CN104046940B - A kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride - Google Patents

A kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride Download PDF

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CN104046940B
CN104046940B CN201410312136.6A CN201410312136A CN104046940B CN 104046940 B CN104046940 B CN 104046940B CN 201410312136 A CN201410312136 A CN 201410312136A CN 104046940 B CN104046940 B CN 104046940B
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coating
base material
blue
titanium
deposition
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CN104046940A (en
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蒋百铃
高茂松
李洪涛
刘燕婕
施文彦
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The present invention relates to a kind of depositing decorative method of coating, particularly a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride, comprises the following steps, base material clean: base material is put into deionized water, ultrasonic wave water washing; Then base material is put into ultrasonic wave dehydrated alcohol to dewater, and dry up with warm air; Coating deposition pre-preparation: cleaned base material is positioned on the rotatable machine frame of vacuum chamber, the distance on adjustment machine frame between base material and titanium target, vacuumizes whole vacuum chamber; Substrate surface deposits blue coating: comprise titanium prime coat deposition and blue titanium nitride coating deposition.After adopting aforesaid method, the inventive method is based on the blue titanium nitride coating of differential of the arc ion plating technique depositing decorative, the inventive method preparation process is nontoxic, pollution-free, material use efficiency is high, technology stability, reproducible, and the blue coating hardness of obtained titanium nitride is high, wear-resisting, solidity to corrosion is good.

Description

A kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride
Technical field
The present invention relates to a kind of depositing decorative method of coating, particularly a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride.
Background technology
At present, ornamental industry prepares the colorful gorgeous decorative product of color mainly with means such as plating, spraying, electrophoresis, and especially the 3C digital product such as mobile phone, computer, wrist-watch accounts for the very large one piece of market of tool especially.But these conventional surface colouring technology all belongs to high pollution, high waste, highly energy-consuming Technology.Vacuum plating decoration have prepare that binding force of cladding material is good, environmental protection, the advantage such as pollution-free, passing decorative coating process aspect in replacement has some superiority.
Titanium nitride coating is first industrialization of vacuum plating decoration industry and the decorative coating of widespread use, its color is based on gold, be commonly called as " titanium " at furnishing fields, be mainly used in mobile phone, the yellow hard coating of Watchcase deposited gold, Traditional DC magnetron sputtering technique cvd nitride titanium coating is based on yellow, change nitrogen flux and also can prepare dark-brown titanium nitride coating, be in addition difficult to deposit the titanium nitride coating possessing other color again.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of method making the blue titanium nitride coating of depositing decorative that ornamental blue titanium nitride coating hardness is high, wear resistance is good.
For solving above-mentioned technical problem, a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride of the present invention, comprises the following steps:
Base material clean: base material is put into deionized water, ultrasonic wave water washing; Then base material is put into ultrasonic wave dehydrated alcohol to dewater, and dry up with warm air;
Coating deposition pre-preparation: cleaned base material is positioned on the rotatable machine frame of vacuum chamber, the distance on adjustment machine frame between base material and titanium target; Whole vacuum chamber is vacuumized;
Substrate surface deposits blue coating: comprise titanium prime coat deposition and blue titanium nitride coating deposition, adopt differential of the arc power supply supply model, described titanium prime coat is deposited as and continues to pass into argon gas in vacuum chamber, ensure vacuum chamber internal gas pressure 0.2-1Pa, machine frame rotating speed 5-50r/min, titanium target mean power 0.1-3w/cm 2, deposition 2-30min; After described blue titanium nitride coating has been deposited as titanium prime coat, in vacuum chamber, continue the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure 10-80%, vacuum chamber internal gas pressure 0.5-1Pa, titanium target mean power 0.2-4w/cm 2, deposit blue coating 30-50min.
Further, in described step base material clean, ultrasonic wave water washing 1min, dewater in ultrasonic wave dehydrated alcohol 5min.
Further, described base material is phone housing or metalwork, needs oil removal treatment, base material is put into the solution containing degreaser, ultrasonic oil removal process 7min in described step base material clean before ultrasonic wave water washing.
Further, in described coating deposition pre-preparation step, the vacuum tightness of vacuum chamber is not more than 6.0 × 10 -3pa.
Further, in described coating deposition pre-preparation step, the distance on machine frame between base material and titanium target is 60-180mm.
After adopting aforesaid method, the inventive method is based on the blue titanium nitride coating of differential of the arc ion plating technique depositing decorative, the inventive method preparation process is nontoxic, pollution-free, material use efficiency is high, technology stability, reproducible, and the blue coating hardness of obtained titanium nitride is high, wear-resisting, solidity to corrosion is good.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the schematic diagram of the blue titanium nitride coating method of depositing decorative of the present invention.
Fig. 2 is depositing decorative of the present invention blue titanium nitride coating scanning electronic microscope surface topography map.
Fig. 3 is depositing decorative of the present invention blue titanium nitride coating scanning electronic microscope Cross Section Morphology figure.
Fig. 4 is the blue titanium nitride coating XRD figure of depositing decorative of the present invention.
Embodiment
As shown in Figure 1, a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride of the present invention, comprises the following steps:
Step S1: base material clean, puts into deionized water by base material, ultrasonic wave water washing; Then base material is put into ultrasonic wave dehydrated alcohol to dewater, and dry up with warm air.
Step S2: coating deposition pre-preparation, is positioned over cleaned base material on the rotatable machine frame of vacuum chamber, the distance on adjustment machine frame between base material and titanium target; Whole vacuum chamber is vacuumized.
Step S3: substrate surface deposits blue coating, step S3 can be divided into again step S301 titanium prime coat to deposit and the blue titanium nitride coating deposition of step S302.Step S301 and step S302 adopts differential of the arc power supply supply model, under differential of the arc ion plating condition, by differential of the arc ion-plating deposition titanium nitride coating.
Wherein step S301 titanium prime coat is deposited as and continues to pass into argon gas in vacuum chamber, ensure vacuum chamber internal gas pressure, for different substrate materials adjustment machine frame rotating speed, and the distance between titanium target and machine frame is set, selected titanium target mean power and depositing time, thus titanium deposition prime coat.
After the blue titanium nitride coating of step S302 has been deposited as titanium prime coat, the mixed gas passing into argon gas and nitrogen is continued in vacuum chamber, nitrogen partial pressure ratio and vacuum chamber internal gas pressure is kept to stablize, selected titanium target mean power and the blue plating time of deposition, thus blue titanium nitride coating is deposited on titanium prime coat.
Embodiment 1
Choose phone housing as base material, on phone housing, the blue titanium nitride coating of depositing decorative comprises the following steps.
Base material clean: base material is put into the solution containing degreaser, ultrasonic oil removal process 7min, removing substrate surface greasy dirt; Again base material is put into deionized water, ultrasonic wave water washing 1min; Finally base material is put into ultrasonic wave dehydrated alcohol to dewater 5min, and dry up with warm air.
Coating deposition pre-preparation: be positioned on machine frame by cleaned base material, the distance controlled on machine frame between matrix and titanium target is 120mm.Close fire door, whole vacuum chamber is vacuumized, makes the background vacuum of vacuum chamber be not more than 6.0 × 10 -3pa.Work rest keeps 5r/min uniform rotation in coating deposition process.Titanium target be titanium content higher than 99% pure metal target, select rectangular target.
Substrate surface deposits blue coating: adopt differential of the arc power supply supply model, first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 1w/cm 2carry out the deposition of titanium prime coat, depositing time is at 10min.And ensure that gas pressure in vacuum is at 0.5Pa.
After having deposited titanium prime coat, continue at vacuum chamber the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure to be 30%, vacuum chamber operating air pressure is 1Pa, keeps titanium target mean power 0.5w/cm simultaneously 2carry out blue coating deposition, depositing time 30min.
Present embodiment prepares blue coating thickness 0.2 μm, and sedimentation rate is about 5nm/min.
Embodiment 2
Choose magnesium table embryo (Watchcase) after differential arc oxidation process, as base material, to comprise the following steps at the ornamental blue titanium nitride coating of Watchcase deposited on substrates.
Base material clean: base material is put into deionized water, ultrasonic wave water washing 1min; Again base material is put into ultrasonic wave dehydrated alcohol to dewater 5min, and dry up with warm air.
Coating deposition pre-preparation: be positioned on machine frame by cleaned base material, the distance controlled on machine frame between matrix and titanium target is 90mm.Close fire door, whole vacuum chamber is vacuumized, makes the background vacuum of vacuum chamber be not more than 6.0 × 10 -3pa.Work rest keeps 20r/min uniform rotation in coating deposition process.Titanium target be titanium content higher than 99% pure metal target, select round target.
Substrate surface deposits blue coating: employing rate differential of the arc power supply supply model, and first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 0.8w/cm 2carry out the deposition of titanium prime coat, depositing time is at 10min.And ensure that gas pressure in vacuum is at 0.3Pa.
After having deposited titanium prime coat, continue at vacuum chamber the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure to be 20%, vacuum chamber operating air pressure is 0.8Pa, keeps titanium target mean power 0.2w/cm simultaneously 2carry out blue titanium nitride coating deposition, depositing time 40min.
The implementation case prepares blue coating thickness 0.39 μm, and sedimentation rate is about 13nm/min.
Embodiment 3
Choose twist drill, gong cutter as base material, comprise the following steps at twist drill, the ornamental blue titanium nitride coating of gong cutter deposited on substrates.
Base material clean: base material is put into the solution containing degreaser, ultrasonic oil removal process 7min, removing substrate surface greasy dirt; Again base material is put into deionized water, ultrasonic wave water washing 1min; Finally base material is put into ultrasonic wave dehydrated alcohol to dewater 5min, and dry up with warm air.
Coating deposition pre-preparation: be positioned on machine frame by cleaned base material, the distance controlled on machine frame between matrix and titanium target is 180mm.Close fire door, whole vacuum chamber is vacuumized, makes the background vacuum of vacuum chamber be not more than 6.0 × 10 -3pa.Work rest keeps 10r/min uniform rotation in coating deposition process.Titanium target be titanium content higher than 99% pure metal target, select rotary target.
Substrate surface deposits blue coating: adopt superpower differential of the arc power supply supply model, first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 0.1w/cm 2carry out the deposition of titanium prime coat, depositing time is at 30min.And ensure that gas pressure in vacuum is at 0.2Pa.
After having deposited prime coat, continue at vacuum chamber the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure to be 10%, vacuum chamber operating air pressure is 0.5Pa, keeps titanium target mean power 2.5w/cm simultaneously 2carry out blue titanium nitride coating deposition, depositing time 50min.
The implementation case prepares blue coating thickness 0.98 μm, and sedimentation rate is about 15.1nm/min.
Embodiment 4
Choosing sheet glass is base material, and on sheet glass base material, the blue titanium nitride coating of depositing decorative comprises the following steps.
Base material clean: base material is put into deionized water, ultrasonic wave water washing 1min; Again base material is put into ultrasonic wave dehydrated alcohol to dewater 5min, and dry up with warm air.
Coating deposition pre-preparation: be positioned on machine frame by cleaned base material, the distance controlled on machine frame between matrix and titanium target is 60mm.Close fire door, whole vacuum chamber is vacuumized, makes the background vacuum of vacuum chamber be not more than 6.0 × 10 -3pa.Work rest protects 50r/min uniform rotation in coating deposition process.Titanium target be titanium content higher than 99% pure metal target, select round target.
Substrate surface deposits blue coating: adopt differential of the arc power supply supply model, first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 1.5w/cm 2carry out the deposition of titanium prime coat, depositing time is at 2min.And ensure that gas pressure in vacuum is at 0.9Pa.
After having deposited prime coat, continue at vacuum chamber the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure to be 40%, vacuum chamber operating air pressure is 0.5Pa, keeps titanium target mean power 1.7W/cm simultaneously 2carry out blue coating deposition, depositing time 40min.
The implementation case prepares blue coating thickness 0.51 μm, and sedimentation rate is about 8.5nm/min.
Embodiment 5
Choosing high-speed steel is base material, comprises the following steps at the ornamental blue titanium nitride coating of high-speed steel deposited on substrates.
Base material clean: base material is put into the solution containing degreaser, ultrasonic oil removal process 7min, goes out substrate surface greasy dirt; Again base material is put into deionized water, ultrasonic wave water washing 1min; Finally base material is put into ultrasonic wave dehydrated alcohol to dewater 5min, and dry up with warm air.
Coating deposition pre-preparation: be positioned on machine frame by base material cleaned before step 1, the distance controlled on machine frame between matrix and titanium target is 120mm.Close fire door, whole vacuum chamber is vacuumized, makes the background vacuum of vacuum chamber be not more than 6.0 × 10 -3pa.Work rest keeps 10r/min uniform rotation in coating deposition process.Titanium target be titanium content higher than 99% high pure metal target, select round target.
Substrate surface deposits blue coating: adopt differential of the arc power supply supply model, first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 3W/cm 2carry out the deposition of titanium prime coat, depositing time is at 10min.And ensure that gas pressure in vacuum is at 1Pa.
After having deposited prime coat, continue at vacuum chamber the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure to be 80%, vacuum chamber operating air pressure is 1Pa, keeps titanium target mean power 4W/cm simultaneously 2carry out blue coating deposition, depositing time 30min.
The implementation case prepares blue coating thickness 0.302 μm, and sedimentation rate is about 7.6nm/min.
As shown in Figure 2, Figure 3 and Figure 4, in Fig. 2, blue titanium nitride coating surface has just started to occur prismatic, has crystallization, and Fig. 3 coating tee section pattern is fine and close, does not see the defects such as hole, and film is combined well with matrix simultaneously.Fig. 4 is the XRD figure spectrum of blue coating, and the obvious broadening of this blue coating diffraction peak as seen from the figure, illustrate that this coating degree of crystallization is lower, prismatic appears in this and Fig. 2 surface, and it is consistent that coating starts crystallization result.It is sharply symmetrical that conventional nitridation titan yellow look coating has diffraction peak usually, and intensity is high, and coating degree of crystallization is high, completely contrary with blue titanium nitride coating.
Certainly, titanium target of the present invention also can select other shapes be suitable for, and such conversion all drops within protection scope of the present invention.
Although the foregoing describe the specific embodiment of the present invention; but those skilled in the art are to be understood that; these only illustrate; various changes or modifications can be made to present embodiment; and not deviating from principle of the present invention and essence, protection scope of the present invention is only defined by the appended claims.

Claims (5)

1. adopt a method for the blue coating of differential of the arc ion-plating deposition titanium nitride, it is characterized in that, comprise the following steps:
Base material clean: base material is put into deionized water, ultrasonic wave water washing; Then base material is put into ultrasonic wave dehydrated alcohol to dewater, and dry up with warm air;
Coating deposition pre-preparation: cleaned base material is positioned on the rotatable machine frame of vacuum chamber, the distance on adjustment machine frame between base material and titanium target, vacuumizes whole vacuum chamber;
Substrate surface deposits blue coating: comprise titanium prime coat deposition and blue titanium nitride coating deposition, adopt differential of the arc power supply supply model, described titanium prime coat is deposited as and continues to pass into argon gas in vacuum chamber, ensure vacuum chamber internal gas pressure 0.2-1Pa, machine frame rotating speed 5-50r/min, titanium target mean power 0.1-3w/cm 2, deposition 2-30min; After described blue titanium nitride coating has been deposited as titanium prime coat, in vacuum chamber, continue the mixed gas passing into argon gas and nitrogen, keep nitrogen partial pressure 10-80%, vacuum chamber internal gas pressure 0.5-1Pa, titanium target mean power 0.2-4w/cm 2, deposit blue coating 30-50min.
2., according to a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride according to claim 1, it is characterized in that: in described step base material clean, ultrasonic wave water washing 1min, dewater in ultrasonic wave dehydrated alcohol 5min.
3. according to a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride according to claim 2, it is characterized in that: described base material is phone housing or metalwork, oil removal treatment is needed before ultrasonic wave water washing in described step base material clean, base material is put into the solution containing degreaser, ultrasonic oil removal process 7min.
4. according to a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride according to claim 1, it is characterized in that: in described coating deposition pre-preparation step, the vacuum tightness of vacuum chamber is not more than 6.0 × 10 -3pa.
5. according to a kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride according to claim 1, it is characterized in that: in described coating deposition pre-preparation step, the distance on machine frame between base material and titanium target is 60-180mm.
CN201410312136.6A 2014-07-02 2014-07-02 A kind of method adopting the blue coating of differential of the arc ion-plating deposition titanium nitride Expired - Fee Related CN104046940B (en)

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CN104746072B (en) * 2015-03-30 2017-06-13 创金美科技(深圳)有限公司 A kind of magnesium alloy differential arc ion plating surface treatment method
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CN102230153A (en) * 2011-06-22 2011-11-02 西安理工大学 Method for self-lubricating steel balls for precision bearing by ion-plating GLC (graphite-like carbon) coating
CN103397304A (en) * 2013-08-21 2013-11-20 南京浩穰环保科技有限公司 Micro-arc ion plating method

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CN102230153A (en) * 2011-06-22 2011-11-02 西安理工大学 Method for self-lubricating steel balls for precision bearing by ion-plating GLC (graphite-like carbon) coating
CN103397304A (en) * 2013-08-21 2013-11-20 南京浩穰环保科技有限公司 Micro-arc ion plating method

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