CN104513960A - Method for preparing color titanium nitride film through magnetron sputtering - Google Patents
Method for preparing color titanium nitride film through magnetron sputtering Download PDFInfo
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- CN104513960A CN104513960A CN201310459978.XA CN201310459978A CN104513960A CN 104513960 A CN104513960 A CN 104513960A CN 201310459978 A CN201310459978 A CN 201310459978A CN 104513960 A CN104513960 A CN 104513960A
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- film
- plated film
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- color
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Physical Vapour Deposition (AREA)
Abstract
The present invention provides a method for preparing a color titanium nitride film through magnetron sputtering. According to the present invention, according to important influence of the nitrogen gas flow rate on the film layer color during a film plating process, the nitrogen gas flow rate is adjusted, such that the titanium nitride film layer color is effectively changed, and the color film layer with multiple color effects and the decoration effect are obtained; and with the method of the present invention, a variety of the film layer effects required by production decorations can be obtained, and good application effects and economic benefits are provided.
Description
Technical field
The invention belongs to physical vapor deposition surface decoration coating film treatment technical field.Relate to colored titanium nitride film preparation method.It is more particularly a kind of method utilizing magnetically controlled DC sputtering technology to prepare titanium nitride film.
Background technology
Colored titanium nitride film also has broad application prospects in decoration plating industry, and in occupation of consequence, this is because not only have good wear resistance and solidity to corrosion, and being generally golden yellow, is desirable imitation gold decorative film.Usually adopt arc ion plating mode to be coated on as imitating gold decorating on metallic matrix using colored titanium nitride film at present, existing Partial coatings processing parameter is on the report affecting aspect of coating color.But form macrobead because splash usual when high-temperature electric arc burns to target goes out drop at coating surface in arc ion plating membrane process to pollute, affect color and luster and surface smoothness to a certain extent, in addition, during plated film, substrate temperature is higher, limits colored titanium nitride film for decorating the range of application of plating
Magnetron sputtering is emerging a kind of film coating method, and compared with plating with electric arc, the method depositing temperature is low, and the film surface obtained is smooth, is well suited for decoration film coating.But, with magnetically controlled sputter method, colored titanium nitride film is applied to the research also rarely seen report of decoration industry.
Summary of the invention
In order to meet the market requirement of the polychromy plated film day by day strengthened, the present invention has investigated the impact of nitrogen flow on the colored titanium nitride film color and luster of reaction magnetocontrol sputtering, is intended to by means of only changing one of processing parameter i.e. nitrogen flow to obtain rete color and luster required in production reality.
For achieving the above object, the invention provides following technical scheme:
Utilize magnetically controlled DC sputtering technology to prepare a method for colored titanium nitride membrane, it is characterized in that entering by following step
1) employing makes matrix through polishing, ganoid high speed steel or stainless steel;
2) matrix is immersed ultrasonic action 10-20 minute in the ethanolic soln of 95%, then use acetone soln dipping bath, dry with blower;
3) specimen mounting then matrix being fixed on vacuum deposition chamber carries out plated film, and before plated film, back end vacuum is evacuated to 3 × 10
-3pa, and effects on surface carries out icon bombardment cleaning 3-50min; Distance between matrix and sputtering target is 150mm, not biasing.
4) keep sputtering power to be 200W during plated film, to be coated with the titanium nitride thin membrane sample of different colours under different nitrogen flow (deposition pressure), the nitrogen flow used is controlled by under meter, be respectively 0.59,0.84,1.99,2.21,2.37sccm, corresponding deposition pressure is respectively 0.11,0.16,0.36,0.39,0.42Pa.Depositing time is 20min.Operating air pressure is respectively between 0.11-0.42Pa.
5) observed by the surface topography of scanning electronic microscope to sample; Colourimeter is utilized to measure the colourity of film surface.
The more detailed preparation method of the present invention is as follows
1, experimental technique
Rich sharp permanent MP-3P type ion film coating machine utilize DC magnetron sputtering method to prepare colored titanium nitride membrane sample.Specimen size 15mm × 10mm × 10mm, body material is high speed steel or stainless steel, respectively with sand papering from coarse to fine, then polishing, until surface presentation minute surface.
Sample to be immersed in spirituous solution ultrasonic action 20 minutes, then use acetone soln dipping bath, dry with blower.Then specimen mounting matrix sample being fixed on vacuum deposition chamber carries out plated film.Before plated film, back end vacuum is evacuated to 3 × 10
-3pa, and effects on surface carries out icon bombardment cleaning 3-5min.
Under different nitrogen flow, be coated with different film samples, in coating process, all the other parameters are substantially constant.
Coating process parameter is in table 1.
| Sample number into spectrum | Nitrogen flow | Deposition pressure | Sputtering power | Bias voltage | Depositing time |
| 1 | 0.59sccm | 0.11Pa | 400W | 0V | 20min |
| 2 | 0.84sccm | 0.16Pa | 400W | 0V | 20min |
| 3 | 1.99sccm | 0.36Pa | 400W | 0V | 20min |
| 4 | 2.21sccm | 0.39Pa | 400W | 0V | 20min |
| 5 | 2.37sccm | 0.42Pa | 400W | 0V | 20min |
Observed by the surface topography of scanning electronic microscope to sample.Colourimeter is utilized to determine the colourity of film surface.
Result and discussion
Surface topography
The surface topography that each film sample is observed under 1000 times of magnifications by scanning electronic microscope.Can find out that the nitrogenize titanizing film surface quality of sputtering sedimentation is good, smooth, fine and close, exist without obvious hole, also do not have the macrobead of arc ion plating film surface to pollute this bright and clean surface and have good reflective function, the homogeneity for its color and luster is highly profitable.
Color
The color of the film obtained under different nitrogen flow condition has notable difference.This is because nitrogen is reactant gases, in coating process during nitrogen flow change, the participation nitrogen-atoms of film forming and the component of titanium atom change, and tissue and the color of rete also change all thereupon.When nitrogen flow is very little, team and titanium nitride titanium nitride react insufficient, and main generation color sample is silvery white, along with the increase of nitrogen flow, nitrogen and titanium sufficient reacting, have light yellow and deep yellow, nitrogen ratios increases gradually, and film surface color also gradually becomes golden yellow.When nitrogen is excessive, color is blue and purple.Utilize colourimeter to the test result of sample during different nitrogen flow in table 2.Can find out, along with the increase (deposition pressure increase) of nitrogen flow, the color of the titanium nitride membrane obtained from light to dark.Visible, as long as regulation and control entraining air stream amount (or deposition pressure), just can obtain required film color, this technology can be widely used in polychromy plated film.
Table 2 chromascope test result
| Sample number into spectrum | Nitrogen flow | Color |
| 1 | 0.59sccm | Silver color |
| 2 | 0.84sccm | Golden |
| 3 | 1.99sccm | Pale blue |
| 4 | 2.21sccm | Dark blue |
| 5 | 2.37sccm | Purple |
On MP-3P type ion plating equipment, by changing nitrogen flow, utilize magnetically controlled sputter method can prepare the film of different colours.Want to obtain decorative coating that is a certain or multiple color, only need to regulate this processing parameter of nitrogen flow, simple possible, is expected to be widely used in polychromy plated film industry.
Invent the positively effect utilizing magnetron sputtering to prepare polychromy film coating method had compared with prior art to be:
1) this technology utilizes the feature that magnetron sputtering deposition temperature is low, can at the lower material even plastic plating polychromy rete of fusing point.
2) magnetron sputtering be coated with film surface impermanence arc ion plating time surface produce macrobead pollute, surface smoothness is higher.
3) by regulating this processing parameter of nitrogen flow, simple possible, is expected to be widely used in polychromy plated film industry.
Embodiment
Embodiment 1
Use MP-3P type vaccum ion coater
Preparation work before experiment: ganoid rapid steel or stainless steel base to be immersed in the spirituous solution of 95% ultrasonic action 10 minutes, then use acetone soln dipping bath; Dry with blower, be then fixed on the specimen mounting of vacuum deposition chamber.
Coating process parameter:
Background vacuum: 3 × 10
-3pa plasma sputter source processing parameter: sputtering voltage 200V, sputtering line 2A sputtering energy 400W.
Other processing parameter: acceleration voltage is 0, auxiliary energy 0, auxiliary line 0; Substrate is Heating temperature not.
In deposition process, sputter gas selects nitrogen, and keep its flow to be respectively 0.59,0.84,1.99,2.21,2^.37sccm by flow director, corresponding operating air pressure is respectively 0.11,0.16,0.36,0.39,0.42Pa.Observed by the surface topography of scanning electronic microscope to sample; Colourimeter is utilized to measure the colourity of film surface.
From above-mentioned, the present invention except electrodeposited chromium layers, all in once shaped after repeatedly plated film in vaccum ion coater, therefore easily manufactured, and without the environmental pollution such as waste gas, waste liquid, the rete formed to human body skin also without any stimulation.
Embodiment 2
Use MP-3P type vaccum ion coater
Preparation work before experiment: ganoid rapid steel or stainless steel base to be immersed in the spirituous solution of 95% ultrasonic action 20 minutes, then use acetone soln dipping bath, dry with blower, be then fixed on the specimen mounting of vacuum deposition chamber.
Coating process parameter:
Background vacuum: 3 × 10
-3pa plasma sputter source processing parameter: sputtering voltage 200V, sputtering line 2A sputtering energy 400W.
Other processing parameter: acceleration voltage is 0, auxiliary energy 0, auxiliary line 0; Substrate is Heating temperature not.
In deposition process, sputter gas selects nitrogen, keeps its flow to be respectively 0.59,0.84,1.99.2.21.2.37 by flow director
Sccm; Operating air pressure is respectively at 0.42Pa.Observed by the surface topography of scanning electronic microscope to sample; Colourimeter is utilized to measure the colourity of film surface.
Embodiment 3
1) employing makes matrix plated film through polishing, ganoid high speed steel or stainless steel;
2) will the matrix of plated film be needed to immerse ultrasonic action 15 minutes in the spirituous solution of 95%, then use acetone soln dipping bath, dry with blower;
3) then carry out plated film by the specimen mounting needing the matrix of plated film to be fixed on vacuum deposition chamber, before plated film, back end vacuum is evacuated to 3 × 10
-3pa, and effects on surface carries out icon bombardment cleaning 30min; Distance between matrix and sputtering target is 150mm, not biasing;
4) sputtering power is kept to be 200W during matrix plated film, to be coated with the film sample of different colours under different nitrogen flow, different deposition pressure; Wherein used nitrogen flow is controlled by under meter, is respectively 0.59,0.84,1.99,2.21.2.37sccm, and corresponding deposition pressure is respectively 0.11,0.16,0.36,0.39,0.42Pa; Depositing time is 20min; Operating air pressure is respectively at 0.25Pa.
5) observed by the surface topography of scanning electronic microscope to sample; Colourimeter is utilized to measure the colourity of film surface.
Claims (1)
1. magnetron sputtering prepares a method for colored titanium nitride film, it is characterized in that being undertaken by following step:
1) employing makes matrix plated film through polishing, ganoid high speed steel or stainless steel;
2) will the matrix of plated film be needed to immerse ultrasonic action 10-20 minute in the ethanolic soln of 95%, then use acetone soln dipping bath, dry with blower;
3) then carry out plated film by the specimen mounting needing the matrix of plated film to be fixed on vacuum deposition chamber, before plated film, back end vacuum is evacuated to 3 × 10
-3pa, and effects on surface carries out icon bombardment cleaning 3-5min; Distance between matrix and sputtering target is 150mm, not biasing;
4) sputtering power is kept to be 200W during matrix plated film, to be coated with the titanium nitride thin membrane sample of different colours under different nitrogen flow, different deposition pressure; Wherein used nitrogen flow is controlled by under meter, is respectively 0.59,0.84,1.99,1.21,2.378sccm, and corresponding deposition pressure is respectively 0.11,0.16,0.36,0.39,0.42Pa; Depositing time is 20min; Operating air pressure is respectively between 0.11-0.42Pa;
5) observed by the surface topography of scanning electronic microscope to sample; Colourimeter is utilized to measure the colourity of film surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310459978.XA CN104513960A (en) | 2013-09-29 | 2013-09-29 | Method for preparing color titanium nitride film through magnetron sputtering |
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| CN201310459978.XA CN104513960A (en) | 2013-09-29 | 2013-09-29 | Method for preparing color titanium nitride film through magnetron sputtering |
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| CN104513960A true CN104513960A (en) | 2015-04-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588585A (en) * | 2018-04-03 | 2018-09-28 | 瑞信五金(河源)有限公司 | A kind of preparation method of 316 stainless steel watchband |
| CN110923629A (en) * | 2019-12-06 | 2020-03-27 | 宁波鑫星汽车部件有限公司 | Titanium nitride plating process for automobile label |
-
2013
- 2013-09-29 CN CN201310459978.XA patent/CN104513960A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588585A (en) * | 2018-04-03 | 2018-09-28 | 瑞信五金(河源)有限公司 | A kind of preparation method of 316 stainless steel watchband |
| CN110923629A (en) * | 2019-12-06 | 2020-03-27 | 宁波鑫星汽车部件有限公司 | Titanium nitride plating process for automobile label |
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Addressee: WUXI HUIMING ELECTRONIC TECHNOLOGY CO., LTD. Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Application publication date: 20150415 |
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