CN110002496A - A kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder - Google Patents
A kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder Download PDFInfo
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Abstract
The invention discloses a kind of anti-preparation methods for peeling off zirconia coating Zirconium oxide powder, belong to technical field of nanometer material preparation.Zirconium oxide powder is mixed with additive 3:1~5:1 in mass ratio, after being stirred, concentrated by rotary evaporation, obtain concentrate, under conditions of being 70~80 DEG C in temperature by concentrate after dry 1~2h, obtain anti-peeling zirconia coating Zirconium oxide powder blank, anti- peeling zirconia coating is mixed with Zirconium oxide powder blank with toluene 1:8~1:10 in mass ratio, and the anti-toluene di-isocyanate(TDI) for peeling off 0.2~0.3 times of zirconia coating Zirconium oxide powder blank quality is added, after being stirred to react, filtering, washing, it is dry, obtain anti-peeling zirconia coating Zirconium oxide powder.Gained anti-peeling zirconia coating Zirconium oxide powder of the invention has excellent wear-resisting property, and adhesive force is preferable when product use.
Description
Technical field
The invention discloses a kind of anti-preparation methods for peeling off zirconia coating Zirconium oxide powder, belong to nano material system
Standby technical field.
Background technique
The compressor delivery temperature of modern aeroengine can achieve 600 DEG C or more, and general material is at such a temperature
Performance can be remarkably decreased, and can not fully meet requirement.Coating is often referred to one layer of special material coated on piece surface, Ke Yixian
The performance and working life for improving part are write, is that aero-engine manufactures essential technological means.Modern aeroengine
There is 75% or more part to be all coated with the coatings of various functions to increase the service life of part, reliability and antifatigue etc.
Performance etc..
Ceramic material has high rigidity and high temperature resistant, corrosion-resistant and anti abrasive characteristic, protective as mechanical part
Surface covering is concerned by people.
Zirconium oxide plasma dusty spray is the important materials that layer (TBCs) is removed for the advanced thermal boundary of spray.It is this for spray
Coating, the main technique requirements to dusty spray are: chemical constituent is uniform, phase composition is uniform, good fluidity, grain graininess 5
~125 μm.Traditional zirconia coating has shown good performance in application process, but exists in its internal structure
It is unevenly distributed, larger-size various defects, often occurs phenomena such as cracking, peel off in use.Nano zircite applies
The appearance of layer is resolved these problems to a certain extent.Composition particle inside nanostructured zirconia coating is very tiny
And be evenly distributed, internal defects are less than traditional zirconia coating；Moreover, the uniformity of defect distribution is also superior to traditional oxygen
Change zirconium coating, therefore its performance is better than traditional zirconia coating.Existing document further demonstrates that, applies with traditional zirconium oxide
Layer shows more superior performance compared to nanostructured zirconia coating, as chemical stability is good, thermal conductivity is low, thermal expansion coefficient is high,
Hardness is high, with the binding force of matrix is strong, high temperature oxidation resistance is good, resistance to high temperature corrosion and thermal shock resistance are excellent.In addition, nanometer
A large amount of interface area is formd between fine particle inside zirconia coating, is easier the sliding of crystal boundary, thus deformation
More easily；Therefore the toughness of nanostructured zirconia coating is better than the existing Zirconium oxide plasma spray coating powder of traditional zirconia coating
The preparation method at end mainly have arc it is molten/crush method and spray drying/plasma spheroidization method.Arc is molten/and the made powder corner angle of crush method are more,
Shattering process is easily introduced impurity, and the distribution of stabilizer, phase constituent and granularity is also not satisfactory；Spray drying/plasma spheroidization method cost
Higher, made powder is mostly hollow powder, and there is also the above problems for their stabilizer, phase constituent and size distribution.In nanometer
It is found in the comparative study of zirconia coating and non-nano zirconia coating, under identical preparation process condition, nano zircite
The binding force of coating and matrix, wear-corrosion resistance and toughness are better than non-nano zirconia coating.In research nano zircite
It is found when the structure and property of coating, the stratiform and cavity-like structure inside nanostructured zirconia coating facilitate its thermal shock resistance
It improves.Spherical nano particle improves the slipping property of crystal boundary, so that the toughness of coating be made to be improved, and prevents coating
The diffusion of middle crackle improves the binding force of coating and matrix.In research nanostructured zirconia coating and non-nano zirconia coating
Thermal shock resistance when, in nanostructured zirconia coating is about 10 μm of stomata there is size, is evenly distributed and coat inside
Particle size very little, and traditional non-nano zirconia coating is unlike nanostructured zirconia coating, in coating there is
The stomata of similar triangle and be unevenly distributed, particle size it is larger, so as to cause the thermal shock resistance of non-nano zirconia coating
It is poor.
Simultaneously as due to nano zirconium oxide powder large specific surface area, density is small, adsorption capacity is strong, in spraying process easily
Cause difficulty of transportation and line clogging；In addition, nanometer powder momentum is small, can not deposit to form fine and close coating in substrate surface,
Nano zirconium oxide powder is caused to use difficulty, and being easy to run off due to nanometer powder in spraying process, to make product
Wearability can not further increase.
Therefore research and develop that a kind of service performance is good, and the high nano zirconium oxide powder of wear-resisting property has good city
Field prospect.
Summary of the invention
The present invention solves the technical problem of: it is directed to Conventional nano Zirconium oxide powder, since surface area is big, density
It is small, adsorption capacity is strong, difficulty of transportation and line clogging are easily caused in spraying process, and nanometer powder is easy to run off, lead to product
The problem of wearability can not further increase provides a kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
1. a kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder, specific preparation step are as follows:
Alkali lignin is mixed with water 1:3~1:5 in mass ratio 2.(1), and adjusts pH to 10.5~11.0, it is molten to obtain alkali lignin
Liquid mixes alkali lignin solution with formaldehyde 15:1~25:1 in mass ratio, and after being stirred to react, heating adds alkali lignin
The sodium sulfite that 0.1~0.2 times of solution quality continues after being stirred to react, obtains pre-polymer mixture；
Pre-polymer mixture is mixed with potassium iodide 100:1~120:1 in mass ratio 3.(2), and pre-polymer mixture matter is added
1, the 6- dibromo-hexane solution of 0.1~0.2 times of amount, after being stirred to react, extracts, and filtering obtains filtrate to get additive；
Dichloro oxidation chromium solution is mixed with precipitating reagent 1:2~1:3 in mass ratio 4.(3), and dichloro oxidation chromium solution matter is added
The dispersing agent of 0.2~0.5 times of amount is stirred to react, and still aging after adjusting pH, is filtered, and washing obtains pretreatment gel, will be pre-
After treatment gel high temperature high pressure process, Zirconium oxide powder is obtained；
5.(4) Zirconium oxide powder is mixed with additive 1:2~1:3 in mass ratio, concentrated by rotary evaporation, it is dry, obtain anti-peeling oxidation
Zirconium coating Zirconium oxide powder blank, by anti-peeling zirconia coating Zirconium oxide powder blank and toluene 1:8 in mass ratio~
1:10 mixing, and the anti-toluene diisocynate for peeling off 0.2~0.3 times of zirconia coating Zirconium oxide powder blank quality is added
Ester after being stirred to react, is filtered, is washed, dry, obtains anti-peeling zirconia coating Zirconium oxide powder.
Extractant used in step (2) described extraction is petroleum ether.
Step (2) the 1,6- dibromo-hexane solution is by 1,6- dibromo-hexane and dehydrated alcohol 5:1~6:1 in mass ratio
Mixing, obtains 1,6- dibromo-hexane solution.
Step (3) described precipitating reagent is the ammonium hydroxide that mass fraction is 10~12% or the sodium hydroxide that mass fraction is 2~5%
In any one.
Step (3) dispersing agent is to mix polyethylene glycol 2000 with ammonium citrate 3:1 in mass ratio, and poly- second is added
The ammonium polymethacrylate of 0.1~0.2 times of 2000 mass of glycol, after being stirred, obtains dispersing agent.
The condition of step (3) described high temperature high pressure process is that temperature is 800~1000 DEG C, and pressure is 1.8~2.0MPa.
The anti-method therefor for peeling off zirconia coating Zirconium oxide powder is to aoxidize anti-peeling zirconia coating
Zirconium powder immerses the second that mass fraction is 90% after plasma spray system is sprayed at metal surface, and by the metal after spraying
In alcoholic solution, after impregnating 1~2h, filter, it is dry, obtain wear-resisting zirconia coating.
0.1~0.3 times of toluene di-isocyanate(TDI) quality of asphalt mixtures modified by epoxy resin can be added in step (4) described toluene di-isocyanate(TDI)
Rouge, the epoxy resin are any one in epoxy resin E-44 or epoxy resin E-51.
0.1~0.2 times of additive quality of dopamine can be added in step (2) described additive.
The beneficial effects of the present invention are:
14.(1) additive is added when preparing anti-peeling zirconia coating Zirconium oxide powder in the present invention, firstly, in additive
Lignin containing alkane bridging has excellent greasy property, after being added in product, can effectively reduce product and was using
The resistance generated when being sprayed in journey, to make the spraying uniformity of product improve, also, since additive can be adsorbed on nanometer
Zirconium surface so that the absorption property of low nano zircite is reduced the autohemagglutination situation of nano zircite, and then makes to reduce and produce
Product to the blocking of pipeline, spray product more easily in use, secondly, the additive being added in product can be in product
After use, immerse ethanol solution in after, can make additive product surface occur autohemagglutination, formed lamellar structure, and with
The extension of soaking time further can stack to form block structure, to form concave-convex structure in product surface, make product
Friction area is reduced, and then improves the wearability of product, furthermore, due to the addition of alkane in additive shield it is intermolecular
Repulsion so that additive be made to be easily adsorbed to metal surface, and then can make product be easy to be sprayed at metal surface, improve product
Adhesive force improves product resistance to flaking, simultaneously as so that lignin is formed three-dimensional net structure after alkane modified lignin resin,
And after immersing in ethanol solution, each intermolecular active force in product can be made to improve, to enable the anti-flaking of product
It further increases；
15.(2) isocyanates is added when preparing anti-peeling zirconia coating Zirconium oxide powder in the present invention, on the one hand, isocyanide
The addition of acid esters can make the hydroxyl on nano zirconium dioxide surface in conjunction with the hydroxyl in additive is under the action of cyano, mention
Binding force between high additive and nano zircite, so that the wearability of product is further increased, on the other hand, isocyanic acid
Ester can be such that hydroxyl remaining in additive crosslinks, so that nano zircite to be fixed on to the three-dimensional net structure of additive
In, while improving product adhesive force, the wearability of product is further increased, also, a certain amount of due to that can be added in product
Epoxy resin, so as to make the epoxy group in epoxy resin graft on nano zircite surface, and then make in product each point
Binding force between son further increases, and can be further improved the wear-resisting sexual desire anti-flaking of product.
Specific embodiment
Alkali lignin and water 1:3~1:5 in mass ratio are mixed in beaker, and the hydrogen for being 15~25% with mass fraction
Sodium hydroxide solution adjusts the pH to 10.5~11.0 of material in beaker, alkali lignin solution is obtained, by alkali lignin solution and formaldehyde
15:1~25:1 is mixed in three-necked flask in mass ratio, is 65~75 DEG C in temperature, revolving speed is the condition of 300~400r/min
Under, after being stirred to react 60~80min, temperature is warming up to 85 DEG C, then alkali lignin solution quality 0.1 is added into three-necked flask
~0.2 times of sodium sulfite, continuing at temperature is 85 DEG C, and revolving speed is stirred to react 2~3h under conditions of being 280~350r/min
Afterwards, pre-polymer mixture is obtained；Pre-polymer mixture and potassium iodide 100:1~120:1 in mass ratio are mixed in four-hole boiling flask,
And 0.1~0.2 times of pre-polymer mixture quality of 1,6- dibromo-hexane solution is added into four-hole boiling flask, in temperature be 65~70
DEG C, under conditions of revolving speed is 280~320r/min, after being stirred to react 1~2h, additive blank is obtained, by additive blank stone
After oily ether extracts 2~3 times, filtering obtains filtrate to get additive；By mass fraction be 5~12% dichloro aoxidize chromium solution with
Precipitating reagent 1:2~1:3 in mass ratio is mixed in flask, and dichloro is added into flask and aoxidizes 0.2~0.5 times of chromium solution quality
Dispersing agent, control dichloro oxidation chromium solution addition rate be 2~3mL/min, and with mass fraction for 5~12% hydrogen-oxygen
Change the pH to 10.0 that sodium solution adjusts material in flask, is 60~80 DEG C in temperature, revolving speed is the condition of 260~360r/min
Under, after being stirred to react 2~3h, by material in flask after still aging 12~13h under room temperature, filtering must be pre-processed solidifying
Compound blank material after treatment gel blank is washed with deionized 8~10 times, obtains pretreatment gel, by pretreatment gel in high temperature
Under condition of high voltage, after constant temperature and pressure handles 1~2h, Zirconium oxide powder is obtained；By Zirconium oxide powder and additive 1:2 in mass ratio~
1:3 mixing, in temperature be 30~50 DEG C, revolving speed be 300~350r/min under conditions of, after being stirred 30~60min, and in
Temperature is 60~70 DEG C, and revolving speed is 120~150r/min, under conditions of pressure is 500~600kPa after 3~6h of concentrated by rotary evaporation,
Concentrate is obtained, under conditions of being 70~80 DEG C in temperature by concentrate after dry 1~2h, obtains anti-peeling zirconia coating oxidation
Zirconium powder blank, by anti-peeling zirconia coating Zirconium oxide powder blank and toluene 1:8~1:10 hybrid reaction in mass ratio
In kettle, and it is different that the anti-toluene two for peeling off 0.2~0.3 times of zirconia coating Zirconium oxide powder blank quality is added into reaction kettle
Cyanate is 80~85 DEG C in temperature, and after revolving speed is stirred to react 1~2h under conditions of being 250~320r/min, filtering is obtained pre-
Anti- peeling zirconia coating Zirconium oxide powder blank is handled, anti-peeling zirconia coating Zirconium oxide powder blank will be pre-processed
Anti- peelings zirconia coating use is obtained after dry 1~2h after acetone washing 4~5 times, and under conditions of being 60~80 DEG C in temperature
Zirconium oxide powder.The 1,6- dibromo-hexane solution is to mix 1,6- dibromo-hexane and dehydrated alcohol 5:1~6:1 in mass ratio
It closes, obtains 1,6- dibromo-hexane solution.The precipitating reagent is the ammonium hydroxide that mass fraction is 10~12% or mass fraction is 2~5%
Any one in sodium hydroxide.The dispersing agent is to mix polyethylene glycol 2000 with ammonium citrate 3:1 in mass ratio, and be added
The ammonium polymethacrylate that 0.1~0.2 times of polyethylene glycol 2000 quality after being stirred, obtains dispersing agent.At the high temperature and pressure
The condition of reason is that temperature is 800~1000 DEG C, and pressure is 1.8~2.0MPa.The anti-peeling zirconia coating zirconia powder
End method therefor be by anti-peeling zirconia coating with Zirconium oxide powder after plasma spray system is sprayed at metal surface,
And immerse the metal after spraying in the ethanol solution that mass fraction is 90%, after impregnating 1~2h, filter, it is dry, obtain wear-resisting oxygen
Change zirconium coating.0.1~0.3 times of toluene di-isocyanate(TDI) quality of epoxy resin, institute can be added in the toluene di-isocyanate(TDI)
Stating epoxy resin is any one in epoxy resin E-44 or epoxy resin E-51.Additive quality can be added in the additive
0.1~0.2 times of dopamine.
Example 1
Alkali lignin and water 1:5 in mass ratio are mixed in beaker, and the sodium hydroxide solution for being 25% with mass fraction is adjusted
The pH to 11.0 of material, obtains alkali lignin solution in beaker, and alkali lignin solution and formaldehyde 25:1 in mass ratio are mixed in three
In mouth flask, it is 75 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 80min, temperature is warming up to 85
DEG C, then 0.2 times of alkali lignin solution quality of sodium sulfite is added into three-necked flask, continuing at temperature is 85 DEG C, and revolving speed is
After being stirred to react 3h under conditions of 350r/min, pre-polymer mixture is obtained；In mass ratio by pre-polymer mixture and potassium iodide
120:1 is mixed in four-hole boiling flask, and 1, the 6- dibromo-hexane of 0.2 times of pre-polymer mixture quality of addition is molten into four-hole boiling flask
Liquid is 70 DEG C in temperature, under conditions of revolving speed is 320r/min, after being stirred to react 2h, additive blank is obtained, by additive blank
After petroleum ether extraction 3 times, filtering obtains filtrate to get additive；The dichloro that mass fraction is 12% is aoxidized into chromium solution and is sunk
Agent 1:3 in mass ratio in shallow lake is mixed in flask, and the dispersing agent of 0.5 times of chromium solution quality of dichloro oxidation, control are added into flask
The addition rate of dichloro oxidation chromium solution processed is 3mL/min, and the sodium hydroxide solution for being 12% with mass fraction is adjusted in flask
The pH to 10.0 of material, in temperature be 80 DEG C, revolving speed be 360r/min under conditions of, after being stirred to react 3h, by material in flask
After still aging 13h under room temperature, filtering must pre-process gel blank, treatment gel blank is washed with deionized
After 10 times, pretreatment gel is obtained, by pretreatment gel under high-temperature and high-pressure conditions, after constant temperature and pressure handles 2h, obtains zirconia powder
End；Zirconium oxide powder is mixed with additive 5:1 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 350r/min, stirs
After mixing mixing 60min, and in temperature be 70 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of after concentrated by rotary evaporation 6h,
Concentrate is obtained, under conditions of being 80 DEG C in temperature by concentrate after dry 2h, obtains anti-peeling zirconia coating Zirconium oxide powder
Blank, by anti-peeling zirconia coating Zirconium oxide powder blank and toluene 1:10 hybrid reactor in mass ratio, and to anti-
It answers and the anti-toluene di-isocyanate(TDI) for peeling off 0.3 times of zirconia coating Zirconium oxide powder blank quality is added in kettle, be in temperature
85 DEG C, after revolving speed is stirred to react 2h under conditions of being 320r/min, filtering must pre-process anti-peeling zirconia coating zirconium oxide
Powder batch, after anti-peeling zirconia coating Zirconium oxide powder blank acetone washing 5 times will be pre-processed, and in temperature be 80
Under conditions of DEG C after dry 2h, anti-peeling zirconia coating Zirconium oxide powder is obtained.The 1,6- dibromo-hexane solution be by 1,
6- dibromo-hexane is mixed with dehydrated alcohol 6:1 in mass ratio, obtains 1,6- dibromo-hexane solution.The precipitating reagent is that mass fraction is
Any one in the sodium hydroxide that 12% ammonium hydroxide or mass fraction is 5%.The dispersing agent is by polyethylene glycol 2000 and lemon
Sour ammonium 3:1 in mass ratio mixing, and 0.2 times of polyethylene glycol 2000 quality of ammonium polymethacrylate is added, after being stirred, obtain
Dispersing agent.The condition of the high temperature high pressure process is that temperature is 1000 DEG C, pressure 2.0MPa.The anti-peeling zirconia coating
It is to be sprayed at anti-peeling zirconia coating through plasma spray system with Zirconium oxide powder with the method therefor of Zirconium oxide powder
Behind metal surface, and the metal after spraying is immersed in the ethanol solution that mass fraction is 90%, after impregnating 2h, is filtered, it is dry,
Obtain wear-resisting zirconia coating.0.3 times of toluene di-isocyanate(TDI) quality of epoxy resin can be added in the toluene di-isocyanate(TDI),
The epoxy resin is epoxy resin E-44.0.2 times of additive quality of dopamine can be added in the additive.
Example 2
The dichloro that mass fraction is 12% is aoxidized into chromium solution and precipitating reagent 1:3 in mass ratio is mixed in flask, and into flask
The dispersing agent that dichloro aoxidizes 0.5 times of chromium solution quality is added, the addition rate of control dichloro oxidation chromium solution is 3mL/min, and
The pH to 10.0 that material in flask is adjusted with the sodium hydroxide solution that mass fraction is 12% is 80 DEG C in temperature, and revolving speed is
Under conditions of 360r/min, after being stirred to react 3h, by material in flask after still aging 13h under room temperature, filtering is obtained pre-
Treatment gel blank after treatment gel blank is washed with deionized 10 times, obtains pretreatment gel, by pretreatment gel in height
Under warm condition of high voltage, after constant temperature and pressure handles 2h, Zirconium oxide powder is obtained；The nanometer two for being 5% by Zirconium oxide powder and mass fraction
Silica dispersion liquid 1:3 in mass ratio mixing is 50 DEG C in temperature, under conditions of revolving speed is 350r/min, is stirred 60min
Afterwards, and in temperature it is 70 DEG C, revolving speed 150r/min, under conditions of pressure is 600kPa after concentrated by rotary evaporation 6h, obtains concentrate, it will
Under conditions of concentrate is 80 DEG C in temperature after dry 2h, anti-peeling zirconia coating Zirconium oxide powder blank is obtained, by anti-stripping
It falls in zirconia coating Zirconium oxide powder blank and toluene 1:10 hybrid reactor in mass ratio, and is added and prevents into reaction kettle
0.3 times of Zirconium oxide powder blank quality of toluene di-isocyanate(TDI) of zirconia coating is peeled off, is 85 DEG C in temperature, revolving speed is
After being stirred to react 2h under conditions of 320r/min, filtering must pre-process anti-peeling zirconia coating Zirconium oxide powder blank, will
After pre-processing anti-peeling zirconia coating Zirconium oxide powder blank acetone washing 5 times, and under conditions of temperature is 80 DEG C
After dry 2h, anti-peeling zirconia coating Zirconium oxide powder is obtained.The precipitating reagent is the ammonium hydroxide or quality that mass fraction is 12%
Any one in the sodium hydroxide that score is 5%.The dispersing agent is by polyethylene glycol 2000 and ammonium citrate 3:1 in mass ratio
Mixing, and 0.2 times of polyethylene glycol 2000 quality of ammonium polymethacrylate is added, after being stirred, obtain dispersing agent.The high temperature
The condition of HIGH PRESSURE TREATMENT is that temperature is 1000 DEG C, pressure 2.0MPa.The anti-peeling zirconia coating Zirconium oxide powder
Method therefor be by anti-peelings zirconia coating with Zirconium oxide powder after plasma spray system is sprayed at metal surface, and general
Metal after spraying immerses in the ethanol solution that mass fraction is 90%, after impregnating 2h, filters, dry, obtains wear-resisting zirconia painting
Layer.0.3 times of toluene di-isocyanate(TDI) quality of epoxy resin can be added in the toluene di-isocyanate(TDI), the epoxy resin is
Epoxy resin E-44.
Example 3
Alkali lignin and water 1:5 in mass ratio are mixed in beaker, and the sodium hydroxide solution for being 25% with mass fraction is adjusted
The pH to 11.0 of material, obtains alkali lignin solution in beaker, and alkali lignin solution and formaldehyde 25:1 in mass ratio are mixed in three
In mouth flask, it is 75 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 80min, temperature is warming up to 85
DEG C, then 0.2 times of alkali lignin solution quality of sodium sulfite is added into three-necked flask, continuing at temperature is 85 DEG C, and revolving speed is
After being stirred to react 3h under conditions of 350r/min, pre-polymer mixture is obtained；In mass ratio by pre-polymer mixture and potassium iodide
120:1 is mixed in four-hole boiling flask, and 1, the 6- dibromo-hexane of 0.2 times of pre-polymer mixture quality of addition is molten into four-hole boiling flask
Liquid is 70 DEG C in temperature, under conditions of revolving speed is 320r/min, after being stirred to react 2h, additive blank is obtained, by additive blank
After petroleum ether extraction 3 times, filtering obtains filtrate to get additive；The dichloro that mass fraction is 12% is aoxidized into chromium solution and is sunk
Agent 1:3 in mass ratio in shallow lake is mixed in flask, and the dispersing agent of 0.5 times of chromium solution quality of dichloro oxidation, control are added into flask
The addition rate of dichloro oxidation chromium solution processed is 3mL/min, and the sodium hydroxide solution for being 12% with mass fraction is adjusted in flask
The pH to 10.0 of material, in temperature be 80 DEG C, revolving speed be 360r/min under conditions of, after being stirred to react 3h, by material in flask
After still aging 13h under room temperature, filtering must pre-process gel blank, treatment gel blank is washed with deionized
After 10 times, pretreatment gel is obtained, by pretreatment gel under high-temperature and high-pressure conditions, after constant temperature and pressure handles 2h, obtains zirconia powder
End；Zirconium oxide powder is mixed with additive 1:3 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 350r/min, stirs
After mixing mixing 60min, and in temperature be 70 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of after concentrated by rotary evaporation 6h,
Concentrate is obtained, under conditions of being 80 DEG C in temperature by concentrate after dry 2h, obtains anti-peeling zirconia coating Zirconium oxide powder.
1, the 6- dibromo-hexane solution is to mix 1,6- dibromo-hexane with dehydrated alcohol 6:1 in mass ratio, obtains 1,6- dibromo-hexane
Solution.Any one in the sodium hydroxide that the precipitating reagent is the ammonium hydroxide that mass fraction is 12% or mass fraction is 5%.Described point
Powder be polyethylene glycol 2000 is mixed with ammonium citrate 3:1 in mass ratio, and be added 0.2 times of polyethylene glycol 2000 quality gather
Ammonium methacrylate after being stirred, obtains dispersing agent.The condition of the high temperature high pressure process is that temperature is 1000 DEG C, and pressure is
2.0MPa.The anti-method therefor for peeling off zirconia coating Zirconium oxide powder is by anti-peeling zirconia coating zirconium oxide
Powder immerses the ethyl alcohol that mass fraction is 90% after plasma spray system is sprayed at metal surface, and by the metal after spraying
In solution, after impregnating 2h, filter, it is dry, obtain wear-resisting zirconia coating.0.2 times of additive quality can be added in the additive
Dopamine.
Comparative example: the dichloro that mass fraction is 12% is aoxidized into chromium solution and precipitating reagent 1:3 in mass ratio is mixed in flask
In, and addition dichloro aoxidizes 0.5 times of chromium solution quality of dispersing agent, the addition rate of control dichloro oxidation chromium solution into flask
For 3mL/min, and the sodium hydroxide solution for being 12% with mass fraction adjusts the pH to 10.0 of material in flask, in temperature be 80
DEG C, under conditions of revolving speed is 360r/min, after being stirred to react 3h, by material in flask after still aging 13h under room temperature,
Filtering, must pre-process gel blank, after treatment gel blank is washed with deionized 10 times, obtain pretreatment gel, will locate in advance
Gel is managed under high-temperature and high-pressure conditions, after constant temperature and pressure handles 2h, obtains Zirconium oxide powder；It is by Zirconium oxide powder and mass fraction
5% nano silicon dioxide dispersion 1:3 in mass ratio mixing is 50 DEG C in temperature, under conditions of revolving speed is 350r/min, stirs
After mixing mixing 60min, and in temperature be 70 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of after concentrated by rotary evaporation 6h,
Concentrate is obtained, under conditions of being 80 DEG C in temperature by concentrate after dry 2h, obtains anti-peeling zirconia coating Zirconium oxide powder.
Any one in the sodium hydroxide that the precipitating reagent is the ammonium hydroxide that mass fraction is 12% or mass fraction is 5%.The dispersing agent
To mix polyethylene glycol 2000 with ammonium citrate 3:1 in mass ratio, and 0.2 times of polyethylene glycol 2000 quality of poly- methyl is added
Ammonium acrylate after being stirred, obtains dispersing agent.The condition of the high temperature high pressure process is that temperature is 1000 DEG C, and pressure is
2.0MPa.The anti-method therefor for peeling off zirconia coating Zirconium oxide powder is by anti-peeling zirconia coating zirconium oxide
Powder immerses the ethyl alcohol that mass fraction is 90% after plasma spray system is sprayed at metal surface, and by the metal after spraying
In solution, after impregnating 2h, filter, it is dry, obtain wear-resisting zirconia coating.
The anti-peeling zirconia coating Zirconium oxide powder of 1 to 3 gained of example and comparative example product are subjected to performance detection, had
Body detecting method is as follows:
1. wearability: using Metco-9MB type high energy plasma paint finishing by 1 to the 3 anti-peeling zirconia coating of gained of example
It is sprayed at Zirconium oxide powder and comparative example product on the stainless steel test specimen of the mm × 6 of 20 mm × 15 mm, it will be stainless after spraying
Steel test specimen immerses in the ethanol solution that mass fraction is 90%, and after impregnating 2h, after dry, test specimen is worn in MM-200 type for filtering
On testing machine under conditions of 200N, the wearability examination of coating is carried out, observation coating grinds off the time used completely, specifically examined
The results are shown in Table 1 for survey:
2. adhesive force: using Metco-9MB type high energy plasma paint finishing by 1 to the 3 anti-peeling zirconia coating of gained of example
It is sprayed at Zirconium oxide powder and comparative example product on the stainless steel test specimen of the mm × 6 of 20 mm × 15 mm, it will be stainless after spraying
Steel test specimen immerses in the ethanol solution that mass fraction is 90%, after impregnating 2h, filtering, after dry, by test specimen in temperature be 60 DEG C
Under the conditions of stand 30 days after, observe the state of surface of test piece, specific testing result is as shown in table 1:
Table 1: wearability and adhesion performance detect table
By 1 testing result of table it is found that the anti-peeling zirconia coating of present invention gained has excellent wearability with Zirconium oxide powder
Can, and adhesive force is preferable when product use.
Claims (9)
1. a kind of anti-preparation method for peeling off zirconia coating Zirconium oxide powder, which is characterized in that specific preparation step are as follows:
(1) alkali lignin is mixed with water 1:3~1:5 in mass ratio, and adjusts pH to 10.5~11.0, it is molten to obtain alkali lignin
Liquid mixes alkali lignin solution with formaldehyde 15:1~25:1 in mass ratio, and after being stirred to react, heating adds alkali lignin
The sodium sulfite that 0.1~0.2 times of solution quality continues after being stirred to react, obtains pre-polymer mixture；
(2) pre-polymer mixture is mixed with potassium iodide 100:1~120:1 in mass ratio, and pre-polymer mixture quality is added
0.1~0.2 times of 1,6- dibromo-hexane solution, after being stirred to react, extracts, and filtering obtains filtrate to get additive；
(3) dichloro oxidation chromium solution is mixed with precipitating reagent 1:2~1:3 in mass ratio, and dichloro oxidation chromium solution quality is added
0.2~0.5 times of dispersing agent is stirred to react, and still aging after adjusting pH, is filtered, and washing obtains pretreatment gel, will locate in advance
After managing gel high temperature high pressure process, Zirconium oxide powder is obtained；
(4) Zirconium oxide powder is mixed with additive 1:2~1:3 in mass ratio, concentrated by rotary evaporation, it is dry, obtain anti-peeling zirconium oxide
Coating Zirconium oxide powder blank, by anti-peeling zirconia coating Zirconium oxide powder blank and toluene 1:8~1 in mass ratio:
10 mixing, and the anti-toluene di-isocyanate(TDI) for peeling off 0.2~0.3 times of zirconia coating Zirconium oxide powder blank quality is added,
It after being stirred to react, filters, washs, it is dry, obtain anti-peeling zirconia coating Zirconium oxide powder.
2. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: extractant used in step (2) described extraction is petroleum ether.
3. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: step (2) 1, the 6- dibromo-hexane solution is to mix 1,6- dibromo-hexane with dehydrated alcohol 5:1~6:1 in mass ratio,
Obtain 1,6- dibromo-hexane solution.
4. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: step (3) described precipitating reagent is to appoint in the ammonium hydroxide that mass fraction is 10~12% or the sodium hydroxide that mass fraction is 2~5%
It anticipates one kind.
5. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: step (3) dispersing agent is to mix polyethylene glycol 2000 with ammonium citrate 3:1 in mass ratio, and polyethylene glycol is added
The ammonium polymethacrylate of 2000 0.1~0.2 times of mass, after being stirred, obtains dispersing agent.
6. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: the condition of step (3) described high temperature high pressure process is that temperature is 800~1000 DEG C, and pressure is 1.8~2.0MPa.
7. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: the anti-method therefor for peeling off zirconia coating Zirconium oxide powder is by anti-peeling zirconia coating Zirconium oxide powder
The ethanol solution that mass fraction is 90% is immersed after plasma spray system is sprayed at metal surface, and by the metal after spraying
In, after impregnating 1~2h, filter, it is dry, obtain wear-resisting zirconia coating.
8. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: 0.1~0.3 times of toluene di-isocyanate(TDI) quality of epoxy resin, institute can be added in step (4) described toluene di-isocyanate(TDI)
Stating epoxy resin is any one in epoxy resin E-44 or epoxy resin E-51.
9. the anti-preparation method for peeling off zirconia coating Zirconium oxide powder of one kind according to claim 1, feature exist
In: 0.1~0.2 times of additive quality of dopamine can be added in step (2) described additive.
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