CN105568263A - Method for preparing SiOC ceramic coating through CO2 laser cracking of polysiloxane material - Google Patents
Method for preparing SiOC ceramic coating through CO2 laser cracking of polysiloxane material Download PDFInfo
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- CN105568263A CN105568263A CN201610140988.0A CN201610140988A CN105568263A CN 105568263 A CN105568263 A CN 105568263A CN 201610140988 A CN201610140988 A CN 201610140988A CN 105568263 A CN105568263 A CN 105568263A
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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
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5603—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides with a well-defined oxygen content, e.g. oxycarbides
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Abstract
The invention relates to a method for preparing a SiOC ceramic coating through CO2 laser cracking of a polysiloxane material. According to the method, firstly, a mixed solution of the polysiloxane material is prepared, and a coating A is prepared on the surface of a Fe-based metal with a brush-coating or spray-coating method; under protection of inert gas, the coating A is scanned by the aid of continuous high-energy controlled laser to react, and the SiOC ceramic coating is prepared. The ceramic coating is prepared through laser cracking of the polysiloxane material with the method, the preparation period is short, the ceramic surface is smooth, the porosity is low, and the prepared ceramic coating has good anti-corrosion and wear-resistant characteristics. A new method is provided for solving the problem that reliable service of pure Fe-based metal materials under some harsh working conditions is difficult to realize.
Description
Technical field
The present invention relates to one and utilize CO
2laser pyrolysis prepares the method for SiOC ceramic coating on ferrous metals surface, belongs to technical field of metal surface modification.Be mainly used in improving ferrous metals surface anticorrosive, wear-resistant, high temperature resistant property.
Background technology
Along with mechanized equipment constantly at a high speed, heavily loaded, integrated, high precision, the harsh future development such as long lifetime, its sliding friction movement parts must in the face of day by day harsh Working environment, as high temperature resistance, protection against corrosion, wear-resistant etc., simple metals material has been difficult to meet these requirements, coated material is prepared on metallic element surface, give the high-performance that metallic substance is special, become and solved metallic element reliable effective way of being on active service under some severe rugged environment.Ceramic coating material has high temperature resistance, the excellent properties such as anti-wear, corrosion-resistant, ceramic coating is prepared at metallic element surface in situ, make component both possess intensity and the toughness of metallic substance, high temperature resistant, corrosion-resistant, the anti abrasive advantage of stupalith can be had again.In recent years, people have developed some effective ways preparing ceramic coating material, as laser cladding, chemical Vapor deposition process (CVD), sol-gel method, polymer pyrolysis pottery (PDC) method, wherein precursor pyrolysis and hot pressing (PDC) is that a kind of up-and-coming original position prepares ceramic coating technology.PDC method is through Pintsch process process by polymer precursor, making it is method and the technique of inorganic ceramic material from polymer transition, has preparation technology simple, and precursor is enriched, the advantages such as pottery composition, stuctures and properties can design and regulate and control, shaping and handling ease.But at present also there is hole in Ceramic Coatings on Stainless Steel via Precursor Pyrolysis material, crackle is not easy to control, the heating pyrolyze time is long, can not meet people on a large scale, the preparation demand of high quality, structure-controllable.Laser have energy density high and concentrate, super rapid heating and cooling, material pointwise consolidation and setting rate soon, be easy to the features such as plurality of advantages such as controlling.Therefore, utilize controlled superlaser to organic polymer material system by rapid heating with solidify that to prepare ceramic coating be a kind of new method, there is preparation cycle short, ceramic yield is high and ceramic porosity is low, can meet extensive, high quality, structure-controllable the requirement preparing ceramic coating in metallic surface.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of laser pyrolysis silicone materials and prepares the method for ceramic coating on ferrous metals surface, and material system involved by the method and laser scanning technique.The ceramic coating that the method obtains, can significantly improve the performance of the protection against corrosion on ferrous metals surface, wear-resistant, high temperature resistance.It is simple that the method has technique, and preparation cycle is short, and efficiency is high, reliable in quality, the feature that can be mass-produced.
The present invention is the design optimization by silicone materials; and be made into mixing solutions, adopt brushing or spraying method to prepare organic coating on ferrous metals surface, under the protection of rare gas element; by the controlled laser scanning of high energy, obtain ceramic coating of good performance on ferrous metals surface.Particularly, method of the present invention is embodied in:
In order to realize above excellent technique effect, the invention provides a kind of CO
2the method of SiOC ceramic coating prepared by laser pyrolysis organosilicon polymer material, and described method in turn includes the following steps: (1) prepares the mixing solutions of organosilicon polymer material; (2) adopt brushing or spraying method that step (1) gained mixing solutions is evenly coated in ferrous metals surface; (3) coating A is obtained after drying at room temperature; (4) under protection of inert gas, adopt the controlled laser scanning coating A of continuous high-energy, thus prepare SiOC ceramic coating on ferrous metals surface.
Preferably, in step (1), described material comprises: polysiloxane or polysiloxane+filler.Wherein the molecular weight of polysiloxane is 770 ~ 13900, fusing point < 40 °, boiling point is greater than > 205 °, relative density is 0.918 ~ 0.977, filler comprises: the one in Ti, Fe, Ni, Si and Al or two kinds, and filler particles diameter is not more than 75 μm.
In step (1), ultrasonic disperse 10 ~ 30min in dimethylbenzene by polysiloxane or polysiloxane+filler, wherein control the massfraction of polysiloxane solution between 50% ~ 75%, the massfraction of polysiloxane+filler mixing solutions is between 75% ~ 88%, and the mass ratio of polysiloxane and filler is 1:2 ~ 3:1; Further, preferably gained mixing solutions evenly brushed or be sprayed at pretreated ferrous metals surface.
In addition, in step (3), preferably at room temperature dry 1 ~ 3h, obtains the coating A of thickness between 0.2 ~ 0.6mm.
In step (4), preferred inert protective gas used is argon gas, and its flow control is between 350 ~ 500mL/min.Described optical maser wavelength is 10.6 μm, and output rating is 100 ~ 800W, and sweep trace speed is 5 ~ 40mm/s, and spot size is 3mm × 3mm.Preferably, described scanning overlapping rate is 3% ~ 5%, and scanning pattern is S type.
According to method gained coatingsurface flat smooth of the present invention, porosity is low, has good anticorrosion, wear resisting property.
Preferably, the present invention also comprises before the step (1) and carries out pretreated step to ferrous metals surface.More preferably, described pre-treatment step is with sand papering, organic solvent immersion and ultrasonic cleaning or its combination, then drying at room temperature.
In addition, present invention provides according to the preparation-obtained ferrous metals surface ceramic coat of aforesaid method.
Present invention also offers aforesaid method and improve the application in anticorrosive metal performance.
The invention provides aforesaid method and improve the application in metal high temperature resistance, abrasion resistance properties.
Core of the present invention is to solve two key technical problems:
One is Design and optimization and the solidification of laser pyrolysis silicone materials.Adopt laser scanning ceramic coating to be prepared by silicone materials pointwise rapid heating and solidifying and must solve two crucial technological difficulties: one is that the ceramic yield obtained wants high; Two is that the porosity of ceramic coating is low.Solve Design and optimization and solidification that one of key of these two technological difficulties is material system.Laser pyrolysis silicone materials of the present invention is polysiloxane or polysiloxane+filler.Wherein filler comprises one in Ti, Fe, Ni, Si and Al or two kinds, and its particle diameter is not more than 75 μm.Observe by experiment, the ceramic yield that after adding filler, cracking obtains significantly improves, and the porosity of pottery obtains effective control.
Two be laser scanning processing parameter optimization solidification.Laser scanning technique is one of key problem in technology obtaining high quality ceramic coating.Laser power is too high, and sweep velocity is excessively slow, and the energy that coating A absorbs is too high, polysiloxane can be caused to be burnt, cannot obtain pottery.Laser power is too low, and sweep velocity is too fast, and coating A cannot obtain enough energy cracking and transform, and also cannot generate pottery.The laser scanning technique of the present invention's solidification: optical maser wavelength is 10.6 μm, and spot size is 3mm × 3mm, and power is 100 ~ 800W, and sweep trace speed is 5 ~ 40mm/s, scanning overlapping rate is 3% ~ 5%, and shielding gas is argon gas.Scanning pattern is S type.This laser scanning technique can obtain that productive rate is higher, the desirable ceramic coating of porosity.
The technical process preparing ceramic coating provided by the invention is as shown in Figure 1:
The present invention has following beneficial effect:
(1) silicone materials composition is simple, and raw material valency is low to be easy to get.
(2) preparation technology is simple and practical, and preparation cycle is short, and the porosity of gained ceramic coating is lower, has good anticorrosion antiwear performance.
(3) laser scanning can not have an impact to the shape of iron-based component metal and structure property.
The present invention solves simple ferrous metals material to be difficult to reliably be on active service under some harsh operating mode provide new method.
Accompanying drawing explanation
Fig. 1 is that laser pyrolysis silicone materials system prepares ceramic coating technology schema.
Embodiment
Example of the present invention prepares the specific embodiments of the method for ceramic coating by further illustrating laser pyrolysis silicone materials system, but the present invention is not limited in subordinate's embodiment.
Embodiment 1:
Step 1: pretreatment of metal surface.After the 45 steel surface use P1000 sand paperings of 15mm × 15mm × 3mm will be of a size of, ultrasonic cleaning 5min, drying at room temperature 5min in sherwood oil.
Step 2: prepare mixing solutions.Take polysiloxane 50g respectively, dimethylbenzene 20g, in beaker, stir 2min, then beaker is put into the ultrasonic 10min of ultrasonic unit, obtain the polysiloxane mixing solutions mixed.
Step 3: preparation coating A.Polysiloxane mixing solutions is sprayed to 45 steel surfaces, ambient temperatare puts 1.5h, and acquisition surfacing, thickness are the coating A of 0.3mm.
Step 4: laser scanning.Coating A step 3 obtained is placed in heat insulation furnace, and with laser scanning coating A under argon shield, wherein argon flow amount is 350mL/min.Laser scanning processing parameter is optical maser wavelength: 10.6 μm, spot size: 3 × 3mm, power: 300W, sweep velocity: 20mm/s, overlapping rate: 5%, set scanning pattern be S type.
Step 5: obtain ceramic coating.After laser scanning coating A, naturally cooling 5min in atmosphere, takes out sample, can obtain SiOC ceramic coating.
The multi-functional reciprocating friction Wear Tester of MFT-R4000 type is investigated the SiOC ceramic coating of embodiment 1 acquisition and the abrasion resistance properties of 45 steel, and its test conditions is: frequency 5Hz, load 20N, friction stroke 10mm, test period 30min.Wear volume after the test of SiOC ceramic coating measured by three-dimensional appearance instrument is only 20% of the wear volume after 45 steel tests, shows that this ceramic coating has the wear resisting property of excellence.
Embodiment 2:
Step 1: pretreatment of metal surface.After the 45 steel surface use P1000 sand paperings of 15mm × 15mm × 3mm will be of a size of, ultrasonic cleaning 5min, drying at room temperature 5min in sherwood oil.
Step 2: prepare mixing solutions.Weighing particle diameter is the Ti powder 80g of 48 μm, polysiloxane 60g, dimethylbenzene 40g, first by Polycarbosilane together with dimethylbenzene after ultrasonic disperse 10min, then add Ti powder and continue ultrasonic disperse 10min, obtain finely dispersed mixing solutions.
Step 3: preparation coating A.Mixing solutions step 2 obtained brushes 45 steel surfaces, and ambient temperatare puts 2.0h, and obtaining surfacing thickness is the coating A of 0.5mm.
Step 4: laser scanning.Coating A step 3 obtained is placed in heat insulation furnace; take argon gas as shielding gas; argon flow amount is 500mL/min; then use laser scanning coating A, wherein laser technical parameters is optical maser wavelength: 10.6 μm, spot size: 3 × 3mm, power: 150W, sweep velocity: 10mm/s, overlapping rate be 3%, setting scanning pattern is S type.
Step 5: obtain ceramic coating.After laser scanning coating A, naturally cooling 5min in atmosphere, takes out sample, can obtain SiOC ceramic coating.
SiOC ceramic coating embodiment 2 obtained adopts the test conditions of GB/T10125-1997 standard specifications to carry out salt-fog test, after test 1000h, SiOC ceramic coating does not corrode, and 45 steel just corrode after test 0.5h, show the corrosion resistance nature that this ceramic coating has had.
SiOC ceramic coating embodiment 2 obtained is positioned in tube furnace, in 1200 DEG C of air, be incubated 72h, this ceramic coating oxidation weight gain 0.25mg/cm
2, and 45 steel oxidation weightening finish 1.4mg/cm under the same terms
2, show that this ceramic coating has excellent high temperature resistant property.
Claims (8)
1. one kind utilizes CO
2laser pyrolysis silicone materials prepares the method for SiOC ceramic coating, it is characterized in that: prepare silicone materials mixing solutions, adopts brushing or spraying method that it is evenly coated in ferrous metals surface, obtains coating A after drying at room temperature; Under protection of inert gas, adopt the controlled laser scanning coating A of continuous high-energy, thus prepare ceramic coating on ferrous metals surface.
2. method according to claim 1, is characterized in that: described silicone materials is polysiloxane or polysiloxane+filler, and wherein the molecular weight of polysiloxane is 770 ~ 13900, and relative density is 0.918 ~ 0.977; Filler comprises: the one in Ti, Fe, Ni, Si and Al or two kinds, and the particle diameter of filler is not more than 75 μm.
3. method according to claim 1, it is characterized in that: ultrasonic disperse 10 ~ 30min in dimethylbenzene by polysiloxane or polysiloxane+filler, wherein control the massfraction of polysiloxane solution between 50% ~ 75%, the massfraction of polysiloxane+filler mixing solutions is between 75% ~ 88%.
4. method according to claim 3, is characterized in that: the mass ratio of polysiloxane and filler is 1:2 ~ 3:1.
5. method according to claim 1, is characterized in that: described drying at room temperature refers at room temperature dry 1 ~ 3h, obtains the coating A of thickness between 0.2 ~ 0.6mm.
6. method according to claim 1, is characterized in that: described rare gas element is argon gas, and its flow control is between 350 ~ 500mL/min.
7. method according to claim 1, is characterized in that: the optical maser wavelength that described laser scanning adopts is 10.6 μm, and output rating is 100 ~ 800W, sweep trace speed is 5 ~ 40mm/s, spot size is 3mm × 3mm, and scanning overlapping rate is 3% ~ 5%, and scanning pattern is S type.
8. the arbitrary described method of claim 1-7 is improving the application in anticorrosive metal, high temperature resistance, abrasion resistance properties.
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| CN201610140988.0A CN105568263B (en) | 2016-03-11 | 2016-03-11 | It is a kind of to utilize CO2The method that laser pyrolysis silicone materials prepare SiOC ceramic coatings |
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| CN201610140988.0A CN105568263B (en) | 2016-03-11 | 2016-03-11 | It is a kind of to utilize CO2The method that laser pyrolysis silicone materials prepare SiOC ceramic coatings |
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| CN108911752A (en) * | 2018-08-01 | 2018-11-30 | 渤海大学 | A method of synthesizing ceramic material under the conditions of extra electric field |
| CN113278973A (en) * | 2021-05-24 | 2021-08-20 | 中山大学 | Titanium-based alloy part with nickel-modified silicon-based protective coating and preparation method thereof |
| CN113684467A (en) * | 2021-07-26 | 2021-11-23 | 中国科学院金属研究所 | Method for preparing amorphous SiOC coating by adopting chemical vapor deposition process |
| CN114901104A (en) * | 2019-12-25 | 2022-08-12 | 太阳星光齿磨公司 | Tooth brush |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108911752A (en) * | 2018-08-01 | 2018-11-30 | 渤海大学 | A method of synthesizing ceramic material under the conditions of extra electric field |
| CN114901104A (en) * | 2019-12-25 | 2022-08-12 | 太阳星光齿磨公司 | Tooth brush |
| CN113278973A (en) * | 2021-05-24 | 2021-08-20 | 中山大学 | Titanium-based alloy part with nickel-modified silicon-based protective coating and preparation method thereof |
| CN113684467A (en) * | 2021-07-26 | 2021-11-23 | 中国科学院金属研究所 | Method for preparing amorphous SiOC coating by adopting chemical vapor deposition process |
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