CN104046940A - Method for depositing blue titanium nitride plating layer by using micro-arc ion plating - Google Patents
Method for depositing blue titanium nitride plating layer by using micro-arc ion plating Download PDFInfo
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- CN104046940A CN104046940A CN201410312136.6A CN201410312136A CN104046940A CN 104046940 A CN104046940 A CN 104046940A CN 201410312136 A CN201410312136 A CN 201410312136A CN 104046940 A CN104046940 A CN 104046940A
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Abstract
The invention relates to a method for depositing a decorative plating layer and particularly relates to a method for depositing a blue titanium nitride plating layer by using micro-arc ion plating. The method comprises the following steps of substrate cleaning treatment: placing a substrate into deionized water, carrying out ultrasonic washing, then, placing the substrate into ultrasonic absolute ethyl alcohol to dehydrate, and drying by using hot air through blowing; plating layer deposition prepreparation: placing the cleaned substrate on a rotatable tool rack in a vacuum chamber, regulating the distance from the substrate on the tool rack to a titanium target, and vacuumizing the whole vacuum chamber; blue plating layer deposition on the surface of the substrate: depositing a titanium base layer and depositing the blue titanium nitride plating layer. The method provided by the invention is used for depositing the decorative blue titanium nitride plating layer on the basis of a micro-arc ion plating technology. The method is nontoxic and pollution-free in the preparation process, high in material utilization rate and good in process stability and repeatability; in addition, the prepared blue titanium nitride plating layer is high in hardness and good in wear and corrosion resistance.
Description
Technical field
The present invention relates to a kind of deposition decorative coating method, particularly a kind of method that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride.
Background technology
At present, ornamental industry is prepared 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 market of tool especially.But these conventional surface colouring technology all belong to high pollution, high waste, highly energy-consuming Technology.Vacuum plating decorate have that the binding force of cladding material of preparation is good, environmental protection, the advantage such as pollution-free, pass decorative coating process aspect and have some superiority replacing.
Titanium nitride coating is the decorative coating of first industrialization of vacuum plating decoration industry widespread use, its color be take gold as main, in decoration field, be commonly called as " titanium ", be mainly used in mobile phone, the yellow hard coating of Watchcase deposited gold, tradition magnetically controlled DC sputtering deposition techniques titanium nitride coating be take yellow as main, change nitrogen flux and also can prepare dark-brown titanium nitride coating, be in addition difficult to deposit again the titanium nitride coating that possesses other color.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of method that makes the ornamental blue titanium nitride coating of deposition that ornamental blue titanium nitride coating hardness is high, wear resistance is good.
For solving above-mentioned technical problem, a kind of method that adopts 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 and dewatered, and dry up with warm air;
Coating deposition pre-preparation: cleaned base material is positioned on the rotatable machine frame of vacuum chamber to 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 in vacuum chamber, continues to pass into argon gas, guarantee 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; Described blue titanium nitride coating has been deposited as after titanium prime coat, continues to pass into the mixed gas of argon gas and nitrogen in vacuum chamber, keeps 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, 5min dewaters in ultrasonic wave dehydrated alcohol.
Further, described base material is phone housing or metalwork, in described step base material clean, before ultrasonic wave water washing, needs oil removal treatment, base material is put into the solution that contains degreaser, ultrasonic wave oil removal treatment 7min.
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.
Adopt after aforesaid method, the inventive method is based on the ornamental blue titanium nitride coating of differential of the arc ion plating technique deposition, the inventive method preparation process is nontoxic, pollution-free, material use efficiency is high, technology stability, reproducible, and makes that the blue coating hardness of 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 that the present invention deposits ornamental blue titanium nitride coating method.
Fig. 2 is that the present invention deposits ornamental blue titanium nitride coating scanning electronic microscope surface topography map.
Fig. 3 is that the present invention deposits ornamental blue titanium nitride coating scanning electronic microscope Cross Section Morphology figure.
Fig. 4 is that the present invention deposits ornamental blue titanium nitride coating XRD figure.
Embodiment
As shown in Figure 1, a kind of method that adopts 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, base material is put into deionized water, ultrasonic wave water washing; Then base material is put into ultrasonic wave dehydrated alcohol and dewatered, 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 deposition and the blue titanium nitride coating deposition of step S302.Step S301 and step S302 adopt 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 in vacuum chamber, continues to pass into argon gas, guarantee vacuum chamber internal gas pressure, for different substrate materials, adjust machine frame rotating speed, and the distance between titanium target and machine frame is set, selected titanium target mean power and depositing time, thereby titanium deposition prime coat.
The blue titanium nitride coating of step S302 has been deposited as after titanium prime coat, in vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keep nitrogen partial pressure ratio and vacuum chamber internal gas pressure stable, selected titanium target mean power and blue coating time of deposition, thus on titanium prime coat, deposit blue titanium nitride coating.
Embodiment 1
Choose phone housing as base material, on phone housing, deposit ornamental blue titanium nitride coating and comprise the following steps.
Base material clean: base material is put into the solution that contains degreaser, ultrasonic wave oil removal treatment 7min, removes substrate surface greasy dirt; Again base material is put into deionized water, ultrasonic wave water washing 1min; Finally base material is put into the ultrasonic wave dehydrated alcohol 5min that dewaters, and dried up with warm air.
Coating deposition pre-preparation: cleaned base material is positioned on machine frame, and the distance on control machine frame between matrix and titanium target is 120mm.Close fire door, whole vacuum chamber is vacuumized, make the base vacuum degree 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
2the deposition of carrying out titanium prime coat, depositing time is at 10min.And guarantee that gas pressure in vacuum is at 0.5Pa.
After having deposited titanium prime coat, at vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keeping nitrogen partial pressure is 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 is prepared blue coating thickness 0.2 μ m, and sedimentation rate is about 5nm/min.
Embodiment 2
Choose magnesium table embryo (Watchcase) after differential arc oxidation is processed, as base material, deposits ornamental blue titanium nitride coating and comprises the following steps on Watchcase base material.
Base material clean: base material is put into deionized water, ultrasonic wave water washing 1min; Again base material is put into the ultrasonic wave dehydrated alcohol 5min that dewaters, and dried up with warm air.
Coating deposition pre-preparation: cleaned base material is positioned on machine frame, and the distance on control machine frame between matrix and titanium target is 90mm.Close fire door, whole vacuum chamber is vacuumized, make the base vacuum degree 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, first titanium deposition prime coat, continues to pass into argon gas at vacuum chamber, keeps titanium target mean power 0.8w/cm
2the deposition of carrying out titanium prime coat, depositing time is at 10min.And guarantee that gas pressure in vacuum is at 0.3Pa.
After having deposited titanium prime coat, at vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keeping nitrogen partial pressure is 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 is prepared blue coating thickness 0.39 μ m, and sedimentation rate is about 13nm/min.
Embodiment 3
Choose twist drill, gong cutter as base material, on twist drill, gong cutter base material, deposit ornamental blue titanium nitride coating and comprise the following steps.
Base material clean: base material is put into the solution that contains degreaser, ultrasonic wave oil removal treatment 7min, removes substrate surface greasy dirt; Again base material is put into deionized water, ultrasonic wave water washing 1min; Finally base material is put into the ultrasonic wave dehydrated alcohol 5min that dewaters, and dried up with warm air.
Coating deposition pre-preparation: cleaned base material is positioned on machine frame, and the distance on control machine frame between matrix and titanium target is 180mm.Close fire door, whole vacuum chamber is vacuumized, make the base vacuum degree 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
2the deposition of carrying out titanium prime coat, depositing time is at 30min.And guarantee that gas pressure in vacuum is at 0.2Pa.
After having deposited prime coat, at vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keeping nitrogen partial pressure is 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 is prepared blue coating thickness 0.98 μ m, and sedimentation rate is about 15.1nm/min.
Embodiment 4
Choosing sheet glass is base material, deposits ornamental blue titanium nitride coating and comprise the following steps on sheet glass base material.
Base material clean: base material is put into deionized water, ultrasonic wave water washing 1min; Again base material is put into the ultrasonic wave dehydrated alcohol 5min that dewaters, and dried up with warm air.
Coating deposition pre-preparation: cleaned base material is positioned on machine frame, and the distance on control machine frame between matrix and titanium target is 60mm.Close fire door, whole vacuum chamber is vacuumized, make the base vacuum degree of vacuum chamber be not more than 6.0 * 10
-3pa.Work rest is protected 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
2the deposition of carrying out titanium prime coat, depositing time is at 2min.And guarantee that gas pressure in vacuum is at 0.9Pa.
After having deposited prime coat, at vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keeping nitrogen partial pressure is 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 is prepared blue coating thickness 0.51 μ m, the about 8.5nm/min of sedimentation rate.
Embodiment 5
Choosing high-speed steel is base material, deposits ornamental blue titanium nitride coating and comprise the following steps on high-speed steel base material.
Base material clean: base material is put into the solution that contains degreaser, ultrasonic wave oil removal treatment 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 the ultrasonic wave dehydrated alcohol 5min that dewaters, and dried up with warm air.
Coating deposition pre-preparation: the front cleaned base material of step 1 is positioned on machine frame, and the distance on control machine frame between matrix and titanium target is 120mm.Close fire door, whole vacuum chamber is vacuumized, make the base vacuum degree 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
2the deposition of carrying out titanium prime coat, depositing time is at 10min.And guarantee that gas pressure in vacuum is at 1Pa.
After having deposited prime coat, at vacuum chamber, continue to pass into the mixed gas of argon gas and nitrogen, keeping nitrogen partial pressure is 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 is prepared blue coating thickness 0.302 μ m, 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 blueness coating diffraction peak, illustrates that this coating degree of crystallization is lower as seen from the figure, and prismatic appears in this and Fig. 2 surface, and it is consistent that coating starts crystallization result.It is sharply symmetrical that the yellow coating of tradition titanium nitride has diffraction peak conventionally, 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 be selected other applicable shapes, within such conversion all drops on protection scope of the present invention.
Although more than described the specific embodiment of the present invention; but those skilled in the art are to be understood that; these only illustrate; can make various changes or modifications to present embodiment; and not deviating from principle of the present invention and essence, protection scope of the present invention is only limited by appended claims.
Claims (5)
1. a method that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride, is characterized in that, 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 and dewatered, 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 in vacuum chamber, continues to pass into argon gas, guarantee 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; Described blue titanium nitride coating has been deposited as after titanium prime coat, continues to pass into the mixed gas of argon gas and nitrogen in vacuum chamber, keeps 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 that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride claimed in claim 1, it is characterized in that: in described step base material clean, ultrasonic wave water washing 1min, 5min dewaters in ultrasonic wave dehydrated alcohol.
3. according to a kind of method that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride claimed in claim 2, it is characterized in that: described base material is phone housing or metalwork, in described step base material clean, before ultrasonic wave water washing, need oil removal treatment, base material is put into the solution that contains degreaser, ultrasonic wave oil removal treatment 7min.
4. according to a kind of method that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride claimed in 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 that adopts the blue coating of differential of the arc ion-plating deposition titanium nitride claimed in 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.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104746072A (en) * | 2015-03-30 | 2015-07-01 | 创金美科技(深圳)有限公司 | Magnesium alloy microarc ion plating surface treatment method |
CN112144012A (en) * | 2019-06-28 | 2020-12-29 | 陕西航天时代导航设备有限公司 | Process method for depositing TiN thick film on inner surface of GT35 ball bowl part |
Citations (3)
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US20020104756A1 (en) * | 2001-01-26 | 2002-08-08 | Seiko Epson Corporation | Sputtering apparatus |
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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2014
- 2014-07-02 CN CN201410312136.6A patent/CN104046940B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020104756A1 (en) * | 2001-01-26 | 2002-08-08 | Seiko Epson Corporation | Sputtering apparatus |
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 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104746072A (en) * | 2015-03-30 | 2015-07-01 | 创金美科技(深圳)有限公司 | Magnesium alloy microarc ion plating surface treatment method |
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 |
CN112144012A (en) * | 2019-06-28 | 2020-12-29 | 陕西航天时代导航设备有限公司 | Process method for depositing TiN thick film on inner surface of GT35 ball bowl part |
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