CN209024637U - A kind of nitridation titanium compound film - Google Patents
A kind of nitridation titanium compound film Download PDFInfo
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- CN209024637U CN209024637U CN201821485195.3U CN201821485195U CN209024637U CN 209024637 U CN209024637 U CN 209024637U CN 201821485195 U CN201821485195 U CN 201821485195U CN 209024637 U CN209024637 U CN 209024637U
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Abstract
The utility model discloses a kind of nitridation titanium compound film, including the metal back layer, supporting layer and titanium nitride layer sequentially formed outward by substrate surface.Bottom is prepared using cathodic arc technique, supporting layer is prepared using magnetron sputtering technique, titanium nitride layer is that the mixture layer that the two kinds of different structure film layers to be formed are staggeredly stacked is worked at the same time using two kinds of technologies of magnetron sputtering and cathode arc, and the thickness of the desalination titanium layer is between 1~5 μm.The utility model deft design, structure is simple, the structure that titanium nitride layer uses two kinds of different structure film layers to be alternately stacked.Give full play to the few advantage of the high compactness of magnetron sputtering film layer, defect, cathode arc prepares the advantages of high rigidity of film layer, good binding force, realize that film layer internal structure is fine and close, can guarantee that the hardness of coating is high again, ultimately form with good binding force, high rigidity, compact structure hard coat.
Description
Technical field
The utility model relates to a kind of composite membrane, especially a kind of nitridation titanium compound film.
Background technique
Titanium nitride membrane is a kind of metal nitride, have high rigidity and high elastic modulus, low-friction coefficient, it is wear-resistant with
And good acid-alkali-corrosive-resisting characteristic, it is well suited as wear-resistant coating, thus the nitridation obtained by physical gas-phase deposition
Titanium film it is numerous have wear-resisting, hardness, acid-alkali-corrosive-resisting requirement part on be used widely.
Conventional titanium nitride thin film preparation often uses single arc technology or magnetron sputtering technique, and single skill
There are certain defects when preparing titanium nitride coating for art.Such as use the titanium nitride of cathodic arc technique preparation, meeting in preparation process
There is more bulky grain to be deposited on inside film and form defect, the biggish internal stress of coat inside generation and coating structure is caused to be dredged
Pine, these defects can reduce the acid-alkali-corrosive-resisting of coating；The titanium nitride prepared using magnetron sputtering, with the binding force of substrate compared with
Difference, lower hardness and abrasion resistance properties are poor.The grain structure of the coating of single technique preparation is column crystal, from substrate bottom
Through entire coat inside, there are gap between crystal grain and crystal grain, these gaps can equally become some defects of coating.
Product uses under different operating conditions, and performance requirement emphasis is different, as the coating on tool and mould surface needs to have
The features such as high rigidity, good wearability；Auto parts and components need coating to have good toughness, good adhesive force and good
The characteristics of good compactness；The coating of medical instrument needs to have high rigidity, good bio-compatibility, acid-alkali-corrosive-resisting, resistance to
The features such as high-temperature steam corrosivity.Cathodic arc technique can satisfy the coating performance requirement of the products such as tool and mould, magnetron sputtering
Can satisfy the performance of the products such as auto parts and components, but both requirements for medical instrument are unable to satisfy, especially without
Method meets high temperature steam corrosion, because medical device product is using preceding needing to carry out at sterilizing in high-temp steam sterilizing pot
Reason, temperature reach 150 DEG C or more, and vapor can enter coat inside, coating by the gap between the defect and crystal grain of coating
Potential difference is formed between substrate, so that the structure of titanium nitride changes, and then is corroded, is led to coating failure.Therefore,
Titanium nitride coating high-temperature corrosion resistance problem become can security application in the critical issue on medical instrument.
Summary of the invention
The purpose of this utility model is exactly that it is multiple to provide a kind of titanium nitride in order to solve the above-mentioned problems in the prior art
Close film.
The purpose of this utility model is achieved through the following technical solutions:
A kind of nitridation titanium compound film, including the metal back layer, supporting layer and titanium nitride sequentially formed outward by substrate surface
Layer, the bottom are prepared using cathodic arc technique, and supporting layer is prepared using magnetron sputtering technique, and titanium nitride layer is using magnetic control
Sputtering and two kinds of technologies of cathode arc work at the same time the mixture layer that the two kinds of different structure film layers to be formed are staggeredly stacked, the nitrogen
Change the thickness of titanium layer between 1~5 μm.
Preferably, a kind of nitridation titanium compound film, in which: one in described metal back layer Cr layers, Ti layers or Ni layers
Kind, and prepared by cathodic arc technique, thickness is between 0.2~0.8 μm.
Preferably, a kind of nitridation titanium compound film, in which: the thickness of the supporting layer is between 0.8~2 μm.
Preferably, a kind of nitridation titanium compound film, in which: the supporting layer is CrN layers of either AlTiN
Layer.
Preferably, a kind of nitridation titanium compound film, in which: the titanium nitride layer, and by magnetron sputtering and
Cathodic arc technique works together to complete to prepare.
A kind of preparation method nitrogenizing titanium compound film, includes the following steps:
S1 is put into vacuum chamber after cleaning substrate, carries out plasma etching；
S2, under the technique vacuum degree of 0.3~1.2Pa, using Cr, Ti or Ni as target, in the substrate surface through over cleaning
One layer of metal back layer is prepared using cathodic arc technique；
S3 opens the magnetron sputtering shielding power supply of Cr or TiAl target, in gold under the technique vacuum degree of 1.0~2.0Pa
Belong to bottom surface and forms supporting layer；
S4 using the Ti target of two kinds of different structures as target, while opening yin under the technique vacuum degree of 2.0-4.0Pa
Pole electrical arc power supply and magnetron sputtering power supply prepare titanium nitride layer, and the power proportion for passing through two targets of control is 1:2,
The TiN layer of support layer surface formation structure composite.
Preferably, a kind of preparation method nitrogenizing titanium compound film, it is characterised in that: the S1 step comprises the following processes:
Substrate is put into ultrasonic cleaning in alkaline solution by S11；
S12, by the substrate Jing Guo S11 step, ultrasonic oscillation is cleaned in filtering pure water；
Substrate Jing Guo S12 step is completed drying by S13 in drying box；
S14 starts after the substrate of S13 step is put into vacuum chamber to vacuumize vacuum chamber, reaches 3 × 10-3Pa's
After vacuum degree, heater heating is kept for 400 DEG C, then passes to argon gas, and continue to vacuumize, and holding technique vacuum degree is
0.3~1.0Pa, open electron beam, voltage be 1000V~1500V, open grid bias power supply, grid bias power supply be set in 1000V~
1500V carries out the ion etching of 60~120min to substrate.
Preferably, a kind of preparation method of nitridation titanium compound film, in which: the cathode of Cr, Ti or Ni target
The power control of arc power is between 1~3kW, and application -80V~-1000V back bias voltage on workpiece, sedimentation time 10
~40min, the thickness of the metal back layer of formation is between 0.2 μm~0.8 μm.
Preferably, a kind of preparation method of nitridation titanium compound film, in which: the magnetic control of the Cr or TiAl target
Shielding power supply 2~3.5kW of power, and application -80V~-1000V back bias voltage on workpiece, the time of deposition are 60~100min,
The thickness of the supporting layer of formation is between 0.8~2 μm.
Preferably, described based on a kind of preparation method for nitrogenizing titanium compound film, in which: the arc power of the Ti target
Power be 500~1500W, the power of magnetron sputtering target power supply is 1000~3000W, and the two power ratio is 1:2, sedimentation time
For 60~200min, the titanium nitride layer thickness of formation is between 1~5 μm.
The advantages of technical solutions of the utility model, is mainly reflected in:
The characteristics of the utility model deft design, thin film preparation process step is simple, gives full play to every kind of coating technology, bottom
Layer is prepared using cathodic arc technique, and coating is made to have good adhesive force；Supporting layer uses magnetron sputtering technique, gives full play to
The feature that magnetron sputtering film layer structure is fine and close, internal stress is small；Titanium nitride layer is using magnetron sputtering and cathodic arc technique while work
Make to prepare titanium nitride, the titanium nitride of two kinds of technique preparation, by the hard of the compactness of magnetron sputtering film layer and cathode arc film layer
Degree effectively combines, it is possible to reduce the defect inside film layer not only guarantees that the film layer of preparation has good compactness, but also can guarantee
Film layer hardness with higher, and the internal stress of coating can also reduce, and then improve the internal stress of film layer.The preparation of this film layer
Method, using the method for cathode arc, magnetron sputtering and cathode arc in conjunction with magnetron sputtering, the film layer of this method preparation is brilliant
The structure of grain is column crystal, but the continuity of column crystal is interrupted, and forms discontinuous grain structure, can be further reduced
The defect of film layer.
The preparation method of the utility model film layer, process is simple, control convenience, is individually plated using two kinds of different film plating process
Film works at the same time plated film, and the high temperature corrosion for the nitridation titanium compound film that this method obtains is better than traditional titanium nitride film
Layer.Meanwhile titanium nitride layer is prepared using the method for cathode arc and the method for magnetron sputtering, two kinds of film plating process work at the same time,
So that deposition rate is fast, film layer preparation efficiency can effectively improve.Pass through the fusion of a variety of PVD techniques and setting for technological parameter
It sets, provides a kind of preparation method for the nitridation titanium compound film that technology stability is high, effect is good.
The utility model combines multiple coating films method, whole process pollution-free, environmentally protective.
Detailed description of the invention
Fig. 1 is the membrane structure schematic diagram of the utility model.
Specific embodiment
The purpose of this utility model, advantage and feature will carry out figure by the non-limitative illustration of preferred embodiment below
Show and explains.These embodiments are only the prominent examples using technical solutions of the utility model, all to take equivalent replacement or wait
Effect transformation and formed technical solution, all fall within the requires of the utility model protection within the scope of.
The utility model discloses a kind of nitridation titanium compound film, including the metal bottom sequentially formed outward by 4 surface of substrate
Layer 1, supporting layer 2 and titanium nitride layer 3, wherein the metal back layer 1 is one of Cr layers, Ti layers or Ni layers, and passes through yin
Pole electrical arc technology generates, thickness between 0.2~0.8 μm, metal Cr, Ti or Ni be conducive to enhance entire composite thick film with
The binding force of substrate.
The supporting layer 2 is prepared using magnetron sputtering technique, the film layer in the supporting layer be CrN layers either
AlTiN layers, and prepared by cathodic arc technique, the thickness of supporting layer is between 0.8~2 μm.
Also, due to when titanium nitride film carries out disinfection under high-temperature vapor environment to sterilize, it may occur that electrochemical reaction,
And then the performance of film layer is influenced, therefore TiN layer is worked together by magnetron sputtering and cathodic arc technique to complete to prepare, it is described
The thickness of TiN layer 3 is between 1~5 μm.
The utility model further discloses a kind of a kind of above-mentioned nitridation titanium compound film, includes the following steps:
S1 is put into vacuum chamber after cleaning substrate, carries out plasma etching；
It is specific and includes the following steps:
Substrate is put into ultrasonic cleaning in alkaline solution by S11；
S12, by the substrate Jing Guo S11 step, ultrasonic oscillation is cleaned in filtering pure water；
Substrate Jing Guo S12 step is completed drying by S13 in drying box；
S14 starts after the substrate of S13 step is put into vacuum chamber to vacuumize vacuum chamber, reaches 3 × 10-3Pa's
After vacuum degree, heater heating is kept for 400 DEG C, is then passed to the high-purity argon gas that purity is 99.999%, is controlled argon gas
Being passed through flow is 10~50sccm, and continues to vacuumize, and holding technique vacuum degree is 0.3~1.0Pa, then, opens electron beam,
Voltage is 1000V~1500V, opens grid bias power supply, and grid bias power supply is set in 1000V~1500V, 60 is carried out to substrate~
The ion etching of 120min.
S2, under the technique vacuum degree of 0.5~3.0Pa, using Cr, Ti or Ni as target, in the substrate Jing Guo ion etching
Surface prepares one layer of metal back layer 1 using cathodic arc method, in coating process, the cathode electricity of Cr, Ti or Ni target
The power control of arc power is between 1~3kW, and application -80V~-1000V back bias voltage on workpiece, sedimentation time be 10~
40min, to form metal back layer 1 of the thickness between 0.2 μm~0.8 μm in substrate 4.
S3 is extracted into 3.0 × 10 in vacuum degree-3When Pa, the high pure nitrogen that purity is 99.999% is passed through into vacuum chamber, and
The flow that is passed through of control nitrogen is 30~80sccm, and under the technique vacuum degree of 1.0~2.0Pa, opens Cr or TiAl target
Magnetron sputtering shielding power supply, the Cr or TiAl are target, magnetron sputtering 2~3.5kW of power of target, and on workpiece
Application -80V~-1000V back bias voltage, time of deposition are 60~100min, metal back layer surface formed thickness 0.8~
CrN either TiAlN supporting layer between 2 μm.
S4 using Ti target as target, while opening cathode arc power supply and magnetic under the technique vacuum degree of 2.0-4.0Pa
The power ratio controlled shielding power supply, and control the power supply of two targets is 1:2, specifically, controls the function of cathode arc power supply
Rate is 500~1500W,；The magnetron sputtering power is 1000~3000W, is controlled described using cathode arc and magnetic control
The time that sputtering technology deposits simultaneously is 60~200min, to form TiN layer of the thickness at 1-5 μm in support layer surface.
Through inventor the study found that the bottom is prepared using cathodic arc technique, since arc technology prepares film layer mistake
Cheng Zhong, particle ionization level is high, and bottom can be made to have good adhesive force.The supporting layer uses magnetron sputtering technique system
It is standby, bottom can be interrupted and supporting layer forms continuous columnar crystal structure, reduce the defect between crystal grain or vacancy, and then reduce
The internal stress that column crystal self-defect generates.
Adhesive force for improving coating and substrate has obvious action, supporting layer to prepare using magnetron sputtering technique,
The coated grains structure of two kinds of different technologies preparations is different, not will form the column crystal through coating whole thickness, so that brilliant
Defect between grain is reduced.The ion of ion and cathode arc that magnetron sputtering comes out forms staggered combination, makes inside film layer
Internal stress be greatly reduced, while the ion of magnetron sputtering has filled up the gap of cathode arc, keeps film layer structure finer and close.
Still there are many embodiment, all technologies formed using equivalents or equivalent transformation for the utility model
Scheme is all fallen within the protection scope of the utility model.
Claims (5)
1. a kind of nitridation titanium compound film, it is characterised in that: including sequentially formed outward by substrate (4) surface metal back layer (1),
Supporting layer (2) and titanium nitride layer (3), the bottom (1) are prepared using cathodic arc technique, and the supporting layer (2) uses magnetic
Control sputtering technology preparation, the functional layer that the titanium nitride layer is prepared using magnetron sputtering and cathodic arc technique, the titanium nitride
The thickness of layer (3) is between 1~5 μm.
2. nitridation titanium compound film according to claim 1, it is characterised in that: the metal back layer (1) be Cr layers, Ti layers or
One of Ni layers, and prepared by cathodic arc technique, thickness is between 0.2~0.8 μm.
3. nitridation titanium compound film according to claim 2, it is characterised in that: the thickness of the supporting layer (2) is in 0.8~2 μ
Between m.
4. nitridation titanium compound film according to claim 3, it is characterised in that: the film layer in the supporting layer (2) is CrN layers
Either AlTiN layers, and prepared by magnetron sputtering technique.
5. nitridation titanium compound film according to claim 1 to 4, it is characterised in that: the titanium nitride layer (3) passes through magnetic
Control sputtering and cathodic arc technique work together to complete to prepare.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201821485195.3U CN209024637U (en) | 2018-09-12 | 2018-09-12 | A kind of nitridation titanium compound film |
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| CN201821485195.3U CN209024637U (en) | 2018-09-12 | 2018-09-12 | A kind of nitridation titanium compound film |
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| CN201821485195.3U Expired - Fee Related CN209024637U (en) | 2018-09-12 | 2018-09-12 | A kind of nitridation titanium compound film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823544A (en) * | 2018-09-12 | 2018-11-16 | 杨杰平 | Based on nitridation titanium compound film and preparation method thereof |
| CN113881917A (en) * | 2021-12-07 | 2022-01-04 | 河南科技学院 | Port crane anticorrosive coating and preparation method thereof |
-
2018
- 2018-09-12 CN CN201821485195.3U patent/CN209024637U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823544A (en) * | 2018-09-12 | 2018-11-16 | 杨杰平 | Based on nitridation titanium compound film and preparation method thereof |
| CN113881917A (en) * | 2021-12-07 | 2022-01-04 | 河南科技学院 | Port crane anticorrosive coating and preparation method thereof |
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