CN103233227B - Preparation method of composite ceramic layer with conductive property - Google Patents
Preparation method of composite ceramic layer with conductive property Download PDFInfo
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- CN103233227B CN103233227B CN201310181678.XA CN201310181678A CN103233227B CN 103233227 B CN103233227 B CN 103233227B CN 201310181678 A CN201310181678 A CN 201310181678A CN 103233227 B CN103233227 B CN 103233227B
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Abstract
The invention discloses a preparation method of a composite ceramic layer with conductive property. The preparation method comprises the following steps: preprocessing the surface of a light-metal (Al, Mg and Ti) test sample by cleaning; preparing a ceramic layer by micro-arc oxidation technology; and depositing a titanium nitride coating on the ceramic layer by magnetron sputtering to form a composite ceramic layer containing a light-metal substrate, the ceramic layer and the titanium nitride coating. The composite ceramic layer prepared by micro-arc oxidation and magnetron sputtering has conductive property, has the advantages of high conductivity, high resistance to abrasion and corrosion, and strong film-base bonding force, and can meet the requirement that the existing light metal serving as a circuit wiring box not only has abrasive resistance, corrosion resistance but also has conductivity.
Description
Technical field
The invention belongs to light metal surface technical field of modification, particularly a kind of preparation method with the composite ceramic layer of conductivity.
Background technology
Differential arc oxidization technique is a kind of process for treating surface of rising in recent years, it breaches the restriction of conventional anodization technical work voltage, work area is incorporated into high voltage discharge field, utilizes the instantaneous high-temperature nodulizing of differential of the arc district directly at light metal or its alloy surface in-situ preparation ceramic layer.Improve the performance such as anti-corrosion, wear-resisting, high temperature resistant of matrix this technology effective, but there is the defects such as surface insulation, cause the terminal box of some light metal materials, should wear resistance electroconductibility and being restricted again.
Publication number CN102220027A " a kind of grapheme/electroconductive polymer composite and preparation method thereof " adopts the Graphene that can conduct electricity to be electro-conductive material preparation conduction compound coating, but its intensity is low, and easy loss, easily comes off.Publication number CN102222565A " carbon-based composite electrode material and preparation method thereof and the application in ultracapacitor " adopts plain steel to be that compound coating prepared by electro-conductive material, but its corrosive nature is low, and power consumption is large.
Titanium nitride is a kind of novel multi-function metal stupalith, and its fusing point is high, hardness is large, frictional coefficient is little, is the good conductor of heat and electricity.Literature research shows to adopt the particle diameter of magnetron sputtering titanium-nitride between 100-175nm, and the particle diameter of electroless plating titanium nitride is between 80-200nm, and composite ceramic layer surface particles is relatively discrete and electroconductibility is low.
If at light metal (Al, Mg, Ti) surface directly magnetron sputtering titanium-nitride, because titanium nitride is too hard, base material is too soft, then conductive coating easily comes off.
Summary of the invention
The object of the invention is should have wear resistance, solidity to corrosion to solve some light metal product surfaces at present, there is the requirement of electroconductibility again, and provide a kind of preparation method with the composite ceramic layer of conductivity.
The present invention adopts differential arc oxidization technique to prepare one deck ceramic layer at light metal surface, ceramic layer adopts magnetron sputtering technique Coating of TiN Film, form the composite ceramic layer of light metal matrix and ceramic layer and titanium nitride coating, and make it have conducting function, and electric conductivity is large, wear resistance and solidity to corrosion is good, film-substrate cohesion strong, coating difficult drop-off.
The technical scheme realizing the object of the invention is: a kind of composite ceramics Rotating fields with conductivity, be that light metal (AL, Mg, Ti) substrate surface is provided with arc differential oxide ceramic layer, arc differential oxide ceramic layer adopt magnetron sputtering technique deposit titanium nitride coating.
There is a preparation method for the composite ceramic layer of conductivity, comprise the steps: (1) by base material through cold work, cut sample thereon; (2) pre-treatment is carried out to the specimen surface cut: sand papering → tap water cleaning → acetone cleaning → washed with de-ionized water → dry up; (3) be placed in micro-arc oxidation device and carry out differential arc oxidation process, prepare one deck ceramic layer; (4) sample after differential arc oxidation is carried out ultrasonic cleaning; (5) Coating of TiN Film in magnetic control sputtering device, realizes composite ceramic layer and has conductivity; (6) cleaning is also dry, obtains the composite ceramic layer with conductivity.
Differential arc oxidation described in step (3) is placed as constant current and powers, and the power supply of use is MAO-65D type, and electrolyzer is diameter is 200mm, and the degree of depth is 300mm plastic tank, and solution maximum volume is 5L, and adopt 1 piece of stainless steel plate to do negative electrode, test specimen is anode.Adopt the method process 15 ~ 100min of constant current, the thickness of film is 30 ~ 100 μm.Concentration of electrolyte and electrical parameter range are: sodium metaaluminate 10 ~ 20g/L, sodium hydroxide 0.5 ~ 4g/L, Sodium hexametaphosphate 99 5 ~ 18g/L, and current density is 8 ~ 25A/dm2, frequency 200 ~ 700HZ, and positive negative pulse stuffing number is 5: 2, and dutycycle is 5 ~ 40%.
The processing parameter of the magnetron sputtering described in step (5) is: vacuum tightness is 10-5 ~ 10-4Pa, passes into argon gas to 1 ~ 35 Pa, with bias voltage cleaning ceramic layer 10 ~ 50 min of-500 ~-1500V; Depositing temperature: room temperature ~ 400 DEG C, deposition pressure is 0. 5 ~ 10Pa, and substrate bias is-100 ~-300V, and depositing time is 20 ~ 90min.
Beneficial effect of the present invention: adopt differential arc oxidization technique to prepare one deck ceramic layer at light metal surface, ceramic layer adopts magnetron sputtering technique Coating of TiN Film, achieves the conductivity of arc differential oxide ceramic layer; Solve some light metal product surfaces and should have wear resistance, solidity to corrosion, there is the requirement of electroconductibility again; And the composite ceramic layer of preparation has that electric conductivity is large, wear resistance and solidity to corrosion is good, film-substrate cohesion strong, the feature of compound coating difficult drop-off.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation with the composite ceramic layer of conductivity;
In figure, 1. light metal base material 2. arc differential oxide ceramic layer 3. nitride coatings;
Fig. 2 is the surface topography map that embodiment 1 has the composite ceramic layer of conductivity.
Embodiment
Below by embodiment, content of the present invention is further elaborated, but is not limitation of the invention.
With reference to Fig. 1, a kind of composite ceramics Rotating fields with conductivity, is that light metal (AL, Mg, Ti) base material 1 surface is provided with arc differential oxide ceramic layer 2, arc differential oxide ceramic layer 2 is provided with magnetron sputtering deposition nitride coatings 3.
Starting material are that the sheet material of 7075 type aluminium alloys is through cold work by embodiment 1, the test specimen being of a size of 30mm × 20mm × 3mm is cut with Linear cut, use 400# successively, 600#, 800# waterproof abrasive paper is polished, through clear water, acetone, washed with de-ionized water 20min, taking-up dries up.
Test specimen is put into the micro-arc oxidation device of 65kw, solution formula is: sodium metaaluminate 10g/L, sodium hydroxide 2g/L, Sodium hexametaphosphate 99 15g/L, concrete electrical parameter is current density 12A/dm2, frequency 500HZ, positive negative pulse stuffing number is 5:2, dutycycle is 16%, adopts constant current oxidation 60min, adopts washed with de-ionized water, dries up after oxidation.Totally and dry, put into TSU-650 magnetron sputtering equipment Coating of TiN Film, equipment vacuum degree is evacuated to 10-4Pa to the sample ultrasonic cleaning obtained by differential arc oxidation, passes into argon gas to 6Pa, with the bias voltage washed samples 20min of-700V; After cleaning, depositing temperature rises to 300 DEG C, deposition pressure 0.8 Pa, bias voltage-200 V, and the working hour is 60 min, target arc current 70A, argon oxide gas ratio 1:8, and furnace cooling after terminating, specimen surface can obtain the titanium nitride coating of surface compact.
After completing sputtering plating, taken out by test specimen, cleaning is also dry, and just obtain the composite ceramic layer with conductivity, thickness is 55 μm.
Even with its tight zone pattern of transmission electron microscope observation, space is obviously reduced; Be 178GPa with resistance strain-ga(u)ge measurement Young's modulus, far above the independent test specimen through differential arc oxidation process; Composite ceramic layer electric conductivity obtained is after testing 70%.
Embodiment 2 material for test is AZ80 magnesium alloy, is of a size of 20mm × 20mm × 2mm.Preparation technology is identical with embodiment 1.Obtained composite ceramics layer thickness is 80 μm, and electric conductivity is 85%.
Embodiment 3 sample material is TC4 titanium alloy, is of a size of 20mm × 20mm × 2mm.Preparation technology is identical with embodiment 1.Obtained composite ceramics layer thickness is 92 μm, and electric conductivity is 92%.
Claims (1)
1. there is a preparation method for the composite ceramic layer of conductivity, it is characterized in that: comprise the following steps:
(1) by base material through cold work, cut sample thereon;
(2) pre-treatment is carried out to the specimen surface cut: sand papering → tap water cleaning → acetone cleaning → washed with de-ionized water → dry up;
(3) be placed in micro-arc oxidation device and carry out differential arc oxidation process, prepare one deck ceramic layer;
Described micro-arc oxidation device is that constant current is powered, and adopt the method process 15 ~ 100min of constant current, the thickness of film is 30 ~ 100 μm; Concentration of electrolyte and electrical parameter range are: sodium metaaluminate 10 ~ 20g/L, sodium hydroxide 0.5 ~ 4g/L, Sodium hexametaphosphate 99 5 ~ 18g/L, and current density is 8 ~ 25A/dm
2, frequency 200 ~ 700HZ, positive negative pulse stuffing number is 5: 2, and dutycycle is 5 ~ 40%;
(4) sample after differential arc oxidation is carried out ultrasonic cleaning;
(5) Coating of TiN Film in magnetic control sputtering device, realizes composite ceramic layer and has conductivity;
The processing parameter of magnetron sputtering is: vacuum tightness is 10
-5~ 10
-4pa, passes into argon gas to 1 ~ 35 Pa, with bias voltage cleaning ceramic layer 10 ~ 50 min of-500 ~-1500V; Depositing temperature: room temperature ~ 400 DEG C, deposition pressure is 0.5 ~ 10Pa, and substrate bias is-100 ~-300V, and depositing time is 20 ~ 90min;
(6) cleaning is also dry, obtains the composite ceramic layer with conductivity.
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| CN201310181678.XA CN103233227B (en) | 2013-05-16 | 2013-05-16 | Preparation method of composite ceramic layer with conductive property |
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| CN201310181678.XA CN103233227B (en) | 2013-05-16 | 2013-05-16 | Preparation method of composite ceramic layer with conductive property |
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| CN103233227B true CN103233227B (en) | 2015-06-03 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104418595B (en) * | 2013-08-22 | 2016-12-28 | 宁波江丰电子材料股份有限公司 | A kind of manufacture method of Sialon ceramics target |
| CN104195569B (en) * | 2014-08-21 | 2016-08-17 | 中国电子科技集团公司第三十八研究所 | A kind of magnesium alloy microwave components lid surface compounding method |
| CN104879109B (en) * | 2015-04-22 | 2018-08-14 | 中国石油天然气股份有限公司 | Decomposable asymmetric choice net pressure break ball holder surface composite film and ball seat and ball seat preparation method |
| CN104805438B (en) * | 2015-04-22 | 2017-10-27 | 中国石油天然气股份有限公司 | Decomposable asymmetric choice net pressure break ball holder surface wear-resistance film layer and ball seat and ball seat preparation method |
| CN105040071B (en) * | 2015-07-03 | 2017-08-22 | 中国兵器科学研究院宁波分院 | Surface treatment method of Mg alloy |
| CN108118380A (en) * | 2017-11-27 | 2018-06-05 | 贵州理工学院 | A kind of preparation method of high compactness corrosion-proof wear magnesium alloy differential arc oxidation film |
| CN108624882B (en) * | 2018-05-18 | 2019-12-27 | 天津师范大学 | Zirconium oxide/chromium nitride composite film on surface of zirconium alloy and preparation method and application thereof |
| CN111647925A (en) * | 2020-07-02 | 2020-09-11 | 广西大学 | Micro-arc oxidation antifriction composite coating on aluminum alloy surface and preparation method thereof |
| CN112226768B (en) * | 2020-10-13 | 2022-09-23 | 辽宁科技大学 | Composite preparation method of micro-arc oxidation CrAlN coating |
| CN112064037A (en) * | 2020-10-13 | 2020-12-11 | 贵州电网有限责任公司 | Preparation method of corrosion-resistant magnesium alloy sacrificial anode |
| CN113416955A (en) * | 2021-06-25 | 2021-09-21 | 浙江天力机车部件有限公司 | Titanium alloy fastener anodic oxidation and magnetron sputtering surface composite treatment method |
| CN114737162A (en) * | 2022-04-08 | 2022-07-12 | 西安热工研究院有限公司 | Non-stoichiometric TiNxNano coating, preparation method and application thereof |
| CN114990482A (en) * | 2022-06-15 | 2022-09-02 | 西安热工研究院有限公司 | Ti-doped TiN conductive coating and preparation method thereof |
| CN115852367A (en) * | 2022-12-06 | 2023-03-28 | 西北有色金属研究院 | Method for preparing high-corrosion-resistance conductive composite coating on surface of magnesium alloy |
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| CN102634796A (en) * | 2012-04-28 | 2012-08-15 | 桂林电子科技大学 | Preparation method of composite ceramic layer with antibacterial properties |
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