CN108149230B - High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating - Google Patents

High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating Download PDF

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CN108149230B
CN108149230B CN201711482218.5A CN201711482218A CN108149230B CN 108149230 B CN108149230 B CN 108149230B CN 201711482218 A CN201711482218 A CN 201711482218A CN 108149230 B CN108149230 B CN 108149230B
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speed steel
high speed
steel plate
composite coating
beaker
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CN108149230A (en
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曾群锋
蔡双利
李双江
陈通
陈萱
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Xian Jiaotong University
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Xian Jiaotong University
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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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material

Abstract

High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating forms colloidal sol by the hydrolysis condensation reaction of presoma using sol-gal process, and colloidal sol forms wet gel after standing a couple of days, and wet gel is coated on high speed steel substrate surface, a nanometer γ-Fe is obtained after Overheating Treatment2O3/SiO2Composite coating, the obtained nanometer γ-Fe of the present invention2O3/SiO2Composite coating has core-shell structure, and the low friction less than 0.1 may be implemented under high temperature environment.

Description

High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating
Technical field
The present invention relates to the preparation method of composite coating, in particular to low friction nanometer in steel matrix under a kind of worst hot case γ-Fe2O3/SiO2The preparation method of composite coating, the disengagement area and sol volume of container when according to colloidal sol to gel conversion Ratio control nanometer γ-Fe2O3/SiO2The particle size distribution of compound, and then control the high Temperature Tribological of composite coating Energy.
Background technique
Nano-composite coating, which refers to, to be added nano material in matrix surface coating by specific technique or will directly receive Coating is made in rice material.Nano coating has the characteristics that high rigidity, high-wearing feature, excellent toughness, while having inoxidizability, resistance to High temperature, therefore nano-composite coating is to solve the problems, such as high temperature friction effective scheme.
Nanometer γ-Fe2O3/SiO2Composite coating refers to, with unformed cellular SiO2Wrap up nanometer γ-Fe2O3Particle, with Core-shell structure is formed, matrix surface is then coated in by special process.As a kind of anti-friction coating applied to worst hot case, Nanometer γ-Fe2O3/SiO2γ-Fe in compound2O3Play main antifriction function, cellular SiO2It is conducive to reduce as carrier The agglomeration of particle.Nanometer γ-Fe2O3/SiO2Composite coating have high temperature antifriction performance is good, property is stable, to environment without dirt Dye and it is low in cost the advantages that, but the Ratio control of the container disengagement area of gelation link and sol volume is not in preparation process Strictly there is great influence to the nucleation process of nano-complex and particle size distribution, be likely to result in particle size distribution not , core-shell structure can not generate.
Summary of the invention
In order to solve above-mentioned high temperature low friction nano-composite coating because gelation disengagement area volume ratio state modulator not The bad problem of coating performance that is sufficient and generating, the present invention provides high temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2It is multiple The preparation method for closing coating, for the sol-gal process technique of nano-composite coating, especially gelation disengagement area volume ratio Control, can effectively improve antifriction performance at a high temperature of the coating that sol-gal process obtains.
To achieve the goals above, the technical solution adopted by the present invention is that:
High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating, comprising the following steps:
The first step prepares colloidal sol: taking nine water ferric nitrate lavender crystal and ethyl orthosilicate colourless liquid molar ratio is 0.57:1 is successively poured into beaker, adds ethanol solution, is made the molar ratio 1:17.5 of ethyl orthosilicate and ethyl alcohol, is used glass The stirring of glass stick makes it after mixing, and hydrochloric acid is added dropwise, is configured to the solution of PH=0.9, beaker is placed on magnetic stirring apparatus, Magnetic agitation 2h forms transparent colloidal sol；
Second step prepares wet gel: colloidal sol being transferred in teflon pipe, is then allowed to stand in drying box in 50-80 DEG C of drying A couple of days generates wet gel, and the evaporation surface of teflon pipe and the volume ratio of colloidal sol are 0.01-0.04, i.e. S/V=0.01- 0.04；
The processing of third step high speed steel substrate: being rinsed using a large amount of deionized waters, and big of the attachment of removal high speed steel plate surface Grain pollutant；10~20min is steeped with acetone in draught cupboard, such as finds that there are Visible pollutants on high speed steel plate surface, use third The wiping of ketone cotton balls；High speed steel plate is put into the beaker equipped with ethyl alcohol, is put into supersonic cleaning machine and is cleaned by ultrasonic 10~20min； High speed steel plate is taken out, is rinsed with a large amount of deionized waters；High speed steel plate is put into the beaker cleaned up, with preservative film to beaker It is sealed, is put into drying box dry；
Coat gel on 4th step matrix: the high speed steel plate that third step is handled well takes two to be placed on testing stand, so The wet gel for taking out preparation afterwards is placed on a high speed steel plate, and two high speed steel plates are combined rotary squeezing, enable gel It is enough evenly distributed on two disks, enables thickness of the gel on high speed steel plate not less than 0.5mm.
The heat treatment of 5th step: two high speed steel plates are placed in 50 DEG C of vacuum ovens dry 1h, in Muffle furnace After 400~600 DEG C of heat treatment 4h, separated after two high-speed steel steel disks are taken out to get composite coating sample is arrived.
Advantages of the present invention are as follows: process equipment requires simple, low processing cost, is suitble to be prepared in large quantity.
Specific embodiment
Embodiment one
The production technology of the present embodiment is achieved in that
The first step prepares colloidal sol: taking nine water ferric nitrate lavender crystal of 10.261g (0.0254mol) and 10ml (0.044mol) ethyl orthosilicate colourless liquid, is successively poured into beaker, adds 45ml ethanol solution, is made with glass bar stirring It is added dropwise hydrochloric acid, makes solution PH=0.9 after mixing.Beaker is placed on magnetic stirring apparatus, magnetic agitation 2h, is formed Transparent colloidal sol.
Second step prepares wet gel: it is 36mm that colloidal sol, which is transferred to bore, and volume is the teflon pipe (S/V=of 100ml 0.02) it in, is then allowed to stand in drying box in 50 DEG C of dry 8 days generation wet gels.
The processing of third step high speed steel substrate: the high speed steel plate that diameter is 30mm is rinsed using a large amount of deionized waters, removal is high The bulky grain pollutant of fast steel disk surface attachment；10min is steeped with acetone in draught cupboard, such as discovery high speed steel plate surface exists can See pollutant, is wiped using acetone cotton balls；High speed steel plate is put into the beaker equipped with ethyl alcohol, is put into supersonic cleaning machine ultrasonic Clean 20min；High speed steel plate is taken out, is rinsed with a large amount of deionized waters；High speed steel plate is put into the beaker cleaned up, is used Preservative film is sealed beaker, is put into dried for standby in drying box.
Coat gel on 4th step matrix: the high speed steel plate that third step is handled well takes two to be placed on testing stand, so The wet gel 2ml for taking out preparation afterwards is placed on a high speed steel plate, and two high speed steel plates are combined rotary squeezing, make gel It can be evenly distributed on two disks.Enable thickness 0.7mm of the gel on high speed steel plate；
The heat treatment of 5th step: two high speed steel plates are placed in 50 DEG C of vacuum ovens dry 1h, in Muffle furnace After 400 DEG C of heat treatment 4h, separated after two high-speed steel steel disks are taken out to get composite coating sample is arrived.
Nanometer γ-Fe manufactured in the present embodiment2O3/SiO2The TEM shape appearance figure of composite material is as shown in Figure 1, can be with by figure Find out that the surface of nano iron oxide coats really and gone up layer of silicon dioxide, wadding poly structure is presented in final sample, shows nucleocapsid The nanometer particle of structure.
Fig. 2 gives the nanometer γ-Fe of the preparation of embodiment 12O3/SiO2The XRD phenogram of composite material, in 2 θ of the angle of diffraction Spike at=29.58 °, 34.96 °, 40.26 °, 42.85 °, 53.48 °, 56.87 °, 62.37 ° belongs to γ-Fe2O3.The angle of diffraction Disperse peak and unformed SiO near 2 27 ° of θ ≈2Corresponding disperse peak is consistent.
By the nanometer γ-Fe in embodiment 12O3/SiO2Composite coating carries out high temperature friction and wear experiment.Fig. 3 is nanometer γ-Fe2O3/SiO2The relational graph that the coefficient of friction of composite coating at different temperatures changes over time.At 500 DEG C~600 DEG C Temperature section, there is the value less than 0.1 in coefficient of friction during changing, minimum to reach 0.06, and maintains a period of time.
Embodiment two
The production technology of the present embodiment is achieved in that
The first step prepares colloidal sol: taking nine water ferric nitrate lavender crystal of 10.261g (0.0254mol) and 10ml (0.044mol) ethyl orthosilicate colourless liquid, is successively poured into beaker, adds 45ml ethanol solution, is made with glass bar stirring It is added dropwise hydrochloric acid, makes solution PH=0.9 after mixing.Beaker is placed on magnetic stirring apparatus, magnetic agitation 2h, is formed Transparent colloidal sol.
Second step prepares wet gel: it is 18mm that colloidal sol, which is transferred to bore, and volume is the teflon pipe (S/V=of 100ml 0.01) it in, is then allowed to stand in drying box in 80 DEG C of dry 5 days generation wet gels.
The processing of third step high speed steel substrate: the high speed steel plate that diameter is 30mm is rinsed using a large amount of deionized waters, removal is high The bulky grain pollutant of fast steel disk surface attachment；10min is steeped with acetone in draught cupboard, such as discovery high speed steel plate surface exists can See pollutant, is wiped using acetone cotton balls；High speed steel plate is put into the beaker equipped with ethyl alcohol, is put into supersonic cleaning machine ultrasonic Clean 20min；High speed steel plate is taken out, is rinsed with a large amount of deionized waters；High speed steel plate is put into the beaker cleaned up, is used Preservative film is sealed beaker, is put into dried for standby in drying box.
Coat gel on 4th step matrix: the high speed steel plate that third step is handled well takes two to be placed on testing stand, so The wet gel 2ml for taking out preparation afterwards is placed on a high speed steel plate, and two high speed steel plates are combined rotary squeezing, make gel It can be evenly distributed on two disks, enable thickness 0.5mm of the gel on high speed steel plate；
The heat treatment of 5th step: two high speed steel plates are placed in 50 DEG C of vacuum ovens dry 1h, in Muffle furnace After 450 DEG C of heat treatment 4h, separated after two high-speed steel steel disks are taken out to get composite coating sample is arrived.
The performance of sample obtained by the present embodiment: during 500 DEG C~600 DEG C of temperature section, coefficient of friction variation not Reach the stable value less than 0.1.
Embodiment three
The production technology of the present embodiment is achieved in that
The first step prepares colloidal sol: taking nine water ferric nitrate lavender crystal of 10.261g (0.0254mol) and 10ml (0.044mol) ethyl orthosilicate colourless liquid, is successively poured into beaker, adds 45ml ethanol solution, is made with glass bar stirring It is added dropwise hydrochloric acid, makes solution PH=0.9 after mixing.Beaker is placed on magnetic stirring apparatus, magnetic agitation 2h, is formed Transparent colloidal sol.
Second step prepares wet gel: it is 36mm that colloidal sol, which is transferred to bore, and volume is the teflon pipe (S/V=of 100ml 0.02) it in, is then allowed to stand in drying box in 80 DEG C of dry 5 days generation wet gels.
The processing of third step high speed steel substrate: the high speed steel plate that diameter is 30mm is rinsed using a large amount of deionized waters, removal is high The bulky grain pollutant of fast steel disk surface attachment；10min is steeped with acetone in draught cupboard, such as discovery high speed steel plate surface exists can See pollutant, is wiped using acetone cotton balls；High speed steel plate is put into the beaker equipped with ethyl alcohol, is put into supersonic cleaning machine ultrasonic Clean 20min；High speed steel plate is taken out, is rinsed with a large amount of deionized waters；High speed steel plate is put into the beaker cleaned up, is used Preservative film is sealed beaker, is put into dried for standby in drying box.
Coat gel on 4th step matrix: the high speed steel plate that third step is handled well takes two to be placed on testing stand, so The wet gel 4ml for taking out preparation afterwards is placed on a high speed steel plate, and two high speed steel plates are combined rotary squeezing, make gel It can be evenly distributed on two disks, enable thickness 0.6mm of the gel on high speed steel plate；
The heat treatment of 5th step: two high speed steel plates are placed in 50 DEG C of vacuum ovens dry 1h, in Muffle furnace After 450 DEG C of heat treatment 4h, separated after two high-speed steel steel disks are taken out to get composite coating sample is arrived.
The performance of sample obtained by the present embodiment: during 500 DEG C~600 DEG C of temperature section, coefficient of friction variation not Reach the stable value less than 0.1.

Claims (1)

1. high temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating, which is characterized in that including with Lower step:
The first step prepares colloidal sol: taking nine water ferric nitrate lavender crystal and ethyl orthosilicate colourless liquid is 0.57:1 in molar ratio It successively pours into beaker, adds ethanol solution, make the molar ratio 1:17.5 of ethyl orthosilicate and ethyl alcohol, stirred with glass bar Make it after mixing, hydrochloric acid is added dropwise, is configured to the solution of pH=0.9, beaker is placed on magnetic stirring apparatus, magnetic agitation 2h forms transparent colloidal sol；
Second step prepares wet gel: colloidal sol being transferred in teflon pipe, is then allowed to stand in drying box in 50-80 DEG C of dry a couple of days Wet gel is generated, the evaporation surface of teflon pipe and the volume ratio of colloidal sol are 0.01-0.04, i.e. S/V=0.01-0.04；
The processing of third step high speed steel substrate: being rinsed with deionized water, the bulky grain pollutant of removal high speed steel plate surface attachment；? 10~20min is steeped with acetone in draught cupboard, such as finds that there are Visible pollutants on high speed steel plate surface, are wiped using acetone cotton balls； High speed steel plate is put into the beaker equipped with ethyl alcohol, is put into supersonic cleaning machine and is cleaned by ultrasonic 10~20min；Take out high-speed steel Disk is rinsed with deionized water；High speed steel plate is put into the beaker cleaned up, beaker is sealed with preservative film, is put into It is dry in drying box；
Coat gel on 4th step matrix: the high speed steel plate that third step is handled well takes two to be placed on testing stand, then takes The wet gel prepared out is placed on a high speed steel plate, and two high speed steel plates are combined rotary squeezing, keep gel equal It is distributed on two disks evenly, enables thickness of the gel on high speed steel plate not less than 0.5mm；
The heat treatment of 5th step: being placed in 50 DEG C of vacuum ovens dry 1h for two high speed steel plates, 400 in Muffle furnace~ After 600 DEG C of heat treatment 4h, separated after two high-speed steel steel disks are taken out to get composite coating sample is arrived.
CN201711482218.5A 2017-12-29 2017-12-29 High temperature low friction nanometer γ-Fe in steel matrix2O3/SiO2The preparation method of composite coating Active CN108149230B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105113213A (en) * 2015-07-21 2015-12-02 上海工程技术大学 Method for preparation of antioxidant composite coating on carbon fiber surface
CN105289659A (en) * 2015-09-29 2016-02-03 合肥学院 SiO2-MoS2 mesoporous composite nano material and preparation method and application thereof
CN105948817A (en) * 2016-04-18 2016-09-21 江苏大学 Preparation method for superhydrophilic-underwater superoleophobic composite film coating
CN107337423A (en) * 2017-07-03 2017-11-10 南京凤源新材料科技有限公司 A kind of nano-cellulose enhancing silicon dioxide silica aerogel composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105113213A (en) * 2015-07-21 2015-12-02 上海工程技术大学 Method for preparation of antioxidant composite coating on carbon fiber surface
CN105289659A (en) * 2015-09-29 2016-02-03 合肥学院 SiO2-MoS2 mesoporous composite nano material and preparation method and application thereof
CN105948817A (en) * 2016-04-18 2016-09-21 江苏大学 Preparation method for superhydrophilic-underwater superoleophobic composite film coating
CN107337423A (en) * 2017-07-03 2017-11-10 南京凤源新材料科技有限公司 A kind of nano-cellulose enhancing silicon dioxide silica aerogel composite material and preparation method thereof

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