CN105177536A - Method for preparing micrometer-particle-contained high-temperature-oxidation-resistant composite coating on surface of niobium alloy - Google Patents
Method for preparing micrometer-particle-contained high-temperature-oxidation-resistant composite coating on surface of niobium alloy Download PDFInfo
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- CN105177536A CN105177536A CN201510584794.5A CN201510584794A CN105177536A CN 105177536 A CN105177536 A CN 105177536A CN 201510584794 A CN201510584794 A CN 201510584794A CN 105177536 A CN105177536 A CN 105177536A
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Abstract
The invention discloses a method for preparing a micrometer-particle-contained high-temperature-oxidation-resistant composite coating on the surface of niobium alloy. The method comprises the steps that firstly, a Ni-CeO2 plating is deposited on a substrate through a composite chemical plating process; and an Al-rich penetration layer is deposited on the plating through a pack cementation process, and the composite coating is formed. The composite coating prepared through the method can be well combined with the substrate, the coating is uniform and compact and good in high-temperature oxidation resistance and can bear oxidation at the temperature at 1200 DEG C, the service life of the coating is prolonged, and the process is simple.
Description
Technical field
The present invention relates to high-temperature protection coating technical field, be specifically related to the preparation method of a kind of niobium alloy surface containing the resistance to high temperature oxidation compound coating of micron particle.
Background technology
During the work of aerospace, nuclear industry and internal combustion turbine, blade must bear the high temperature of 1000 DEG C ~ 1200 DEG C.Nickel-base high-temperature is by the restriction (about 1400 DEG C) of self fusing point, and its service temperature upper limit is only 1100 DEG C, and the high-temperature structural material therefore developing more operation at high temperature is imperative.Metal niobium (Nb) has that fusing point is high, density is little and the advantage such as high temperature specific tenacity is large, but the oxidation-resistance of Nb and Nb-based alloys is poor, calamity " efflorescence " oxidative phenomena can be there is in pure metal Nb at 600 DEG C, its oxidation belongs to the system with obvious oxide skin crackle, along with thickening of zone of oxidation, the internal stress that oxide compound and metal interface produce can make zone of oxidation ftracture, and calamitous oxidation occurs subsequently.Therefore, improving the high-temperature oxidation resistance of niobium alloy, is the key widening its application.
The current intended application temperature of niobium alloy is 1200 DEG C, and alloying and surface-coated effectively improve the method for niobium alloy oxidation-resistance, but the addition of alloying element need control within zone of reasonableness, otherwise can fall low-alloyed mechanical property; At alloy surface coating protective coating, improve alloy high-temp oxidation-resistance and corrosion proof while can also have both good mechanical property, therefore top coat is widely used, and the document of related application is as 1. " a kind of low density niobic alloy high temperature antioxidation material and prepared the method for high-temperature oxidation resistant coating by it " (application number: 201210237037.7); The coating prepared of the method is adopted to efficiently solve low density niobium alloy more than 800 DEG C, especially vigorous oxidation problem in atmospheric environment about 1100 DEG C; 2. " on niobium tungstenalloy, prepare the method for high-temperature oxidation resistant coating " (application number: 201110024937.9), this technology is mainly by preparing high-temperature oxidation resistant nano-composite coating with cold spraying and laser melting and coating technique on niobium tungstenalloy (Nb521) surface; 3. " high-temperature oxidation-resistant material and high-temperature oxidation resistant coating prepared therefrom " (application number: 200610137224.2), this technology, mainly by high-temperature oxidation-resistant material is made powder, carries out fusing preparation coating after being coated on matrix after adding the mixing of other coating; 4. " niobic alloy high temperature antioxidation silicide coating and preparation method thereof " (application number: 200710192652.X); this technology be first at niobium alloy matrix skin by vacuum sintering granularity molybdenum layer; then, under argon shield, coating is prepared by bag siliconising.Though the standby coating of above 4 patent systems solves niobium alloy problem of oxidation in high temperature air environment, but this coating is mainly by the preparation of the method such as slurry process and spraying method, and after coating oxidation, concrete test result (as material phase analysis and shape characteristic etc.) is not yet clear.
Summary of the invention
The technical problem to be solved in the present invention is to provide one and is combined with matrix, coating uniform is fine and close, has good high-temperature oxidation resistance, can bear the oxidation of 1200 DEG C, extend coating work-ing life, the simple niobium alloy surface of technique is containing the preparation method of the resistance to high temperature oxidation compound coating of micron particle.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
Niobium alloy surface, containing a preparation method for the resistance to high temperature oxidation compound coating of micron particle, comprises the following steps:
(1) pre-treatment: by base material successively mass concentration be 99.9% acetone and dehydrated alcohol in each 10min of ultrasonic cleaning respectively, dry up;
(2) coating pre-treatment: base material carried out successively electrochemical deoiling, pickling, once soak zinc, move back zinc, secondary soaking zinc and washing;
(3) particle activation: by CeO
2micron particle soaks each 10min of activation treatment with alcohol-pickled, deionized water that mass concentration is 99.9% successively;
(4) Ni-CeO is prepared
2coating: electroplate liquid formulation is: single nickel salt 25 ~ 35g/L, inferior sodium phosphate 15 ~ 25g/L, trisodium citrate 15 ~ 20g/L, ammonium chloride 10 ~ 25g/L, sodium acetate 15 ~ 25g/L; After above-mentioned formulated plating solution, regulate bath pH value to 8 with ammoniacal liquor, this process is placed in magnetic stirring apparatus and reacts, at plating temperature 70 ~ 85 DEG C of CeO that will have activated
2micron particle adds in plating solution by 8 ~ 10g/L, is hung on by sample in plating solution, reaction times t=1h;
(5) pack cementation aluminizing: by following mass percent preparation penetration enhancer: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%, mixing grinding; Sample containing coating is put into crucible and embedded penetration enhancer, and crucible is placed in the silica tube of vacuum tube furnace, is evacuated to 100 ~ 900mtorr, at furnace temperature 860 ~ 940 DEG C, be incubated 3 ~ 4h; After being incubated, furnace cooling, to room temperature, obtains described compound coating.
In described step (2), the degreaser formula of electrochemical deoiling is: 25g/LNa
3pO
412H
2o, 30g/LNa
2cO
3, 10g/LNa
2siO
3; Pickling adopts mixing acid, and proportioning is water and sulphuric acid soln volume ratio is 1:1, and wherein the mass concentration of sulphuric acid soln is 95 ~ 98%; The zinc dipping solution formula once soaking zinc employing is: 50g/LNaOH, 2g/LKNaC
4h
4o
6h
2o, 5g/LZnO, 2g/LFeCl
36H
2o, 1g/LNaNO
3; The dezincifying solution moving back zinc employing is: the water of volume ratio 1:1 and salpeter solution, and wherein salpeter solution mass concentration is 65 ~ 68%; Secondary soaking zinc is identical with a zinc dipping solution; Washing is distillation washing.
The alcohol-pickled of described step (3) is by CeO
2micron particle add mass concentration be 99.9% spirituous solution soak, and stir after the Nonionic surfactant OP-21 adding 2g/L, soak 10min, treat that spirituous solution clarify, outwell spirituous solution and add deionized water immersion 10min.
Described step (5) vacuum tube furnace temperature rise rate is 10 DEG C/min.
The invention has the beneficial effects as follows:
1, the present invention adopts chemical plating technology and pack cementation technique to prepare compound coating, is combined with matrix, and coating uniform is fine and close.
2, this compound coating is at Ni-CeO
2coating surface deposits the rich Al coating of one deck again, is a kind of novel alloy means, is different from the method that the elements such as Al, Ni, Ce are directly added to Nb alloy by other.
3, the work-ing life of coating is effectively extended.Coatingsurface rich Al, Ni, add rare earth element ce, coating is with AlNi phase, Al
3nb phase and CeO
2xiang Weizhu, generates Al fine and close continuously in hot environment
2o
3film, thus the degeneration delaying coating, show good high-temperature oxidation resistance.
4, can obtain the coating of heterogeneity and thickness by controlling deposition parameter, technique is simple and reproducible, is applicable to suitability for industrialized production.
5, this compound coating can stand the long oxidation of 1200 DEG C.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 compound coating XRD figure spectrum.
Fig. 2 is that the embodiment of the present invention 1 oozes state compound coating surface topography.
Fig. 3 is that the embodiment of the present invention 1 oozes state compound coating Cross Section Morphology.
Fig. 4 is the oxidation weight gain curve of the embodiment of the present invention 1 compound coating at 1200 DEG C of oxidation 20h.
Fig. 5 is that the embodiment of the present invention 1 compound coating is at 1200 DEG C of oxidation 20hXRD collection of illustrative plates.
Fig. 6 is the Cross Section Morphology of the embodiment of the present invention 1 compound coating at 1200 DEG C of oxidation 20h, in figure, and 1.Al
2o
3film; 2. compound coating; 3.Nb base material.
Fig. 7 is that the embodiment of the present invention 2 compound coating is at 1000 DEG C of oxidation 20hXRD collection of illustrative plates.
Fig. 8 is the Cross Section Morphology of the embodiment of the present invention 2 compound coating at 1000 DEG C of oxidation 20h, in figure, and 1.Al
2o
3film; 2. compound coating; 3.Nb base material.
Fig. 9 is the oxidation weight gain curve of the embodiment of the present invention 1,2 compound coating at 1000 DEG C of oxidation 20h, in figure, rich Al/Ni-P-CeO2/C103 coating (b) of (a) 860 DEG C 940 DEG C of rich Al/Ni-P-CeO2/C103 coating (c) matrixes.
Figure 10 is the embodiment of the present invention 3 compound coating Cross Section Morphology.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described, but do not form the restriction to the claims in the present invention protection domain.
Embodiment 1:
Niobium alloy surface, containing a preparation method for the resistance to high temperature oxidation compound coating of micron particle, comprises the following steps:
1, pre-treatment: base material is niobium alloy, by base material successively mass concentration be 99.9% acetone and dehydrated alcohol in each 10min of ultrasonic cleaning respectively, dry up;
2, coating pre-treatment:
Base material is carried out following pre-treatment successively:
Electrochemical deoiling, degreaser formula is: 25g/LNa
3pO
412H
2o, 30g/LNa
2cO
3, 10g/LNa
2siO
3;
Pickling, mixing acid proportioning is: water: sulfuric acid volume ratio=1:1, and wherein h 2 so 4 concentration is 95%;
Once soak zinc, zinc dipping solution formula is: 50g/LNaOH, 2g/LKNaC
4h
4o
6h
2o, 5g/LZnO, 2g/LFeCl
36H
2o, 1g/LNaNO
3;
Move back zinc, dezincifying solution is water: nitric acid volume ratio=1:1, and wherein nitric acid mass concentration is 65%;
Secondary soaking zinc is identical with a zinc dipping solution;
Distillation washing;
3, particle activation: by CeO
2micron particle adds the spirituous solution immersion that mass concentration is 99.9%, and the OP-21 adding 2g/L stirs, soaks, and treats that spirituous solution is clarified, and outwell spirituous solution and add deionized water immersion, spirituous solution and deionized water soak each 10min of activation treatment;
4, Ni-CeO is prepared
2coating:
Electroplate liquid formulation is: single nickel salt 25g/L, inferior sodium phosphate 20g/L, trisodium citrate 18g/L, ammonium chloride 18g/L, sodium acetate 18g/L;
Regulating the pH value to 8 of plating solution with ammoniacal liquor, is 80 DEG C of CeO that will have activated at plating temperature
2micron particle adds in plating solution by 10g/L, hangs sample plating 1h in the plating solution, preparation Ni-CeO
2coating, this process is placed in magnetic stirring apparatus and reacts;
5, pack cementation aluminizing:
By following mass percent preparation penetration enhancer: Al
2o
3powder 87%, Al powder 10%, NaF powder 3%, mixing grinding;
Sample containing coating is put into crucible and embedded penetration enhancer, crucible is placed in the silica tube of vacuum tube furnace, be evacuated to 100mtorr, aluminising in vacuum tube furnace, vacuum tube furnace temperature rise rate is 10 DEG C/min, aluminising temperature 940 DEG C, soaking time is 4h, and after being incubated, furnace cooling is to room temperature, obtain compound coating, compound coating thickness is 40 μm.
Embodiment 2
1, pre-treatment is with embodiment 1.
2, coating pre-treatment:
Base material is carried out following pre-treatment successively:
Electrochemical deoiling is with embodiment 1.
Pickling, mixing acid proportioning is: water: sulfuric acid volume ratio=1:1, and wherein sulfuric acid concentration is 97%;
Once soak zinc, secondary soaking zinc all identical with embodiment 1.
Move back zinc, dezincifying solution is water: nitric acid volume ratio=1:1, and wherein nitric acid mass concentration is 66%;
Distillation washing;
3, particle activation: by CeO
2micron particle adds the spirituous solution immersion that mass concentration is 99.9%, and the OP-21 adding 2g/L stirs, soaks, and treats that spirituous solution is clarified, and outwells spirituous solution and adds deionized water immersion; Spirituous solution and deionized water soak each 10min of activation treatment.
4, Ni-CeO is prepared
2coating:
Electroplate liquid formulation: single nickel salt 28g/L, inferior sodium phosphate 15g/L, trisodium citrate 15g/L, ammonium chloride 10g/L, sodium acetate 15g/L; Regulating the pH value to 8 of plating solution with ammoniacal liquor, is 70 DEG C of CeO that will have activated at plating temperature
2nano particle adds in plating solution by 8g/L, hangs sample plating 1h in the plating solution, preparation Ni-CeO
2coating, this process is placed in magnetic stirring apparatus and reacts;
5, pack cementation aluminizing:
By following mass percent preparation penetration enhancer: Al
2o
3powder 85%, Al powder 11%, NaF powder 4%, mixing grinding;
Sample containing coating is put into crucible and embedded penetration enhancer, crucible is placed in the silica tube of vacuum tube furnace, be evacuated to 900mtorr, aluminising in vacuum tube furnace, vacuum tube furnace temperature rise rate is 10 DEG C/min, aluminising temperature 860 DEG C, soaking time is 3h, and after being incubated, furnace cooling is to room temperature, obtain compound coating, compound coating thickness is 20 μm.
Embodiment 3:
1, pre-treatment is with embodiment 1.
2, coating pre-treatment:
Sample is carried out following pre-treatment successively:
Electrochemical deoiling is with embodiment 1.
Pickling, mixing acid proportioning is: water: sulfuric acid volume ratio=1:1, and wherein sulfuric acid concentration is 98%;
Once soak zinc, secondary soaking zinc all identical with embodiment 1.
Move back zinc, dezincifying solution is water: nitric acid volume ratio=1:1, and wherein nitric acid mass concentration is 68%;
3, particle activation: by CeO
2micron particle adds the spirituous solution immersion that mass concentration is 99.9%, and the OP-21 adding 2g/L stirs, soaks, and treats that spirituous solution is clarified, and outwells spirituous solution and adds deionized water immersion; Spirituous solution and deionized water soak each 10min of activation treatment.
4, Ni-CeO is prepared
2coating:
Electroplate liquid formulation: single nickel salt 35g/L, inferior sodium phosphate 25g/L, trisodium citrate 20g/L, ammonium chloride 25g/L, sodium acetate 25g/L;
Regulating the pH value to 8 of plating solution with ammoniacal liquor, is 75 DEG C of CeO that will have activated at plating temperature
2micron particle adds in plating solution by 9g/L, hangs sample plating 1h in the plating solution, preparation Ni-CeO
2coating, this process is placed in magnetic stirring apparatus and reacts;
5, pack cementation aluminizing:
By following mass percent preparation penetration enhancer: Al
2o
3powder 89%, Al powder 9%, NaF powder 2%, mixing grinding;
Sample containing coating is put into crucible and embedded penetration enhancer, crucible is placed in the silica tube of vacuum tube furnace, be evacuated to 500mtorr, aluminising in vacuum tube furnace, vacuum tube furnace temperature rise rate is 10 DEG C/min, aluminising temperature 900 DEG C, soaking time is 4h, and after being incubated, furnace cooling is to room temperature, obtain compound coating, compound coating thickness is about 40 μm.
One, by high-temperature oxidation resistant compound coating obtained for embodiment 1, utilize XRD diffraction to detect the phase structure of coating respectively, utilize scanning electron microscope (SEM) to observe surface and the Cross Section Morphology of coating, measurement result is shown in Fig. 1-Fig. 7, and measurement result shows:
As shown in Figure 1, state compound coating is oozed primarily of Al
3nb, Al
3ni, AlNi, CeO
2phase composite, illustrates, at the Al of aluminising process mesectoderm and the Ni element of internal layer and matrix, obvious diffusion reaction all occurs, thus generate Al-Ni, Al-Nb phase.
As shown in Figure 2, compound coating surface in cotton-shaped weave construction, and containing micropore, without cracking and obscission, is combined well with matrix.
As shown in Figure 3, coatings growth even compact, be combined densification with matrix.
As seen from Figure 4, after 1200 DEG C of oxidation 20h, 2.7mg/cm is only containing weightening finish after the sample oxidation 20h of compound coating
2, in Fig. 9, matrix is in the weightening finish of 1000 DEG C/20h.
As seen from Figure 5, after 1200 DEG C of oxidation 20h, coating sample Surface Creation Al
2o
3phase.
As seen from Figure 6, after 1200 DEG C/20h is oxidized, coating skin generates zone of oxidation, and coating is through long high temperature oxidation, and hole appears in skin, and internal layer remains good continuity and compactness, combines and be still closely between coating and matrix.
As seen from Figure 9, the weightening finish after 1000 DEG C of oxidation 20h of niobium alloy matrix is 254.1mg/cm
2, after the sample oxidation 20h after 940 DEG C of platings are oozed, weightening finish is 2.2mg/cm
2, illustrating that the sample high-temperature oxidation resistance containing compound coating is good, improve 114 times through calculating than matrix.
Two, embodiment 2 measurement result shows:
As seen from Figure 7, after 1000 DEG C of oxidation 20h, the sample containing compound coating mainly generates Al
2o
3phase.
As seen from Figure 8, after 1000 DEG C of oxidation 20h, first plate the sample surfaces oozing compound coating afterwards and generate the evenly Al of densification
2o
3layer.Al
2o
3the interbed of layer, compound coating, matrix is combined with layer well, without obscission.
As seen from Figure 9, the weightening finish after 1000 DEG C of oxidation 20h of niobium alloy matrix is 254.0653mg/cm
2, oozing weightening finish after compound coating sample oxidation 20h through 860 DEG C of platings is 3.6mg/cm
2, illustrating that the sample containing compound coating has good high temperature oxidation resistance, improve 70 times through calculating than matrix.
Three, embodiment 3 measurement result shows:
As seen from Figure 10, compound coating is smooth and continuous, combines closely between coating and niobium alloy matrix, occurs without hole, crackle.
Claims (4)
1. niobium alloy surface is containing a preparation method for the resistance to high temperature oxidation compound coating of micron particle, it is characterized in that, comprises the following steps:
(1) pre-treatment: by base material successively mass concentration be 99.9% acetone and dehydrated alcohol in each 10min of ultrasonic cleaning respectively, dry up;
(2) coating pre-treatment: base material carried out successively electrochemical deoiling, pickling, once soak zinc, move back zinc, secondary soaking zinc and washing;
(3) particle activation: by CeO
2micron particle soaks each 10min of activation treatment with alcohol-pickled, deionized water that mass concentration is 99.9% successively;
(4) Ni-CeO is prepared
2coating: electroplate liquid formulation is: single nickel salt 25 ~ 35g/L, inferior sodium phosphate 15 ~ 25g/L, trisodium citrate 15 ~ 20g/L, ammonium chloride 10 ~ 25g/L, sodium acetate 15 ~ 25g/L; After above-mentioned formulated plating solution, regulate bath pH value to 8 with ammoniacal liquor, this process is placed in magnetic stirring apparatus and reacts, at plating temperature 70 ~ 85 DEG C of CeO that will have activated
2micron particle adds in plating solution by 8 ~ 10g/L, is hung on by sample in plating solution, reaction times t=1h;
(5) pack cementation aluminizing: by following mass percent preparation penetration enhancer: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%, mixing grinding; Sample containing coating is put into crucible and embedded penetration enhancer, and crucible is placed in the silica tube of vacuum tube furnace, is evacuated to 100 ~ 900mtorr, at furnace temperature 860 ~ 940 DEG C, be incubated 3 ~ 4h; After being incubated, furnace cooling, to room temperature, obtains described compound coating.
2. a kind of niobium alloy surface is containing the preparation method of the resistance to high temperature oxidation compound coating of micron particle as described in the appended claim 1, and it is characterized in that, in described step (2), the degreaser formula of electrochemical deoiling is: 25g/LNa
3pO
412H
2o, 30g/LNa
2cO
3, 10g/LNa
2siO
3; Pickling adopts mixing acid, and proportioning is water and sulphuric acid soln volume ratio is 1:1, and wherein the mass concentration of sulphuric acid soln is 95 ~ 98%; The zinc dipping solution formula once soaking zinc employing is: 50g/LNaOH, 2g/LKNaC
4h
4o
6h
2o, 5g/LZnO, 2g/LFeCl
36H
2o, 1g/LNaNO
3; The dezincifying solution moving back zinc employing is: the water of volume ratio 1:1 and salpeter solution, and wherein salpeter solution mass concentration is 65 ~ 68%; Secondary soaking zinc is identical with a zinc dipping solution; Washing is distillation washing.
3. a kind of niobium alloy surface is containing the preparation method of the resistance to high temperature oxidation compound coating of micron particle as described in the appended claim 1, and it is characterized in that, the alcohol-pickled of described step (3) is by CeO
2micron particle add mass concentration be 99.9% spirituous solution soak, and stir after the Nonionic surfactant OP-21 adding 2g/L, soak 10min, treat that spirituous solution clarify, outwell spirituous solution and add deionized water immersion 10min.
4. a kind of niobium alloy surface is containing the preparation method of the resistance to high temperature oxidation compound coating of micron particle as described in the appended claim 1, and it is characterized in that, described step (5) vacuum tube furnace temperature rise rate is 10 DEG C/min.
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| CN105714339A (en) * | 2016-04-01 | 2016-06-29 | 上海交通大学 | Zr doped Ni-Al adhesive layer material with Ni-Zr diffusion obstacle layer and preparation method thereof |
| CN106591773A (en) * | 2016-12-14 | 2017-04-26 | 哈尔滨工业大学 | Preparation method of high-temperature oxidation resistant radiative thermal protection coating for metal surface applicable to high temperature |
| CN108642535A (en) * | 2018-05-31 | 2018-10-12 | 上海工程技术大学 | A kind of preparation method of ceria modified aluminide gradient coating system |
| CN113046671A (en) * | 2021-03-11 | 2021-06-29 | 南京工程学院 | Nano CeO2Method for enhancing corrosion resistance of ZnAl-based composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714339A (en) * | 2016-04-01 | 2016-06-29 | 上海交通大学 | Zr doped Ni-Al adhesive layer material with Ni-Zr diffusion obstacle layer and preparation method thereof |
| CN106591773A (en) * | 2016-12-14 | 2017-04-26 | 哈尔滨工业大学 | Preparation method of high-temperature oxidation resistant radiative thermal protection coating for metal surface applicable to high temperature |
| CN106591773B (en) * | 2016-12-14 | 2019-01-18 | 哈尔滨工业大学 | A kind of high temperature metal surface resistance to high temperature oxidation radiation thermal protection coating preparation method |
| CN108642535A (en) * | 2018-05-31 | 2018-10-12 | 上海工程技术大学 | A kind of preparation method of ceria modified aluminide gradient coating system |
| CN113046671A (en) * | 2021-03-11 | 2021-06-29 | 南京工程学院 | Nano CeO2Method for enhancing corrosion resistance of ZnAl-based composite material |
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