CN105986219B - A kind of process preparing titanium boride coating in metal surface - Google Patents
A kind of process preparing titanium boride coating in metal surface Download PDFInfo
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- CN105986219B CN105986219B CN201610521817.2A CN201610521817A CN105986219B CN 105986219 B CN105986219 B CN 105986219B CN 201610521817 A CN201610521817 A CN 201610521817A CN 105986219 B CN105986219 B CN 105986219B
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- coating
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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 kind of process for preparing titanium boride coating in metal surface, which combines the advantages of plasma spraying handles two kinds of technologies with laser remolten, overcomes the TiB of plasma spraying acquisition2The defects of coating thermal shock resistance is poor, and compactness is insufficient, while avoiding the problems such as laser melting and coating process is difficult to boride cladding, and coating stress is big, uniformity is poor.The present invention passes through plasma spraying technology prefabricated one layer of TiB on metallic matrix first2Coating, by process parameter control coating porosity, then to coated laser re melting process, to obtain with matrix in metal surface in metallurgical bonding, fine and close TiB2Coating.This method TiB obtained2Coating can significantly improve metal base surface intensity and the active time in corrosive environment.
Description
Technical field
The invention belongs to metal coating preparation field, in particular to a kind of technique for preparing titanium boride coating in metal surface
Method.
Background technique
Titanium diboride (TiB2) a kind of metalloid compound as hexagonal crystal, crystal structure is by boron atom face and titanium
Atomic plane is alternately present and constitutes two-dimensional network structure, and wherein the B in boron atom face is combined with other 3 B with covalent bond, more
Remaining one electronically forms big pi bond, imparts TiB2Excellent electric conductivity, and Ti-B key is determined between boron atom face and titanium atom face
TiB is determined2Hardness it is higher.Just because of TiB2High conductivity and chemical stability, be widely used in metal all the time
Surfacecti proteon field.The method for usually preparing this metal-cermic coating includes: physics, chemical vapour deposition technique；Pulsed electrode
Sedimentation；Plasma spraying method etc..
Plasma spray coating process has that deposition velocity is fast, high production efficiency, coating uniformity are good, applied widely etc. excellent
Gesture also solves the problems, such as the spraying of refractory ceramic material, is currently used preparation technology of coating method.However, plasma spray
Painting have the defects that it is some intrinsic, if ceramic particle successively accumulation formed in coating procedure, be inevitably generated more split
Line, and coating porosity is higher, thus its corrosion resistance cannot be guaranteed with inoxidizability.Moreover, plasma spraying institute
The principal mode of interface cohesion is mechanical bond between the coating and substrate of acquisition, and thermal shock resistance is poor, cannot be by TiB2Coating
Excellent performance give full play of.
As another Surface-micromachining process, it can pass through the powder to be applied for being placed on matrix surface laser melting and coating technique
Laser beam irradiation is allowed to matrix surface while fusing forms thin layer, and quickly solidification forms the extremely low surface covering of dilution,
To significantly improve wear-resisting, anti-corrosion, the heat-resisting and inoxidizability of substrate material surface, in addition, being obtained by laser melting and coating process
The coating structure obtained is fine and close, and coating and matrix knot are in metallurgical bonding, better assure that the long service performance of coating.However
Laser melting coating work is more suitable for some materials such as self-melting alloy, and to carbide, the cladding of boride is difficult, and laser melting coating institute
Often uniformity is poor for the coating of acquisition.
Summary of the invention
The present invention proposes that a kind of rationally efficient and practicability is stronger for the deficiency illustrated in background above technology
Scheme: using the TiB of the prefabricated certain hole of plasma spraying2Laser remolten is carried out after coating, can be effectively eliminated in coating and be answered
Power can increase coating compactness and bond strength again, so as to improve TiB2Thermal shock resistance and corrosion resistant of the coating in practical application
Corrosion.
The present invention is realized particular by following four step:
1, surface preparation is carried out to metallic matrix,
Metallic matrix includes but is not limited to stainless steel, titanium alloy,
Pretreatment operation are as follows: by metallic matrix respectively through 400 and 800#SiC sand paper grinding process, and cleaned and done with acetone
It is dry, 5~10min then is handled to its surface sand-blasting (corundum sand), until metal surface loses metallic luster, and clear with acetone
It is dried after washing shot blasting particles remained on surface；
2、TiB2The preparation of sprayed on material,
By TiB2Metal ceramic powder is mixed with dissolved polyvinyl alcohol (PVA) by the mass fraction ratio of 20:1, dry
By star row ball mill ball milling, 100 are then used#、200#Sieve takes sieve step by step, and final partial size of choosing is 100~200 mesh ranges
TiB2Powder is as sprayed on material；
3, by TiB obtained in step (2)2Sprayed on material is pre-processed by plasma spray coating process by step (1)
The pre-prepared TiB of metal base surface2Coating,
The concrete operations of plasma spray coating process are as follows: set distance between spray gun and metallic matrix and spray function as 90~110mm
Rate be 80~85kW, argon gas flow velocity be 38~42L/min, hydrogen flow rate be 15~18L/min, powder feeding rate 28g/min,
Pre-prepared TiB2Coating layer thickness is controlled at 10~15 μm,
In this step, by plasma spraying technology come the boride coating of prefabricated certain hole, the presence of certain hole
Coating can be eliminated in subsequent laser remolten treatment process because coating crack caused by the factors such as internal stress, peel off
Problem also avoids exclusive use laser melting coating and is difficult to the excellent borided layer of processability；
4, re melting process is carried out to prefabricated coating obtained in step (3) using laser melting and coating technique, obtains TiB2Coating,
The power setting of laser melting coating is 60~80W/mm2, frequency be 5~10Hz, electric current pulsewidth is 6~8 μ s, electric current is
220A, sweep speed are 3~8mm/s, protective gas nitrogen flow rate is 15L/min.
To above-mentioned prepared TiB2The performance test methods of coating include:
1, thermal shock resistance test: coating sample being placed at 800 DEG C after keeping the temperature 30min and taken out, be put into quenching in room temperature water, weight
Multiple more than 20 times, and observe coating surface variation；
2, dynamic potential scanning: coating sample is placed in the sulfuric acid solution of 0.5mol/L, evaluates it by electro-chemical test
In acidic environment corrosion resistance.
Specific embodiment
Embodiment 1
(1) metallic matrix selects commercially available 304L stainless steel, is cut to 10mm × 10mm × 3mm sheet substrate,
400 and 800 are respectively adopted#SiC sand paper makees grinding process, and is cleaned and dried with acetone, then using corundum sand to its sandblasting
After handling 10min, its surface is set to lose metallic luster, and be cleaned and dried with acetone；
(2) by the TiB of 200g2Metal ceramic powder is sufficiently mixed with the dissolved polyvinyl alcohol of 10g (PVA), after dry
Through star row ball mill ball milling 3h, revolving speed 450r/min；Then use 100#、200#Sieve takes sieve step by step, and final partial size of choosing is
The TiB of 100~200 mesh2Powder is as spraying powder；
(3) by TiB obtained in step (2)2Sprayed on material is pre-processed by plasma spray coating process by step (1)
The pre-prepared TiB of metal base surface2Coating: distance is 100mm, spray power 80kW, argon gas between spray gun and metallic matrix
Flow velocity is 40L/min, hydrogen flow rate 15L/min, and powder feeding rate remains 28g/min, is sprayed 4 minutes.
This example coating layer thickness obtained is 12 μm, and prepared coating is directly carried out performance survey without re melting process
Examination, find after 20 thermal shock resistance tests, coating appearance significantly fall off, skin effect phenomenon, it is not high with substrate combinating strength；
Using potentiodynamic polarization technology in 0.5mol/L H2SO4Test finds the coating relative to matrix, corrosion in solution
Current potential promotes 130mV, and corrosion current decreases.
Embodiment 2
Step (1), (2), (3) are the same as embodiment 1；
(4) use laser melting and coating technique to prefabricated coating obtained in step (3) carry out re melting process: cladding power for
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 rate
For 15L/min.
This example coating layer thickness obtained is 12 μm, and prepared coating is directly carried out performance survey without re melting process
Examination finds that after 20 thermal shock resistance tests, coating does not occur the sign that falls off, and significantly changing does not occur yet in coating surface, still
It is firmly combined；
Using potentiodynamic polarization 0.5mol/L H2SO4It is tested in solution, finds the coating relative to matrix, corrosion electricity
Position promotes 312mV, and corrosion rate decline is obvious, and corrosion resisting property improves.The TiB of direct spraying in comparative example 12Layer, remelting
Treated thermal shock resistance, corrosion resistance significantly improve, and the binding force of coating and matrix is good.
Embodiment 3
Step (1), (2) are the same as embodiment 1；
(3) by TiB obtained in step (2)2Sprayed on material is pre-processed by plasma spray coating process by step (1)
The pre-prepared TiB of metal base surface2Coating: distance is 100mm, spray power 80kW, argon gas between spray gun and metallic matrix
Flow velocity is 40L/min, hydrogen flow rate 15L/min, and powder feeding rate remains 28g/min, is sprayed 5 minutes；
(4) use laser melting and coating technique to prefabricated coating obtained in step (3) carry out re melting process: cladding power for
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 rate
For 15L/min.
This example coating layer thickness obtained is 14 μm, and prepared coating is directly carried out performance survey without re melting process
Examination finds that after 20 thermal shock resistance tests, coating does not occur the sign that falls off, and significantly changing does not occur yet in coating surface, still
It is firmly combined；
Using potentiodynamic polarization 0.5mol/L H2SO4It is tested in solution, finds the coating relative to matrix, corrosion electricity
Position promotes 291mV, and corrosion rate decline is obvious, and corrosion resisting property improves.The TiB of direct spraying in comparative example 12Layer, remelting
Treated thermal shock resistance, corrosion resistance significantly improve, and the binding force of coating and matrix is good.
Embodiment 4
Step (1), (2) are the same as embodiment 1；
(3) by TiB obtained in step (2)2Sprayed on material is pre-processed by plasma spray coating process by step (1)
The pre-prepared TiB of metal base surface2Coating: distance is 100mm, spray power 80kW, argon gas between spray gun and metallic matrix
Flow velocity is 40L/min, hydrogen flow rate 15L/min, and powder feeding rate remains 28g/min, is sprayed 4 minutes；
(4) use laser melting and coating technique to prefabricated coating obtained in step (3) carry out re melting process: cladding power for
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 rate
For 15L/min.
This example coating layer thickness obtained is 14 μm, and prepared coating is directly carried out performance survey without re melting process
Examination finds that after 20 thermal shock resistance tests, coating does not occur the sign that falls off, but subtle crackle occurs in coating surface, this
It is since sweep speed is comparatively fast caused；
Using potentiodynamic polarization 0.5mol/L H2SO4It is tested in solution, finds the coating relative to matrix, corrosion electricity
Position promotes 223mV, and corrosion rate decline is obvious, and corrosion resisting property improves.
Claims (3)
1. a kind of process for preparing titanium boride coating in metal surface, it is characterised in that: the method are as follows:
(1), surface preparation is carried out to metallic matrix；
(2)、TiB2The preparation of sprayed on material: by TiB2Metal ceramic powder and dissolved polyvinyl alcohol, through row after drying
Celestial body grinding machine ball milling then uses 100#、200#Sieve takes sieve step by step, final to choose the TiB that partial size is 100~200 mesh ranges2Powder
End is used as sprayed on material；
(3), by TiB obtained in step (2)2Sprayed on material is passing through step (1) pretreated gold by plasma spray coating process
Belong to the pre-prepared TiB of matrix surface2Coating, the concrete operations of plasma spray coating process are as follows: distance between setting spray gun and metallic matrix
For 90~110mm, spray power is 80~85kW, and argon gas flow velocity is 38~42L/min, and hydrogen flow rate is 15~18L/min, is sent
Powder rate is 28g/min；
(4), re melting process is carried out to prefabricated coating obtained in step (3) using laser melting and coating technique, obtains TiB2Coating swashs
The power of light cladding is 60~80W/mm2, frequency be 5~10Hz, electric current pulsewidth is 6~8 μ s, electric current 220A, sweep speed
It is 15L/min for 3~8mm/s, protective gas nitrogen flow rate.
2. the process of titanium boride coating is prepared in metal surface as described in claim 1, it is characterised in that: step (1)
Described in metallic matrix be stainless steel or titanium alloy.
3. the process of titanium boride coating is prepared in metal surface as described in claim 1, it is characterised in that: step (1)
In, by metallic matrix respectively through 400#With 800#SiC sand paper grinding process, and be cleaned and dried with acetone, then to its surface sand-blasting
5~10min is handled, until metal surface loses metallic luster, and is dried with after the remaining shot blasting particles of acetone clean the surface.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2812935C1 (en) * | 2023-04-11 | 2024-02-05 | Федеральное государственное унитарное предприятие "Центральный научно-исследовательский институт конструкционных материалов "Прометей" имени И.В. Горынина Национального исследовательского центра "Курчатовский институт" (НИЦ "Курчатовский институт" - ЦНИИ КМ "Прометей") | METHOD FOR MICROPLASMA SPRAYING OF WEAR-RESISTANT COATINGS BASED ON CLAD POWDERS OF Ti/TiB2 SYSTEM |
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| 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 |
| CN107998814B (en) * | 2017-11-24 | 2020-06-16 | 中南大学 | Fluorine-containing flue gas treatment system and application method thereof |
| CN108326384B (en) * | 2017-12-11 | 2021-07-02 | 蚌埠市启典金属制品有限公司 | Brazing process of high-strength corrosion-resistant aluminum-copper joint |
| CN109989059B (en) * | 2019-03-06 | 2021-01-05 | 莆田学院 | TiBw-Ti composite layer and laser in-situ preparation method thereof |
| 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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| JP2728264B2 (en) * | 1988-06-23 | 1998-03-18 | トーカロ株式会社 | Method for producing conductor roll having excellent electrical conductivity and conductor roll |
| DE19714433C2 (en) * | 1997-04-08 | 2002-08-01 | Celanese Ventures Gmbh | Process for producing a coating with a titanium boride content of at least 80% by weight |
| CA2504831C (en) * | 2005-04-21 | 2010-10-19 | Standard Aero Limited | Wear resistant ceramic composite coatings and process for production thereof |
| CN102864404B (en) * | 2012-09-03 | 2014-01-22 | 昆明冶金研究院 | Method for preparing aluminum electrolytic cell TiB2 cathode coating by adopting plasma spraying technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2812935C1 (en) * | 2023-04-11 | 2024-02-05 | Федеральное государственное унитарное предприятие "Центральный научно-исследовательский институт конструкционных материалов "Прометей" имени И.В. Горынина Национального исследовательского центра "Курчатовский институт" (НИЦ "Курчатовский институт" - ЦНИИ КМ "Прометей") | METHOD FOR MICROPLASMA SPRAYING OF WEAR-RESISTANT COATINGS BASED ON CLAD POWDERS OF Ti/TiB2 SYSTEM |
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