CN103952663A - Metal bottoming technology in diamond like coating - Google Patents
Metal bottoming technology in diamond like coating Download PDFInfo
- Publication number
- CN103952663A CN103952663A CN201410193574.5A CN201410193574A CN103952663A CN 103952663 A CN103952663 A CN 103952663A CN 201410193574 A CN201410193574 A CN 201410193574A CN 103952663 A CN103952663 A CN 103952663A
- Authority
- CN
- China
- Prior art keywords
- plasma
- metal
- workpiece
- deposition
- coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a metal bottoming technology in diamond like coating. The metal bottoming technology comprises two steps of plasma cleaning, and metal net plasma deposition or metal organic matter steam input deposition, wherein in the step of plasma cleaning, rare gases like Ar and Kr are filled into a vacuum tank, and plasma of the rare gases is generated through applying high pressure on a workpiece; in the step of metal net plasma deposition, pure Ti and Cr metal sheets and the workpiece are put into a metal net for coating a film, and the high energy plasma bombards pure Ti and Cr, so that the metal elements sputter or escape to deposit a thin Ti or Cr metal base layer on the surface of the workpiece; in the step of metal organic matter steam input deposition, an organic matter liquid containing metal elements like Ti and Cr is put in an external metal tank, is heated to become steam and is then introduced into the vacuum tank, and under ion bombardment, the steam becomes plasma so as to form a metal base layer on the surface of the workpiece.
Description
Technical field
The present invention relates to field of vacuum coating, specifically a kind of coating process that improves diamond-like coating and basal body binding force.
Background technology
The comprehensive ion technology of plasma (Plama Immersion Ion Deposition-PIID) is a kind of process for treating surface growing up in recent years, its advantage is to carry out plated film to complex part surfaces externally and internally simultaneously, especially with the obvious advantage to Tube plating.Utilizing PIID technology to be prepared into one of maximum coating is exactly diamond-like coating (Diamond Like Carbon-DLC).But, because the internal stress of DLC coating is higher, and the reasons such as bonding force is poor, mass stability is low between matrix, make its Application Areas be subject to very big constraint.
One, for improving in the method for its bonding force, research direction mainly comprises the following aspects:
(1) surface preparation
The difference of workpiece material and surface appearance, also difference to some extent of the surface pre-treating process of taking, conventional surface pre-treating process has the operations such as dry type sandblast, wet sand blast, pickling, alkali cleaning, rinsing, oven dry, uses sometimes in conjunction with ultrasonic wave.
(2) transition layer
Transition layer technology plates one deck transition tunic between DLC coating and matrix, the thickness of this tunic only has hundreds of nanometer conventionally to several micron thick, it not only can and matrix atom between can form stable chemical bond, can also form chemical bond with the C element of outer DLC coating the inside, thereby can significantly improve the bonding force of DLC coating.
(3) plasma nitriding
Plasma nitriding technology is in vacuum chamber, to be filled with N2 before plating DLC coating, under the bombardment of high-energy N plasma body, it is dark that part N atom can infiltrate several microns to tens microns of matrixes, can form nitride with matrix atom simultaneously, can significantly improve bonding force like this after skin plating DLC.
(4) plasma injects
Plasma injects similar with nitriding, and difference is that the former carries out under several ten thousand volt high pressure, and latter is several kilovolts, and the element that plasma injects is all generally less atom, and its bonding force is than the better effects if of plasma nitriding.
Two, for reducing in the method for internal stress, research direction mainly comprises the following aspects:
(1) doped with non-metals/metallic element in coating
Internal stress height is one of feature of traditional DLC coating, and high internal stress makes it under higher stress, produce fragility to burst apart.Scientific research personnel finds that some nonmetal/metallic elements that adulterate in DLC coating coating process can reduce its internal stress, generally realizes by being filled with gas, and the unit of doping have Si, F, P, Cr, Ti, Al etc.
(2) reduce plated film frequency/plated film voltage
Coating process parameter also can significantly reduce internal stress, generally takes to reduce plated film frequency or reduces plated film voltage and realize.But the reduction of plated film frequency declines plated film speed, has extended the plated film time, has reduced efficiency; The reduction of plated film voltage can make ionization level decline, and the hardness of coating also can decline in various degree simultaneously.Therefore, choose reasonable is very crucial.
Three, for improving in the method for mass stability, research direction mainly comprises the following aspects:
(1) reasonable in design, special fixture
For PIID technology, the fixture that the workpiece of different shapes, different size uses is completely different, the fundamental principle of jig Design is that good conductivity, portability, batch maximize, ionization level is high, the life-span is long etc., designs reasonable, a professional fixture and realize the prerequisite of mass, stabilization plated film.
(2) inflation mechanism reasonable in design and air extractor, the stability of guarantee vacuum tank internal gas pressure
Research shows: inflate and the quality of bleeding can affect the distribution of vacuum chamber internal gas pressure, thereby can affect the homogeneity of coating.Inflation mechanism is generally made up of source of the gas, under meter, gas ducting, stopping valve etc., and air extractor generally has the composition such as off-gas pump group (mechanical pump, lobe pump, diffusion pump, molecular pump), throttling valve (Throttle Valve).
(3) uncontrollability of minimizing manual intervention
In modern industrial equipments, due to popularizing of computer, the use of intelligentized program can reduce the uncontrollability of manual intervention, substantially realizes zero error, thereby can ensure the quality product of every batch.For filming equipment, by implanting good PLC program, substantially realize operating in a key, so only need in device prompts, carry out reasonable operation.
Summary of the invention
The invention provides the technique of metal bottoming in a kind of diamond-like carbon film-coating process, reach the object of the bonding force that strengthens diamond-like coating and matrix.
Technical solution problem of the present invention adopts following scheme:
A technique for metal bottoming in diamond-like carbon film-coating process, described technique comprises plasma clean, metal net mask plasma deposition/metallorganics steam input deposition two step compositions.This process characteristic is:
Described plasma clean is by Ar, and the rare gas such as Kr are filled with in vacuum tank, applies the plasma body of high pressure generation rare gas on workpiece, and in these plasma bodys, the ion bombardment workpiece surface of positively charged reaches the effect of plasma cleaning.
Described metal net mask plasma deposition is that the tinsels such as pure Ti, Cr are placed in and in metal net mask, carry out plated film together with workpiece, at this moment energy of plasma ratio is high a lot of while cleaning, high-octane plasma is known from experience bombardment pure Ti, Cr, make these metallic elements produce sputter or effusion effect, because workpiece and these tinsels are separated by very near, thereby can deposit at workpiece surface the metal prime coat of Ti, the Cr of thin layer, sometimes also can in tank body, be filled with as required N
2, the nitride of generation Ti, Cr, forms gradient film.
Described metallorganics steam input deposition is that the organism liquid that contains the metallic element such as Ti, Cr is placed in external metal tin, after making it become steam by heating, pass in vacuum tank, under ion bombardment effects, steam can become plasma body, thereby forms metal prime coat at workpiece surface.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, prime coat quality is high.At the inner pure Ti of high-octane plasma bombardment producing of metal net mask, the metal block of Cr, can deposit at workpiece surface the amorphous metal prime coat of higher degree.
2, technological operation is convenient.Metallorganics steam input deposition has just increased an input aperture on existing equipment, can realize metal prime coat and deposits not changing the simple source of the gas that switches under processing parameter.
3 compare with nonmetal prime coat, and metal prime coat can make the bonding force of DLC coating significantly improve, thereby widens its Application Areas.
Brief description of the drawings
Fig. 1 is the process device figure of metal net mask plasma deposition of the present invention.
Fig. 2 plasma cleaning power supply of the present invention output waveform figure.
Fig. 3 metal net mask plasma deposition of the present invention power supply output waveform figure.
Embodiment
A technique for metal bottoming in diamond-like carbon film-coating process, this technique mainly realizes by plasma cleaning, metal net mask plasma deposition or metallorganics steam input deposition, and concrete principle and working method are as follows:
One, plasma cleaning
Plasma cleaning is the indispensable program before DLC plated film.Its primary process is as follows: the workpiece cleaning up in ultrasonic equipment is dried, be installed on vacuum tank, utilize off-gas pump group that vacuum tank air pressure is evacuated to 3 × 10
-3below Pa, vacuum tank is carried out being filled with rare gas (Ar or Kr) after bakeout degassing, reach after operating air pressure (0.5～10Pa), on workpiece, apply negative bias (500～-8KV), the unbound electron of assembling on workpiece escapes out from its surface under vacuum state, electronics is subject to the attraction of anode (vacuum tank) and accelerates, in traveling process with vacuum chamber in rare gas molecule bump, cause the ionization of gas molecule, form the plasmoid of rare gas.The noble gas ion of positively charged bombards workpiece surface, causes the oxide compound of workpiece surface and impurity to be etched, and has realized the plasma clean of workpiece surface.
Two, metal net mask plasma deposition
Fig. 1 is the process device figure of metal net mask plasma deposition, and this device is made up of metal net mask 1, workpiece 2, support 3, tinsel 4.Metal net mask plasma deposition is that the tinsels 4 such as pure Ti, Cr are placed in and in metal net mask 1, carry out plated film together with workpiece 2.This technique is relatively suitable for flat-type workpiece plated film, and in order to improve batch and coating quality, flat-type workpiece adopts " back-to-back " Method for Installation.In order to ensure good electroconductibility, workpiece is supported by aluminum metal frame.After plasma cleaning completes, in the situation that not changing source of the gas and air pressure, supply frequency is adjusted to 3000Hz by 1000Hz, voltage 1500V is adjusted to 4100V, realizes metal bottoming technique, makes a concrete analysis of as follows:
Sparking voltage and current waveform figure when Fig. 2 is the interior plasma clean of vacuum chamber, in figure, upper part is voltage waveform, and lower part is current waveform, and 1V is 1KV corresponding to real voltage, and 1V is 25A corresponding to real peak electric current, pulsewidth is set as 20 microseconds.In figure, voltage is close to 1500V, frequency is close to 1000Hz, voltage waveform is square wave output, current waveform similar " mountain peak " form, peak point current 50A left and right, continuous discharge chronic (100 microsecond left and right), be that voltage pulse finishes to still have electric current to produce in final vacuum tank, this is because plasma discharge is continuous collision type discharge process, in a pulse, voltage-drop loading moment produces discharging current, along with the prolongation electric current of time increases gradually, it is maximum that the immediate current of loss of voltage reaches, then in the hundreds of microsecond of loss of voltage, electric current is not to disappear at once, but along with collision frequency reduces gradually, electric current is decayed gradually.
Fig. 3 is metal net mask plasma deposition power supply output waveform figure.As can be seen from the figure, compared with plasma cleaning, voltage rises to 4100V, frequency rises to after 3000Hz, and peak point current is promoted to rapidly 90A left and right by 50A, much higher when now the energy of plasma in metal net mask is than cleaning.This is because the raising of voltage and frequency can make the dynamics of ion impact and probability improve, thereby causes more atom ionization, and plasma density significantly improves.After highdensity plasma body and workpiece and tinsel effect, can cause the temperature of Ti, Cr tinsel and workpiece surface to raise, under high temperature and violent ion bombardment dual function, can there is sputter or escape in the metal ion on Ti, Cr tinsel surface, be similar to magnetron sputtering ion bombardment target process, because workpiece and these tinsels are separated by very near, thereby can deposit at workpiece surface the metal prime coat of Ti, the Cr of thin layer, sometimes also can in tank body, be filled with as required N
2, the nitride of generation Ti, Cr, forms gradient film, realizes thus the deposition of metal prime coat.
Table 1 is performance and the Application Areas comparison of different prime coats in diamond-like carbon film-coating process.As can be seen from the table, with respect to for prime coat and nonmetal prime coat, metal prime coat can significantly improve bonding force (according to German VDI3198 coating binding force examination criteria), HF1-HF6 bonding force weakens successively, the coating that bonding force is high can significantly improve its service life, taking field, colliery centrifugal machine sieve basket sheet as example, the life-span that normally there is no plated film is about 17 days, the diamond-like coating life-span of nonmetal prime coat is improved 4-7 days, the diamond-like coating life-span of metal bottoming of the present invention is improved 30-32 days, this means after whizzer uses the diamond-like coating of metal bottoming and can reduce shutdown number of times in the time of work, improve production capacity.For operability, metal bottoming technique and do not improve process complexity, only need to or change source of the gas by power parameter adjustment, and easy to operate, workpiece is without any need for the rotation of mechanism.For Application Areas, the adaptable environment of coating that bonding force is better is more harsh, diamond-like coating without prime coat can only be used for simple decoration, nonmetal prime coat can be applied to the field that surging force is little, have the field of certain impact power and metal bottoming diamond-like coating of the present invention can be applied to cutter, colliery basket sheet etc., application prospect is very open.
The performance of different prime coats and Application Areas comparison in table 1 diamond-like carbon film-coating process
Claims (4)
1. a technique for metal bottoming in diamond-like carbon film-coating process, described technique comprises: plasma clean, metal net mask plasma deposition/metallorganics steam input deposition two step compositions.
2. technique according to claim 1, wherein said plasma clean is by Ar, the rare gas such as Kr are filled with in vacuum tank, on workpiece, apply the plasma body that high pressure produces rare gas, in these plasma bodys, the ion bombardment workpiece surface of positively charged reaches the effect of plasma cleaning.
3. technique according to claim 1, wherein said metal net mask plasma deposition is that the tinsels such as pure Ti, Cr are placed in and in metal net mask, carry out plated film together with workpiece, at this moment energy of plasma ratio is high a lot of while cleaning, high-octane plasma is known from experience bombardment pure Ti, Cr, make these metallic elements produce sputter or effusion effect, because workpiece and these tinsels are separated by very near, thereby can deposit at workpiece surface the metal prime coat of Ti, the Cr of thin layer, sometimes also can in tank body, be filled with as required N
2, the nitride of generation Ti, Cr, forms gradient film.
4. technique according to claim 1, wherein said metallorganics steam input deposition is that the organism liquid that contains the metallic element such as Ti, Cr is placed in external metal tin, after making it become steam by heating, pass in vacuum tank, under ion bombardment effects, steam can become plasma body, thereby forms metal prime coat at workpiece surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410193574.5A CN103952663A (en) | 2014-05-02 | 2014-05-02 | Metal bottoming technology in diamond like coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410193574.5A CN103952663A (en) | 2014-05-02 | 2014-05-02 | Metal bottoming technology in diamond like coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103952663A true CN103952663A (en) | 2014-07-30 |
Family
ID=51330007
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410193574.5A Pending CN103952663A (en) | 2014-05-02 | 2014-05-02 | Metal bottoming technology in diamond like coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103952663A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420673A (en) * | 2015-12-09 | 2016-03-23 | 上海应用技术学院 | Diamond-like micro-nano coating for rubber mold and preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768724A (en) * | 2008-12-29 | 2010-07-07 | 中国科学院兰州化学物理研究所 | Method for preparing film on stainless steel |
| CN202558926U (en) * | 2012-05-30 | 2012-11-28 | 合肥永信等离子技术有限公司 | Equipment capable of realizing high-speed deposited diamond-like film on surface of three-dimensional workpiece |
| CN103469205A (en) * | 2013-08-01 | 2013-12-25 | 合肥永信等离子技术有限公司 | Coating process for lotus leaf-like diamond film |
| CN203382818U (en) * | 2013-08-01 | 2014-01-08 | 合肥永信等离子技术有限公司 | Device for plating diamond-like film on surface of flat plate |
| CN103510053A (en) * | 2012-06-29 | 2014-01-15 | 陈伟 | Method for plating metal surface with diamond-like carbon (DLC) film |
-
2014
- 2014-05-02 CN CN201410193574.5A patent/CN103952663A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768724A (en) * | 2008-12-29 | 2010-07-07 | 中国科学院兰州化学物理研究所 | Method for preparing film on stainless steel |
| CN202558926U (en) * | 2012-05-30 | 2012-11-28 | 合肥永信等离子技术有限公司 | Equipment capable of realizing high-speed deposited diamond-like film on surface of three-dimensional workpiece |
| CN103510053A (en) * | 2012-06-29 | 2014-01-15 | 陈伟 | Method for plating metal surface with diamond-like carbon (DLC) film |
| CN103469205A (en) * | 2013-08-01 | 2013-12-25 | 合肥永信等离子技术有限公司 | Coating process for lotus leaf-like diamond film |
| CN203382818U (en) * | 2013-08-01 | 2014-01-08 | 合肥永信等离子技术有限公司 | Device for plating diamond-like film on surface of flat plate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420673A (en) * | 2015-12-09 | 2016-03-23 | 上海应用技术学院 | Diamond-like micro-nano coating for rubber mold and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107142463B (en) | A kind of coating method that plasma activated chemical vapour deposition is compound with magnetron sputtering or ion plating | |
| CN109797363B (en) | Arc light electron source assisted ion nitriding process | |
| CN109778136B (en) | Method for preparing diamond-like coating by adopting thermionic plasma technology | |
| CN110098044B (en) | Composite modification method for surface protection of neodymium iron boron magnet | |
| CN105200381B (en) | The auxiliary magnetic control sputtering film plating device of anodic field | |
| CN110400738B (en) | Method for improving micro-channel plate resolution and evaporation method thereof | |
| JP5607760B2 (en) | CVD apparatus and CVD method | |
| CN109055901A (en) | A kind of device and technique improving hard coat and substrate binding force | |
| CN107858684B (en) | Metal-diamond-like composite coating, preparation method and application thereof and coated tool | |
| CN114481071B (en) | Coating device and DLC coating process | |
| CN106048531A (en) | ICP reinforced multi-target magnetron sputtering device and method for preparing TiO2 film by using device | |
| CN202558926U (en) | Equipment capable of realizing high-speed deposited diamond-like film on surface of three-dimensional workpiece | |
| CN111321384A (en) | Method for preparing zirconium dioxide film on nickel-based alloy | |
| CN102534514A (en) | Method for plating films of multi-arc ion plating | |
| CN108085651B (en) | Electron beam bombardment resistant secondary electron emission composite film and preparation method thereof | |
| CN105200390A (en) | Method for restraining secondary electron emission by directly depositing nano-graphene | |
| CN102330057B (en) | Method for preparing metal ruthenium film for hard semiconductor component | |
| CN111378947B (en) | Preparation method of diamond-like thin film | |
| CN106319468A (en) | Method for increasing quality of magnetron sputtering coating | |
| CN103952663A (en) | Metal bottoming technology in diamond like coating | |
| US20120237790A1 (en) | Housing and method for making the same | |
| CN201793721U (en) | Vacuum electronic gun coating machine | |
| CN114134566B (en) | Method for improving heterogeneous epitaxial nucleation uniformity of diamond | |
| US8512859B2 (en) | Housing and method for making the same | |
| CN209307474U (en) | A kind of device improving hard coat and substrate binding force |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140730 |