CN1680618A - Method for impulsive bias arc ion plating multi-player super-hard nano films of titanium/titanium nitrate - Google Patents
Method for impulsive bias arc ion plating multi-player super-hard nano films of titanium/titanium nitrate Download PDFInfo
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- CN1680618A CN1680618A CN 200410155489 CN200410155489A CN1680618A CN 1680618 A CN1680618 A CN 1680618A CN 200410155489 CN200410155489 CN 200410155489 CN 200410155489 A CN200410155489 A CN 200410155489A CN 1680618 A CN1680618 A CN 1680618A
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Abstract
A surface modification technology of nanometer multi-layer hard membrane of Ti/ titanium oxide by way of pulsed biasing. Apply to pulsed biasing to improve deposit quality of membrane in the arc process. Interchange Ar and N2 interchange and control the time interval. Then cover is fit on the preface of metal.
Description
Technical field
The invention belongs to the metal surface properties modification technical field.
Background technology
Titanium nitride membrane is plated on cutter or the die surface life-span is significantly improved, and has once caused cutting-tool engineering revolution widely in the eighties, and the rapid industrialization for the mechanical industry automatic production line provides key condition.In recent years, machine adds industry will be to high speed and serialization producer will use under the rugged environment more to development and tool and mould more, the simple performance that titanium nitride membrane had (film-substrate cohesion 40N-50N, hardness 24GPa) with the usual way preparation can not satisfy this requirement fully.
Thin-film material is made nano-multilayered structures can improve and improve its over-all properties, promptly reflect the strengthening effect of nano-scale; Though being plated in synthesizing of nitride-based ganoine thin film, arc ions has irreplaceable effect, mix reasons such as interface and sedimentation rate are difficult for controlling soon but contaminated surface, ion energy are high owing to always there is the macrobead defective in common arc ion plating, be not suitable for being used for preparing meticulous ganoine thin film so it is generally acknowledged arc ion plating with nano-multilayered structures, at present this class film also mainly adopts method such as magnetic controlled sputtering ion plating to prepare, but shortcoming such as the ubiquity sedimentation rate is low, the not strong and actual usage performance of film-substrate cohesion is not really outstanding.
Summary of the invention
The purpose of this invention is to provide a kind of easy and simple to handle, sedimentation velocity fast, be easy to produce in batches, preparation is by the method for a kind of multi-player super-hard nano films of simple binary titanium, nitrogen element set structure, i.e. the method for pulsed bias arc ions titanizing/titanium nitride nano multi-player super-hard film.
Technical solution of the present invention is that workpiece through putting into the vacuum chamber of arc ion plating apparatus behind the cleaning-drying, is all installed pure titanium target on all cathode arc source positions; Be evacuated down to 5 * 10
-3-2 * 10
-2Pa; Logical argon gas opens the titanium arc to 0.30-0.60Pa, and arc stream fixes on 50-70A, adds dc negative bias voltage and carries out sputter clean 3-8 minute to-800--1000V; Begin plated film then; Plated film falls bias voltage after finishing, stops arc, stops the supple of gas or steam, cuts off the power supply, and stove is chilled to 20-30 ℃ under natural vacuum, bleeds off vacuum at last and takes out workpiece; In the plated film stage, titanium negative electrode target arc stream is adjusted to 60-80A; Apply pulsed negative bias to workpiece, the bias voltage amplitude is that 20-40KHz, dutycycle are 20-40% for-800--1000V, frequency; Adopt argon/nitrogen repeatedly over-over mode supply gas to vacuum chamber, and the control argon gas feeding time be 50-100 second, stop argon gas then and send into nitrogen, the feeding time is 20-40 second, and then changes argon gas into, and 50-100 changes nitrogen again into after second ... so alternately repeat, total plated film time is 40-60 minute.Wherein pulsed negative bias guarantees to obtain enough to lack the good thin film deposition quality of macrobead quantity and enough high-compactness; Deposition obtains pure titanium layer when feeding argon gas, and deposition obtains titanium nitride layer when feeding nitrogen, alternately ventilate repeatedly and then obtain the membrane structure that adds up that repeats of titanium and titanium nitride layer, replace the element thickness that is then determining each individual layer pitch time of ventilation, total number of plies of unit layer depends on total depositing time; Last one deck finishes with the titanium nitride layer of logical nitrogen.
Workpiece is with rapid steel.
Workpiece is a Wimet.
The invention has the beneficial effects as follows, the ganoine thin film of the synthetic alternately repeated titanium/titanium nitride nano multilayered structure that is elementary cell by titanium layer and the 15-25nm titanium nitride layer of 20-30nm, the film-substrate cohesion of film is greater than 70N, and hardness is higher than 40GPa.
Embodiment
The present invention is described further below in conjunction with embodiment.
The rapid steel workpiece through putting into the vacuum chamber of arc ion plating apparatus behind the cleaning-drying, is all installed pure titanium target on all cathode arc source positions; Be evacuated down to 5 * 10
-3Pa; Logical argon gas opens the titanium arc to 0.36Pa, and arc stream fixes on 60A, adds dc negative bias voltage and carries out sputter clean 5 minutes to-1000V; Adjust arc stream to 80A; Bias voltage makes pulse mode into, and the bias voltage amplitude is that 30KHz, dutycycle are 40% for-900V, frequency; The logical nitrogen of disconnected simultaneously argon gas also arrives 0.36Pa, the beginning titanium nitride layer, stop nitrogen after 30 seconds, continue to change logical argon gas, air pressure is 0.36Pa still, begins to deposit pure titanium layer, stop argon gas after 90 seconds again and feed nitrogen, continue to feed argon gas again after 30 seconds ..., so alternate repetition carries out, and the titanium nitride layer with 30 seconds logical nitrogen finishes at last; Total deposition plating time is 40 minutes 30 seconds, falls bias voltage after then, stops arc, stops the supple of gas or steam, cuts off the power supply, and stove is cold 1 hour under vacuum, bleeds off vacuum at last and takes out workpiece.
So having produced by the titanium layer of about 25nm and the titanium nitride layer of about 20nm in the workpiece surface deposition is elementary cell, be and alternately repeat the nano-multilayer film of the titanium/titanium nitride of totally 20.5 formations, though these film starting material are simple, cost is low, but film-substrate cohesion can promptly have superhard characteristic up to 85N and hardness up to 48Gpa.
Claims (4)
1. the method for pulsed bias arc ions titanizing/titanium nitride nano multi-player super-hard film is to put into the vacuum chamber of arc ion plating apparatus behind the workpiece process cleaning-drying, pure titanium target all is installed on all cathode arc source positions; Be evacuated down to 5 * 10-3-2 * 10-2Pa; Logical argon gas opens the titanium arc to 0.30-0.60Pa, and arc stream fixes on 50-70A, adds dc negative bias voltage and carries out sputter clean 3-8 minute to-800--1000V; Begin plated film then; Plated film falls bias voltage after finishing, stops arc, stops the supple of gas or steam, cuts off the power supply, and stove is chilled to 20-30 ℃ under vacuum; Bleed off vacuum at last and take out workpiece; It is characterized in that,, titanium negative electrode target arc stream is adjusted to 60-80A in the plated film stage; Apply pulsed negative bias to workpiece, the bias voltage amplitude is that 20-40KHz, dutycycle are 20-40% for-800--1000V, frequency; Employing argon/nitrogen over-over mode is repeatedly supplied gas to vacuum chamber, and the control argon gas feeding time is 50-100 second, stop argon gas then and send into nitrogen, the feeding time is 20-40 second, and then change argon gas into, the same 50-100 that continues changes nitrogen again into after second, so alternately repeat, and total plated film time is 40-60 minute.
2. the method for pulsed bias arc ions titanizing according to claim 1/titanium nitride nano multi-player super-hard film, it is characterized in that, employing has the arc ion plating apparatus in two arc sources, pure titanium target is installed on negative electrode position, arc source, will accept the rapid steel workpiece of coating film treatment and put into vacuum chamber through behind the cleaning-drying: in the plated film stage, titanium negative electrode target arc stream is 80A; Negative bias is an impulse form, and amplitude is that 30KHz, dutycycle are 40% for-900V, frequency; Supplying gas is repetition alternatively form, repeats by the principle separately of then 30 seconds logical nitrogen of 90 seconds logical argon gas, and total deposition plating time is 40 minutes 30 seconds.
3. the method for pulsed bias arc ions titanizing according to claim 1/titanium nitride nano multi-player super-hard film is characterized in that workpiece is with rapid steel.
4. the method for pulsed bias arc ions titanizing according to claim 1/titanium nitride nano multi-player super-hard film is characterized in that workpiece is a Wimet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410155489 CN1680618A (en) | 2004-11-30 | 2004-11-30 | Method for impulsive bias arc ion plating multi-player super-hard nano films of titanium/titanium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410155489 CN1680618A (en) | 2004-11-30 | 2004-11-30 | Method for impulsive bias arc ion plating multi-player super-hard nano films of titanium/titanium nitrate |
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| Publication Number | Publication Date |
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| CN1680618A true CN1680618A (en) | 2005-10-12 |
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| CN 200410155489 Pending CN1680618A (en) | 2004-11-30 | 2004-11-30 | Method for impulsive bias arc ion plating multi-player super-hard nano films of titanium/titanium nitrate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395060C (en) * | 2006-02-16 | 2008-06-18 | 华南理工大学 | TiN two-layer film cladding for cutting tool material surface and its preparing method |
| CN102094180A (en) * | 2010-06-04 | 2011-06-15 | 中国科学院金属研究所 | Multi-layer film deposition method |
| CN102230159A (en) * | 2011-05-27 | 2011-11-02 | 沈阳市红十字会医院 | Preparation method of surface hard protective film for guide wire/tunnel needle used in peritoneal dialysis catheter insertion |
| CN102634753A (en) * | 2011-02-12 | 2012-08-15 | 深圳职业技术学院 | Hard coating and preparation method thereof |
| CN101983253B (en) * | 2008-04-03 | 2012-10-24 | Oc欧瑞康巴尔查斯股份有限公司 | Apparatus for sputtering and a method of fabricating a metallization structure |
| CN104911551A (en) * | 2015-06-03 | 2015-09-16 | 陕西航天导航设备有限公司 | Preparation method for TiN film with thickness of 21.5mu m |
| CN108823544A (en) * | 2018-09-12 | 2018-11-16 | 杨杰平 | Based on nitridation titanium compound film and preparation method thereof |
| CN109913797A (en) * | 2017-12-13 | 2019-06-21 | 维达力实业(深圳)有限公司 | Case-hardened graphite jig and its case-hardened method |
| CN110257780A (en) * | 2019-06-28 | 2019-09-20 | 长安大学 | A kind of multicomponent alloy target, multi-element metal/nitride composite coating and preparation method thereof |
-
2004
- 2004-11-30 CN CN 200410155489 patent/CN1680618A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395060C (en) * | 2006-02-16 | 2008-06-18 | 华南理工大学 | TiN two-layer film cladding for cutting tool material surface and its preparing method |
| CN101983253B (en) * | 2008-04-03 | 2012-10-24 | Oc欧瑞康巴尔查斯股份有限公司 | Apparatus for sputtering and a method of fabricating a metallization structure |
| CN102094180A (en) * | 2010-06-04 | 2011-06-15 | 中国科学院金属研究所 | Multi-layer film deposition method |
| CN102094180B (en) * | 2010-06-04 | 2013-04-03 | 中国科学院金属研究所 | Multi-layer film deposition method |
| CN102634753B (en) * | 2011-02-12 | 2016-04-27 | 深圳职业技术学院 | Hard coat and preparation method thereof |
| CN102634753A (en) * | 2011-02-12 | 2012-08-15 | 深圳职业技术学院 | Hard coating and preparation method thereof |
| CN102230159B (en) * | 2011-05-27 | 2013-07-10 | 沈阳市红十字会医院 | Preparation method of surface hard protective film for guide wire/tunnel needle used in peritoneal dialysis catheter insertion |
| CN102230159A (en) * | 2011-05-27 | 2011-11-02 | 沈阳市红十字会医院 | Preparation method of surface hard protective film for guide wire/tunnel needle used in peritoneal dialysis catheter insertion |
| CN104911551A (en) * | 2015-06-03 | 2015-09-16 | 陕西航天导航设备有限公司 | Preparation method for TiN film with thickness of 21.5mu m |
| CN109913797A (en) * | 2017-12-13 | 2019-06-21 | 维达力实业(深圳)有限公司 | Case-hardened graphite jig and its case-hardened method |
| CN108823544A (en) * | 2018-09-12 | 2018-11-16 | 杨杰平 | Based on nitridation titanium compound film and preparation method thereof |
| CN110257780A (en) * | 2019-06-28 | 2019-09-20 | 长安大学 | A kind of multicomponent alloy target, multi-element metal/nitride composite coating and preparation method thereof |
| CN110257780B (en) * | 2019-06-28 | 2021-07-06 | 长安大学 | Multi-element alloy target, multi-element metal/nitride composite coating and preparation method thereof |
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