CN105986219A - Technique for preparing titanium diboride (TiB2) coating on metal surface - Google Patents
Technique for preparing titanium diboride (TiB2) coating on metal surface Download PDFInfo
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- CN105986219A CN105986219A CN201610521817.2A CN201610521817A CN105986219A CN 105986219 A CN105986219 A CN 105986219A CN 201610521817 A CN201610521817 A CN 201610521817A CN 105986219 A CN105986219 A CN 105986219A
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- coating
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- metal surface
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- preparing titanium
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Classifications
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
Abstract
The present invention relates to a technique for preparing a titanium diboride (TiB2) coating on a metal surface. In the technique, advantages of a plasma spraying technique and a laser remelting technique are combined, defects such as poor thermal shock resistance and bad compactness of the TiB2 coating obtained by the plasma spraying technique are overcome, and problems that fusion covering of a boride is difficult by a laser fusion covering technique and the coating is large in stress and poor in uniformity are solved. A layer of TiB2 coating is prefabricated on a metal matrix through the laser spraying technique, a porosity factor of the coating is controlled through technological parameters, and then laser remelting treatment is performed on the coating, thus to obtain a dense TiB2 coating in metallurgical bonding with the matrix on the metal surface. With adoption of the obtained TiB2 coating, the surface strength of the metal matrix and the service time of the metal matrix in a corrosive environment can be notably raised.
Description
Technical field
The invention belongs to metal coating preparation field, particularly to a kind of process preparing titanium boride coating in metal surface.
Background technology
Titanium diboride (TiB2) as the metalloid compound of a kind of hexagonal crystal, its crystal structure is to be handed over by boron atomic plane and titanium atom face
Constituting two-dimensional network structure for occurring, wherein the B in boron atomic plane combines with covalent bond with other 3 B, unnecessary one
Individual electronically form big π key, impart TiB2Excellent electric conductivity, and between boron atomic plane and titanium atom face, Ti-B key determines
TiB2Hardness higher.Just because of TiB2High conductivity and chemical stability, be widely used in metal surface all the time
Protection field.The method generally preparing this metal-cermic coating includes: physics, chemical vapour deposition technique；Pulsed electrode deposits
Method；Plasma spraying method etc..
Plasma spray coating process has the advantages such as deposition velocity is fast, production efficiency is high, coating uniformity is good, applied widely, also
Solve the spraying problem of refractory ceramic material, be preparation technology of coating method conventional at present.But, plasma spraying exists
Some intrinsic defects, if ceramic particle is in piling up formation coating procedure successively, are inevitably generated compared with multiple cracks, and apply
Layer porosity is higher, thus its corrosion resistance can not be guaranteed with non-oxidizability.Moreover, the painting that plasma spraying is obtained
Between layer and base material, the principal mode of interface cohesion is mechanical bond, thermal shock resistance difference, it is impossible to by TiB2The premium properties of coating
Give full play of.
Laser melting and coating technique is as another kind of Surface-micromachining process, and it can will be placed on the powder to be applied of matrix surface through laser beam
Irradiation, is allowed to melt formation thin layer with matrix surface simultaneously, and rapid solidification forms the extremely low face coat of dilution factor, thus aobvious
Write and improve the wear-resisting, anti-corrosion, heat-resisting of substrate material surface and non-oxidizability, additionally, the painting being obtained by laser melting and coating process
Layer tissue is fine and close, and coating is tied in metallurgical binding with matrix, better assures that the long service performance of coating.But laser melts
Cover work and be more suitable for some materials such as self-melting alloy, and to carbide, the cladding difficulty of boride, and laser melting coating obtained
Coating often uniformity is poor.
Content of the invention
The present invention is directed to the deficiency being illustrated in background above technology, propose a kind of rationally efficiently and the stronger scheme of practicality:
Use the TiB of the prefabricated certain hole of plasma spraying2Carry out laser remolten after coating, can effectively eliminate coating internal stress, again can
Increase coating compactness and bond strength, improve TiB with this2The thermal shock resistance when reality is applied for the coating and corrosion resistance.
The present invention realizes particular by following four step:
1st, surface preparation is carried out to metallic matrix,
Metallic matrix includes but is not limited to stainless steel, titanium alloy,
Pretreatment operation is: by metallic matrix respectively through 400 and 800#SiC sand papering process, and use acetone cleaning-drying,
Subsequently 5～10min is processed to its surface sand-blasting (corundum sand), until metal surface loses metallic luster, and clean surface with acetone
It is dried after the shot blasting particles of residual；
2、TiB2The preparation of sprayed on material,
By TiB2Metal ceramic powder is mixed by the mass fraction ratio of 20:1 with the polyvinyl alcohol (PVA) after dissolving, through star after being dried
Row ball mill ball milling, uses 100 subsequently#、200#Sieve sieve step by step takes, and finally chooses the TiB that particle diameter is 100～200 mesh scopes2Powder
End is as sprayed on material；
3rd, the TiB that will obtain in step (2)2Sprayed on material is being pre-processed through step (1) by plasma spray coating process
The pre-prepared TiB of metal base surface2Coating,
The concrete operations of plasma spray coating process are: setting spray gun with metallic matrix spacing as 90～110mm, spray power is
80～85kW, argon gas flow velocity is 38～42L/min, and hydrogen flow rate is 15～18L/min, and powder feeding rate is 28g/min,
Pre-prepared TiB2Coating layer thickness controls at 10～15 μm,
In this step, being carried out the boride coating of prefabricated certain hole by plasma spraying technology, the existence of certain hole can be
Follow-up laser remolten processing procedure eliminates coating crack, the problem of peeling that coating is caused because of factors such as internal stress, also
Avoid and be used alone laser melting coating and be difficult to the excellent borided layer of processability；
4th, laser melting and coating technique is used to carry out re melting process to the prefabricated coating obtaining in step (3), it is thus achieved that TiB2Coating,
The power setting of laser melting coating is 60～80W/mm2, frequency be 5～10Hz, electric current pulsewidth be 6～8 μ s, electric current be 220A,
Sweep speed be 3～8mm/s, protective gas nitrogen flow rate be 15L/min.
To above-mentioned prepared TiB2The performance test methods of coating includes:
1st, thermal shock resistance test: take out after coating sample being placed at 800 DEG C insulation 30min, put into quenching in room temperature water, repeat
More than 20 times, and observe coating surface change；
2nd, dynamic potential scanning: be placed in coating sample in the sulfuric acid solution of 0.5mol/L, evaluates it in acid by electro-chemical test
Property environment corrosion resistance.
Detailed description of the invention
Embodiment 1
(1) metallic matrix selects commercially available 304L stainless steel, is cut to the flat substrates of 10mm × 10mm × 3mm,
It is respectively adopted 400 and 800#Grinding process made by SiC sand paper, and uses acetone cleaning-drying, uses corundum sand to its sandblasting subsequently
After processing 10min so that it is surface loses metallic luster, and uses acetone cleaning-drying；
(2) by the TiB of 200g2Polyvinyl alcohol (PVA) after metal ceramic powder dissolves with 10g is sufficiently mixed, through star after being dried
Row ball mill ball milling 3h, rotating speed is 450r/min；Use 100 subsequently#、200#Sieve sieve step by step takes, and finally choosing particle diameter is 100～200
Purpose TiB2Powder is as spraying powder；
(3) TiB that will obtain in step (2)2Sprayed on material is being pre-processed through step (1) by plasma spray coating process
The pre-prepared TiB of metal base surface2Coating: spray gun and metallic matrix spacing are 100mm, and spray power is 80kW, argon gas
Flow velocity is 40L/min, and hydrogen flow rate is 15L/min, and powder feeding rate remains 28g/min, sprays 4 minutes.
The coating layer thickness that this example is obtained is 12 μm, and prepared coating directly carries out performance test without re melting process, sends out
After the thermal shock resistance test of present 20 times, coating appearance significantly comes off, skin effect phenomenon, not high with substrate combinating strength；
Use potentiodynamic polarization technology at 0.5mol/L H2SO4Test in solution finds that this coating carries relative to matrix, corrosion potential
Rising 130mV, corrosion current decreases.
Embodiment 2
Step (1), (2), (3) are with embodiment 1；
(4) laser melting and coating technique is used to carry out re melting process to the prefabricated coating obtaining in step (3): cladding power is
80W/mm2；Frequency is 10Hz；Electric current pulsewidth is 8 μ s；Electric current is 220A；Sweep speed is 3mm/s；Protective gas nitrogen
Flow velocity is 15L/min.
The coating layer thickness that this example is obtained is 12 μm, and prepared coating directly carries out performance test without re melting process, sends out
After the thermal shock resistance test of present 20 times, there is not the sign that comes off in coating, and significantly changing, still with jail does not occurs yet in coating surface
Gu；
Use potentiodynamic polarization at the H of 0.5mol/L2SO4Solution is tested, finds that this coating carries relative to matrix, corrosion potential
Rising 312mV, corrosion rate declines substantially, and corrosion resisting property improves.The TiB of direct spraying in comparative example 12Layer, at remelting
Thermal shock resistance after reason, corrosion resistance significantly improve, and coating is good with the adhesion of matrix.
Embodiment 3
Step (1), (2) are with embodiment 1；
(3) TiB that will obtain in step (2)2Sprayed on material is being pre-processed through step (1) by plasma spray coating process
The pre-prepared TiB of metal base surface2Coating: spray gun and metallic matrix spacing are 100mm, and spray power is 80kW, argon
Gas velocity is 40L/min, and hydrogen flow rate is 15L/min, and powder feeding rate remains 28g/min, sprays 5 minutes；
(4) laser melting and coating technique is used to carry out re melting process to the prefabricated coating obtaining in step (3): cladding power is
80W/mm2；Frequency is 10Hz；Electric current pulsewidth is 8 μ s；Electric current is 220A；Sweep speed is 5mm/s；Protective gas nitrogen
Flow velocity is 15L/min.
The coating layer thickness that this example is obtained is 14 μm, and prepared coating directly carries out performance test without re melting process, sends out
After the thermal shock resistance test of present 20 times, there is not the sign that comes off in coating, and significantly changing, still with jail does not occurs yet in coating surface
Gu；
Use potentiodynamic polarization at the H of 0.5mol/L2SO4Solution is tested, finds that this coating carries relative to matrix, corrosion potential
Rising 291mV, corrosion rate declines substantially, and corrosion resisting property improves.The TiB of direct spraying in comparative example 12Layer, at remelting
Thermal shock resistance after reason, corrosion resistance significantly improve, and coating is good with the adhesion of matrix.
Embodiment 4
Step (1), (2) are with embodiment 1；
(3) TiB that will obtain in step (2)2Sprayed on material is being pre-processed through step (1) by plasma spray coating process
The pre-prepared TiB of metal base surface2Coating: spray gun and metallic matrix spacing are 100mm, and spray power is 80kW, argon
Gas velocity is 40L/min, and hydrogen flow rate is 15L/min, and powder feeding rate remains 28g/min, sprays 4 minutes；
(4) laser melting and coating technique is used to carry out re melting process to the prefabricated coating obtaining in step (3): cladding power is
80W/mm2；Frequency is 10Hz；Electric current pulsewidth is 8 μ s；Electric current is 220A；Sweep speed is 8mm/s；Protective gas nitrogen
Flow velocity is 15L/min.
The coating layer thickness that this example is obtained is 14 μm, and prepared coating directly carries out performance test without re melting process, sends out
After the thermal shock resistance test of present 20 times, there is not the sign that comes off in coating, but coating surface occurs in that trickle crackle, this be due to
Sweep speed comparatively fast causes；
Use potentiodynamic polarization at the H of 0.5mol/L2SO4Solution is tested, finds that this coating carries relative to matrix, corrosion potential
Rising 223mV, corrosion rate declines substantially, and corrosion resisting property improves.
Claims (6)
1. the process preparing titanium boride coating in metal surface, it is characterised in that: described method is,
(1) surface preparation is carried out to metallic matrix；
(2)TiB2The preparation of sprayed on material；
(3) TiB that will obtain in step (2)2Sprayed on material is being pre-processed through step (1) by plasma spray coating process
The pre-prepared TiB of metal base surface2Coating；
(4) laser melting and coating technique is used to carry out re melting process to the prefabricated coating obtaining in step (3), it is thus achieved that TiB2Coating.
2. the process preparing titanium boride coating in metal surface as claimed in claim 1, it is characterised in that: step (1)
Described in metallic matrix be stainless steel or titanium alloy.
3. the process preparing titanium boride coating in metal surface as claimed in claim 1, it is characterised in that: step (1)
In, by metallic matrix respectively through 400 and 800#SiC sand papering process, and use acetone cleaning-drying, subsequently its surface is sprayed
Sand processes 5～10min, until metal surface is dried after losing metallic luster, and the shot blasting particles with acetone cleaning remained on surface.
4. the process preparing titanium boride coating in metal surface as claimed in claim 1, it is characterised in that: step (2)
In, by TiB2Polyvinyl alcohol after metal ceramic powder and dissolving, through star row ball mill ball milling after being dried, uses 100 subsequently#、
200#Sieve sieve step by step takes, and finally chooses the TiB that particle diameter is 100～200 mesh scopes2Powder is as sprayed on material.
5. the process preparing titanium boride coating in metal surface as claimed in claim 1, it is characterised in that: step (3)
In, the concrete operations of plasma spray coating process are, set spray gun and with metallic matrix spacing as 90～110mm, spray power are
80～85kW, argon gas flow velocity is 38～42L/min, and hydrogen flow rate is 15～18L/min, and powder feeding rate is 28g/min.
6. the process preparing titanium boride coating in metal surface as claimed in claim 1, it is characterised in that: step (4)
In, the power of laser melting coating is 60～80W/mm2, frequency be 5～10Hz, electric current pulsewidth be that 6～8 μ s, electric current are 220A, sweep
Retouch speed be 3～8mm/s, protective gas nitrogen flow rate be 15L/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935613A (en) * | 2017-11-24 | 2018-04-20 | 中南大学 | A kind of inner lining material and preparation method and application of anti-smoking gas containing fluorine corrosion |
| CN107998814A (en) * | 2017-11-24 | 2018-05-08 | 中南大学 | The processing system and its application process of a kind of smoking gas containing fluorine |
| CN108326384A (en) * | 2017-12-11 | 2018-07-27 | 安徽宝辰机电设备科技有限公司 | A kind of soldering processes of high-strength corrosion-resistant erosion joint of aluminium and copper |
| CN109989059A (en) * | 2019-03-06 | 2019-07-09 | 莆田学院 | A kind of TiBw-Ti composite layer and its laser in-situ preparation method |
| CN110818421A (en) * | 2019-12-13 | 2020-02-21 | 哈尔滨理工大学 | Preparation method of compact composite coating based on reactive plasma spraying and laser remelting |
| CN115537810A (en) * | 2022-10-14 | 2022-12-30 | 中国兵器装备集团西南技术工程研究所 | Method for preparing composite component based on plasma spraying-laser cladding |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935613A (en) * | 2017-11-24 | 2018-04-20 | 中南大学 | A kind of inner lining material and preparation method and application of anti-smoking gas containing fluorine corrosion |
| CN107998814A (en) * | 2017-11-24 | 2018-05-08 | 中南大学 | The processing system and its application process of a kind of smoking gas containing fluorine |
| CN107998814B (en) * | 2017-11-24 | 2020-06-16 | 中南大学 | Fluorine-containing flue gas treatment system and application method thereof |
| CN107935613B (en) * | 2017-11-24 | 2020-06-23 | 中南大学 | Lining material resisting corrosion of fluorine-containing flue gas and preparation method and application thereof |
| CN108326384A (en) * | 2017-12-11 | 2018-07-27 | 安徽宝辰机电设备科技有限公司 | A kind of soldering processes of high-strength corrosion-resistant erosion joint of aluminium and copper |
| CN109989059A (en) * | 2019-03-06 | 2019-07-09 | 莆田学院 | A kind of TiBw-Ti composite layer and its laser in-situ preparation method |
| CN110818421A (en) * | 2019-12-13 | 2020-02-21 | 哈尔滨理工大学 | Preparation method of compact composite coating based on reactive plasma spraying and laser remelting |
| CN115537810A (en) * | 2022-10-14 | 2022-12-30 | 中国兵器装备集团西南技术工程研究所 | Method for preparing composite component based on plasma spraying-laser cladding |
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