CN105220128A - A kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat - Google Patents
A kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat Download PDFInfo
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Abstract
A preparation method for Zr alloy surface original position vertical-growth Graphene preservative coat, the present invention relates to the preparation method of Zr alloy surface preservative coat.It is poor that the present invention will solve existing zirconium alloy cladding water-fast side corrosive nature, the problem that work-ing life of fuel sheath is short.Method: one, Zr alloy surface pre-treatment; Two, utilize PECVD method at the vertical Graphene of Zr alloy surface growth in situ.The present invention is used for the preparation of Zr alloy surface original position vertical-growth Graphene preservative coat.
Description
Technical field
The present invention relates to the preparation method of Zr alloy surface preservative coat.
Background technology
Along with increasingly sharpening of energy dilemma, nuclear energy is paid close attention to widely as the energy of clean and effective, and the electric energy in the whole world about 16% comes from nuclear energy.Wherein the generated energy of light-water reactor account for 87% of whole world nuclear power, 14% of world's gross generation.And zirconium alloy is little with its thermal neutron absorption cross section, at 350 DEG C, there is excellent mechanical property and the features such as advantage of lower cost, be widely used in water reactor fuel involucrum and other heap inner structural member.In recent years, along with nuclear power develop rapidly and the mankind to the raising of nuclear reactor safety and cost-effectiveness requirement, improve the performance of zirconium alloy under reactor high burnup further, extend its working life and become an important problem.Zirconium alloy cladding under arms time contact with coolant water for a long time, generally in actual applications in addition in refrigerant, add reaction toxicant B, generally with H
3bO
3form adds, but add rear refrigerant in acid, in order to regulate the pH value of refrigerant, also can add LiOH etc. and make refrigerant meta-alkalescence, the refrigerant of meta-alkalescence can accelerate zircaloy corrosion, so the improvement of corrosion resistance nature is depended in the prolongation of zirconium alloy cladding working life to a great extent, in order to improve the corrosion resistance nature of zirconium alloy, except designing new Zirconium alloy material, process for treating surface just becomes important process means, these technology comprise the pre-film of autoclave, laser surface alloying, surface laser process, ion implantation, ion irradiation and anodizing technology etc., corrosion resistance nature and the antiwear property of zirconium alloy is mainly improved by the approach of surface modification.
Summary of the invention
It is poor that the present invention will solve existing zirconium alloy cladding water-fast side corrosive nature, the problem that work-ing life of fuel sheath is short, and provide a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat.
A preparation method for Zr alloy surface original position vertical-growth Graphene preservative coat, specifically carries out according to following steps:
One, zirconium alloy is placed in plasma enhanced chemical vapor deposition vacuum unit, being evacuated to pressure is 5Pa, pass into argon gas and hydrogen, the gas flow regulating argon gas is 20sccm, the gas flow regulating hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 100Pa, then be under the condition of 100Pa at pressure, by temperature most 300 DEG C ~ 1000 DEG C, after intensification, open radio-frequency power supply, adjustment radio frequency power is 150W, be 150W at radio frequency power, pressure is 100Pa and temperature is carry out surface treatment under the condition of 300 DEG C ~ 1000 DEG C, the surface treatment time is 30min,
Two, after surface treatment, close radio-frequency power supply, pass into methane gas, the gas flow regulating methane gas is 5sccm ~ 50sccm, the gas flow regulating argon gas is 50sccm ~ 200sccm, the gas flow keeping hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 50Pa ~ 500Pa, open radio-frequency power supply, then radio frequency power be 200W, pressure deposits under be 50Pa ~ 500Pa and temperature being the condition of 300 DEG C ~ 1000 DEG C, depositing time is 10min ~ 60min;
Three, after deposition terminates; close heating power supply and radio-frequency power supply; stop passing into methane gas; with argon gas and hydrogen for shielding gas; be 300 DEG C ~ 1000 DEG C cool to room temperature from temperature; obtain the zirconium alloy that Graphene preservative coat thickness is the surface in situ vertical-growth Graphene preservative coat of 50nm ~ 500nm, namely complete a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat.
The principle that the present invention improves corrosion resistance nature is: utilize plasma enhanced chemical vapor deposition method, without the need to the auxiliary lower original position of catalyzer at Zr alloy surface direct growth graphene film, improve Zr alloy surface state, Graphene is combined with zirconium alloy well, the wetting angle of orthotropic Graphene and water brings up to 130 °, nonwetting with water, the water side corrosion resistance nature of zirconium alloy can be improved, Graphene has good heat conductivility simultaneously, and the heat being conducive to fuel sheath shifts to refrigerant.In addition, the thermal neutron absorption cross section of carbon is little, can not affect the irradiation behaviour of zirconium alloy cladding.
The invention has the beneficial effects as follows: 1. the problem solving the refrigerant corrosion of existing zirconium alloy cladding water resistant lateral deviation alkalescence, contributes to the life-span of improving zirconium alloy cladding.Zirconium alloy cladding can with 300 of meta-alkalescence DEG C about water coolant Long Term Contact, for improving Qi Shui side corrosion resistance nature, at the vertical Graphene of Zr alloy surface growth in situ, due to Graphene and water nonwetting, thermal conductivity is good, and has good mechanical property, ductility, low thermal neutron absorption cross section, thus can improve the corrosion resistance nature of zirconium alloy, extend the work-ing life of involucrum, meet engineering service requirements.
2. the present invention can assist without the need to catalyzer at low ambient temperatures, and direct in-situ, at Zr alloy surface vertical-growth graphene film, avoids the large element of some impurity, particularly thermal neutron absorption cross section and introduces.
3. simple, efficient, the low cost of plasma enhanced chemical vapor deposition method used in the present invention, be convenient to suitability for industrialized production.
The present invention is used for a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat.
Accompanying drawing explanation
Fig. 1 is the zirconium alloy stereoscan photograph of surface in situ vertical-growth Graphene preservative coat prepared by embodiment one.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat described in present embodiment, specifically carry out according to following steps:
One, zirconium alloy is placed in plasma enhanced chemical vapor deposition vacuum unit, being evacuated to pressure is 5Pa, pass into argon gas and hydrogen, the gas flow regulating argon gas is 20sccm, the gas flow regulating hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 100Pa, then be under the condition of 100Pa at pressure, by temperature most 300 DEG C ~ 1000 DEG C, after intensification, open radio-frequency power supply, adjustment radio frequency power is 150W, be 150W at radio frequency power, pressure is 100Pa and temperature is carry out surface treatment under the condition of 300 DEG C ~ 1000 DEG C, the surface treatment time is 30min,
Two, after surface treatment, close radio-frequency power supply, pass into methane gas, the gas flow regulating methane gas is 5sccm ~ 50sccm, the gas flow regulating argon gas is 50sccm ~ 200sccm, the gas flow keeping hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 50Pa ~ 500Pa, open radio-frequency power supply, then radio frequency power be 200W, pressure deposits under be 50Pa ~ 500Pa and temperature being the condition of 300 DEG C ~ 1000 DEG C, depositing time is 10min ~ 60min;
Three, after deposition terminates; close heating power supply and radio-frequency power supply; stop passing into methane gas; with argon gas and hydrogen for shielding gas; be 300 DEG C ~ 1000 DEG C cool to room temperature from temperature; obtain the zirconium alloy that Graphene preservative coat thickness is the surface in situ vertical-growth Graphene preservative coat of 50nm ~ 500nm, namely complete a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat.
The beneficial effect of present embodiment is: 1. the problem solving the refrigerant corrosion of existing zirconium alloy cladding water resistant lateral deviation alkalescence, contributes to the life-span of improving zirconium alloy cladding.Zirconium alloy cladding can with 300 of meta-alkalescence DEG C about water coolant Long Term Contact, for improving Qi Shui side corrosion resistance nature, at the vertical Graphene of Zr alloy surface growth in situ, due to Graphene and water nonwetting, thermal conductivity is good, and has good mechanical property, ductility, low thermal neutron absorption cross section, thus can improve the corrosion resistance nature of zirconium alloy, extend the work-ing life of involucrum, meet engineering service requirements.
2. present embodiment can be assisted without the need to catalyzer at low ambient temperatures, and direct in-situ, at Zr alloy surface vertical-growth graphene film, avoids the large element of some impurity, particularly thermal neutron absorption cross section and introduces.
3. simple, efficient, the low cost of the plasma enhanced chemical vapor deposition method that uses of present embodiment, be convenient to suitability for industrialized production.
Embodiment two: present embodiment and embodiment one unlike: the zirconium alloy described in step one is nuclear industry level M5, Zr-2 or Zr-4 zirconium alloy for canning nuclear fuel.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two unlike: in step one then under pressure is the condition of 100Pa, by temperature most 500 DEG C.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: in step one then under pressure is the condition of 100Pa, by temperature most 800 DEG C.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: in step one then under pressure is the condition of 100Pa, by temperature most 510 DEG C ~ 790 DEG C.Other is identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: in step one then under pressure is the condition of 100Pa, by temperature most 700 DEG C.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: regulate the gas flow of methane gas to be 30sccm in step 2.Other is identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: regulate the gas flow of argon gas to be 70sccm in step 2.Other is identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: regulate vacuum pumping rate to control pressure in plasma enhanced chemical vapor deposition vacuum unit for 300Pa in step 2.Other is identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: in step 2 then be 200W at radio frequency power, pressure deposits under be 50Pa ~ 500Pa and temperature being 300 DEG C ~ 1000 DEG C conditions, depositing time is 20min.Other is identical with embodiment one to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat described in the present embodiment, specifically carries out according to following steps:
One, zirconium alloy is placed in plasma enhanced chemical vapor deposition vacuum unit, being evacuated to pressure is 5Pa, pass into argon gas and hydrogen, the gas flow regulating argon gas is 20sccm, the gas flow regulating hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 100Pa, then be under the condition of 100Pa at pressure, by temperature most 700 DEG C, after intensification, open radio-frequency power supply, adjustment radio frequency power is 150W, be 150W at radio frequency power, pressure is 100Pa and temperature is carry out surface treatment under 700 DEG C of conditions, the surface treatment time is 30min,
Two, after surface treatment, close radio-frequency power supply, pass into methane gas, the gas flow regulating methane gas is 30sccm, and the gas flow regulating argon gas is 70sccm, and the gas flow keeping hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 300Pa, open radio-frequency power supply, then be 200W at radio frequency power, pressure deposits under be 300Pa and temperature being 700 DEG C of conditions, depositing time is 10min;
Three, after deposition terminates, close heating power supply and radio-frequency power supply, stop passing into methane gas, with argon gas and hydrogen for shielding gas, be 700 DEG C of cool to room temperature from temperature, obtain the zirconium alloy that Graphene preservative coat thickness is the surface in situ vertical-growth Graphene preservative coat of 50nm, namely complete a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat;
Zirconium alloy described in step one is zirconium-4 alloy.
Fig. 1 is the zirconium alloy stereoscan photograph of surface in situ vertical-growth Graphene preservative coat prepared by embodiment one.As seen from the figure, the Graphene prepared in the present embodiment is all perpendicular to Zr alloy surface growth, and be evenly distributed, size is less.The Graphene defect obtained is less, and quality is higher.
Carry out wettability test to the zirconium alloy of surface in situ vertical-growth Graphene preservative coat prepared by embodiment one, the wetting angle obtaining Graphene and water is 130 °.
Claims (10)
1. a preparation method for Zr alloy surface original position vertical-growth Graphene preservative coat, is characterized in that it carries out according to following steps:
One, zirconium alloy is placed in plasma enhanced chemical vapor deposition vacuum unit, being evacuated to pressure is 5Pa, pass into argon gas and hydrogen, the gas flow regulating argon gas is 20sccm, the gas flow regulating hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 100Pa, then be under the condition of 100Pa at pressure, by temperature most 300 DEG C ~ 1000 DEG C, after intensification, open radio-frequency power supply, adjustment radio frequency power is 150W, be 150W at radio frequency power, pressure is 100Pa and temperature is carry out surface treatment under the condition of 300 DEG C ~ 1000 DEG C, the surface treatment time is 30min,
Two, after surface treatment, close radio-frequency power supply, pass into methane gas, the gas flow regulating methane gas is 5sccm ~ 50sccm, the gas flow regulating argon gas is 50sccm ~ 200sccm, the gas flow keeping hydrogen is 20sccm, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum unit as 50Pa ~ 500Pa, open radio-frequency power supply, then radio frequency power be 200W, pressure deposits under be 50Pa ~ 500Pa and temperature being the condition of 300 DEG C ~ 1000 DEG C, depositing time is 10min ~ 60min;
Three, after deposition terminates; close heating power supply and radio-frequency power supply; stop passing into methane gas; with argon gas and hydrogen for shielding gas; be 300 DEG C ~ 1000 DEG C cool to room temperature from temperature; obtain the zirconium alloy that Graphene preservative coat thickness is the surface in situ vertical-growth Graphene preservative coat of 50nm ~ 500nm, namely complete a kind of preparation method of Zr alloy surface original position vertical-growth Graphene preservative coat.
2. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that the zirconium alloy described in step one is nuclear industry level M5, Zr-2 or Zr-4 zirconium alloy for canning nuclear fuel.
3. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that in step one then under pressure is the condition of 100Pa, by temperature most 500 DEG C.
4. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that in step one then under pressure is the condition of 100Pa, by temperature most 800 DEG C.
5. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that in step one then under pressure is the condition of 100Pa, by temperature most 510 DEG C ~ 790 DEG C.
6. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that in step one then under pressure is the condition of 100Pa, by temperature most 700 DEG C.
7. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that regulating in step 2 the gas flow of methane gas to be 30sccm.
8. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that regulating in step 2 the gas flow of argon gas to be 70sccm.
9. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, is characterized in that regulating vacuum pumping rate to control pressure in plasma enhanced chemical vapor deposition vacuum unit for 300Pa in step 2.
10. the preparation method of a kind of Zr alloy surface original position vertical-growth Graphene preservative coat according to claim 1, to it is characterized in that in step 2 then be 200W at radio frequency power, pressure deposits under be 50Pa ~ 500Pa and temperature being 300 DEG C ~ 1000 DEG C conditions, depositing time is 20min.
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| CN105603393A (en) * | 2016-02-22 | 2016-05-25 | 中国石油大学(北京) | Magnesium alloy provided with graphene protection film and preparation method thereof |
| CN105755447A (en) * | 2016-01-29 | 2016-07-13 | 中国科学院重庆绿色智能技术研究院 | Low-cost method for uniformly preparing graphene film |
| CN106784915A (en) * | 2016-11-30 | 2017-05-31 | 哈尔滨工业大学 | A kind of preparation method of stainless steel surfaces Graphene corrosion-inhibiting coating |
| CN106835066A (en) * | 2017-01-14 | 2017-06-13 | 太原理工大学 | A kind of method of metal surface Graphene Passivation Treatment corrosion-inhibiting coating |
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| CN109052379A (en) * | 2018-09-04 | 2018-12-21 | 山西大学 | A kind of preparation method of blacker-than-black light absorbent |
| CN110106492A (en) * | 2019-05-05 | 2019-08-09 | 苏州大学 | Quickly prepare the method for vertical graphene |
| CN112011783A (en) * | 2020-09-03 | 2020-12-01 | 太原理工大学 | Low-temperature chemical vapor deposition method for zirconium oxide on surface of zirconium alloy to catalyze growth of graphene |
| CN112011783B (en) * | 2020-09-03 | 2022-09-09 | 太原理工大学 | Low-temperature chemical vapor deposition method for zirconium oxide on surface of zirconium alloy to catalyze growth of graphene |
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