CN103014621A - Preparation method of Cr-Si-C-N nanoscale composite coating - Google Patents
Preparation method of Cr-Si-C-N nanoscale composite coating Download PDFInfo
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Abstract
The invention belongs to a preparation method of a coating and especially relates to a preparation method of a Cr-Si-C-N nanoscale composite coating on the surface of a super-critical water-cooled reactor casing. The preparation method comprises the following steps of 1, carrying out a matrix plating pretreatment and backwash washing process by grinding and polishing a matrix by a metallographic abrasive paper of 300 to 1200 meshes to obtain a matrix with a mirror surface, putting the matrix with the mirror surface into an ultrasonic container, carrying out degreaser cleaning, carrying out pickling and deionized water rinsing, drying in a vacuum drying oven, putting the dried matrix into a deposition vacuum chamber and carrying out plasma backwash washing, 2, carrying out Cr(C,N) gradient transition layer deposition, 3, carrying out Cr-Si-C-N nanoscale composite coating deposition, and 4, carrying out coating heat treatment. The preparation method has the advantages of high hardness, high antioxidation degree and good coating adhesion.
Description
Technical field
The invention belongs to the preparation method of coating, be specifically related to a kind of preparation method of Supercritical-Pressure Light Water Cooled Reactor fuel sheath surface C r-Si-C-N nano-composite coating.
Background technology
Compare with all multiple-energy-sources such as coal, oil, sun power, water energy, nuclear power is as a kind of efficient, economic and lasting energy, and the comprehensive advantage of the aspects such as the energy dilemma that faces in the solution whole world, protection of the environment quality is remarkable.Supercritical-Pressure Light Water Cooled Reactor has the advantages such as thermo-efficiency height, designs simplification, security are good, good economy performance.The research of Supercritical-Pressure Light Water Cooled Reactor fuel canning material is one of key of Supercritical-Pressure Light Water Cooled Reactor technical research.At present, low swelling austenitic stainless steel such as D9,1.4970,316Ti etc. are main Supercritical-Pressure Light Water Cooled Reactor fuel canning materials, and these materials have the advantages such as intensity height, void swelling is low, weldability good, neutron economy is better.Yet, the high temperature oxidation corrosion resistance poor-performing of above-mentioned materials in supercritical water, in the long service process, excessive oxidation corrosion speed certainly will affect the structural integrity of fuel sheath.
Nano-composite coating in Supercritical-Pressure Light Water Cooled Reactor fuel sheath surface deposition high temperature oxidation resistance excellence can solve an above-mentioned difficult problem effectively, and this also becomes the in recent years study hotspot of academia and engineering circles.At the research initial stage, people trend towards the alloy coat at involucrum surface deposition Cr, because it can form the Fe-Cr compound with steel substrate at the interface, and realization chemical metallurgy combination, thereby have good coating/base material bonding force.Simultaneously, the Cr element can form the protection by oxide films layer by the O in surface and corrosive environment in the coating, hinders soaking into of corrosive medium, thereby has preferably high temperature oxidation resistance.But, the alloy coat that Cr and other metals form is in the aspects such as intensity, hardness, wear resistance shortcoming advantage, strong high-temperature water thermal shocking may cause the distortion of coating ductility, premature failure is such as document [Wang Jianping, Xu Lianyong, permitted the Yongtai, the resistance to high temperature corrosion performance research of Li Jia .FeCrAl and nickelic chromium alloy coating. China Power, 2007,40 (4): 54-57].Afterwards, more research then trends towards paying close attention to the metal nitride coatings such as CrN, TiN and CrAlN.With respect to the Cr alloy coat, nitride coatings has more advantage at aspects such as corrosion resistance, hardness and wear resistancies.For example, the TiN coating has higher hardness, and about 20GPa, its oxidation resistance temperature are 400 ℃～500 ℃, as document [Song Guihong, Du Hao, He Chunlin. hard and superhard coating-properity, the preparation with the sign, Beijing: Chemical Industry Press, 2007]; The CrN coating also has higher hardness, about 18GPa, also have good toughness and high temperature oxidation resistance, such as document [M.A.Djouadi, C.Nouveau, P.Beer, M.Lambertin.CrxNy hard coatings deposited with PVD method on tools for wood machining.Surface and Coatings Technology, 2000,133,478-483].In recent years, along with developing rapidly of nanotechnology, nano-composite coating is owing to all have very significant advantage with respect to conventional washcoat material at aspect of performances such as resistance to high temperature oxidation, hardness, frictional wear, anti-thermal shocks, thereby caused investigator's extensive concern.For example, the hardness of Ti-Al-Si-N nano-composite coating can be lower than 1.0 * 10 up to 45GPa, wear rate
-14m
2N
-1Such as document [E.Ribeiro, A.Malczyk, S.Carvalho, et al.Effects of ion bombardment on properties of d.c.sputtered superhard (Ti, Si, Al) N nanocomposite coatings.Surface and Coatings Technology, 2002,151-152,515-520]; The resistance to high temperature oxidation temperature of Ti-Si-C-N nano-composite coating can reach more than 900 ℃, and at high temperature it still has excellent mechanical property, can reach about 40GPa such as the coating hardness value 900 ℃ the time, such as document [D.Ma, S.Ma, K.Xu.Superhard nanocomposite Ti-Si-C-N coatings prepared by pulsed-d.c plasma enhanced CVD.Surface and Coatings Technology, 2005,200,382-386].Suchlike studies show that, nano-composite coating have more excellent high temperature oxidation corrosion resistance performance and mechanical property.At present, the research of nano-composite coating is mainly comprised in the following areas: the first, develop the nano-composite coating novel material of various element constituent elements, such as Cr-Al-Si-N, Ti-Si-C-N, W-Si-C-N etc.; The second, Reasonable Regulation And Control design coating forms structure, makes it have the pattern structure of (amorphous phase+nanometer crystalline phase) form; The 3rd, optimize buffer layer material, to improve bonding strength between nano-composite coating and the matrix etc., such as document [P.Holubar, M.Jilek, M.Sima.Present and possible future applications of superhard nanocomposite coatings.Surface and Coatings Technology, 2000,133-134,145-151].
To sum up, at present also not at satisfactory alloy all in nature such as hardness, intensity, wear resistance, erosion resistance.
Summary of the invention
The present invention is directed to the defective of prior art, provide a kind of hardness high, the preparation method of the Cr-Si-C-N nano-composite coating of oxidation-resistance number.
Technical scheme of the present invention is: a kind of preparation method of Cr-Si-C-N nano-composite coating comprises the steps
Step 1: matrix plating pre-treatment and backwash clean
With 300 orders～1200 purpose abrasive paper for metallograph base material is carried out grinding and polishing, reaching mirror status gets final product, then base material being placed ultrasonic container to carry out degreaser cleans, degreaser carries out drying in vacuum drying oven after pickling and the rinsed with deionized water after cleaning and finishing, to dry at last base material places deposition vacuum chamber to carry out the cleaning of plasma body backwash
Step 2: Cr (C, N) gradient transitional lay deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment to deposit Cr (C, N) gradient transitional lay at substrate surface, at first the vacuum tightness with environment is extracted into 5 * 10
-4Then Pa is filled with Ar gas, and the Ar airshed is 50sccm, and air pressure is 0.5Pa, ventilates 10 minutes, then with N
2With CH
4The flow of gas is adjusted to 50sccm and 40sccm gradually from 0sccm and 0sccm respectively, and air pressure also is 0.5Pa, and 3 kinds of source of the gas purity are 99.99%; The sputtering power of 1 magnetic control Cr target is transferred to the arc current of 2.0kW, 2 post arc Cr targets and is transferred to 70A, Cr target purity is 99.99%, will deposit bias voltage to be transferred to-50V, depositing temperature is transferred to 200 ℃, open subsequently the chip bench baffle plate, deposition 30min, deposit thickness is about 1 μ m
Step 3: Cr-Si-C-N nano-composite coating deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment, behind the deposition transition layer, under the condition of uninterrupted vacuum environment, continue deposition Cr-Si-C-N nano-composite coating, in deposition process, environment vacuum tightness, Ar, N
2With CH
4The parameters such as gas flow and air pressure, magnetic control Cr target sputtering power, post arc Cr target arc current, depositing temperature all remain unchanged, magnetic control Si target sputtering power is transferred to 0.5kW, and matrix is deposited bias voltage is transferred to-200V by-50V, depositing time is 1.5～2.0h, deposit thickness is about 2～3 μ m
Step 4: coating thermal treatment
Behind deposition Cr-Si-C-N nano-composite coating, uninterrupted vacuum environment is carried out in-situ annealing to sample, and its processing parameter is: vacuum tightness 5 * 10
-4Pa, 500 ℃ of annealing temperatures, 10 ℃/min of temperature rise rate, soaking time 60 minutes, insulation is chilled to room temperature with stove after finishing, and takes out subsequently.
The preparation method of aforesaid a kind of Cr-Si-C-N nano-composite coating, wherein, the base material described in the step 1 comprises D9,1.4970,316Ti austenitic stainless steel.
The preparation method of aforesaid a kind of Cr-Si-C-N nano-composite coating, wherein, ultrasonic container that base material is placed described in the step 1 carries out the degreaser cleaning, the composition of degreaser comprises yellow soda ash 180g/L, Trisodium Citrate 50g/L, fatty alcohol-polyoxyethylene ether 5g/L, sodium phosphate 40g/L, and scavenging period is 10～15min.
The preparation method of aforesaid a kind of Cr-Si-C-N nano-composite coating, wherein, in vacuum drying oven, dry after pickling described in the step 1 and the rinsed with deionized water and comprise, it is that 10% hydrochloric acid soln at room temperature cleans about 5min that concentration is adopted in pickling, washes several with deionized water subsequently; The vacuum tightness of vacuum drying oven is 300Pa, and bake out temperature is 150 ℃, and storing time was longer than 1 hour.
The preparation method of aforesaid a kind of Cr-Si-C-N nano-composite coating, wherein, the backwash cleaning parameters described in the step 1 is: base vacuum degree 5 * 10
-4Pa, backwash bias voltage-200V, sputter Ar air pressure 0.3Pa, backwash time 15min.
Effect of the present invention is: (1) is because the dense oxidation film protective layer that Cr and O form can effectively stop the transmission of corrosive medium; and adopt Cr-Si-C-N coating process of the present invention can form the composite structure of amorphous phase+nanometer crystalline phase; thereby this nano-composite coating possesses excellent resistance to high temperature corrosion performance and mechanical property; its oxidation resistance temperature can reach 900 ℃, and hardness value can reach 35GPa.(2) Cr (C, N) gradient transitional lay structure is so that Cr-Si-C-N nano-composite coating and stainless steel substrate have good interface bond strength, and coating adhesion can reach 35N.Adopt coating on the Supercritical-Pressure Light Water Cooled Reactor fuel sheath of Cr-Si-C-N nano-composite coating technique of the present invention can realize being coated with the coordinating and unifying of sheet building and function, use properties and the work-ing life of having improved the Supercritical-Pressure Light Water Cooled Reactor fuel sheath.
Embodiment
A kind of preparation method of Cr-Si-C-N nano-composite coating comprises the steps
Step 1: matrix plating pre-treatment and backwash clean
With 300 orders～1200 purpose abrasive paper for metallograph base material is carried out grinding and polishing, reach mirror status and get final product, described base material comprises D9,1.4970,316Ti austenitic stainless steel, and above-mentioned three kinds of base materials are the commercially available material.Then base material is placed ultrasonic container to carry out degreaser and clean, the composition of degreaser comprises yellow soda ash 180g/L, Trisodium Citrate 50g/L, fatty alcohol-polyoxyethylene ether 5g/L, sodium phosphate 40g/L.Scavenging period is 10～15min.Degreaser carries out drying in vacuum drying oven after pickling and the rinsed with deionized water after cleaning and finishing.It is that 10% hydrochloric acid soln at room temperature cleans about 5min that concentration is adopted in pickling, washes several with deionized water subsequently; The vacuum tightness of vacuum drying oven is 300Pa, and bake out temperature is 150 ℃, and storing time was longer than 1 hour.To dry at last base material and place deposition vacuum chamber to carry out the cleaning of plasma body backwash, the backwash cleaning parameters is: base vacuum degree 5 * 10
-4Pa, backwash bias voltage-200V, sputter Ar air pressure 0.3Pa, backwash time 15min.
Step 2: Cr (C, N) gradient transitional lay deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment to deposit Cr (C, N) gradient transitional lay at substrate surface.At first the vacuum tightness with environment is extracted into 5 * 10
-4Then Pa is filled with Ar gas, and the Ar airshed is 50sccm (standard cubic centimeters per minute), and air pressure is 0.5Pa, ventilates 10 minutes, then with N
2With CH
4The flow of gas is adjusted to 50sccm and 40sccm gradually from 0sccm and 0sccm respectively, and air pressure also is 0.5Pa, and 3 kinds of source of the gas purity are 99.99%; The sputtering power of 1 magnetic control Cr target is transferred to the arc current of 2.0kW, 2 post arc Cr targets and is transferred to 70A, Cr target purity is 99.99%, will deposit bias voltage to be transferred to-50V, depositing temperature is transferred to 200 ℃, opens subsequently the chip bench baffle plate, deposition 30min, deposit thickness is about 1 μ m.
Step 3: Cr-Si-C-N nano-composite coating deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment, behind the deposition transition layer, under the condition of uninterrupted vacuum environment, continue deposition Cr-Si-C-N nano-composite coating.Used target also has 2 magnetic control Si targets except 1 magnetic control Cr target and 2 post arc Cr targets, the purity of Si target also is 99.99%.In deposition process, environment vacuum tightness, Ar, N
2With CH
4The parameters such as gas flow and air pressure, magnetic control Cr target sputtering power, post arc Cr target arc current, depositing temperature all remain unchanged, magnetic control Si target sputtering power is transferred to 0.5kW, and matrix is deposited bias voltage be transferred to-200V by-50V, depositing time is 1.5～2.0h, deposit thickness is about 2～3 μ m.
Step 4: coating thermal treatment
Behind deposition Cr-Si-C-N nano-composite coating, uninterrupted vacuum environment is carried out in-situ annealing to sample, and its processing parameter is: vacuum tightness 5 * 10
-4Pa, 500 ℃ of annealing temperatures, 10 ℃/min of temperature rise rate, soaking time 60 minutes, insulation is chilled to room temperature with stove after finishing, and takes out subsequently.
Claims (5)
1. the preparation method of a Cr-Si-C-N nano-composite coating is characterized in that: comprise the steps
Step 1: matrix plating pre-treatment and backwash clean
With 300 orders～1200 purpose abrasive paper for metallograph base material is carried out grinding and polishing, reaching mirror status gets final product, then base material being placed ultrasonic container to carry out degreaser cleans, degreaser carries out drying in vacuum drying oven after pickling and the rinsed with deionized water after cleaning and finishing, to dry at last base material places deposition vacuum chamber to carry out the cleaning of plasma body backwash
Step 2: Cr (C, N) gradient transitional lay deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment to deposit Cr (C, N) gradient transitional lay at substrate surface, at first the vacuum tightness with environment is extracted into 5 * 10
-4Then Pa is filled with Ar gas, and the Ar airshed is 50sccm, and air pressure is 0.5Pa, ventilates 10 minutes, then with N
2With CH
4The flow of gas is adjusted to 50sccm and 40sccm gradually from 0sccm and 0sccm respectively, and air pressure also is 0.5Pa, and 3 kinds of source of the gas purity are 99.99%; The sputtering power of 1 magnetic control Cr target is transferred to the arc current of 2.0kW, 2 post arc Cr targets and is transferred to 70A, Cr target purity is 99.99%, will deposit bias voltage to be transferred to-50V, depositing temperature is transferred to 200 ℃, open subsequently the chip bench baffle plate, deposition 30min, deposit thickness is about 1 μ m
Step 3: Cr-Si-C-N nano-composite coating deposition
Adopt JW-500 type arc ion intensified response magnetron sputtering equipment, behind the deposition transition layer, under the condition of uninterrupted vacuum environment, continue deposition Cr-Si-C-N nano-composite coating, in deposition process, environment vacuum tightness, Ar, N
2With CH
4The parameters such as gas flow and air pressure, magnetic control Cr target sputtering power, post arc Cr target arc current, depositing temperature all remain unchanged, magnetic control Si target sputtering power is transferred to 0.5kW, and matrix is deposited bias voltage is transferred to-200V by-50V, depositing time is 1.5～2.0h, deposit thickness is about 2～3 μ m
Step 4: coating thermal treatment
Behind deposition Cr-Si-C-N nano-composite coating, uninterrupted vacuum environment is carried out in-situ annealing to sample, and its processing parameter is: vacuum tightness 5 * 10
-4Pa, 500 ℃ of annealing temperatures, 10 ℃/min of temperature rise rate, soaking time 60 minutes, insulation is chilled to room temperature with stove after finishing, and takes out subsequently.
2. the preparation method of a kind of Cr-Si-C-N nano-composite coating as claimed in claim 1, it is characterized in that: the base material described in the step 1 comprises D9,1.4970,316Ti austenitic stainless steel.
3. the preparation method of a kind of Cr-Si-C-N nano-composite coating as claimed in claim 2, it is characterized in that: the ultrasonic container that base material is placed described in the step 1 carries out the degreaser cleaning, the composition of degreaser comprises yellow soda ash 180g/L, Trisodium Citrate 50g/L, fatty alcohol-polyoxyethylene ether 5g/L, sodium phosphate 40g/L, and scavenging period is 10～15min.
4. the preparation method of a kind of Cr-Si-C-N nano-composite coating as claimed in claim 3, it is characterized in that: in vacuum drying oven, dry after the pickling described in the step 1 and the rinsed with deionized water and comprise, it is that 10% hydrochloric acid soln at room temperature cleans about 5min that concentration is adopted in pickling, washes several with deionized water subsequently; The vacuum tightness of vacuum drying oven is 300Pa, and bake out temperature is 150 ℃, and storing time was longer than 1 hour.
5. the preparation method of a kind of Cr-Si-C-N nano-composite coating as claimed in claim 4, it is characterized in that: the backwash cleaning parameters described in the step 1 is: base vacuum degree 5 * 10
-4Pa, backwash bias voltage-200V, sputter Ar air pressure 0.3Pa, backwash time 15min.
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Cited By (5)
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| CN106381471A (en) * | 2016-09-19 | 2017-02-08 | 中国科学院宁波材料技术与工程研究所 | Hardness-width-variable wear-resistant coating, and preparation method and application of wear-resistant coating |
| CN109957757A (en) * | 2019-04-04 | 2019-07-02 | 中国核动力研究设计院 | A kind of method of two-step method PVD technique preparation super thick Ti-Al-C ternary coating |
| CN110484867A (en) * | 2018-05-15 | 2019-11-22 | 蓝思科技（长沙）有限公司 | Furvous coating Logo and preparation method thereof for nonmetallic cover board |
| CN111826616A (en) * | 2020-07-23 | 2020-10-27 | 北京市辐射中心 | Nuclear fuel cladding coating and preparation method thereof |
| CN112281125A (en) * | 2020-09-29 | 2021-01-29 | 维达力实业(深圳)有限公司 | Composite metal film and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381471A (en) * | 2016-09-19 | 2017-02-08 | 中国科学院宁波材料技术与工程研究所 | Hardness-width-variable wear-resistant coating, and preparation method and application of wear-resistant coating |
| CN110484867A (en) * | 2018-05-15 | 2019-11-22 | 蓝思科技（长沙）有限公司 | Furvous coating Logo and preparation method thereof for nonmetallic cover board |
| CN110484867B (en) * | 2018-05-15 | 2021-09-21 | 蓝思科技（长沙）有限公司 | Dark black coating Logo for non-metal cover plate and preparation method thereof |
| CN109957757A (en) * | 2019-04-04 | 2019-07-02 | 中国核动力研究设计院 | A kind of method of two-step method PVD technique preparation super thick Ti-Al-C ternary coating |
| CN111826616A (en) * | 2020-07-23 | 2020-10-27 | 北京市辐射中心 | Nuclear fuel cladding coating and preparation method thereof |
| CN111826616B (en) * | 2020-07-23 | 2022-05-13 | 北京市辐射中心 | Nuclear fuel cladding coating and preparation method thereof |
| CN112281125A (en) * | 2020-09-29 | 2021-01-29 | 维达力实业(深圳)有限公司 | Composite metal film and preparation method and application thereof |
| CN112281125B (en) * | 2020-09-29 | 2022-07-12 | 维达力实业(深圳)有限公司 | Composite metal film and preparation method and application thereof |
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