CN106811782A - Nickel cobalt/chromium aluminium/yittrium oxide coating and its composite plating method - Google Patents
Nickel cobalt/chromium aluminium/yittrium oxide coating and its composite plating method Download PDFInfo
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- CN106811782A CN106811782A CN201710073911.0A CN201710073911A CN106811782A CN 106811782 A CN106811782 A CN 106811782A CN 201710073911 A CN201710073911 A CN 201710073911A CN 106811782 A CN106811782 A CN 106811782A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The present invention relates to one kind (Ni Co)/CrAl/Y2O3Coating and its composite plating method, the composite plating method comprise the following steps：CrAl/Y2O3It is prepared by alloy powder：According to weight than 80~120：1 mixing CrAl alloy powders and Y2O3Powder, then carries out ball milling, obtains CrAl/Y2O3Alloy powder；It is prepared by coating：Substrate is taken, composite plating is carried out：By the CrAl/Y2O3Alloy powder is added into electroplate liquid, and addition is 20~50g/L；Then electroplated using reverse pulse electric current, obtained final product.(Ni Co)/CrAl/Y that the composite plating method is prepared2O3The careful, adhesion of coating crystallization is good, and plated layer compact is smooth, voidage is low, and toughness, resistance to high temperature oxidation and hot corrosion resistance are good, while low production cost.
Description
Technical field
The present invention relates to electroplating technology field, more particularly to nickel-cobalt/chromium-aluminium/yittrium oxide coating and its composite plating side
Method.
Background technology
High temperature coating such as Ni-Cr, Ni-Al, MCrA1Y etc. have good toughness, good corrosion and heat resistant, anti-oxidant and heat resistanceheat resistant
The features such as mechanical fatigue, receive the widely studied of domestic and international researcher.Research of the domestic and international researcher to MCrA1Y coating
Focus primarily upon improvement coating composition and the optimization aspect such as coating structure, conventional method be by increase in coating Ti, Si,
The multiple elements such as Ta, Re, Ru, and using the method for Multi-layer design, improve coating performance.At present, above-mentioned high temperature coating is prepared
Method have：Electron beam-physical vapor spraying, low pressure or vacuum plasma spray coating, detonation flame spraying, vacuum arc deposition, three poles
High speed pigment spraying that sputtering and latest developments are got up etc..But be present high cost, apparatus expensive in method made above, obtained
The shortcomings of there is crackle in coating, porosity is high.
Composite plating is to make matrix metal micro- with insoluble solid by chemistry or electrochemical method in electrolyte solution
Grain is co-deposited and obtain the new technology of composite layer.Recent years, there is researcher to prepare Ni- using composite plating technology
The composite deposites such as CrAl, Ni-CrAl-Y and MCrA1Y.But the structure of the high temperature coating such as gained Ni-Cr, Ni-Al, MCrA1Y is also
It is that not enough fine and close, porosity is higher, therefore toughness, resistance to high temperature oxidation and hot corrosion resistance are bad, and obtained MCrA1Y coating
There is the phase counterdiffusion of element in high temperature environments, between coating and matrix for a long time, cause coating performance to deteriorate, high temperature resistance
Heat erosion and mechanical performance decline.
The content of the invention
Based on this, it is necessary to provide a kind of low production cost, the nickel that plated layer compact, light, porosity are low, adhesion is good-
The composite plating method of cobalt/chromium-aluminium/yittrium oxide coating.
A kind of nickel-cobalt/chromium-aluminium/yittrium oxide ((Ni-Co)/CrAl/Y2O3) coating composite plating method, including following step
Suddenly：
CrAl/Y2O3It is prepared by alloy powder：
According to weight than 80~120：1 mixing CrAl alloy powders and Y2O3Powder, then carries out ball milling, obtains CrAl/
Y2O3Alloy powder；
It is prepared by coating：Substrate is taken, composite plating is carried out：With including 115~180g/L nickel sulfates, 10~30g/L nickel chlorides,
2~5g/L cobaltous sulfates, 20~50g/LH3BO3, 0.1~0.2g/L surfactants the aqueous solution as electroplate liquid, and will be described
CrAl/Y2O3Alloy powder is added into the electroplate liquid, and addition is 20~50g/L；Then reverse pulse electric current is used
Electroplated, i.e., prepared (the Ni-Co)/CrAl/Y on the surface of the substrate2O3Coating.
(Ni-Co)/CrAl/Y of the invention2O3The composite plating method of coating, by using reverse pulse electric current,
With reference to CrAl/Y2O3Alloy powder, using Ni, Co as the composite plating method of coating main element, is prepared as solia particle
(the Ni-Co)/CrAl/Y for obtaining2O3The careful, adhesion of coating crystallization is good, and plated layer compact is smooth, voidage is low, toughness, high temperature resistance
Oxidation and hot corrosion resistance are good.Meanwhile, the method is without the use of HTHP, and equipment is simple, and easy to operate, process conditions can
Control, suitable production line balance, and the more existing electron beam of production cost-physical vapor spraying, low pressure or vacuum plasma spray coating,
The methods such as detonation flame spraying, vacuum arc deposition, triode sputtering, the spraying of high speed pigment are greatly reduced.Its principle and advantage are as follows：
(1) it is using the principle and advantage of reverse pulse electric current：A () plates in the presence of rp pulse electric current
The hydrogen of layer surface attachment is aoxidized, and eliminates hydrogen embrittlement, and coating becomes smooth because the burr above it dissolves；(b) anti-phase arteries and veins
The anodic dissolution effect of electric current is rushed, the ion solubility near substrate surface is increased rapidly, surface is also constantly in the state of activation,
Subsequent direct impulse electric current can cause that the formation speed of nucleus has been more than the speed of growth of crystal, the coating crystal grain because obtained from
Tiny, general effect shows as that coating is finer and close, bright, porosity is low, and adhesion is good；C () organic impurities is in rp pulse
It is easier to disengage it from matrix surface in the presence of electric current, this just can greatly reduce the amount of such impurity in coating, improves
Coating purity, meanwhile, the internal stress of coating is reduced, increase the adhesion between coating and matrix.
(2) with CrAl/Y2O3Alloy powder as solia particle, using Ni, Co as the principle and advantage of coating main element
It is：The essential element of coating is constituted using Ni, Co, high performance intermetallic compound (NiAl, Ni can be formed with Al3Al,
CoAl)；In addition in corrosive environment, particularly in corrosive environment containing S, the coating shows excellent corrosion resistance, and this is
The sulfate of stabilization can be formed with S due to Co, and the Cr and Al in coating can form protective oxide film in oxidizing process；
Y can effectively improve the adhesiveness of the protective oxide film of formation in coating simultaneously.
Wherein in one embodiment, the average grain diameter of the CrAl alloy powders is 20~100um；The Y2O3Powder
Average grain diameter be 50~150nm.
Wherein in one embodiment, the average grain diameter of the CrAl alloy powders is 50~70um；The Y2O3Powder
Average grain diameter is 50~150nm.
Wherein in one embodiment, the current density of the reverse pulse electric current is 2~3A/dm2, the cycle is for just
To 50~150ms of burst length, 10~50ms of negative-going pulse time.
Wherein in one embodiment, the cycle of the reverse pulse electric current is 90~110ms of direct impulse time,
25~35ms of negative-going pulse time.
Further rationally control CrAl alloy powders and Y2O3The particle diameter of powder, and reverse pulse electric current electric current
Density and pulse period, (the Ni-Co)/CrAl/Y for preparing can be made2O3Coating has more excellent combination property.
Wherein in one embodiment, the method for the ball milling is：The rotating speed for controlling ball mill is 500~550 revs/min
Clock, Ball-milling Time is 2~6h.
Wherein in one embodiment, during the composite plating, using intermittent airflow stirring, stir and stop
The ratio between time of stirring is 1:2~4, speed of agitator is 100~150 revs/min.
Wherein in one embodiment, the time of the composite plating is 120~180min.
Wherein in one embodiment, before carrying out the composite plating, 160~200 mesh, 380~420 are first used successively
Mesh, the sand paper of 580~620 mesh are polished the substrate.
Wherein in one embodiment, before the polishing is carried out, also including oil removing and/or descaling step；Wherein, it is described
Deoiling step is：The degreasing fluid for using is for including 20g/LNa3PO4, 2g/LOP emulsifying agents, 20g/LNa2CO3, 65g/LNaOH's
The aqueous solution；Treatment temperature is 80~90 DEG C, 3~8min of time.
The descaling step is：The rust removing solution for using for including 0.2~0.5L/L38%HCl, 0.5~1.5L/LH2SO4, 0
The aqueous solution of~0.6wt%OP-10 emulsifying agents, 0.6~1.2wt% methenamines；Treatment temperature is normal temperature, the time is 1~
5min。
Wherein in one embodiment, the material of described matrix is stainless steel.
Wherein in one embodiment, the surfactant is cationic surfactant, preferably cetyl three
Methyl bromide ammonium.
The present invention also provides described (Ni-Co)/CrAl/Y2O3(the Ni- that the composite plating method of coating is prepared
Co)/CrAl/Y2O3Coating.
Compared with prior art, the invention has the advantages that：
(Ni-Co)/CrAl/Y of the invention2O3The composite plating method of coating, by using reverse pulse electric current,
With reference to CrAl/Y2O3Alloy powder, using Ni, Co as the composite plating method of coating main element, is prepared as solia particle
(the Ni-Co)/CrAl/Y for obtaining2O3The careful, adhesion of coating crystallization is good, and plated layer compact is smooth, voidage is low, toughness, high temperature resistance
Oxidation and hot corrosion resistance are good.
Meanwhile, the composite plating method is without the use of HTHP, and equipment is simple, and easy to operate, process conditions are controllable, fits
Close production line balance, and the more existing electron beam of production cost-physical vapor spraying, low pressure or vacuum plasma spray coating, blast
The methods such as spraying, vacuum arc deposition, triode sputtering, the spraying of high speed pigment are greatly reduced.
Brief description of the drawings
(Ni-Co)/CrAl/Y that Fig. 1 is prepared for one embodiment of the invention2O3The energy spectrum diagram of coating；
(Ni-Co)/CrAl/Y that Fig. 2 is prepared for one embodiment of the invention2O3The macro morphology figure of coating；
(Ni-Co)/CrAl/Y that Fig. 3 is prepared for one embodiment of the invention2O3The microscopic appearance figure of coating.
Specific embodiment
Below in conjunction with specific embodiment to (Ni-Co)/CrAl/Y of the invention2O3Coating and its composite plating method make into
One step is described in detail.
Embodiment 1
The present embodiment one kind (Ni-Co)/CrAl/Y2O3The composite plating method of coating, the substrate for using is Q235 steel, step
It is rapid as follows：
(1) pretreatment of substrate：
A. substrate goes oil processing：The degreasing fluid for using is for including Na3PO420g/L, OP emulsifying agent 2g/L, Na2CO320g/
The aqueous solution of L, NaOH65g/L；Treatment temperature is 80~90 DEG C, 3~8min of time；
B. the processing of rust removing of substrate：The rust removing solution for using is for including 38%HCl0.2~0.5L/L, H2SO40.5~1.5L/
0~0.6wt% of L, OP-10 emulsifying agent, the aqueous solution of 0.6~1.2wt% of methenamine；Treatment temperature is normal temperature, the time is 1~
5min；
C. polish：The substrate after degreasing and rust removal is polished successively with 180#, 400#, 600#, 600#, is rushed with distilled water
Wash, then carrying out ultrasonic wave to the substrate after polishing with alcohol cleans, dry for standby.
(2)CrAl/Y2O3It is prepared by alloy powder：
It is the spherical Y of 100nm that 2 grams of average grain diameters are added in 200 grams of average grain diameters are for the CrAl powder of 60um2O3, mixed powder
Refined using QM-3SP2 planetary ball mills, wherein the agate tank volume for using is 100mL, argon gas be passed through in ball grinder,
Sealing, controls the rotating speed of ball mill for 525 revs/min, per the operation of half an hour positive and negative alternate, ball milling 4h.
(3) substrate surface reverse pulse composite plating：
Composite plating is carried out to the substrate that step (1) treatment is obtained：The formula of electroplate liquid is：NiSO4·6H2O250g/L,
NiCl2·6H2O35g/L, CoSO4·7H2O6g/L, H3BO330g/L, CrAl/Y2O330g/L, cetyl trimethylammonium bromide
0.1g/L；Electroplating temperature is room temperature, and pH is 3.5~4.2, and current density is 2~3A/dm2, reverse pulse TF(just)
100ms, TR(negative) 30ms；Using intermittent air stirring mode, the make-to-break ratio of intermittence stirring is 1:3, speed of agitator is 120
Rev/min；Plating time is 150min, i.e., prepare (Ni-Co)/CrAl/Y on the surface of substrate2O3Coating.
Embodiment 2
The present embodiment one kind (Ni-Co)/CrAl/Y2O3The composite plating method of coating, the substrate for using is Q235 steel, step
It is rapid as follows：
(1) preprocess method of substrate is with embodiment 1.
(2)CrAl/Y2O3It is prepared by alloy powder：
It is the spherical Y of 150nm that 2 grams of average grain diameters are added in 160 grams of average grain diameters are for the CrAl powder of 20um2O3, mixed powder
Refined using QM-3SP2 planetary ball mills, wherein the agate tank volume for using is 100mL, argon gas be passed through in ball grinder,
Sealing, controls the rotating speed of ball mill for 500 revs/min, per the operation of half an hour positive and negative alternate, ball milling 6h.
(3) substrate surface reverse pulse composite plating：
Composite plating is carried out to the substrate that step (1) treatment is obtained：The formula of electroplate liquid is：NiSO4·6H2O300g/L,
NiCl2·6H2O20g/L, CoSO4·7H2O9g/L, H3BO350g/L, CrAl/Y2O320g/L, cetyl trimethylammonium bromide
0.2g/L；Electroplating temperature is room temperature, and pH is 3.5~4.2, and current density is 2~3A/dm2, reverse pulse TF(just) 50T/
Ms, TR(negative) 50T/ms；Using intermittent air stirring mode, the make-to-break ratio of intermittence stirring is 1:3, speed of agitator is 100
Rev/min；Plating time is 120min, i.e., prepare (Ni-Co)/CrAl/Y on the surface of substrate2O3Coating.
Embodiment 3
The present embodiment one kind (Ni-Co)/CrAl/Y2O3The composite plating method of coating, the substrate for using is T92 steel, step
It is as follows：
(1) preprocess method of substrate is with embodiment 1.
(2)CrAl/Y2O3It is prepared by alloy powder：
It is the spherical Y of 50nm that 2 grams of average grain diameters are added in 240 grams of average grain diameters are for the CrAl powder of 100um2O3, mixed powder
Refined using QM-3SP2 planetary ball mills, wherein the agate tank volume for using is 100mL, argon gas be passed through in ball grinder,
Sealing, controls the rotating speed of ball mill for 550 revs/min, per the operation of half an hour positive and negative alternate, ball milling 2h.
(3) substrate surface reverse pulse composite plating：
Composite plating is carried out to the substrate that step (1) treatment is obtained：The formula of electroplate liquid is：NiSO4·6H2O200g/L,
NiCl2·6H2O50g/L, CoSO4·7H2O5g/L, H3BO320g/L, CrAl/Y2O350g/L, cetyl trimethylammonium bromide
0.1g/L；Electroplating temperature is room temperature, and pH is 3.5~4.2, and current density is 2~3A/dm2, reverse pulse TF(just) 150T/
Ms, TR(negative) 10T/ms；Using intermittent air stirring mode, the make-to-break ratio of intermittence stirring is 1:3, speed of agitator is 150
Rev/min；Plating time is 180min, i.e., prepare (Ni-Co)/CrAl/Y on the surface of substrate2O3Coating.
Comparative example 1
This comparative example one kind (Ni-Co)/CrAl/Y2O3The preparation method of coating, its step similar embodiment 1, difference exists
In：Step uses DC current in (3).
Comparative example 2
This comparative example one kind (Ni-Co)/CrAl/Y2O3The preparation method of coating, its step similar embodiment 1, difference exists
In：Step does not add CrAl/Y in (3)2O3Alloy powder.
(Ni-Co)/CrAl/Y that embodiment 1 is prepared2O3The energy spectrum diagram of coating is as shown in figure 1, macro morphology such as Fig. 2
Shown, microscopic appearance is as shown in Figure 3, it can be seen that, should (Ni-Co)/CrAl/Y2O3Coating structure is smooth, densification.
Further the coating to embodiment 1-3 and comparative example 1-2 carries out performance detection, as a result as shown in table 1.
Table 1
| Porosity | Adhesion (MPa) | Toughness | High temperature oxidation resistance/heat erosion | |
| Embodiment 1 | 0.56% | 59.86 | It is good | It is excellent |
| Embodiment 2 | 0.63% | 62.25 | It is good | It is excellent |
| Embodiment 3 | 0.59% | 59.48 | It is good | It is excellent |
| Comparative example 1 | 1.57% | 48.63 | Typically | It is poor |
| Comparative example 2 | 0.60% | 59.95 | Typically | Difference |
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. one kind (Ni-Co)/CrAl/Y2O3The composite plating method of coating, it is characterised in that comprise the following steps：
CrAl/Y2O3It is prepared by alloy powder：
According to weight than 80~120：1 mixing CrAl alloy powders and Y2O3Powder, mixed-powder carries out ball milling, obtains CrAl/
Y2O3Alloy powder；
It is prepared by coating：Substrate is taken, composite plating is carried out：With including 115~180g/L nickel sulfates, 10~30g/L nickel chlorides, 2~
5g/L cobaltous sulfates, 20~50g/LH3BO3, 0.1~0.2g/L surfactants the aqueous solution as electroplate liquid, and will be described
CrAl/Y2O3Alloy powder is added into the electroplate liquid, and addition is 20~50g/L；Then reverse pulse electric current is used
Electroplated, i.e., prepared (the Ni-Co)/CrAl/Y on the surface of the substrate2O3Coating.
2. (Ni-Co)/CrAl/Y according to claim 12O3The composite plating method of coating, it is characterised in that described
The average grain diameter of CrAl alloy powders is 20~100um；The Y2O3The average grain diameter of powder is 50~150nm.
3. (Ni-Co)/CrAl/Y according to claim 22O3The composite plating method of coating, it is characterised in that described
The average grain diameter of CrAl alloy powders is 50~70um；The Y2O3The average grain diameter of powder is 80~120nm.
4. (Ni-Co)/CrAl/Y according to claim 12O3The composite plating method of coating, it is characterised in that the week
The current density of phase commutating pulse electric current is 2~3A/dm2, the cycle is 50~150ms of direct impulse time, negative-going pulse time
10~50ms.
5. (Ni-Co)/CrAl/Y according to claim 42O3The composite plating method of coating, it is characterised in that the week
The cycle of phase commutating pulse electric current is 90~110ms of direct impulse time, 25~35ms of negative-going pulse time.
6. (the Ni-Co)/CrAl/Y according to claim any one of 1-52O3The composite plating method of coating, its feature exists
In the method for the ball milling is：It is 500~550 revs/min to control the rotating speed of ball mill, and Ball-milling Time is 2~6h.
7. (the Ni-Co)/CrAl/Y according to claim any one of 1-52O3The composite plating method of coating, its feature exists
During the composite plating, using intermittent airflow stirring, the ratio between time of stirring and stopping stirring is 1:2~4,
Speed of agitator is 100~150 revs/min.
8. (the Ni-Co)/CrAl/Y according to claim any one of 1-52O3The composite plating method of coating, its feature exists
In before carrying out the composite plating, first successively using 160~200 mesh, 380~420 mesh, the sand paper of 580~620 mesh to described
Substrate is polished.
9. (the Ni-Co)/CrAl/Y according to claim any one of 1-52O3The composite plating method of coating, its feature exists
In the material of described matrix is stainless steel.
10. (the Ni-Co)/CrAl/Y described in any one of claim 1-92O3What the composite plating method of coating was prepared
(Ni-Co)/CrAl/Y2O3Coating.
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| CN106086997A (en) * | 2016-06-17 | 2016-11-09 | 中国科学院金属研究所 | A kind of thermally grown Al2o3or Cr2o3membranous type M Cr Al nano-composite plate and preparation and application |
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