CN104141122B - A kind of metal base surface aluminum oxide coating layer and preparation method thereof - Google Patents
A kind of metal base surface aluminum oxide coating layer and preparation method thereof Download PDFInfo
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- CN104141122B CN104141122B CN201310517848.7A CN201310517848A CN104141122B CN 104141122 B CN104141122 B CN 104141122B CN 201310517848 A CN201310517848 A CN 201310517848A CN 104141122 B CN104141122 B CN 104141122B
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Abstract
The invention discloses a kind of metal base surface aluminum oxide coating layer and preparation method thereof, aluminum oxide coating layer is mainly made up of γ phase aluminas, between thickness is 1 micron to 10 microns, described matrix is the alloy materials such as Ge Shi hardness ＜ 40 carbon steel, structural steel.By water, the organic alcohol compound of aluminium and inorganic acid, proportionally heating stirring obtains alumina sol, colloidal sol is subjected to hydro-thermal process afterwards, the colloidal sol after hydro-thermal process is subjected to repeatedly coating drying in metal base surface again, calcination processing is finally carried out in the hot environment below 500 DEG C, acquisition has certain thickness, fine and close γ phase alumina coatings.Aluminum oxide coating layer provided by the invention is not only anticorrosive, anti-permeability is good, and has certain thickness and good compactness.
Description
Technical field
The invention belongs to metal surface treatment technology, and in particular to a kind of metal base surface aluminum oxide coating layer and its preparation
Method, it mainly for alloy and other metallic articles surface treatment, more particularly, to high temperature alloy, equipment and various steel
The anticorrosion of pipeline, impermeable and heat insulating coat.
Background technology
Sol-gel process is a kind of coat preparing technology being surface-treated to metal, using sol-gel technique energy
It is enough that ceramics or organic coating with specific function are prepared on the matrixes such as glass, plastics, metal（Chandradass J,
Balasubramanian M,Effect of magnesium oxide on sol-gel spun alumina and
alumina-zirconia fibres[J].Journal of the European Ceramic Society,2006,26
(13):2611-2617）.In the seventies of eighties of last century six, as the energy, manufacture and electronic communication field are to material property
It is required that more and more higher, sol-gel（Sol-Gel）The technology of method prepares coating starts widely to be paid attention to.Colloidal sol is by straight
Footpath only has the dispersion that tens nanometers of colloidal particles and solution are collectively forming, and has a higher surface energy, absorption property compared with
By force, thus easily in substrate deposit.Simultaneously because the sol particles adsorption electric charge of same alike result, makes it due to mutual
Repel and form dispersion steady in a long-term.Sol-Gel methods have following several ways：（1）Organic alkoxide Hydrolyze method；（2）Have
Machine reactive polymeric method；（3）Inorganic dispersion method etc..Figure below is this several process for obtaining gel method.
Method using Sol-Gel prepares coatings is similar, and matrix is infiltrated in colloidal sol or colloidal sol rotary coating is existed
Matrix surface, afterwards drying and certain heat treatment process so that obtain needed for ceramic coating.Using high-temperature calcination
Method prepare aluminum oxide coating layer, it is necessary to which the γ phase oxidation aluminium laminations with corrosion resistance could be formed more than 800 DEG C,
More than 1200 DEG C calcinings could obtain alpha-phase aluminum oxide the most stable, and as the metal material of coated substrate, mostly 600
Undergone phase transition more than DEG C, performance is remarkably decreased.Meanwhile coating layer thickness prepared by conventional sol method is relatively low, is typically 500nm
Hereinafter, the protective effect unobvious for matrix, therefore, the method that under relative low temperature prepared by high thickness oxidation aluminized coating is studied,
There is important theory and engineering significance for the performance such as the efficiency for improving coating and the Mechanics of Machinery for ensureing metallic matrix.
The content of the invention
The purpose of the present invention be for conventional sol method prepare aluminum oxide coating layer thickness is relatively low, heat treatment temperature is higher
Defect, there is provided a kind of aluminum oxide coating layer and preparation method of the processing of hydro-thermal assisting sol.Present invention also offers the γ phase oxidations
The preparation method of aluminized coating.
Metal base surface γ phase alumina coatings provided by the invention, the metal base surface coating is by γ phase aluminas
Form, between 1 micron to 10 microns of thickness, between 200 nanometers to 1000 nanometers of crystallite dimension, described matrix is Ge Shi hardness ＜
40 metal material.
Described metal material is the metals such as iron, carbon steel, nickel-base alloy.
The preparation method of above-mentioned metal base surface aluminum oxide coating layer is：
（1）By the organic alcohol compound of aluminium, water and inorganic acid according to (0.5~1.5):(100~80):(0.05~0.15)
Molar ratio uniformly mix, the stirring reaction between 70 DEG C and 95 DEG C, wherein inorganic acid are added in whipping process, finally
Obtain transparent colloidal sol；
（2）Colloidal sol made above is placed in hydrothermal reaction kettle, between compactedness is 30% to 70%, sealing reaction afterwards
Kettle, heat the colloidal sol of inside and be incubated 6 to 18 hours；
（3）Colloidal sol after isothermal holding is taken out, by the way of rotary coating, i.e., consolidated metallic matrix on spin coater
Fixed rotation, uniform fold surface is allowed to above colloidal sol is constantly dropped into matrix surface, obtains and has cated matrix；
（4）By step（3）The cated matrix drying of tool of acquisition repeats untill surface liquid film solidifies（3）（4）Cross
Journey, obtain the alumina sol coating of different-thickness；
（5）The sample obtained by above procedure is put into high-temperature electric resistance furnace, heating rate be heated to 400 DEG C to 500 DEG C it
Between, after being incubated 1 hour to 6 hours, acquisition has certain thickness aluminum oxide coating layer.
Described inorganic acid is the dilute solution of the strong acid such as nitric acid, hydrochloric acid, sulfuric acid.
The alumina sol that the present invention is crossed using hydro-thermal process, wettability improves, is brilliant after being crossed using its hydro-thermal process
The characteristics of type transition temperature declines, repeatedly coats in matrix surface, forms the higher alumina sol layer of thickness, then by relatively low
Calcining heat complete crystal transfer, can be formed at 500 DEG C with certain thickness, densification, corrosion resistance it is excellent
γ phase alumina coatings, coating layer thickness is high, can be widely used in the technologies such as anti-oxidant, anticorrosion, heat-insulated and gas barrier
Field.
Brief description of the drawings
Fig. 1,2,3,4,5 are according to patent system of the present invention standby coating structure and coating characterization, and Fig. 1 is coating structure signal
Figure；Coating cross sections SEM pictures before Fig. 2 is heat treatment；Fig. 3 is coating cross sections SEM after heat treatment（SEM）
Picture；Fig. 4 is the surface SEM pictures of coating after heat treatment；Fig. 5 is the X-ray diffraction analysis of coating surface thing phase（XRD）.
Fig. 6,7,8 be according to existing conventional method prepare coating and microscopic features, Fig. 6 be the section SEM pictures of coating,
Fig. 7 is the section SEM pictures of coating after heat treatment, and Fig. 8 is the XRD analysis of coating surface thing phase after heat treatment.
Embodiment
As shown in figure 1, metal base surface γ phase aluminas coating provided by the invention by mainly by with matrix surface knot
Close alumina layer to form, total coating thickness is 1 micron to 10 microns.
Matrix can be the various equipment being made up of metal materials such as alloy, structural steel, must be through before coating preparation
Past oil processing.
Example 1：
（1）By distilled water, isobutanol aluminum and hydrochloric acid according to 90:1:0.15 molar ratio is well mixed, in 85 DEG C of stirrings
Reaction 4 hours, wherein hydrochloric acid is added in whipping process, finally obtains transparent colloidal sol；
（2）Colloidal sol made above is placed in hydrothermal reaction kettle, compactedness 70%, seals reactor afterwards, in heating
The colloidal sol in portion is to being incubated 12 hours after 210 DEG C；
（3）By 40# carbon steels（Ge Shi hardness=35）Surface clean is processed by shot blasting after deoiling；
（4）Colloidal sol after isothermal holding is taken out, by the way of rotary coating, i.e., the fixed rotation on spin coater by carbon steel
Turn, be allowed to uniform fold surface above colloidal sol is constantly dropped into matrix surface, spin coater rotating speed is 50 revs/min；
（5）Rotary coating stops colloidal sol and is added dropwise and rotates after 30 seconds, matrix is dried to surface liquid film in atmosphere and solidified
Untill, repeat（3）（4）Process 6 to 10 times, obtain alumina sol coating；
（6）The sample obtained by above procedure is put into high-temperature electric resistance furnace, heated with the heating rate less than 5 DEG C/min
To 460 DEG C, the γ phase alumina coatings for obtaining well-crystallized are taken out in insulation after 3 hours.Example 2：
(1) by deionized water and aluminium isopropoxide（Analyze pure）Added according to the ratio of mol ratio 100 to 1 in there-necked flask,
Magnetic agitation is heated to 85 DEG C in water-bath, adds the nitric acid that molar ratio is 0.1 afterwards, continues insulated and stirred 6 hours, obtains saturating
Bright alumina sol.
(2) experiment is used into 600 mesh, 1500 mesh, 3000 purposes successively with martensite steel (Ge Shi hardness=30) matrix surface
Sand paper carries out sanding and polishing on polishing machine, and matrix is inserted into progress ultrasonic wave cleaning in acetone afterwards, removes the greasy dirt on surface
After be placed in kept dry in vacuum drying chamber.
(3) alumina sol of acquisition is imported in hydrothermal reaction kettle, compactedness 50%, reactor is put into 200 DEG C
Taken out after being incubated 12 hours in baking oven.
(4) matrix is fixed on spin coater, 120 revs/min of rotating speed, uses acid buret by above-mentioned colloidal sol with 10
The speed of drop/minute drops to matrix surface, stops operating and is added dropwise after 30 seconds, and matrix is placed in vacuum desiccator 2 hours,
9 simultaneously drying process of dropwise addition and rotary course are repeated afterwards, it can be seen that coating layer thickness is about 10 microns under ESEM（Figure
2）, and inner homogeneous is fine and close.
(5) coating sample is put into 500 DEG C of electric furnaces, after being incubated 180 minutes, takes out and coating section is observed under ESEM
Face（Fig. 3）, it can be seen that coating layer thickness reaches 10 microns, and there is the densification that particle diameter is 100 nanometers to 1000 nanometers on its surface
Crystal grain（Fig. 4）Form.
(6) using X-ray diffractometer analysis coating surface thing phase, it can be seen that coating is all made up of γ phase aluminas
（Fig. 5）.
Example 3：
(1) by pure water and aluminium isopropoxide（Technical grade）Added according to the ratio of mol ratio 100 to 1 in there-necked flask, in water
Mechanical agitation is heated to 80 DEG C in bath, adds the nitric acid that molar ratio is 0.1 afterwards, continues insulated and stirred 10 hours, is connect
The alumina sol of near-transparent.
(2) it will test and polished successively using the sand paper of 600 mesh, 1500 mesh with 9Cr steel (Ge Shi hardness=35) matrix surface
Sanding and polishing is carried out on machine, matrix is inserted into progress ultrasonic wave cleaning in absolute ethyl alcohol afterwards, is placed in after removing the greasy dirt on surface
Kept dry in vacuum desiccator.
(3) alumina sol of acquisition is imported in hydrothermal reaction kettle, compactedness 70%, reactor is put into 220 DEG C
Taken out after being incubated 12 hours in baking oven.
(4) matrix is fixed on spin coater, 80 revs/min of rotating speed, use acid buret by above-mentioned colloidal sol with 10 drop/
The speed of minute drops to matrix surface, stops operating and is added dropwise after 30 seconds, and matrix is placed 2 hours in atmosphere, repeated afterwards
3 simultaneously drying process of dropwise addition and rotary course, it can be seen that coating layer thickness is about 2 microns under ESEM, and it is internal equal
Even densification.
(5) coating sample is put into 450 DEG C of electric furnaces, after being incubated 300 minutes, takes out the observation coating table under ESEM
Face and section, coating layer thickness are 1 micron, and its surface has the compact-grain that particle diameter is 100 nanometers to 300 nanometers to form.
(6) using X-ray diffractometer analysis coating surface thing phase, it can be seen that coating is all made up of γ phase aluminas.
Comparative example 1:
Aluminum oxide coating layer is prepared using existing conventional sol method：
(1) by deionized water and aluminium isopropoxide（Analyze pure）Added according to the ratio of mol ratio 100 to 0.5 in there-necked flask,
Magnetic agitation is heated to 85 DEG C in a water bath, adds the nitric acid that molar ratio is 0.1 afterwards, continues insulated and stirred 6 hours, obtains
Transparent alumina sol.
(2) experiment is used into 600 mesh, 1500 mesh, 3000 purposes successively with martensite steel (Ge Shi hardness=30) matrix surface
Sand paper carries out sanding and polishing on polishing machine, and matrix is inserted into progress ultrasonic wave cleaning in acetone afterwards, removes the greasy dirt on surface
After be placed in kept dry in vacuum drying chamber.
(3) martensite steel matrix is fixed on spin coater, 120 revs/min of rotating speed, using acid buret by aluminum oxide
Colloidal sol drops to matrix surface with the speed of 10 drops/minute, stops operating and is added dropwise after 30 seconds, and matrix is placed on into vacuum desiccator
In 2 hours, repeat to be added dropwise afterwards with rotary course 9 times and drying process, it can be seen that coating layer thickness is only 2 under ESEM
Micron（Fig. 6）.
(4) coating sample is put into 500 DEG C of electric furnaces, after being incubated 180 minutes, takes out and coating section is observed under ESEM
Face（Fig. 7）, it can be seen that coating layer thickness is 2 microns, and occurs crackle between coating and matrix.
(5) using X-ray diffractometer analysis coating surface thing phase, it can be seen that alumina sol coating is not tied
Crystalline substance, i.e., no γ phase aluminas generation（Fig. 8）.
As can be seen here, aluminum oxide coating layer that patent of the present invention provides and preparation method thereof can be realized at a lower temperature
Prepare the higher γ phase alumina coatings of thickness.The coating can be used as tritium permeation coating and other be related to anticorrosion, anti-oxidation
Etc. the protective coating of equipment.Matrix is the metal material such as steel or other alloys.Mainly using hydro-thermal process assisting sol gel with
It is prepared by the mode of calcining.Colloidal sol is pre-processed using the mode of hydro-thermal process, purpose mainly improves colloidal sol in matrix table
The wettability in face, improves the thickness of coating, and reduces the crystal transfer temperature of aluminum oxide.
Claims (2)
- A kind of 1. metal base surface aluminum oxide coating layer, it is characterised in that：The metal base surface aluminum oxide coating layer is mainly by γ Phase alumina is formed, and between thickness is 1 micron to 10 microns, described matrix is Ge Shi hardness ＜ 40 carbon steel, structural steel, Ni-based Alloy metal material；The metal base surface aluminum oxide coating layer is made by the method comprised the following steps：(1) by water, the organic alcohol compound of aluminium and inorganic acid according to (100~80):(0.5~1.5):(0.05~0.15) rubs You are mixed ratio, and stirring reaction 4 hours to 48 hours between 70 DEG C and 95 DEG C, wherein inorganic acid acid are added in whipping process Enter, finally obtain transparent colloidal sol；(2) colloidal sol made above is placed in hydrothermal reaction kettle, between compactedness is 30% to 70%, sealing reaction afterwards Kettle, heat the colloidal sol of inside insulation 6 to 18 hours to after between 180 DEG C to 230 DEG C；(3) colloidal sol after isothermal holding is taken out, by the way of rotary coating, i.e., the fixed rotation on spin coater by metallic matrix Turn, uniform fold surface is allowed to above colloidal sol is constantly dropped into matrix surface；(4) stop colloidal sol after rotary coating to be added dropwise and rotate, matrix is dried untill surface liquid film solidifies in atmosphere, then is weighed Multiple (3) (4) process several times, obtains certain thickness alumina sol coating；(5) sample obtained by above procedure is put into high-temperature electric resistance furnace, be heated to the heating rate less than 10 DEG C/min Between 300 DEG C to 500 DEG C, insulation is taken out after 1 hour to 6 hours.
- 2. a kind of preparation method of metal base surface aluminum oxide coating layer, it is characterised in that this method comprises the steps：(1) by water, the organic alcohol compound of aluminium and inorganic acid according to (100~80):(0.5~1.5):(0.05~0.15) rubs You are mixed ratio, and stirring reaction 4 hours to 48 hours between 70 DEG C and 95 DEG C, wherein inorganic acid acid are added in whipping process Enter, finally obtain transparent colloidal sol；(2) colloidal sol made above is placed in hydrothermal reaction kettle, between compactedness is 30% to 70%, sealing reaction afterwards Kettle, heat the colloidal sol of inside insulation 6 to 18 hours to after between 180 DEG C to 230 DEG C；(3) colloidal sol after isothermal holding is taken out, by the way of rotary coating, i.e., the fixed rotation on spin coater by metallic matrix Turn, uniform fold surface is allowed to above colloidal sol is constantly dropped into matrix surface；(4) stop colloidal sol after rotary coating to be added dropwise and rotate, matrix is dried untill surface liquid film solidifies in atmosphere, then is weighed Multiple (3) (4) process several times, obtains certain thickness alumina sol coating；(5) sample obtained by above procedure is put into high-temperature electric resistance furnace, be heated to the heating rate less than 10 DEG C/min Between 300 DEG C to 500 DEG C, insulation is taken out after 1 hour to 6 hours.
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| CN108359985A (en) * | 2018-04-16 | 2018-08-03 | 沈阳建筑大学 | A method of hydro-thermal prepares gamma-alumina nano thin-film on FeCrAl alloys |
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| CN105177541A (en) * | 2015-10-15 | 2015-12-23 | 四川大学 | Method for preparing Al2O3 tritium-resistant coating by MOD (metal-organic decomposition) method |
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| CN1278462A (en) * | 2000-07-07 | 2001-01-03 | 清华大学 | Method of coating sol-gel onto surface of easy-to-oxidize metal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108359985A (en) * | 2018-04-16 | 2018-08-03 | 沈阳建筑大学 | A method of hydro-thermal prepares gamma-alumina nano thin-film on FeCrAl alloys |
| CN108359985B (en) * | 2018-04-16 | 2020-03-31 | 沈阳建筑大学 | Method for preparing gamma alumina nano film on FeCrAl alloy in hydrothermal mode |
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