CN104561952A - Composite coating resistant to high temperature oxidation and preparation method thereof - Google Patents
Composite coating resistant to high temperature oxidation and preparation method thereof Download PDFInfo
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- CN104561952A CN104561952A CN201510002563.9A CN201510002563A CN104561952A CN 104561952 A CN104561952 A CN 104561952A CN 201510002563 A CN201510002563 A CN 201510002563A CN 104561952 A CN104561952 A CN 104561952A
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Abstract
The invention discloses a composite coating resistant to high temperature oxidation and a preparation method thereof. The composite coating is prepared through the following steps: depositing an Ni-P coating on a base material by adopting a chemical plating technology; then, enabling aluminum to permeate into the Ni-P coating by adopting an embedding aluminizing technology, so as to form the composite coating resistant to high temperature oxidation, wherein a plating solution of the chemical plating technology comprises the following components: 25-35 g/L of nickel sulfate, 15-25 g/L of sodium hypophosphite, 15-20 g/L of trisodium citrate, 10-25 g/L of ammonium chloride and 15-25 g/L of sodium acetate; an aluminizing agent of the embedding aluminizing technology comprises the following components by weight percent: 85-89% of Al2O3 powder, 9-11% of Al powder and 2-4% of NaF powder. According to invention, the prepared composite coating is bonded well with the base material, is uniform and compact, has good resistance to high temperature oxidation, is simple in technology, has good repeatability, and can be prepared in large area.
Description
Technical field
The present invention relates to high-temperature protection coating technical field, relate in particular to a kind of resistance to high temperature oxidation compound coating and preparation method thereof.
Background technology
High-temperature protection coating is mainly used in the hot-end component that the industry such as aerospace, nuclear industry and internal combustion turbine manufacture.Metal niobium has that fusing point is high, density is little and the advantage such as high temperature specific tenacity is large, is considered to the high-temperature structural material of the existing nickel-base alloy of the most potential replacement.But the oxidation-resistance of Nb and Nb-based alloys is poor, calamitous " efflorescence " oxidative phenomena is 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 Nb and Nb-based alloys, form protective oxide film on its surface, is the key widening its application.
Alloying and top coat protection effectively can improve the oxidation-resistance of metal; alloying is usually to lose intensity and processing characteristics for cost; and to add coating protection very little to the Effect on Mechanical Properties of metal on surface, and can significantly improve oxidation-resistance, experiment proves practicable approach.The document of related application as: 1. application number is the Chinese patent of 201210237037.7, disclose a kind of low density niobic alloy high temperature antioxidation material and prepared the method for high-temperature oxidation resistant coating by it, this patent adopts surface coating process, to component be that " B is 0.5wt%; Si is 10wt%; Ti is 2wt%, and Ge is 1.5wt%, M by weight.For 1wt%, HfO
2for 0.8wt%, W is 0.7wt%, S is 0.25wt%, surplus is Al " coated materials at substrate surface; efficiently solve low density niobium alloy more than 800 DEG C; especially vigorous oxidation problem in atmospheric environment about 1100 DEG C, farthest retains the mechanical behavior under high temperature of alloy, expands the low density niobium alloy scope of application simultaneously and extends its work-ing life.2. application number is the Chinese patent of 201110024937.9, disclose a kind of method preparing high-temperature oxidation resistant coating on niobium tungstenalloy, this patent 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, tissue tight between the party's decree coat powder, substantially increases the compactness of coating; 3. application number is the Chinese patent of 200610137224.2, disclose a kind of high-temperature oxidation-resistant material and high-temperature oxidation resistant coating prepared therefrom, this patent is mainly by making powder by high-temperature oxidation-resistant material, carry out fusing preparation coating after being coated on matrix after adding the mixing of other coating to fuse, this coating has the performance such as antioxidant anticorrosive, antiscour, and can be widely used on engine nozzle, turbine blade, combustion chamber and other high-temperature structural components; 4. application number is the Chinese patent of 200710192652.X; disclose a kind of niobic alloy high temperature antioxidation silicide coating and preparation method thereof; first this patent passes through vacuum sintering granularity molybdenum layer at niobium alloy matrix skin; then under argon shield; prepare coating by bag siliconising, coating ingredients prepared by the method and thickness are comparatively even, and density comparatively slurry reaction sintering process improves a lot; and technique is simple, low for equipment requirements.The present invention adopts chemical plating Ni-P coating and pack cementation aluminizing technology, can significantly improve resistance to high temperature oxidation and the corrosion resistance of Nb and Nb-based alloys, at present, has no pertinent literature report.
Summary of the invention
The object of the invention is the shortcoming for Nb and Nb-based alloys high temperature antioxidant difference, utilize electroless plating technology and pack cementation technology, a kind of novel resistance to high temperature oxidation compound coating and preparation method thereof is provided, the resistance to high temperature oxidation effect that improve compound coating by a relatively large margin, extends the work-ing life of Nb and Nb-based alloys.
Technical scheme of the present invention is:
A kind of resistance to high temperature oxidation compound coating, first by electroless plating technology, at deposited on substrates Ni-P coating; Again by pack cementation aluminizing technology, infiltrate aluminium at Ni-P coating, form resistance to high temperature oxidation compound coating;
The electroplate liquid formulation of described electroless plating technology 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;
The penetration enhancer compositions in weight percentage of described pack cementation aluminizing technology is: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%.
Above-described resistance to high temperature oxidation compound coating, described base material is preferably niobium or niobium alloy, also can be other resistant to elevated temperatures material, as metal, alloy etc.
The preparation method of resistance to high temperature oxidation compound coating described in more than one, comprises pre-treatment, electroless plating pre-treatment, preparation Ni-P coating, pack cementation aluminizing step:
1. pre-treatment: by the base material successively each 10min of difference ultrasonic cleaning in acetone and dehydrated alcohol, dry up;
2. electroless plating pre-treatment: base material good for pre-treatment is carried out electrochemical deoiling, pickling successively, once soaks zinc, move back zinc, secondary soaking zinc, washing;
3. prepare Ni-P coating: prepare plating solution according to the following formulation: 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, pH value to 7.5 ~ 9.0 of plating solution are regulated with ammoniacal liquor, hang in plating solution by the base material that electroless plating pre-treatment is good, putting temperature is react 0.5 ~ 1.5 hour in the water-bath of 70 ~ 85 DEG C;
4. pack cementation aluminizing: prepare penetration enhancer as following weight percent: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%, mixing grinding, puts in tube furnace by the penetration enhancer fully mixed and the base material that plated Ni-P coating, is evacuated to 2 × 10
-1~ 3 × 10
-1pa, tube furnace temperature rise rate is 6 ~ 7 DEG C/min, is to be incubated 3 ~ 4 hours under the furnace temperature of 850 ~ 950 DEG C in temperature, and after being incubated, furnace cooling, to room temperature, obtains resistance to high temperature oxidation compound coating.
Above-described high-temperature oxidation resistant compound coating, described base material is preferably niobium or niobium alloy, also can be other resistant to elevated temperatures material.
The invention has the beneficial effects as follows:
1. the present invention adopts compound coating prepared by electroless plating technology and pack cementation technology, utilizes scanning electron microscope (SEM) to observe: surface is in cotton-shaped weave construction, and containing micropore, not cracking and obscission, thickness is homogeneous, is combined well with base material.
2. this compound coating infiltrates Al again at Ni-P coating surface, be different from the method that the elements such as Al, Ni are directly added to Nb and Nb-based alloys by other, the present invention Al in aluminising process is outer to be occurred significantly to spread with Ni-P internal layer, phenomenon is interpenetrated between coating, thus generate AlNi phase, be a kind of novel alloy means, there is good erosion resistance and wear resistance.
3. this compound coating effectively can extend the work-ing life of Nb and Nb-based alloys.Coatingsurface rich Al, Ni, generate Al fine and close continuously in hot environment
2o
3film, AlNi phase, Al
3nb is equal, thus delays the degeneration of coating, shows good high temperature oxidation resistance, and high temperature oxidation weight increment test shows, the high-temperature oxidation resistance of 1000 DEG C improves 30 ~ 71 times than base material.
4. can obtain the coating of heterogeneity and thickness by controlling deposition parameter, technique is simple and reproducible, can be used for the preparation of industrial big area.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 compound coating XRD figure spectrum
Fig. 2 is the embodiment of the present invention 1 compound coating surface topography
Fig. 3 is the embodiment of the present invention 1 compound coating Cross Section Morphology
Fig. 4 is that the embodiment of the present invention 1 compound coating is 1000 DEG C of oxidation 20h XRD figure spectrums
Fig. 5 is the Cross Section Morphology of the embodiment of the present invention 1 compound coating at 1000 DEG C of oxidation 20h
Fig. 6 is that the embodiment of the present invention 2 compound coating is 1000 DEG C of oxidation 20h XRD figure spectrums
Fig. 7 is the Cross Section Morphology of the embodiment of the present invention 2 compound coating at 1000 DEG C of oxidation 20h
Fig. 8 is base material of the present invention and embodiment 1, the sample of embodiment 2 compound coating is oxidized the oxidation weight gain curve of 20h at 1000 DEG C
Fig. 9 is the embodiment of the present invention 3 compound coating Cross Section Morphology
Sequence number in Fig. 3,5,7,8,9 is respectively:
1. compound coating; 2. transition layer; 3. base material; 4.Al
2o
3film;
(a) embodiment 2 sample (b) embodiment 1 sample (c) niobium alloy base material
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described, but do not limit the scope of the invention and range of application.
One, the preparation method of resistance to high temperature oxidation compound coating
Embodiment 1
A preparation method for resistance to high temperature oxidation compound coating, comprises following operation steps:
1. pre-treatment: (its constituent content is: Hf 10.0% by niobium alloy base material, Ti 1.30%, Zr 0.34%, W 0.31%, Ta 0.30%, C < 0.005%, N < 0.014%, O < 0.013%, surplus is Nb) priority each 10min of difference ultrasonic cleaning in acetone and dehydrated alcohol, dry up;
2. electroless plating pre-treatment: niobium alloy base material good for pre-treatment is first used degreaser, and (degreaser proportioning is: 25g/LNa
3pO
412H
2o, 30g/L Na
2cO
3, 10g/L Na
2siO
3) cleaning, (mixing acid proportioning is: water: sulfuric acid=1:1 (volume ratio) to use mixing acid again, wherein sulfuric acid concentration is 95 ~ 98%) wash, cleaned niobium alloy base material is carried out first time and soak zinc (zinc dipping solution proportioning is: 50g/L NaOH, 2g/L KNaC
4h
4o
6h
2o, 5g/L ZnO, 2g/L FeCl
36H
2o, 1g/L NaNO
3), move back zinc (dezincifying solution proportioning is: water: nitric acid=1:1 (volume ratio), and wherein concentration of nitric acid is 65 ~ 68%), then carry out second time and soak zinc (identical with first time zinc dipping solution), washing;
3. prepare Ni-P coating: prepare plating solution according to the following formulation: single nickel salt 35g/L, inferior sodium phosphate 25g/L, trisodium citrate 20g/L, ammonium chloride 25g/L, sodium acetate 25g/L, the pH value to 8.0 of plating solution is regulated with ammoniacal liquor, hang in plating solution by niobium alloy base material good for electroless plating pre-treatment, putting temperature is react 1.0 hours in the water-bath of 80 DEG C;
4. pack cementation aluminizing: prepare penetration enhancer as following weight percent: Al
2o
3powder 87%, Al powder 10%, NaF powder 3%, mixing grinding, puts in tube furnace by the penetration enhancer fully mixed and the niobium alloy base material that plated Ni-P coating, is evacuated to 2 × 10
-1pa, tube furnace temperature rise rate is 6 DEG C/min, is to be incubated 4 hours under the furnace temperature of 950 DEG C in temperature, and after being incubated, furnace cooling, to room temperature, obtains resistance to high temperature oxidation compound coating, and compound coating thickness is 120 μm.
Embodiment 2
A preparation method for resistance to high temperature oxidation compound coating, comprises following operation steps:
1. pre-treatment: (its constituent content is: Hf 10.0% by niobium alloy base material, Ti 1.30%, Zr 0.34%, W 0.31%, Ta 0.30%, C < 0.005%, N < 0.014%, O < 0.013%, surplus is Nb) priority each 10min of difference ultrasonic cleaning in acetone and dehydrated alcohol, dry up;
2. electroless plating pre-treatment: niobium alloy base material good for pre-treatment is first used degreaser, and (degreaser proportioning is: 25g/LNa
3pO
412H
2o, 30g/L Na
2cO
3, 10g/L Na
2siO
3) cleaning, (mixing acid proportioning is: water: sulfuric acid=1:1 (volume ratio) to use mixing acid again, wherein sulfuric acid concentration is 95 ~ 98%) wash, cleaned niobium alloy base material is carried out first time and soak zinc (zinc dipping solution proportioning is: 50g/L NaOH, 2g/L KNaC
4h
4o
6h
2o, 5g/L ZnO, 2g/L FeCl
36H
2o, 1g/L NaNO
3), move back zinc (dezincifying solution proportioning is: water: nitric acid=1:1 (volume ratio), and wherein concentration of nitric acid is 65 ~ 68%), then carry out second time and soak zinc (identical with first time zinc dipping solution), washing;
3. prepare Ni-P coating: prepare plating solution according to the following formulation: single nickel salt 25g/L, inferior sodium phosphate 15g/L, trisodium citrate 15g/L, ammonium chloride 10g/L, sodium acetate 15g/L, the pH value to 7.5 of plating solution is regulated with ammoniacal liquor, hang in plating solution by niobium alloy base material good for electroless plating pre-treatment, putting temperature is react 1.5 hours in the water-bath of 70 DEG C;
4. pack cementation aluminizing: prepare penetration enhancer as following weight percent: Al
2o
3powder 85%, Al powder 11%, NaF powder 4%, mixing grinding, puts in tube furnace by the penetration enhancer fully mixed and the niobium alloy base material that plated Ni-P coating, is evacuated to 3 × 10
-1pa, tube furnace temperature rise rate is 7 DEG C/min, is to be incubated 4 hours under the furnace temperature of 900 DEG C in temperature, and after being incubated, furnace cooling, to room temperature, obtains resistance to high temperature oxidation compound coating, and compound coating thickness is 95 μm.
Embodiment 3
A preparation method for resistance to high temperature oxidation compound coating, comprises following operation steps:
1. pre-treatment: by the niobium base material successively each 10min of difference ultrasonic cleaning in acetone and dehydrated alcohol, dry up;
2. electroless plating pre-treatment: niobium alloy base material good for pre-treatment is first used degreaser, and (degreaser proportioning is: 25g/LNa
3pO
412H
2o, 30g/L Na
2cO
3, 10g/L Na
2siO
3) cleaning, (mixing acid proportioning is: water: sulfuric acid=1:1 (volume ratio) to use mixing acid again, wherein sulfuric acid concentration is 95 ~ 98%) wash, cleaned niobium alloy base material is carried out first time and soak zinc (zinc dipping solution proportioning is: 50g/L NaOH, 2g/L KNaC
4h
4o
6h
2o, 5g/L ZnO, 2g/L FeCl
36H
2o, 1g/L NaNO
3), move back zinc (dezincifying solution proportioning is: water: nitric acid=1:1 (volume ratio), and wherein concentration of nitric acid is 65 ~ 68%), then carry out second time and soak zinc (identical with first time zinc dipping solution), washing;
3. prepare Ni-P coating: prepare plating solution according to the following formulation: single nickel salt 20g/L, inferior sodium phosphate 20g/L, trisodium citrate 18g/L, ammonium chloride 18g/L, sodium acetate 18g/L, the pH value to 9.0 of plating solution is regulated with ammoniacal liquor, hang in plating solution by niobium base material good for electroless plating pre-treatment, putting temperature is react 0.5 hour in the water-bath of 85 DEG C;
4. pack cementation aluminizing: prepare penetration enhancer as following weight percent: Al
2o
3powder 89%, Al powder 9%, NaF powder 2%, mixing grinding, puts in tube furnace by the penetration enhancer fully mixed and the niobium base material that plated Ni-P coating, is evacuated to 3 × 10
-1pa, tube furnace temperature rise rate is 7 DEG C/min, is to be incubated 3 hours under the furnace temperature of 850 DEG C in temperature, and after being incubated, furnace cooling, to room temperature, obtains resistance to high temperature oxidation compound coating, and compound coating thickness is 50 μm.
Two, the structural characterization of resistance to high temperature oxidation compound coating
The resistance to high temperature oxidation compound coating obtained by embodiment, 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 refers to Fig. 1-Fig. 9.
1. embodiment 1 measurement result situation.
Fig. 1 shows: compound coating, primarily of AlNi phase composite, illustrates that Al skin, with Ni-P internal layer, obvious diffusion reaction occurs in aluminising process, thus generates AlNi phase.
Fig. 2 shows: compound coating surface is in cotton-shaped weave construction, and containing micropore, cracking and obscission, be not combined well with base material.
Fig. 3 shows: generate transition layer between compound coating and base material, and combines fine and close between coating; Due to be first carry out plating Ni-P after carry out aluminising, therefore aluminium lamination and Ni-P layer there occurs diffusion, interpenetrate phenomenon between coating.
Fig. 4 shows: after 1000 DEG C of oxidation 20h, compound coating mainly generates Al
2o
3phase, AlNi phase.
Fig. 5 shows: after 1000 DEG C of oxidation 20h, continuous, the fine and close Al of the Surface Creation of compound coating
2o
3film; Al
2o
3the interbed of film, compound coating, base material is combined with layer well, without obscission.
Fig. 8 shows: the weightening finish after 1000 DEG C of oxidation 20h of niobium alloy base material is 254.0653mg/cm
2, after first plating through 950 DEG C the embodiment 1 sample oxidation 20h oozed afterwards, weightening finish is 7.7143mg/cm
2, illustrating that the sample high temperature oxidation resistance containing compound coating is good, improve 32 ~ 71 times through calculating than niobium alloy base material.
2. embodiment 2 measurement result situation.
Fig. 6 shows: after 1000 DEG C of oxidation 20h, compound coating mainly generates Al
2o
3phase, AlNi phase, Al
3nb phase.
Fig. 7 shows: after 1000 DEG C of oxidation 20h, continuous, the fine and close Al of the Surface Creation of compound coating
2o
3film; Al
2o
3the interbed of film, compound coating, base material is combined with layer well, without obscission.
Fig. 8 shows: the weightening finish after 1000 DEG C of oxidation 20h of niobium alloy base material is 254.0653mg/cm
2, 850 DEG C are first plated weightening finish after the embodiment 2 sample oxidation 20h oozed afterwards is 8.0124mg/cm
2, illustrating that the sample high temperature oxidation resistance containing compound coating is good, improve 30 ~ 70 times through calculating than niobium alloy base material.
3. embodiment 3 measurement result situation.
Fig. 9 shows: compound coating growth is smooth, and combines densification between matrix; Due to be first carry out plating Ni-P after carry out aluminising, therefore aluminium lamination and Ni-P layer there occurs diffusion, interpenetrate phenomenon between coating.But holding temperature is lower, soaking time is shorter, therefore does not occur transition layer.
Claims (3)
1. a resistance to high temperature oxidation compound coating, is characterized in that: first by electroless plating technology, at deposited on substrates Ni-P coating; Again by pack cementation aluminizing technology, infiltrate aluminium at Ni-P coating, form resistance to high temperature oxidation compound coating;
The electroplate liquid formulation of described electroless plating technology 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;
The penetration enhancer compositions in weight percentage of described pack cementation aluminizing technology is: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%.
2. resistance to high temperature oxidation compound coating according to claim 1, is characterized in that: described base material is niobium or niobium alloy.
3. a preparation method for resistance to high temperature oxidation compound coating as claimed in claim 1 or 2, comprises pre-treatment, electroless plating pre-treatment, preparation Ni-P coating, pack cementation aluminizing step, it is characterized in that:
Described preparation Ni-P plating steps is: prepare plating solution according to the following formulation: 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, pH value to 7.5 ~ 9.0 of plating solution are regulated with ammoniacal liquor, hang in plating solution by the base material that pre-treatment is good, putting temperature is react 0.5 ~ 1.5 hour in the water-bath of 70 ~ 85 DEG C;
Described pack cementation aluminizing step is: prepare penetration enhancer as following weight percent: Al
2o
3powder 85 ~ 89%, Al powder 9 ~ 11%, NaF powder 2 ~ 4%, mixing grinding, puts in tube furnace by the penetration enhancer fully mixed and the base material that plated Ni-P coating, is evacuated to 2 × 10
-1~ 3 × 10
-1pa, tube furnace temperature rise rate is 6 ~ 7 DEG C/min, is to be incubated 3 ~ 4 hours under the furnace temperature of 850 ~ 950 DEG C in temperature, and after being incubated, furnace cooling, to room temperature, obtains resistance to high temperature oxidation compound coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177536A (en) * | 2015-09-15 | 2015-12-23 | 广西大学 | Method for preparing micrometer-particle-contained high-temperature-oxidation-resistant composite coating on surface of niobium alloy |
| CN109404077A (en) * | 2018-09-30 | 2019-03-01 | 东方电气集团东方汽轮机有限公司 | A kind of mixed working fluid processing method using steam turbine |
| CN114686872A (en) * | 2022-03-25 | 2022-07-01 | 长沙理工大学 | Strong corrosion-resistant Ta alloy coating and preparation method thereof |
-
2015
- 2015-01-05 CN CN201510002563.9A patent/CN104561952A/en active Pending
Non-Patent Citations (2)
| Title |
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| 樊国福等: "钛合金和钛合金化学镀镍层渗铝的研究", 《材料保护》 * |
| 田晓东等: "铌基超高温合金包埋渗铝改性硅化物涂层结构", 《材料热处理学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177536A (en) * | 2015-09-15 | 2015-12-23 | 广西大学 | Method for preparing micrometer-particle-contained high-temperature-oxidation-resistant composite coating on surface of niobium alloy |
| CN109404077A (en) * | 2018-09-30 | 2019-03-01 | 东方电气集团东方汽轮机有限公司 | A kind of mixed working fluid processing method using steam turbine |
| CN114686872A (en) * | 2022-03-25 | 2022-07-01 | 长沙理工大学 | Strong corrosion-resistant Ta alloy coating and preparation method thereof |
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