CN105177541A - Method for preparing Al2O3 tritium-resistant coating by MOD (metal-organic decomposition) method - Google Patents
Method for preparing Al2O3 tritium-resistant coating by MOD (metal-organic decomposition) method Download PDFInfo
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- CN105177541A CN105177541A CN201510674277.7A CN201510674277A CN105177541A CN 105177541 A CN105177541 A CN 105177541A CN 201510674277 A CN201510674277 A CN 201510674277A CN 105177541 A CN105177541 A CN 105177541A
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Abstract
The invention belongs to the field of materials, and relates to a method for preparing Al2O3 coating on a CLF-1 low-activity ferrite martensite stainless steel substrate. The method comprises the following steps: (1) carrying out surface treatment, according to a sequence of mechanical grinding, mechanical polishing, electrolytic polishing, oil removal and rust removal, on CLF-1 low-activity ferrite martensite steel (RAFM); (2) uniformly coating commercial MOD liquor on the surface of the substrate by utilizing a dip-coating method; (3) baking a test sample prepared in the step (2) for 5-30 minutes at 120 DEG C by use of a glue baking machine, and naturally cooling the test sample to the room temperature; (4) baking the test sample prepared in the step (3) for 5-20 minutes at 500-600 DEG C by use of the glue baking machine, and naturally cooling the test sample to the room temperature; (5) repeating the steps (2) to (4) for 10-20 times; and (6) putting the test sample prepared in the step (5) into a high-temperature tubular furnace to anneal for 30-120 minutes at 600-700 DEG C, thereby obtaining the Al2O3 tritium-resistant coating. The method is simple in operation process; and the prepared Al2O3 tritium-resistant coating is compact, flat and high in binding force with a base material.
Description
Technical field
The invention belongs to Material Field, relate to one and prepare Al in CLF-1 low activity ferrito-martensite steel matrix
2o
3the method of coating, is specially MOD legal system for Al
2o
3the method of resistance tritium coating.
Background technology
The advantage that fusion energy shows in spatter property, security and fuel reserves are rich etc. gets most of the attention, along with the construction of International Thermal-Nuclear Experimental Reactor (ITER) and going deep into of correlative study, the structure of core technology carrier-covering, design of material that fusion energy is moved towards to apply become study hotspot.Wherein, because the important fuel-tritium of D-T thermonuclear reaction has extremely strong infiltration, diffustivity, in addition the complex environment such as high temperature, high heat load, irradiation, very easily cause tritium hypertrophic region structured material in covering, as low activity ferrito-martensite steel, there is hydrogen damage, affect material property, reduce covering effect in reactor; The loss of expensive tritium simultaneously also can cause radiocontamination to environment and equipment.Therefore, the resistance tritium-permeation problem of producing tritium cladding modular structured material causes international concern.
In recent years, propose in the world to reduce tritium-permeation, diffusion in structured material surface-coated tritium permeation barrier (TPB) method.Wherein, Al
2o
3ceramic barrier is owing to having the over-all propertieies such as high infiltration attenuating/descending factors (PRF), excellent mechanical property, good thermal conductivity and resistivity thus being considered to have application potential most.But conventional coatings technology of preparing such as PVD method, CVD method, spraying method are only applicable to the coating of (closely) planar substrates, limited when being applied to complex-shaped surface mould/inner surface of pipeline coating and preparing; Mainly complex process, coating is uneven, poor process control.
Summary of the invention
The object of the invention is to: provide a kind of and be applicable to the simple and Al of excellent performance of complex-shaped surface mould/inner surface of pipeline, preparation technology
2o
3resistance tritium coating production.
Concrete technical scheme is:
MOD legal system is for Al
2o
3the method of resistance tritium coating, comprises the following steps:
(1) with 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper CLF-1 substrate of polishing successively from coarse to fine, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste, electropolishing is used successively after polishing smooth, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment that commercial MOD liquid is evenly coated on CLF-1 substrate surface, the pull rate of this step is that 5 ~ 20cm/min, CLF-1 substrate leaves standstill 300 ~ 2000s in MOD liquid;
(3), after again CLF-1 substrate being suspended 3 ~ 10min in atmosphere, in roasting glue machine, cure 5 ~ 30min at 120 DEG C, naturally cool to room temperature;
(4) roasting glue machine put into again by the CLF-1 substrate being coated with xerogel, cures 5 ~ 20min, naturally cool to room temperature at 500 ~ 600 DEG C;
(5) above-mentioned steps (2) ~ (4) 10 ~ 20 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 600 DEG C ~ 700 DEG C temperature, carries out 1 ~ 2h thermal treatment, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, temperature rise rate 5 ~ 10 DEG C/min of this step, with stove naturally cooling during cooling.
CLF-1 substrate is CLF-1 low activity ferrito-martensite steel.
Preferably, in step (2), pull rate is 10cm/min; CLF-1 substrate leaves standstill 1800s in MOD liquid;
Preferably, 10min is cured at roasting 120 DEG C, glue machine in step (3);
Preferably, in step (4), CLF-1 substrate cures 5min at 500 ~ 600 DEG C, roasting glue machine;
Preferably, the middle repeating step (2) ~ (4) of step (5) 10 times;
Preferably, in step (6), temperature rise rate is 5 DEG C/min, annealing 1h.
MOD legal system provided by the invention is for Al
2o
3the method of resistance tritium coating, can be used for the preparation of complex-shaped surface mould/inner surface of pipeline coating, technological operation is simple, can realize industrialization scale operation; The method is by adjusting pull rate and dipping time, curing and the process parameter control such as annealing temperature, cycle index coating uniformity, sedimentation rate, thickness, and controllability is strong; Obtained Al
2o
3coating is fine and close, even, stronger with basal body binding force.
Accompanying drawing explanation
Fig. 1 is the thermogravimetric analysis figure of the commercial MOD liquid that embodiment 1 ~ 4 uses;
Fig. 2 is Al prepared by embodiment 1
2o
3the FESEM figure of resistance tritium coating;
Fig. 3 is Al prepared by embodiment 1
2o
3the energy spectrum analysis figure of resistance tritium coating;
Fig. 4 is Al prepared by embodiment 1
2o
3the XRD figure of resistance tritium coating;
Fig. 5 is Al prepared by embodiment 2
2o
3the FESEM figure of resistance tritium coating;
Fig. 6 is Al prepared by embodiment 2
2o
3the XRD figure of resistance tritium coating;
Fig. 7 is Al prepared by embodiment 3
2o
3the FESEM figure of resistance tritium coating
Fig. 8 is Al prepared by embodiment 3
2o
3the XRD figure of resistance tritium coating;
Fig. 9 is the metallography microscope shape appearance figure of embodiment 4 sample.
Embodiment:
The specific embodiment of the present invention is described in conjunction with the embodiments.
Embodiment 1:
(1) with 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper CLF-1 substrate of polishing successively from coarse to fine, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste is used successively after polishing smooth, electropolishing, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment by commercial MOD liquid, thermolysis property as shown in Figure 1, is evenly coated on CLF-1 substrate surface, and wherein pull rate is that 10cm/min, CLF-1 substrate leaves standstill 1800s in MOD liquid;
(3), after the CLF-1 substrate after above-mentioned steps (2) being flooded suspends 5min in atmosphere, at 120 DEG C, roasting glue machine, cure 10min, naturally cool to room temperature;
(4) CLF-1 substrate above-mentioned steps (3) being coated with xerogel cures 5min at 500 DEG C, roasting glue machine, naturally cools to room temperature;
(5) above-mentioned steps (2) ~ (4) 10 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 600 DEG C of temperature, carries out 1h thermal treatment, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, the temperature rise rate of this step is 5 DEG C/min, with stove naturally cooling during cooling.With field emission scanning electron microscope to obtained Al
2o
3resistance tritium coating carries out morphology analysis, and as shown in Figure 2, gained coating is fine and close, even, carries out energy spectrum analysis as shown in Figure 3, record Al content 19.36at.%, O content 33.20at.% to coating.Utilize X-ray diffractometer to Al
2o
3resistance tritium coating carries out material phase analysis, and as shown in Figure 4,2 θ occur Al at about 38 °
2o
3the diffraction peak of crystal face.
Embodiment 2:
(1) with 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper CLF-1 substrate of polishing successively from coarse to fine, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste is used successively after polishing smooth, electropolishing, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment by commercial MOD liquid, thermolysis property as shown in Figure 1, is evenly coated on CLF-1 substrate surface, and wherein pull rate is that 10cm/min, CLF-1 substrate leaves standstill 1800s in MOD liquid;
(3), after the CLF-1 substrate after above-mentioned steps (2) being flooded suspends 5min in atmosphere, at 120 DEG C, roasting glue machine, cure 10min, naturally cool to room temperature;
(4) CLF-1 substrate above-mentioned steps (3) being coated with xerogel cures 5min at 500 DEG C, roasting glue machine, naturally cools to room temperature;
(5) above-mentioned steps (2) ~ (4) 10 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 700 DEG C of temperature, carries out 1h thermal treatment, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, the temperature rise rate of this step is 5 DEG C/min, with stove naturally cooling during cooling.With field emission scanning electron microscope to obtained Al
2o
3resistance tritium coating carries out morphology analysis, and as shown in Figure 5, gained coating is fine and close, even.Utilize X-ray diffractometer to Al
2o
3resistance tritium coating carries out material phase analysis, and as shown in Figure 6,2 θ occur Al at about 38 °
2o
3diffraction peak.
Embodiment 3:
(1) with 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper CLF-1 substrate of polishing successively from coarse to fine, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste is used successively after polishing smooth, electropolishing, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment by commercial MOD liquid, thermolysis property as shown in Figure 1, is evenly coated on CLF-1 substrate surface, and wherein pull rate is that 10cm/min, CLF-1 substrate leaves standstill 1800s in MOD liquid;
(3), after the CLF-1 substrate after above-mentioned steps (2) being flooded suspends 5min in atmosphere, at 120 DEG C, roasting glue machine, cure 10min, naturally cool to room temperature;
(4) CLF-1 substrate above-mentioned steps (3) being coated with xerogel cures 5min at 600 DEG C, roasting glue machine, naturally cools to room temperature;
(5) above-mentioned steps (2) ~ (4) 10 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 600 DEG C of temperature, carries out 1h thermal treatment, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, the temperature rise rate of this step is 5 DEG C/min, with stove naturally cooling during cooling.With field emission scanning electron microscope to obtained Al
2o
3resistance tritium coating carries out morphology analysis, and as shown in Figure 7, gained coating is fine and close, even.Utilize X-ray diffractometer to Al
2o
3resistance tritium coating carries out material phase analysis, and as shown in Figure 8,2 θ occur Al at about 38 °
2o
3diffraction peak.
Embodiment 4:
(1) by CLF-1 substrate of polishing successively from coarse to fine for 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste is used successively after polishing smooth, electropolishing, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment by commercial MOD liquid, thermolysis property as shown in Figure 1, is evenly coated on CLF-1 substrate surface, and wherein pull rate is that 10cm/min, CLF-1 substrate leaves standstill 1800s in MOD liquid;
(3), after the substrate after above-mentioned steps (1) being flooded suspends 5min in atmosphere, at 120 DEG C, roasting glue machine, cure 10min, naturally cool to room temperature;
(4) CLF-1 substrate above-mentioned steps (3) being coated with wet gel cures 5min at 500 DEG C, roasting glue machine, naturally cools to room temperature;
(5) above-mentioned steps (2) ~ (4) 10 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 600 DEG C, 700 DEG C temperature, carries out 1h thermal treatment respectively, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, the temperature rise rate of this step is 5 DEG C/min, with stove naturally cooling during cooling.Utilize metallography microscope sem observation CLF-1 substrate, 600 DEG C of annealed sample, 700 DEG C of annealed sample in 2% nital, corrode 30s after microscopic appearance, as shown in Figure 9, Al
2o
3resistance tritium coating plays effective protected effect to matrix, and coating and substrate caking power are by force, have no coating shedding.
Claims (1)
1.MOD legal system is for Al
2o
3the method of resistance tritium coating, is characterized in that, comprise the following steps:
(1) with 180#, 240#, 600#, 1000#, 1200# waterproof abrasive paper CLF-1 substrate of polishing successively from coarse to fine, 1 μm of diamond polishing agent, W1 polishing powder, the polishing of W1 rubbing paste, electropolishing is used successively after polishing smooth, oil removing, rust cleaning, dries up stand-by after finally clean with deionized water rinsing;
(2) at room temperature utilize lift coating equipment that commercial MOD liquid is evenly coated on CLF-1 substrate surface, the pull rate of this step is that 5 ~ 20cm/min, CLF-1 substrate leaves standstill 300 ~ 2000s in MOD liquid;
(3), after again CLF-1 substrate being suspended 3 ~ 10min in atmosphere, in roasting glue machine, cure 5 ~ 30min at 120 DEG C, naturally cool to room temperature;
(4) roasting glue machine put into again by the CLF-1 substrate being coated with xerogel, cures 5 ~ 20min, naturally cool to room temperature at 500 ~ 600 DEG C;
(5) above-mentioned steps (2) ~ (4) 10 ~ 20 times are repeated;
(6) sample that above-mentioned steps (5) obtains is placed in high-temperature tubular sintering oven, at 600 DEG C ~ 700 DEG C temperature, carries out 1 ~ 2h thermal treatment, Al can be obtained on CLF-1 substrate
2o
3resistance tritium coating, temperature rise rate 5 ~ 10 DEG C/min of this step, with stove naturally cooling during cooling.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929831A (en) * | 2015-12-30 | 2017-07-07 | 核工业西南物理研究院 | A kind of preparation method of aluminum oxide tritium permeation coating |
| CN108787402A (en) * | 2018-06-27 | 2018-11-13 | 合肥工业大学 | A method of on tungsten surface, coating TiO2 colloids prepare compound resistance tritium coating |
| CN112657815A (en) * | 2020-12-23 | 2021-04-16 | 合肥工业大学 | Preparation method of Al2O3/SiO2 composite tritium-resistant coating on inner wall of 316L stainless steel pipe |
| CN115747775A (en) * | 2022-11-29 | 2023-03-07 | 四川大学 | Preparation method of high-quality thick tritium-resistant coating |
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| JPS59232273A (en) * | 1983-06-14 | 1984-12-27 | Tokyo Yogyo Co Ltd | Method for coating metal with ceramic |
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| JPS59232273A (en) * | 1983-06-14 | 1984-12-27 | Tokyo Yogyo Co Ltd | Method for coating metal with ceramic |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929831A (en) * | 2015-12-30 | 2017-07-07 | 核工业西南物理研究院 | A kind of preparation method of aluminum oxide tritium permeation coating |
| CN108787402A (en) * | 2018-06-27 | 2018-11-13 | 合肥工业大学 | A method of on tungsten surface, coating TiO2 colloids prepare compound resistance tritium coating |
| CN112657815A (en) * | 2020-12-23 | 2021-04-16 | 合肥工业大学 | Preparation method of Al2O3/SiO2 composite tritium-resistant coating on inner wall of 316L stainless steel pipe |
| CN112657815B (en) * | 2020-12-23 | 2023-08-08 | 合肥工业大学 | Preparation method of 316L stainless steel pipe inner wall Al2O3/SiO2 composite tritium-resistant coating |
| CN115747775A (en) * | 2022-11-29 | 2023-03-07 | 四川大学 | Preparation method of high-quality thick tritium-resistant coating |
| CN115747775B (en) * | 2022-11-29 | 2023-09-08 | 四川大学 | Preparation method of high-quality thick tritium-resistant coating |
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Effective date of registration: 20160229 Address after: 610065 Wuhou District, Chengdu, South Ring Road, No. 1, No. 1, Sichuan Applicant after: Sichuan University Applicant after: Nuclear Industry Xinan Physical Inst. Address before: 610065 Wuhou District, Chengdu, South Ring Road, No. 1, No. 1, Sichuan Applicant before: Sichuan University |
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| CB03 | Change of inventor or designer information |
Inventor after: Yang Jijun Inventor after: Wang Long Inventor after: Feng Yongjin Inventor after: Liao Jiali Inventor after: Yang Yuanyou Inventor after: Liu Ning Inventor after: Feng Kaiming Inventor before: Wang Long Inventor before: Yang Jijun Inventor before: Feng Yongjin Inventor before: Liao Jiali Inventor before: Yang Yuanyou Inventor before: Liu Ning Inventor before: Feng Kaiming |
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