CN106544627A - A kind of thermophilic corrosion-resistance composite coating and preparation method thereof - Google Patents
A kind of thermophilic corrosion-resistance composite coating and preparation method thereof Download PDFInfo
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- CN106544627A CN106544627A CN201610960581.2A CN201610960581A CN106544627A CN 106544627 A CN106544627 A CN 106544627A CN 201610960581 A CN201610960581 A CN 201610960581A CN 106544627 A CN106544627 A CN 106544627A
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/48—Aluminising
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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Abstract
The invention discloses a kind of thermophilic corrosion-resistance composite coating and preparation method thereof, first passes through pack cementation aluminizing process and NbAl is prepared on base material3Aluminized coating, then by differential arc oxidation process in the NbAl3Aluminized coating plates last layer Al2O3Ceramic membrane, is obtained Al2O3 / NbAl3Composite coating；The aluminizing medium that the pack cementation aluminizing is processed is by weight percentage：Al2O384～90wt% of powder, Al 8～12wt% of powder, NaF 2～4wt% of powder；The electrolyte prescription that the differential arc oxidation is processed is：15～25g/L of sodium metaaluminate, 2～6g/L of sodium hydroxide, 2～6g/L of sodium fluoride.Al prepared by the present invention2O3 / NbAl3Composite coating, is combined with base material, coating continuous uniform, shows good thermophilic corrosion-resistance performance；And process is simple and reproducible, can large area prepare.
Description
Technical field
The invention belongs to high-temperature protection coating technical field, is related to a kind of thermophilic corrosion-resistance composite coating and its preparation side
Method.
Background technology
High-temperature protection coating is mainly used in the gas turbine hot-end component of Aero-Space and modern energy industrial circle.Gold
Category niobium（Nb）Fusing point is high（2468℃）, medium density（8.6g/cm3）, high temperature specific strength it is big, with excellent mechanical behavior under high temperature
And processing characteristics, niobium alloy is one of important candidate material of high-temperature structural material.But the non-oxidizability of niobium alloy is poor, simple metal
There is " pest " oxidation at 600 DEG C in Nb, strongly limit the application of niobium alloy.For problem above, carry out both at home and abroad big
The research of amount niobium alloy surface protection coating.At present, the research with regard to niobium alloy protection is concentrated mainly on high temperature oxidation resistance,
And thermophilic corrosion-resistance is mainly for alloys such as Ni, TiAl, and the thermophilic corrosion-resistance to niobium alloy surface protection coating
Can be rarely reported.
The content of the invention
It is an object of the invention to provide a kind of compound with thermophilic corrosion-resistance used in high temperature corrosion medium
Coating and preparation method thereof.
The technical scheme is that：A kind of thermophilic corrosion-resistance composite coating, first passes through pack cementation aluminizing and processes in base material
Upper preparation NbAl3Aluminized coating, then by differential arc oxidation process in the NbAl3Aluminized coating plates last layer Al2O3Ceramic membrane, is obtained
Al2O3 / NbAl3Composite coating.The aluminizing medium that the pack cementation aluminizing is processed is by weight percentage：Al2O384～90wt% of powder,
Al 8～12wt% of powder, NaF 2～4wt% of powder；The electrolyte prescription that the differential arc oxidation is processed is：15～25g/L of sodium metaaluminate, hydrogen
2～6g/L of sodium oxide, 2～6g/L of sodium fluoride.
The base material is niobium or niobium alloy.
A kind of preparation method of thermophilic corrosion-resistance composite coating, comprises the following steps：
（1）Pretreatment：It is cleaned by ultrasonic 10min with acetone after base material is polished step by step, dries up；
（2）Pack cementation aluminizing process：Aluminizing medium is prepared as following weight percent first：Al2O384～90wt% of powder, Al powder 8～
12wt%, NaF 2～4wt% of powder, is then mixed using ball mill, then the abundant aluminizing medium for mixing and base material are sealed in pottery together
In porcelain crucible, finally room temperature is cooled in tube furnace, is obtained after evacuation, heating and insulation in placement vacuum tube furnace
NbAl3The aluminising base material of aluminized coating；
（3）Differential arc oxidation process：From dipulse high voltage power supply as pressure source, aluminising base material is hung on into anode, with stainless
Used as negative electrode, aluminising base material is immersed in electrolyte to steel tank, electrolyte by 15～25g/L of sodium metaaluminate, 2～6g/L of sodium hydroxide and
2～6g/L of sodium fluoride is constituted；Differential arc oxidation process is carried out using constant voltage mode, electrical quantity is adjusted, and is applied mechanical agitation, make molten
Liquid temp be less than 40 DEG C, process time be 10～75min after aluminising base material plate last layer Al2O3Ceramic membrane, is obtained Al2O3
/ NbAl3Composite coating.
The step（2）Arrange parameter in vacuum tube furnace：Vacuum is 0.15 × 10-2～3 × 10-2Pa, 8～12 DEG C/
The heating rate of min rises to 900～1000 DEG C, and is incubated 2～6h.The step（3）Electrical quantity is：350～410V of positive voltage,
Positive dutycycle 10～30%, 200～600Hz of frequency.
The NbAl3The thickness of aluminized coating is 40～85 μm, the Al2O3The thickness of ceramic membrane is 8～12 μm.
Beneficial effects of the present invention：
1. the present invention adopts composite coating prepared by pack cementation aluminizing and differential arc oxidization technique, using scanning electron microscope（SEM）Observation：Table
Face forms the ceramic membrane of loose structure, and micropore distribution is relatively regular, and between coating, coating and base material be well combined.
2. the composite coating is, in niobium or the aluminising of niobium alloy base material elder generation, then to prepare ceramic film, be that a kind of NEW TYPE OF COMPOSITE is applied
Layer preparation method.
3. the composite coating can effectively extend the service life of niobium or niobium alloy under High Temperature Hot-corrosion Behaviorof.Coating mainly by
NbAl3And Al2O3Composition, generates cubic structure NaNbO under High Temperature Hot-corrosion Behaviorof3, part NaNbO3It is deposited in micropore, hinders
Fused salt shows good corrosion and heat resistant to internal diffusion.
4. the painting of different-thickness can be obtained by control pack cementation aluminizing time, temperature and micro-arc oxidation electrolyte, electrical quantity
Layer, process is simple, controllability are strong.
Description of the drawings
Fig. 1 is 1 Al of the embodiment of the present invention2O3 / NbAl3The XRD spectrum of composite coating.
Fig. 2 is 1 Al of the embodiment of the present invention2O3 / NbAl3The surface topography of composite coating.
Fig. 3 is 1 Al of the embodiment of the present invention2O3 / NbAl3The Cross Section Morphology of composite coating.
Fig. 4 is 1 Al of the embodiment of the present invention2O3 / NbAl3XRD spectrum of the composite coating in 900 DEG C of heat erosion 50h.
Fig. 5 is 1 Al of the embodiment of the present invention2O3 / NbAl3Surface topography of the composite coating in 900 DEG C of heat erosion 50h.
Fig. 6 is 2 Al of the embodiment of the present invention2O3 / NbAl3The Cross Section Morphology of composite coating.
Fig. 7 is 2 Al of the embodiment of the present invention2O3 / NbAl3XRD spectrum of the composite coating in 900 DEG C of heat erosion 50h.
Als of the Fig. 8 for Example 1 and Example 2 of the present invention2O3 / NbAl3Composite coating is with niobium alloy base material at 900 DEG C
The surrosion curve of heat erosion 50h.
Sequence number in Fig. 3 and Fig. 6 is respectively：A. Al2O3Ceramic membrane；B. NbAl3Aluminized coating；C. niobium alloy base material.
Specific embodiment
With reference to specific embodiment and accompanying drawing, the invention will be further described, but does not limit the scope of the invention
And range of application.
First, the preparation method of thermophilic corrosion-resistance composite coating
Embodiment 1
A kind of preparation method of niobium alloy surface thermophilic corrosion-resistance composite coating, including following operating procedure：
1. pretreatment：Base material selects niobium alloy C103, and its chemical composition is：Hf 10.0, Ti 1.30, Zr 0.34, W 0.34,
Ta 0.30, C 0.005, N 0.014, O 0.013, Nb surplus（wt.%）, it is cleaned by ultrasonic 10min with acetone after polishing step by step, blows
It is dry；
2. pack cementation aluminizing is processed：Aluminizing medium is prepared as following weight percent first：Al2O3Powder 87wt%, Al powder 10wt%, NaF
Powder 3wt%, is then mixed using ball mill, then the abundant aluminizing medium for mixing and base material are sealed in ceramic crucible together, finally
Place in vacuum tube furnace, be evacuated to 0.15 × 10-2Pa, rises to 940 DEG C with the heating rate of 10 DEG C/min, and it is little to be incubated 4
When, subsequent stove is cooled to room temperature, obtains NbAl3The aluminising niobium alloy base material of aluminized coating；
3. differential arc oxidation is processed：From dipulse high voltage power supply as pressure source, aluminising niobium alloy base material is hung on into anode, with
Used as negative electrode, aluminising niobium alloy is immersed in electrolyte to stainless steel tank, electrolyte by sodium metaaluminate 20g/L, sodium hydroxide 4g/L and
Sodium fluoride 4g/L is constituted；Differential arc oxidation process is carried out using constant voltage mode, and applies mechanical agitation, 25 DEG C of solution temperature is processed
Time 30min；And press following parameter regulation electrical quantity：Positive voltage 380V, positive dutycycle 10%, frequency 500Hz, at differential arc oxidation
Reason obtains Al2O3 / NbAl3Composite coating, composite coating thickness are 82 μm.
Embodiment 2
1. pretreatment：Base material selects niobium alloy C103, and its chemical composition is：Hf 10.0, Ti 1.30, Zr 0.34, W 0.34,
Ta 0.30, C 0.005, N 0.014, O 0.013, Nb surplus（wt.%）, it is cleaned by ultrasonic 10min with acetone after polishing step by step, blows
It is dry；
2. pack cementation aluminizing is processed：Aluminizing medium is prepared as following weight percent first：Al2O3Powder 84wt%, Al powder 12wt%, NaF
Powder 4wt%, is then mixed using ball mill, then the abundant aluminizing medium for mixing and base material are sealed in ceramic crucible together, finally
Place in vacuum tube furnace, be evacuated to 0.75 × 10-2Pa, rises to 900 DEG C with the heating rate of 10 DEG C/min, and it is little to be incubated 4
When, subsequent stove is cooled to room temperature, obtains NbAl3The aluminising niobium alloy base material of aluminized coating；
3. differential arc oxidation is processed：From dipulse high voltage power supply as pressure source, aluminising niobium alloy base material is hung on into anode,
Using stainless steel tank as negative electrode, aluminising niobium alloy is immersed in electrolyte, electrolyte by sodium metaaluminate 15g/L, sodium hydroxide 2g/L,
Sodium fluoride 2g/L is constituted；Differential arc oxidation process is carried out using constant voltage mode, and applies mechanical agitation, 30 DEG C of solution temperature is processed
Time 30min；And press following parameter regulation electrical quantity：Positive voltage 350V, positive dutycycle 20%, frequency 200Hz, at differential arc oxidation
Reason obtains Al2O3 / NbAl3Composite coating, composite coating thickness are 51 μm.
Embodiment 3
1. pretreatment：Base material selects niobium alloy C103, and its chemical composition is：Hf 10.0, Ti 1.30, Zr 0.34, W 0.34,
Ta 0.30, C 0.005, N 0.014, O 0.013, Nb surplus（wt.%）, it is cleaned by ultrasonic 10min with acetone after polishing step by step, blows
It is dry；
2. pack cementation aluminizing is processed：Aluminizing medium is prepared as following weight percent first：Al2O3Powder 90wt%, Al powder 8wt%, NaF
Powder 2wt%, is then mixed using ball mill, then the abundant aluminizing medium for mixing and base material are sealed in ceramic crucible together, finally
Place in vacuum tube furnace, be evacuated to 3 × 10-2Pa, is incubated 3 under the furnace temperature that 940 DEG C are risen to the heating rate of 10 DEG C/min
Hour, subsequent stove is cooled to room temperature, obtains NbAl3The aluminising niobium alloy base material of aluminized coating；
3. differential arc oxidation is processed：From dipulse high voltage power supply as pressure source, aluminising niobium alloy base material is hung on into anode,
Using stainless steel tank as negative electrode, aluminising niobium alloy is immersed in electrolyte, electrolyte by sodium metaaluminate 25g/L, sodium hydroxide 6g/L,
Sodium fluoride 6g/L is constituted；Differential arc oxidation process is carried out using constant voltage mode, and applies mechanical agitation, 32 DEG C of solution temperature is processed
Time 30min；And press following parameter regulation electrical quantity：Positive voltage 410V, positive dutycycle 30%, frequency 600Hz, at differential arc oxidation
Reason obtains thermophilic corrosion-resistance composite coating, and composite coating thickness is 75 μm.
2nd, the structural characterization of thermophilic corrosion-resistance composite coating
By embodiment 1 and Al obtained in embodiment 22O3 / NbAl3Composite coating, is utilized respectively the thing that XRD diffraction detects coating
Phase structure, using scanning electron microscope（SEM）The surface of observation coating and Cross Section Morphology, before observation coating cross sections, in advance with chemistry
It is plated in coating surface and prepares Ni-P layers, shields.Measurement result refers to Fig. 1～Fig. 8.
1. 1 measurement result situation of embodiment.
As shown in Figure 1：Al2O3 / NbAl3Composite coating is mainly by NbAl3And Al2O3Phase composition, during illustrating aluminising
NbAl formed and diffusion reaction with the Al powder of outer layer in niobium alloy base material there is3Phase, and differential arc oxidation is in NbAl3Generate on aluminized coating
Al2O3Ceramic membrane.
As shown in Figure 2：Al2O3 / NbAl3In loose structure, micropore is distributed relatively regular, pore size on composite coating surface
It is more or less the same.
As shown in Figure 3：Al2O3Ceramic membrane and NbAl3Aluminized coating, NbAl3Aluminized coating and niobium alloy base material are well combined；
NbAl3Aluminized coating even compact, Al2O3Ceramic membrane is in cellular.
As shown in Figure 4：The 75wt%Na that 900 DEG C of Jing2SO4After 25wt%NaCl mixed melting salt hot corrosion 50h, Al2O3
/ NbAl3Composite coating is mainly by NaNbO3、Al2O3With Nb phase compositions.
As shown in Figure 5：The 75wt%Na that 900 DEG C of Jing2SO4After 25wt%NaCl mixed melting salt hot corrosion 50h, Al2O3 /
NbAl3There is the NaNbO of cubic structure in composite coating surface3, mainly in Al2O3Ceramic membrane micropore is formed about, and part
NaNbO3It is deposited in micropore, hinders fused salt to internal diffusion, show good corrosion and heat resistant..
As shown in Figure 8：The Al of embodiment 12O3 / NbAl3The 75wt%Na that 900 DEG C of composite coating Jing2SO4And 25wt%
Gain in weight after NaCl mixed melting salt hot corrosion 50h is 55.71mg/cm2；And the weightening after niobium alloy base material heat erosion 50h
Measure as 252.09mg/cm2, illustrate Al2O3 / NbAl3The hot corruption of high temperature resistance of composite coating is good, improves 4～5 times through calculating.
2. 2 measurement result situation of embodiment.
As shown in Figure 6：Al2O3 / NbAl3NbAl in composite coating3Aluminized coating and Al2O3Ceramic membrane, niobium alloy base material
It is well combined, continuous uniform.
As shown in Figure 7：The 75wt%Na that 900 DEG C of Jing2SO4After 25wt%NaCl mixed melting salt hot corrosion 50h, Al2O3 /
NbAl3Composite coating is mainly by NaNbO3、Al2O3With Nb phase compositions.
As shown in Figure 8：The Al of embodiment 22O3 / NbAl3The 75wt%Na that 900 DEG C of composite coating Jing2SO4And 25wt%NaCl
Gain in weight after mixed melting salt hot corrosion 50h is 60.15mg/cm2；And the gain in weight after niobium alloy base material heat erosion 50h is
252.09mg/cm2, illustrate Al2O3 / NbAl3The hot corruption of high temperature resistance of composite coating is good, improves 4～5 times through calculating.
Claims (7)
1. a kind of thermophilic corrosion-resistance composite coating, it is characterised in that：First pass through pack cementation aluminizing process and NbAl is prepared on base material3
Aluminized coating, then by differential arc oxidation process in the NbAl3Aluminized coating plates last layer Al2O3Ceramic membrane, is obtained Al2O3 / NbAl3
Composite coating；The aluminizing medium that the pack cementation aluminizing is processed is by weight percentage：Al2O384～90wt% of powder, Al 8～12wt% of powder,
NaF 2～4wt% of powder；The electrolyte prescription that the differential arc oxidation is processed is：15～25g/L of sodium metaaluminate, 2～6g/ of sodium hydroxide
L, 2～6g/L of sodium fluoride.
2. thermophilic corrosion-resistance composite coating according to claim 1, it is characterised in that：The base material is that niobium or niobium are closed
Gold.
3. a kind of preparation method of thermophilic corrosion-resistance composite coating as claimed in claim 1 or 2, it is characterised in that include
Following steps：
（1）Pretreatment：It is cleaned by ultrasonic 10min with acetone after base material is polished step by step, dries up；
（2）Pack cementation aluminizing process：Aluminizing medium is prepared as following weight percent first：Al2O384～90wt% of powder, Al powder 8～
12wt%, NaF 2～4wt% of powder, is then mixed using ball mill, then the abundant aluminizing medium for mixing and base material are sealed in pottery together
In porcelain crucible, finally room temperature is cooled in tube furnace, is obtained after evacuation, heating and insulation in placement vacuum tube furnace
NbAl3The aluminising base material of aluminized coating；
（3）Differential arc oxidation process：From dipulse high voltage power supply as pressure source, aluminising base material is hung on into anode, with stainless
Used as negative electrode, aluminising base material is immersed in electrolyte to steel tank, electrolyte by 15～25g/L of sodium metaaluminate, 2～6g/L of sodium hydroxide and
2～6g/L of sodium fluoride is constituted；Differential arc oxidation process is carried out using constant voltage mode, electrical quantity is adjusted, and is applied mechanical agitation, make molten
Liquid temp be less than 40 DEG C, process time be 10～75min after aluminising base material plate last layer Al2O3Ceramic membrane, is obtained Al2O3
/ NbAl3Composite coating.
4. the preparation method of thermophilic corrosion-resistance composite coating according to claim 3, it is characterised in that：The step
（2）Arrange parameter in vacuum tube furnace：Vacuum is 0.15 × 10-2～3 × 10-2The heating rate liter of Pa, 8～12 DEG C/min
To 900～1000 DEG C, and it is incubated 2～6h.
5. the preparation method of thermophilic corrosion-resistance composite coating according to claim 3, it is characterised in that：The step
（3）Electrical quantity is：350～410V of positive voltage, positive dutycycle 10～30%, 200～600Hz of frequency.
6. the preparation method of thermophilic corrosion-resistance composite coating according to claim 3, it is characterised in that：The NbAl3Ooze
The thickness of aluminium lamination is 40～85 μm.
7. the preparation method of thermophilic corrosion-resistance composite coating according to claim 3, it is characterised in that：The Al2O3Pottery
The thickness of porcelain film is 8～12 μm.
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| CN108642439A (en) * | 2018-06-05 | 2018-10-12 | 合肥工业大学 | A method of preparing high-strength coating in tungsten alitizing |
| CN110195206A (en) * | 2019-07-16 | 2019-09-03 | 广西大学 | A kind of preparation method of niobium alloy high-temperature corrosion resistance containing scandium oxide coating |
| CN115558886A (en) * | 2022-09-13 | 2023-01-03 | 首钢集团有限公司 | Corrosion-resistant high-carbon steel protective film layer and preparation method thereof |
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| CN110195206A (en) * | 2019-07-16 | 2019-09-03 | 广西大学 | A kind of preparation method of niobium alloy high-temperature corrosion resistance containing scandium oxide coating |
| CN115558886A (en) * | 2022-09-13 | 2023-01-03 | 首钢集团有限公司 | Corrosion-resistant high-carbon steel protective film layer and preparation method thereof |
| CN115558886B (en) * | 2022-09-13 | 2024-06-11 | 首钢集团有限公司 | Corrosion-resistant high-carbon steel protective film and preparation method thereof |
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