CN104694917B - A kind of preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer - Google Patents
A kind of preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer, comprise the following steps：1) Ni (0) solid-solution powder is taken, then sieve takes Ni (0) solid-solution powders that particle diameter is less than 50 μm as cold spraying powder；2) blasting treatment is carried out after carrying out oil removing and cleaning to pending stainless steel base containing Cr；3) using cold spray technique by step 1) obtained cold spraying powder spray is to through step 2) surface of stainless steel base containing Cr of processing, in Cr stainless steel bases surface deposition Ni (0) solid solution layer；4) in step 3) anti-corrosion Ni layers of the surface deposition of obtained Ni (0) solid solution layer；5) Cr stainless steel bases are placed into the container of inert gas shielding, be heat-treated, Cr stainless steel base superficial growths is gone out Cr2O3Diffusion barrier, is then incubated again, obtains the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer.The present invention can prepare continuous fine and close and good with the binding ability of stainless steel base containing Cr anti-corrosion Ni layers.
Description
Technical field
The invention belongs to surface alloying and coating technology field, it is related to a kind of oxide diffusion barrier of stainless steel surfaces containing Cr
And the preparation method of anticorrosion layer.
Background technology
Fusedsalt reactor (Molten Salt Reactor-MSR) is as forth generation nuclear reactor, because of its high neutron
Economy, high power density, inherently load big controllable, negative temperature coefficient, high transformation ratio, high reliability, fuel fabrication expend it is low,
Can proliferative the advantages of, obtain domestic and international extensive concern.But, fuel and the molten fluoride used in cooling agent have in MSR
Extremely strong corrosivity, most of protective oxide film such as Al being stabilized in high-temperature oxidation environment2O3、Cr2O3And SiO2Deng
Will occur active dissolution, so as to cause the failure of hot-end component (mainly stainless steel) material.Chemistry of the Ni in fused salt is steady
It is qualitative higher, it is suitable as the protective coating of MSR environmental structure materials.But, when Ni coatings coordinate matrix alloy long service
When, Ni coatings can not stop the external diffusion of active element in matrix, so as to lose effective protection to matrix.
In view of counterdiffusion is to influence the key factor of anti-corrosion Ni coatings service life, it is necessary to draw between coating and matrix
Enter diffusion impervious layer.The design of " diffusion barrier/metal anticorrosion layer " composite coating system has studied application in high temperature coating field,
For example, the composite coating that nitride diffusion barrier is constituted with Metal Substrate anticorrosion layer is rotten in the high temperature for solving gas turbine high-temperature component
Erosion, abrasion and the problems such as coating degradation caused by element counterdiffusion aspect have broad application prospects；Al2O3、Cr2O3Deng
Oxide diffusion barrier can effectively suppress the element counterdiffusion between MCrAlY coatings and high temperature alloy.The pungent university of University of Wisconsin-Madison
Kinetics of diffusion test result indicates that, due to diffusion coefficient of the alloying element in oxide ceramics much smaller than its in W metal
Numerical value, so as to play significant resistance diffusion effect.
The preparation technology of current oxide ceramics diffusion barrier mainly includes the physical vapors such as magnetron sputtering, multi-arc ion coating and sunk
Product method (PVD) and pre-oxidation heat growth method.Wherein PVD requires equipment vacuum, with high costs, the diffusion impervious layer of preparation with
It is physical bond between matrix, often has that adhesion is poor, caducous problem because thermal coefficient of expansion is mismatched, it is serious to threaten fused salt anti-
Answer the safe operation of heap.Compared with PVD, equipment needed for pre-oxidation heat growth method is simple, cheap；Oxide coating and base
Chemical bond between body can significantly improve oxide and matrix adhesiveness；Can be by controlling reaction condition to enter oxide coating
Row composition thickness regulates and controls.However, preparing diffusion barrier by above-mentioned conventional coating techniques can bring necessarily to anti-corrosion Ni layers preparation
Influence, e.g., oxide diffusion barrier it is non-conductive will to electroplating technology prepare Ni layer have a negative impact, and use spray
Technique prepares Ni layers and easily causes the rupture of diffusion barrier stress again, further influences it to hinder diffusion.In addition, using coating technology
Successively prepare oxide and Ni interlayers be physical bond, under arms during easily because thermophysical property difference ftractures.
It can be seen that, how to obtain continuous fine and close and matrix alloy and the good diffusion barrier of anti-corrosion Ni layers of binding ability is research and development fused salt reaction
The key of heap coating technology.
The content of the invention
It is an object of the invention to the shortcoming for overcoming above-mentioned prior art, there is provided a kind of oxide of stainless steel surfaces containing Cr
The preparation method of diffusion barrier and anticorrosion layer, the preparation method can prepare it is continuous fine and close and with the associativity of stainless steel base containing Cr
Can be good anti-corrosion Ni layers.
To reach above-mentioned purpose, the preparation side of the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer of the present invention
Method comprises the following steps：
1) Ni (O) solid-solution powder is taken, then sieve takes Ni (O) solid-solution powders that particle diameter is less than 50 μm as cold spraying powder
End；
2) blasting treatment is carried out after carrying out oil removing and cleaning to pending stainless steel base containing Cr；
3) using cold spray technique by step 1) obtained cold spraying powder spray is to through step 2) processing to contain Cr stainless
Steel matrix surface, Ni (O) solid solution layer is deposited on Cr stainless steel bases surface；
4) in step 3) anti-corrosion Ni layers of the surface deposition of obtained Ni (O) solid solution layer；
5) by step 4) the obtained deposition container that there are anti-corrosion Ni layers Cr stainless steel bases to be placed into inert gas shielding
It is interior, it is being heat-treated, Cr stainless steel base superficial growths is gone out Cr2O3Diffusion barrier, is then incubated again, obtains stainless containing Cr
Steel surface oxide diffusion barrier and anticorrosion layer.
Step 3) in Ni (O) solid solution layer thickness be 10-100 microns.
Step 4) in anti-corrosion Ni layers thickness be 90-400 microns.
Step 5) in inert gas be argon gas；
Step 5) in container be quartz ampoule or vacuum drying oven.
Step 5) in be heat-treated during temperature be 700-1000 DEG C, soaking time is 4-20h.
Cr content is more than or equal to 18wt.% during stainless steel containing Cr is basic.
The invention has the advantages that：
The preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer of the present invention in concrete operations,
Ni (O) solid solution layer first is deposited in the basic surface of stainless steel containing Cr, then in anti-corrosion Ni layers of the surface deposition of Ni (O) solid solution layer,
Then Cr is gone out in Cr stainless steel base superficial growths2O3Diffusion barrier, forms Cr2O3Diffusion barrier/anti-corrosion Ni Rotating fields, so as to obtain
Continuous fine and close and good with the binding ability of stainless steel base containing Cr anti-corrosion Ni layers, preparation method is simple.
Further, the temperature during heat treatment is 700-1000 DEG C, and soaking time is 4-20h, and low gibbs is free
The Cr of energy2O3Can be in stainless steel base containing Cr/coating interface preferred growth.
Brief description of the drawings
Fig. 1 (a) is the surface topography of original Ni powder；
Fig. 1 (b) is the surface topography of Ni (O) powder after ball-milling treatment；
Fig. 2 (a) is the composite coating Cross Section Morphology after cold spraying Ni (O) layers and the anti-corrosion outer layers of Ni；
Fig. 2 (b) is the enlarged drawing at A in Fig. 2 (a)；
Fig. 3 is Cr at 310ss matrixes/coating interface2O3The pattern of diffusion barrier；
Fig. 4 (a) is Cr2O3The shape appearance figure of diffusion barrier；
Fig. 4 (b) Cr2O3The power spectrum Cr element distribution plots of diffusion barrier；
Fig. 4 (c) Cr2O3The power spectrum Fe element distribution plots of diffusion barrier；
Fig. 4 (d) Cr2O3The power spectrum Ni element distribution plots of diffusion barrier；
Fig. 4 (e) Cr2O3The power spectrum O element distribution plots of diffusion barrier；
Fig. 5 (a) is the shape appearance figure of 316ss matrixes；
Fig. 5 (b) is Cr at coating interface2O3The shape appearance figure of diffusion barrier.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings：
The preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer of the present invention comprises the following steps：
1) Ni (O) solid-solution powder is taken, then sieve takes Ni (O) solid-solution powders that particle diameter is less than 50 μm as cold spraying powder
End；
2) blasting treatment is carried out after carrying out oil removing and cleaning to pending stainless steel base containing Cr；
3) using cold spray technique by step 1) obtained cold spraying powder spray is to through step 2) processing to contain Cr stainless
Steel matrix surface, Ni (O) solid solution layer is deposited on Cr stainless steel bases surface；
4) in step 3) anti-corrosion Ni layers of the surface deposition of obtained Ni (O) solid solution layer；
5) by step 4) the obtained deposition container that there are anti-corrosion Ni layers Cr stainless steel bases to be placed into inert gas shielding
It is interior, it is being heat-treated, Cr stainless steel base superficial growths is gone out Cr2O3Diffusion barrier, is then incubated again, obtains stainless containing Cr
Steel surface oxide diffusion barrier and anticorrosion layer.
Step 3) in Ni (O) solid solution layer thickness be 10-100 microns.
Step 4) in anti-corrosion Ni layers thickness be 90-400 microns.
Step 5) in inert gas be argon gas；
Step 5) in container be quartz ampoule or vacuum drying oven.
Step 5) in be heat-treated during temperature be 700-1000 DEG C, soaking time is 4-20h.
Cr content is more than or equal to 18wt.% during stainless steel containing Cr is basic.
Embodiment 1
Using Cr contents be about 25wt.% 310 stainless steels as base material (composition is shown in Table 1), material is pre-processed：Acetone
Dried up after ultrasonic oil removing, washes of absolute alcohol；
Table 1
The preparation of Ni (O) solid-solution powder uses Mechanical Alloying, and granularity is placed in for 63-75 μm of globular nickel powder
In stainless steel jar mill, ratio of grinding media to material is 10: 1, stainless steel ball big (12mm), in (10mm), the quantitative proportion of small (6mm) ball be about
Powder diameter is about 30 μm after 1: 10: 3, rotating speed 150r/min, mechanical alloying 8h, is determined through apparatus for determination of oxygen (RO-316, LECO),
When being 8h between when treated, the oxygen content of Ni (O) powder is 3.2wt.%, with reference to Fig. 1 (a) and Fig. 1 (b)；
310SS base materials, through blasting treatment, to remove surface contaminant, improve coating and combined by force before depositing anti-corrosion Ni layers
Degree.Cold spray process parameter is listed in table 2, and internal layer uses Ni (O) powder spray after ball-milling treatment, and outer layer is sprayed using original Ni powder
Apply.Fig. 2 (a) and Fig. 2 (b) are respectively the composite coating Cross Section Morphology after cold spraying Ni (O) layers and the anti-corrosion outer layers of Ni, wherein internal layer
Thickness is about 20-50 μm, and outer layer thickness is about 150-200 μm.
Table 2
The 310SS samples that deposited anti-corrosion Ni layers are packaged in the quartz ampoule of argon filling gas shielded, in 900 in Muffle furnace
DEG C insulation 8 hours, obtained oxide diffusion barrier Cross Section Morphology is as shown in figure 3, after heat treatment anti-corrosion Ni layer interior outer boundary
Disappear, and the oxide that continuous average thickness is about 1-3m is generated in 310SS and Ni interfaces.Using power spectrum EDS to sample
It is scanned, the main component of obtained oxide coating is shown in Table 3, and Elemental redistribution result is shown in Fig. 4.With reference to elemental line scan and point
Analysis result can be obtained, and oxide diffusion barrier is mainly made up of rich Cr oxides.
Table 3
Embodiment 2
Using Cr contents be about 18.wt% 316 stainless steels as base material (composition is shown in Table 4), material is pre-processed：Acetone
Dried up after ultrasonic oil removing, washes of absolute alcohol.
Table 4
The preparation of Ni (O) solid-solution powder uses Mechanical Alloying, and granularity is placed in for 63-75 μm of globular nickel powder
In stainless steel jar mill, ratio of grinding media to material is 8: 1, stainless steel ball big (12mm), in (10mm), the quantitative proportion of small (6mm) ball be about 1
: Ni (O) solid-solution powder is made after 10: 3, rotating speed 120r/min, mechanical alloying 15h, the oxygen content of Ni (O) powder is
4.1wt.%.
316SS base materials, through blasting treatment, to remove surface contaminant, improve coating and combined by force before depositing anti-corrosion Ni layers
Degree.Cold spray process parameter is listed in table 2, and internal layer uses Ni (O) powder spray after ball-milling treatment, and outer layer is sprayed using original Ni powder
Apply, wherein internal layer thickness is about 20-50m, and outer layer thickness is about 300-350 μm.
The 316SS samples that deposited anti-corrosion Ni layers are packaged in vacuum drying oven, 8 hours are incubated at 850 DEG C, obtained oxygen
Shown in compound diffusion barrier Cross Section Morphology such as Fig. 5 (a) and Fig. 5 (b).Outer boundary disappears in anti-corrosion Ni layers after heat treatment, and
316SS generates the oxide that continuous average thickness is about 1-3m with Ni interfaces.Sample is scanned using power spectrum EDS,
The main component of obtained oxide coating is shown in Table 5, and the oxide diffusion barrier is mainly made up of rich Cr oxides.
Table 5
Claims (4)
1. the preparation method of a kind of oxide diffusion barrier of stainless steel surfaces containing Cr and anticorrosion layer, it is characterised in that including following step
Suddenly：
1) Ni (O) solid-solution powder is taken, then sieve takes Ni (O) solid-solution powders that particle diameter is less than 50 μm as cold spraying powder；
2) blasting treatment is carried out after carrying out oil removing and cleaning to pending stainless steel base containing Cr；
3) using cold spray technique by step 1) obtained cold spraying powder spray is to through step 2) the stainless base steel containing Cr that handles
Body surface face, Ni (O) solid solution layer is deposited on Cr stainless steel bases surface；
4) in step 3) anti-corrosion Ni layers of the surface deposition of obtained Ni (O) solid solution layer；
5) by step 4) obtained deposition has anti-corrosion Ni layers Cr stainless steel bases to be placed into the container of inert gas shielding,
It is heat-treated, Cr stainless steel base superficial growths is gone out Cr2O3Diffusion barrier, is then incubated again, obtains stainless steel surfaces containing Cr
Oxide diffusion barrier and anticorrosion layer；
Step 3) in Ni (O) solid solution layer thickness be 10-100 microns；
Step 4) in anti-corrosion Ni layers thickness be 90-400 microns.
2. the preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr according to claim 1 and anticorrosion layer, its feature
It is,
Step 5) in inert gas be argon gas；
Step 5) in container be quartz ampoule or vacuum drying oven.
3. the preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr according to claim 1 and anticorrosion layer, its feature
Be, step 5) in be heat-treated during temperature be 700-1000 DEG C, soaking time is 4-20h.
4. the preparation method of the oxide diffusion barrier of stainless steel surfaces containing Cr according to claim 1 and anticorrosion layer, its feature
It is, Cr content is more than or equal to 18wt.% in stainless steel base containing Cr.
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| CN105401147B (en) * | 2015-11-04 | 2018-09-04 | 西安交通大学 | A kind of high temperature anti-corrosion coating of salic diffusion barrier and preparation method thereof |
| CN111763088B (en) * | 2019-04-02 | 2022-03-15 | 上海梅山钢铁股份有限公司 | Spray paint for joint of blast furnace cast iron cooling wall and blast furnace lining and preparation method thereof |
| CN109943872B (en) * | 2019-04-11 | 2021-02-09 | 广西大学 | Preparation method of composite coating for protecting Cr-containing stainless steel in molten fluoride salt |
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| EP1734331A1 (en) * | 2005-06-18 | 2006-12-20 | EADS Deutschland GmbH | High-temperature infrared camouflage coating |
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| EP1734331A1 (en) * | 2005-06-18 | 2006-12-20 | EADS Deutschland GmbH | High-temperature infrared camouflage coating |
Non-Patent Citations (2)
| Title |
|---|
| "Oxidation mechanism of Ni-20Cr foils and its relation to the oxide-scale microstructure";G.Calvarin et al.;《Oxidation of metals》;20001231;第53卷(第1/2期);第25-48页 * |
| "Synthesis and mechanical properties of nanocrystalline Ni coatings produced by cold gas dynamic spraying";L.Ajdelsztajn et al.;《Surface & coatings technology》;20060228;第201卷;第1166-1172页 * |
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