEEK composite coating
Operating current 400A, arc voltage 60V are adjusted, other spraying parameters are identical as example 1, sprayed.? To TiN-PEEK composite coating, the thickness of coating is about 300 μm.
TiH obtained above2As shown with 7, the coated composite powder sphericity of preparation is very high, micron order for the SEM figure of/PEEK coated composite powder TiH2It is wrapped in the surface PEEK well.Fig. 8 is the SEM figure of broken coated composite powder, and the inside bulky grain is PEEK, and outside is by tiny TiH2Closely it is bundled together.
The tissue of composite coating obtained above is similar with example 1, and coating is in typical layer structure, coating texture Comparatively dense, PEEK is evenly distributed in coating, increases the toughness of coating.
The XRD diffracting spectrum class of TiN-PEEK composite coating obtained above is as shown in figure 9, the coating that this method is prepared Main phase is TiN, and secondary phase is Ti3O, TiN are by TiH2The ceramic phase generated is reacted with N2, increases the wearability of coating.Due to The content of PEEK in the coating can't detect less than 10%, therefore in XRD diffraction.
Wear test is carried out to TiN-PEEK composite coating obtained above.For the sake of comparing, with identical spray parameters The single tin coating of lower spraying is as a comparison.Using SFT-2M type pin disk-type friction abrasion tester comparative analysis single tin and Abrasion loss test of the composite coating under 20N and 30N load-up condition, the wear test time is 30min.Pass through frictional wear experiment TiN-PEEK compound painting of the abrasion loss trend of coating similar to example 1, compared with single tin coating, in the present embodiment is measured afterwards The wear rate and coefficient of friction of layer are below single tin coating, and TiN-PEEK composite coating shows more excellent wearability.
Electrochemistry experiment is carried out to TiN-PEEK composite coating obtained above.For the sake of comparing, joined with identical spraying The single tin coating of several lower sprayings is as a comparison.Electrochemistry experiment parameter is the same as example 1, the corrosion potential of composite coating and corrosion Electric current is below single tin coating and shows superior corrosion resistance.
Embodiment 3：It is prepared for BN/PEEK coated composite powder with the method for mist projection granulating, used in 45# steel matrix specimen surface etc. Plasma spray technique prepares BN-PEEK composite coating.
In the present embodiment,
The preparation method of BN/PEEK coated composite powder and composite coating is as follows：
1:The preparation of BN/PEEK coated composite powder
(1) preparation of BN slurry：Weighing granularity is that 30nm~500nmBN powder 180g is placed in beaker 1, weighs deionization Water 170g is poured into beaker 1, is stirred 15 minutes.Then dispersing agent (sodium polyphosphate) 1.8g is added, stirs 15 minutes.Finally plus Enter binder 110g, is mixed 1 hour, prepares TiH2Slurry.
(2) PEEK material by preparation：It weighs the PEEK25g that granularity is 20~40 μm to be placed in beaker 2, be added appropriate anhydrous Ethyl alcohol about 25ml, stirring are completely dissolved PEEK in 10 minutes.Then dispersing agent 0.25g is added, is stirred 10 minutes.It is eventually adding Binder 6g stirs 30 minutes, prepares PEEK slurry.
(3) PEEK slurry is poured into BN slurry to mix together, is stirred when pouring into glass bar, is stirred for after pouring into completely 2~3 hours, it is mixed into the slurry that solid content is 40%.
(4) BN/PEEK coated composite powder is prepared with the method for mist projection granulating；Using air-flowing type spray granulation plant, mist projection granulating Parameter is set as：280 DEG C of inlet air temperature, 130 DEG C of leaving air temp, atomizer frequency is 110Hz, and the control of nozzle air current amount pressure exists Between 0.08-0.1MPa, wriggling revolution speed 30r/min, charging revolution speed is 40r/min, and charging rate is controlled in 10ml/min. It introduces the slurry into, finally obtains dry solid BN/PEEK coated composite powder.
(5) obtained solid BN/PEEK coated composite powder feeding is screened, filtering out size is -200~+300 mesh Suitable spraying powder.
2:The preparation of BN-PEEK composite coating
Operating current 500A, arc voltage 60V are adjusted, other spraying parameters are identical as example 1, sprayed.? To BN-PEEK composite coating, the thickness of coating is about 300 μm.
The SEM of BN/PEEK coated composite powder obtained above is similar to example 1, and the coated composite powder sphericity of preparation is very high, micron order BN It is wrapped in the surface PEEK well.
The SEM figure of BN-PEEK composite coating obtained above is similar to Figure 1, and coating is in typical layer structure, coating Institutional framework is comparatively dense, and PEEK is evenly distributed in coating, increases the toughness of ceramic coating.
Frictional wear experiment is carried out to BN-PEEK composite coating obtained above.For the sake of comparing, joined with identical spraying The single BN coating of several lower sprayings is as a comparison.Using the SFT-2M type pin single BN of disk-type friction abrasion tester comparative analysis and Abrasion loss test of the composite coating under 20N and 30N load-up condition, the wear test time is 30min.By being surveyed after frictional experiment The abrasion loss trend of coating is obtained similar to example 1, compared with single BN coating, the mill of the BN-PEEK composite coating in the present embodiment Loss rate is lower than single BN coating, and BN-PEEK composite coating shows more excellent wearability.
Electrochemistry experiment is carried out to BN-PEEK composite coating obtained above.For the sake of comparing, with identical spray parameters The single BN coating of lower spraying is as a comparison.Electrochemistry experiment parameter is the same as example 1, the corrosion potential and corrosion current of composite coating It is below single BN coating and shows superior corrosion resistance.
Embodiment 4：ZrO is prepared for the method for mist projection granulating2/ PEEK coated composite powder is used in 45# steel matrix specimen surface Reaction and plasma spraying technique prepares ZrO2- PEEK composite coating.
In the present embodiment,
ZrO2The preparation method of/PEEK coated composite powder and composite coating is as follows：
1:ZrO2The preparation of/PEEK coated composite powder
(1)ZrO2The preparation of slurry：Weighing granularity is 40nm~500nmZrO2Powder 180g is placed in beaker 1, is weighed Ionized water 160g is poured into beaker 1, is stirred 15 minutes.Then dispersing agent (sodium polyphosphate) 1.8g is added, stirs 15 minutes.Most Binder 110g is added afterwards, is mixed 1 hour, prepares ZrO2Slurry.
(2) PEEK material by preparation：It weighs the PEEK24g that granularity is 20~40 μm to be placed in beaker 2, be added appropriate anhydrous Ethyl alcohol about 24ml, stirring are completely dissolved PEEK in 10 minutes.Then dispersing agent 0.24g is added, is stirred 10 minutes.It is eventually adding Binder 6g stirs 30 minutes, prepares PEEK slurry.
(3) PEEK slurry is poured into ZrO2Slurry mixes together, is stirred when pouring into glass bar, stirs again after pouring into completely It mixes 2~3 hours, is mixed into the slurry that solid content is 41%.
(4) ZrO is prepared with the method for mist projection granulating2/ PEEK coated composite powder；Using air-flowing type spray granulation plant, make by spraying Grain parameter is set as：280 DEG C of inlet air temperature, 130 DEG C of leaving air temp, atomizer frequency is 110Hz, the control of nozzle air current amount pressure Between 0.08-0.1MPa, wriggling revolution speed 30r/min, charging revolution speed is 40r/min, and charging rate is controlled in 10ml/ min.It introduces the slurry into, finally obtains dry solid ZrO2/ PEEK coated composite powder.
(5) the solid ZrO that will be obtained2/ PEEK coated composite powder feeding is screened, and filtering out size is -200~+300 Purpose is suitble to the powder of spraying.
2:ZrO2The preparation of-PEEK composite coating
Operating current 500A, arc voltage 55V are adjusted, other spraying parameters are identical as example 1, sprayed.? To ZrO2- PEEK composite coating, the thickness of coating are about 300 μm.
ZrO obtained above2The SEM of/PEEK coated composite powder is similar to example 1, and the coated composite powder sphericity of preparation is very high, micron order ZrO2It is wrapped in the surface PEEK well.
ZrO obtained above2The SEM figure of-PEEK composite coating is similar to Figure 1, and coating is in typical layer structure, applies Layer tissue structure is comparatively dense, and PEEK is evenly distributed in coating, increases the toughness of ceramic coating.
To ZrO obtained above2- PEEK composite coating carries out frictional wear experiment.For the sake of comparing, with identical spraying The single ZrO sprayed under parameter2Coating is as a comparison.It is single using SFT-2M type pin disk-type friction abrasion tester comparative analysis ZrO2With abrasion loss test of the composite coating under 20N and 30N load-up condition, the wear test time is 30min.It is real by friction The abrasion loss trend of coating is measured after testing similar to example 1, with single ZrO2Coating is compared, the ZrO in the present embodiment2- PEEK is compound The wear rate of coating is lower than single ZrO2Coating, ZrO2- PEEK composite coating shows more excellent wearability.
To ZrO obtained above2- PEEK composite coating carries out electrochemistry experiment.For the sake of comparing, joined with identical spraying The single ZrO of several lower sprayings2Coating is as a comparison.Electrochemistry experiment parameter is the same as example 1, the corrosion potential of composite coating and corrosion Electric current is below single ZrO2Coating shows superior corrosion resistance.
Embodiment 5：
In the present embodiment, it is prepared for Ti/PEEK composite powder with the method for mist projection granulating, is adopted in 45# steel matrix specimen surface TiN-PEEK composite coating is prepared with reaction and plasma spraying technique.
The preparation method of Ti/PEEK composite powder and coating is as follows：
For other steps with embodiment 2, difference is that the partial size of PEEK with Ti powder is identical；The particle size of PEEK be 20~ 40 μm, the particle size of Ti powder is 20~40 μm.Composite powder obtained is that PEEK packet Ti powder only has a small amount of Ti packet PEEK mostly, And package is not fine and close, and part PEEK is exposed outside.Coated composite powder cannot be formed.With the powder spray obtain the performance of coating compared with Difference, PEEK degrade, and cannot effectively play the self-lubricating function of organic matter.And hole is formed, increase coating porosity, drop Low coating quality.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention, Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Unaccomplished matter of the present invention is well-known technique.

Claims (5)

1. a kind of ceramic coatings organic matter composite powder suitable for spraying, it is characterized in that the composite powder is made by following methods, including Following steps：
(1) preparation of ceramic slurry：Deionized water is added in ceramic powders, stirs, dispersing agent is then added, continues to stir It mixes；Binder is added, obtains ceramic powder slurry after finally agitated；
Wherein, the quality of dispersing agent is the 0.9%~1.1% of ceramic powders quality, and the quality of deionized water is ceramic powders matter The 5/6~10/9 of amount, binder quality are the 5/9~2/3 of ceramic powders quality；
(2) preparation of organic slurry：Dehydrated alcohol is poured into organic matter powder, after stirring dissolves organic matter powder, then Dispersing agent is added, continues to stir, is eventually adding binder, obtains organic slurry after stirring；
Wherein, the quality of the dispersing agent in this step is the 0.9%~1.1% of organic matter powder；The quality of dehydrated alcohol is to have The 3/5~1 of machine amount of substance, bonding agent quality are the 1/4~1/5 of organic matter；
(3) two kinds of slurries are mixed together, is stirred for 2~3 hours, obtain being uniformly mixed solid content being the compound of 30%-50% Slurry material；
Wherein, quality proportioning is ceramic powders：Organic matter powder=9:1~7:1；
Ceramics are Al2O3、TiN、BN、ZrO2、Cr2O3Or Nb2O5, the particle size range of ceramic powders is 30nm~5 μm；
Organic matter is PEEK (polyether-ether-ketone), PTFE (polytetrafluoroethylene (PTFE))；The particle size range of organic matter powder is 20~40 μm；
(4) the organic composite powder of ceramic coatings is prepared with the method for mist projection granulating；It is spraying using air-flowing type spray granulation plant Parameter is granulated to be set as：260 DEG C~300 DEG C of inlet air temperature, 110 DEG C~130 DEG C of leaving air temp, atomizer frequency be 100~ 110Hz, nozzle air current amount pressure control between 0.08-0.1MPa, wriggling revolution speed 35-40r/min, and charging revolution speed is 30 ~40r/min charging rate is controlled in 10~14ml/min；It is multiple to introduce the slurry into the dry solid ceramic cladding organic matter of acquisition Close powder；
(5) dry solid ceramic cladding organic matter composite powder is screened, filtering out size is -200~+300 mesh Powder.
2. the as described in claim 1 ceramic coatings organic matter composite powder for being suitable for spraying, it is characterized in that the binder by Thickener and deionized water stir 40~45 minutes under the conditions of 95 DEG C to be prepared, and mass ratio is thickener：Deionized water= 1：100；The thickener is sodium cellulose glycolate.
3. the ceramic coatings organic matter composite powder as described in claim 1 for being suitable for spraying, it is characterized in that the dispersing agent is Sodium polyphosphate.
4. a kind of spraying method of the ceramic coatings organic matter composite powder suitable for spraying, it is characterized in that including the following steps：
(1) matrix specimen surface is pre-processed；
(2) Ni-10%wtAl self-melting alloy powder is sprayed in advance in matrix surface, obtain the bonding with a thickness of 80~120 μm Bottom；The matrix is metal material；
(3) ceramic coatings organic matter composite powder made from claim 1 is put into powder feeder, using the method for plasma spraying Spray to matrix surface, obtain ceramics-organic matter composite coating, coating with a thickness of 300-500 μm；
Wherein, spray parameters are set as：400~500A of operating current；50~60V of arc voltage；40~60L/ of argon flow Min, 0.6~0.8MPa of pressure；7~10L/min of nitrogen flow, 0.6~0.8MPa of pressure；2~5L/min of powder feeding rate；Spraying 80~110mm of distance；Spray angle is 90 °；Wherein nitrogen is as powder feeding gas, and argon gas is as protection gas.
5. the spraying method of the ceramic coatings organic matter composite powder as claimed in claim 4 for being suitable for spraying, it is characterized in that described Metal material be specially 45# steel, Q235 or Q345.
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