CN106917081B - A method of preparing SiTiOC ceramic coating - Google Patents
A method of preparing SiTiOC ceramic coating Download PDFInfo
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- CN106917081B CN106917081B CN201710198405.4A CN201710198405A CN106917081B CN 106917081 B CN106917081 B CN 106917081B CN 201710198405 A CN201710198405 A CN 201710198405A CN 106917081 B CN106917081 B CN 106917081B
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- silicon compound
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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
- C23C20/00—Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
- C23C20/06—Coating with inorganic material, other than metallic material
- C23C20/08—Coating with inorganic material, other than metallic material with compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
Abstract
The invention discloses a kind of methods for preparing SiTiOC ceramic coating, belong to chemical synthesis and ceramic coating preparation technical field.The method of the present invention includes the following steps that (1) butyl titanate is chemically reacted with organo-silicon compound, prepares titanium organo-silicon compound；(2) titanium organo-silicon compound are coated in matrix surface, solidification；(3) solid-state titanium organic silicon coating made from step (2) is scanned using continuous laser, cracks coating, obtain SiTiOC ceramic coating.The method of the present invention is simple and easy to operate; short preparation period is high-efficient; laser scanning will not have a negative impact to the shape and structure property of matrix; SiTiOC ceramic coating porosity obtained is lower; with excellent anticorrosion antiwear antifriction performance; it is not likely to produce crackle, is suitble to large-scale production, has broad application prospects in fields such as aerospace, national defence, chemical industry, machinery, electric power, electronics.
Description
Technical field
The present invention relates to chemical syntheses and ceramic coating preparation technical field, and in particular, to a kind of to use continuous laser
Cracking the preparation of titanium organo-silicon compound has the method for SiTiOC ceramic coating of anticorrosion antiwear performance.
Background technique
High-performance coating material is prepared in metal material surface, components is made to have both the superiority of metal and coating material
Can, it is the effective means for solving simple metals components and being difficult to meet increasingly harsh military service operating condition.Based on carbon, boron, nitride
Ceramic coating material there are low close, high-strength, high hard, the excellent properties such as wear-resisting, anti-corruption, high temperature resistant, but there are plasticity poor, property
It is crisp, be also easy to produce the deficiencies of crackle, make its application receive certain restrictions.In order to overcome the above-mentioned deficiency of ceramic coating, have developed
Ceramics material used for preparing coated is mainly characterized by a certain temperature, and metal parts surface passes through heating cracking high polymer system
Standby ceramic coating makes the toughness of components combination metal material and the high temperature resistant of ceramic material, corrosion-resistant, wear-resistant.Pottery at present
Porcelain composite coating has been applied to the fields such as aerospace, national defence, chemical industry, machinery, electric power, electronics, and development prospect is wide.
Organic polymer polymer pyrolysis (PDC) method is that the effective of ceramic composite coating is prepared in situ in metal material surface
Approach.Ceramic phase in ceramic composite coating prepared by PDC method is tiny, is evenly distributed, therefore is combined with matrix, wear-resisting, anti-
Corruption is had excellent performance, but there is also porositys the problem of larger, crackle is also easy to produce.To solve the above problems, in polymer precursors
Ti, Al, Ni, Mo, Cr isoreactivity filler are added in cracking system, precursor is made to generate new ceramic phase in cracking process, from
And it reduces the porosity of ceramic coating, ceramic coating crackle is inhibited to generate.But filler micro-nano powder is past in organic polymer
Toward the problems such as there are particle aggregations, dispersion unevenness, it is unfavorable for high performance ceramic composite coating preparation.And it uses and contains metallic element
Organic polymer prepares SiMOC ceramics material used for preparing coated, can effectively avoid the dispersion of filler grain as presoma,
Ceramic coating porosity can be effectively reduced again simultaneously, crackle in ceramic coating is inhibited to generate, but PDC method uses heating cracking, still
The deficiencies of being difficult to control there are preparation step complexity, long preparation period, process.Laser is with light-gathering is good, energy density is high, easy
In accurate the advantages that controlling, therefore using laser as heat source, cracking precursor and obtaining ceramic coating is a kind of novel system
The method of standby ceramic coating.
Summary of the invention
The present invention provides a kind of using laser as heat source, and cracking the preparation of titanium organo-silicon compound has anti-corrosion resistance to
The method for grinding the SiTiOC ceramic coating of performance, to make up the deficiencies in the prior art.
A kind of method preparing SiTiOC ceramic coating provided by the invention, includes the following steps：
(1) butyl titanate is chemically reacted with organo-silicon compound, prepares titanium organo-silicon compound；
(2) titanium organo-silicon compound are coated in matrix surface, solidification；
(3) solid-state titanium organic silicon coating made from step (2) is scanned using continuous laser, cracks coating, obtained
SiTiOC ceramic coating.
The molecular formula of butyl titanate of the present invention is Ti (OCH2-CH2-CH2-CH3)4。
In the above method, step (1) organo-silicon compound be γ-glycidoxypropyl trimethoxy silane and/
Or γ-aminopropyl triethylsilane.
The γ-glycidoxypropyl trimethoxy silane molecular structural formula is：
The γ-aminopropyl triethylsilane molecular structural formula is：
Wherein, butyl titanate and organo-silicon compound mass ratio are 1 in step (1):1~1:4, the temperature chemically reacted
Degree is 20~50 DEG C, and the ultrasound condition lower reaction time is 5~10min.
Further, the molecular structural formula of titanium organo-silicon compound made from the method for the present invention step (1) is：
Matrix described in the method for the present invention step (2) is metallic matrix, preferably ferrous metals matrix.
Those skilled in the art can coat titanium silicon organic coating on ferrous metals surface using brushing or spray coating method.It is preferred that
Ground, iron-based matrix described in step (2) is through surface preparation, it is highly preferred that the pre-treatment step includes sandblasting, You Jirong
Agent immersion and ultrasonic cleaning or combinations thereof, the solvent are preferably ethyl alcohol and acetone.
The method of the present invention step (2) titanium organo-silicon compound are coated in matrix surface with a thickness of 200 μm ± 50 μm.
Wherein, step (2) cured condition is：Solidification temperature is 40~180 DEG C, curing time 20-40min.It is preferred that
Ground, solidification temperature are 90 DEG C, curing time 30min.
The step of the method for the present invention (3), carries out continuous laser scanning under inert gas protection, and the inert gas is argon
Gas or nitrogen, flow control are 350~500mL/min.
Step (3) Laser Scanning is the laser for using wavelength as 980nm, and laser power is 200~800W, scanning
Linear velocity is 5~30mm/s, and spot diameter size is 3mm × 3mm；Scanning overlapping rate is 3%~5%, and scan path is S type.
SiTiOC ceramic coating made from the above method of the present invention belongs to the scope of protection of the present invention.
The present invention provides SiTiOC ceramic coatings obtained by the above method to improve anticorrosive metal, high temperature resistant, wear-resisting
Damage the application in performance.
The process flow provided by the invention for preparing ceramic coating is as shown in Figure 1.
The present invention is that ceramic coating is prepared in situ in metal surface based on polymer pyrolysis china-clay method, and raw material is easy to get, and is used
Simple chemical synthesis process is prepared for the titanium organo-silicon compound precursor of titanium and element silicon one, and the precursor is continuous
There is very high ceramic yield, technique during laser pyrolysis.Ceramics are prepared using laser pyrolysis silicon organo-metallic compound to apply
Layer, will not shape to iron-based components and structure property have a negative impact, simple process, the period is short, while avoiding and filling out
Material particle disperses uneven, serious problem of reuniting in " organic polymer precursor+filler " system, makes metallic element in laser
In-situ preparation cermet phase is cracked, and is evenly distributed in prepared SiTiOC ceramic coating.So that prepared by the present invention
Compared with SiTiOC ceramic coating porous ceramics prepared by the conventional sintering method (porosity is that 40-50% is even higher), hole
Rate is substantially reduced, reach 20% hereinafter, and the ceramic coating coefficient of friction compared with wear volume matrix be decreased obviously, the range of decrease
59% and 38% are respectively reached, in addition, its corrosion potential is obviously shuffled compared to-the 0.8V of matrix, under corrosion current is significant
Drop, therefore the SiTiOC ceramic coating has excellent anti-corrosion, wear-resisting, antifriction performance.
Detailed description of the invention
Fig. 1 is the process flow diagram that the present invention prepares SiTiOC ceramic coating.
Fig. 2 is the surface topography map of SiTiOC ceramic coating prepared by embodiment 3.
Fig. 3 is the polarization curve of the SiTiOC ceramic coating of different instances preparation, and Sample1-Sample 3 divides in figure
It is not SiTiOC ceramic coating made from embodiment 1-3, Coating A is using high temperature pyrolysis titanium valve+polydimethylsiloxanes
Alkane system method refers to 45 steel matrix in SiTiOC ceramic coating A, Blank prepared by 45 steel matrix surfaces.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..Without departing substantially from spirit of that invention
In the case where essence, to modifications or substitutions made by the method for the present invention, step or condition, all belong to the scope of the present invention.
Unless otherwise specified, chemical raw material used in embodiment is conventional commercial raw material, skill used in embodiment
The conventional means that art means are well known to those skilled in the art.
Embodiment 1 prepares the method (1) of SiTiOC ceramic coating
Step 1：The preparation of titanium organo-silicon compound.According to mass ratio 1:1, weigh makes γ-glycidyl-oxypropyl respectively
The two is mixed and is placed in 500mL beaker by each 100g of trimethoxy silane, butyl titanate, sonicating in 50 DEG C of waters bath with thermostatic control
Reaction 5min is learned, the titanium organo-silicon compound of yellow transparent shape are obtained, essential molecular structure formula is：
Step 2：Pretreatment of metal surface to be coated.Sandblasting will be carried out having a size of 45 steel matrix of 15mm × 15mm × 3mm
Processing, and it is cleaned by ultrasonic 15min in acetone soln.
Step 3：The preparation of titanium organo-silicon compound coating.In the titanium organosilicon of 45 steel matrix surface coating steps (1) preparation
Compound obtains the titanium organic silicon coating A with a thickness of 200 μm.
Step 4：The solidification of titanium organic silicon coating.Titanium organic silicon coating A is kept the temperature into 30min under 90 DEG C of constant temperatures, from
So cured titanium organic silicon coating B is obtained after cooling.
Step 5：The preparation of SiTiOC ceramic coating.Adjusting argon flow be 350m/min, use laser power for 350W,
Scanning speed is 14mm/s, spot size 3mm × 3mm, overlapping rate 5%, the continuous laser sweep parameter that scan path is S type.
Under protection of argon gas after laser single pass titanium organic silicon coating B, cooled to room temperature obtains SiTiOC ceramic coating.
Embodiment 2 prepares the method (2) of SiTiOC ceramic coating
Step 1：The preparation of titanium organo-silicon compound.According to mass ratio 3:2, weigh makes γ-glycidyl-oxypropyl respectively
The two is mixed and is placed in a beaker by each 40g of trimethoxy silane 60g, butyl titanate, and sonochemistry is anti-in 40 DEG C of waters bath with thermostatic control
8min is answered, the titanium organo-silicon compound of yellow transparent shape are obtained, essential molecular structure formula is：
Step 2：Pretreatment of metal surface.Blasting treatment will be carried out having a size of 45 steel matrix of 15mm × 15mm × 3mm, and
It is cleaned by ultrasonic 15min in acetone soln.
Step 3：The preparation of titanium organo-silicon compound coating.It is siliconated in the titanium of 45 matrix surface coating steps (1) preparation
Close object, coating titanium organo-silicon compound with a thickness of 180 μm, obtain titanium organic silicon coating A.
Step 4：The solidification of titanium organic silicon coating.Titanium organic silicon coating A is kept the temperature into 20min under 120 DEG C of constant temperatures, from
So cured titanium organic silicon coating B is obtained after cooling.
Step 5：The preparation of SiTiOC ceramic coating.Laser scanning titanium organic silicon coating B under protection of argon gas adjusts argon gas
Flow is 450m/min, laser power 500W, scanning speed 12mm/s, spot size 3mm × 3mm, and overlapping rate 4% is swept
Retouching path is S type.Cooled to room temperature after laser single pass obtains SiTiOC ceramic coating.
Embodiment 3 prepares the method (3) of SiTiOC ceramic coating
Step 1：The preparation of titanium organo-silicon compound.According to mass ratio 4:1, weigh makes γ-aminopropyl triethyl group silicon respectively
The two is mixed and is placed in a beaker by each 20g of alkane 80g, butyl titanate, and sonochemistry reacts 10min in 30 DEG C of waters bath with thermostatic control, is obtained
The titanium organo-silicon compound of pale yellow transparent shape are obtained, essential molecular structure formula is：
Step 2：Pretreatment of metal surface.Blasting treatment will be carried out having a size of 45 steel matrix of 15mm × 15mm × 3mm, and
It is cleaned by ultrasonic 15min in acetone soln.
Step 3：The preparation of titanium organo-silicon compound coating.It is siliconated in the titanium of 45 matrix surface coating steps (1) preparation
Close object, coating titanium organo-silicon compound with a thickness of 210 μm, obtain titanium organic silicon coating A.
Step 4：The solidification of titanium organic silicon coating.Titanium organic silicon coating A is kept the temperature under 60 DEG C of constant temperatures after 40min from
It is so cooling, obtain cured titanium organic silicon coating B.
Step 5：The preparation of SiTiOC ceramic coating.Laser scanning titanium organic silicon coating B under protection of argon gas adjusts argon gas
Flow is 400m/min, laser power 800W, scanning speed 10mm/s, spot size 3mm × 3mm, and overlapping rate 3% is swept
Retouching path is S type.After laser single pass, cooled to room temperature obtains SiTiOC ceramic coating.
In addition, handling using ultrasonic disperse keeps Ti powder evenly dispersed in dimethyl silicone polymer, this is contained into active filler
The dimethyl silicone polymer of titanium valve (Ti) is evenly applied to 45 steel surfaces, under the conditions of 700 DEG C, using high temperature pyrolysis containing activity
Filler titanium valve+dimethyl silicone polymer system is prepared for SiTiOC ceramic coating A on 45 steel matrix surfaces, separately take above-mentioned titanium valve+
Dimethyl silicone polymer system is evenly applied to 45 steel surfaces, takes laser parameter same as Example 3, with laser scanning 45
The titanium valve organic silicon coating of steel surface prepares SiTiOC ceramic coating B.Respectively prepared by ceramic coating A, B and embodiment 1-3
SiTiOC ceramic coating and 45 steel carry out tribological property and are tested, and experimental condition is load 2N, frequency 2Hz, friction row
Journey 5mm, test period 20min obtain all data as shown in Table 1.As can be seen that three kinds of above embodiments preparation
The coefficient of friction and wear volume of SiTiOC ceramic coating are than coating A, the coefficient of friction of coating B and 45 steel matrix and abrasion body
Product is small, and the properties of antifriction and wear resistance for the SiTiOC ceramic coating that wherein prepared by embodiment 2 is best, and coefficient of friction is than 45 steel, coating A
Compare with coating B reduces 59%, 49% and 55% respectively, and wear volume compares difference with coating B than 45 steel, coating A
Reduce 38%, 11% and 32%.
The coefficient of friction and wear volume of the SiTiOC ceramic coating of the different embodiment preparations of table 1
The SEM pattern of SiTiOC ceramic coating prepared by embodiment 3 is as shown in Figure 2, it can be seen that prepared
SiTiOC ceramic coating surface compactness is good, and surface texture is smooth, flawless.The pottery of SiTiOC made from embodiment 1 and embodiment 2
Porcelain coating has SEM pattern similar to Example 3.
As shown in figure 3, compared to 45 steel matrix (corrosion potential is -0.790V) and coating A (corrosion potential is -
0.495V or so), the corrosion potential of SiTiOC ceramic coating prepared by embodiment 1-3 obviously moves to right, this shows to implement
SiTiOC ceramic coating prepared by example 1-3 all has excellent corrosion resistance, wherein the ceramics of SiTiOC prepared by embodiment 3
The corrosion potential highest of coating, about -0.185V show that its antiseptic property is optimal.
As it can be seen that the SiTiOC ceramic coating of the method for the present invention preparation has excellent anti-corrosion, antifriction, abrasion resistance, it can be with
It is insufficient substantially to make up performance of the metal material in terms of these.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of method for preparing SiTiOC ceramic coating, which is characterized in that the method includes the following steps：
(1) butyl titanate is chemically reacted with organo-silicon compound, prepares titanium organo-silicon compound；The organo-silicon compound
For γ-glycidoxypropyl trimethoxy silane and/or γ-aminopropyl triethylsilane；
(2) titanium organo-silicon compound are coated in matrix surface, solidification；
(3) solid-state titanium organic silicon coating made from step (2) is scanned using continuous laser, cracks coating, obtain SiTiOC pottery
Porcelain coating.
2. the method as described in claim 1, which is characterized in that butyl titanate and organo-silicon compound mass ratio in step (1)
It is 1:1~1:4, the temperature chemically reacted is 20~50 DEG C, and the ultrasound condition lower reaction time is 5~10min.
3. the method as described in claim 1, which is characterized in that the molecular structure of titanium organo-silicon compound made from step (1)
Formula is：
4. the method as described in claim 1, which is characterized in that matrix described in step (2) is metallic matrix.
5. method as claimed in claim 4, which is characterized in that matrix described in step (2) is ferrous metals matrix.
6. the method as described in claim 1, which is characterized in that it is thick that step (2) titanium organo-silicon compound are coated in matrix surface
Degree is 200 μm ± 50 μm.
7. the method as described in claim 1, which is characterized in that step (2) cured condition is：Solidification temperature is 40~180
DEG C, curing time 20-40min.
8. method as claimed in claim 1, which is characterized in that step (3) carries out continuously under inert gas protection
Laser scanning, the inert gas are argon gas or nitrogen, and flow control is 350~500mL/min.
9. method as claimed in claim 1, which is characterized in that step (3) Laser Scanning be use wavelength for
The laser of 980nm, laser power are 200~800W, and scanning linear velocity is 5~30mm/s, and spot diameter size is 3mm × 3mm；
Scanning overlapping rate is 3%~5%, and scan path is S type.
10. the SiTiOC ceramic coating that any the method for claim 1-9 obtains is improving anticorrosive metal, high temperature resistant, resistance to
Application in polishing machine.
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