CN108330445B - A method for multi-arc ion plating of titanium-doped diamond-like film on the surface of punching needle - Google Patents
A method for multi-arc ion plating of titanium-doped diamond-like film on the surface of punching needle Download PDFInfo
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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
- C23C14/0021—Reactive sputtering or evaporation
-
- 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
- C23C14/0605—Carbon
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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Abstract
The invention discloses a method for plating a titanium-doped diamond-like film on the surface of a punching needle head by using multi-arc ions, which belongs to the technical field of film plating processes.
Description
Technical Field
The invention belongs to the technical field of film coating processes, and particularly relates to a method for plating a titanium-doped diamond-like film on the surface of a punching needle by multi-arc ions.
Background
The fiber-forming polymer is dissolved in solvent to form solution, or the fiber-forming polymer slices are heated and melted in a screw extruder to form melt, the melt is fed into a spinning machine after the preparation process before spinning, the spinning solution or the melt is quantitatively, continuously and uniformly extruded from the fine holes of a spinning nozzle by a spinning pump (metering pump), the fine flow is solidified in water, coagulating liquid or air to generate nascent fiber, and the process is fiber forming. The spinning nozzle is a key part of a chemical fiber spinning machine and is provided with a plurality of micropores with the same size. Since the surface of chemical fiber product must be smooth, it requires high inner wall smoothness of the spinneret micropores, and therefore, the roughness of the surface of the carbon steel needle used for spinneret punching must be low, otherwise the quality of fiber will be directly affected. The carbon steel needle used at present has some problems which need to be solved urgently: (1) the frequent collision of the needle head and the spinning nozzle during the punching process can cause the needle head to be extruded and even broken; (2) during the punching process, the surface of the needle is abraded by friction. When the problems occur, manual re-grinding or replacement is needed, which can seriously reduce the production efficiency and cause the increase of the production cost, and the economic benefit of the factory is directly influenced. In order to further develop the chemical fiber industry, the hardness and strength, i.e. wear resistance, of carbon steel needles need to be improved, and the carbon steel needles also need to have a small friction coefficient.
The actual punching number of the uncoated high-speed steel needle head is 2100 holes, namely, one high-speed steel needle head can only complete the punching task of one spinning nozzle. In the spinneret punching period, the phenomenon of abrasion and wear-out easily occurs to the pinhead, the pinhead is firstly polished by a numerical control needle grinding machine and then is manufactured by manual multiple grinding and polishing, and finally the shape and the size of the pinhead are checked by a numerical control needle measuring machine, so that time and labor are wasted. Once worn out, the need to immediately replace a new needle and make a spare needle affects the order completion speed and efficiency.
As can be seen from the above, surface engineering of the carbon steel needle is required, and common surface engineering techniques include surface quenching and chemical heat treatment, overlay welding, thermal spraying, electroplating, vapor deposition, which includes Chemical Vapor Deposition (CVD) and Physical Vapor Deposition (PVD). Chemical vapor deposition is currently mainly: the atmospheric pressure chemical vapor deposition, the ultrahigh vacuum chemical vapor deposition, the low pressure chemical vapor deposition and the physical vapor deposition methods mainly comprise: vacuum evaporation, sputter coating, arc plasma coating, and the like. The first three methods in the surface engineering technology have high energy consumption, electroplating not only has high energy consumption but also can bring pollution, and the electroplating is forbidden by the national regulations at present, and vapor deposition has the characteristics of low energy consumption, small pollution, uniform film layer and the like.
A new thin film, namely a diamond-like carbon thin film (DLC), is a metastable material formed by combining sp2 and sp3 bonds, has the properties of high hardness, high elastic modulus, high thermal conductivity, high chemical stability, low friction coefficient, low thermal expansion coefficient and the like, and is an ideal film layer. For diamond-like thin films, because of their unstable materials, there are large internal stresses inside, which can reduce the film-substrate bonding strength; meanwhile, the DLC film is gradually graphitized when the temperature reaches above 350 e.
The main method for depositing DLC film is multi-arc ion plating, which uses multi-arc vacuum ion plating machine, the ion plating is to deposit evaporant or reactant on the substrate in the vacuum chamber by gas discharge or partial separation of evaporant, while the gas ion or evaporant particle bombards. The multi-arc ion plating has the following advantages: (1) the ionization rate is high and can reach 60 to 80 percent; (2) the evaporation rate is high; (3) the incident particle energy is high, and the formed film has high density, good adhesiveness and good durability; (4) the plasma is directly generated from the cathode, and the cathode target can be arranged in any direction according to the shape of the workpiece, so that the clamp can be greatly simplified.
Disclosure of Invention
In order to overcome the defects of the background art, the invention provides a method for plating a titanium-doped diamond-like film on the surface of a punching needle by multi-arc ions.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for multi-arc ion plating of a titanium-doped diamond-like film on the surface of a punching needle head comprises the following steps:
(1) polishing the surface of the punching needle head substrate sample step by using water abrasive paper, and using Al2O3Polishing the powder to a mirror surface state until no obvious scratch is formed on the surface of the substrate;
(2) putting a punching needle head substrate sample into an ultrasonic cleaning machine, sequentially carrying out ultrasonic cleaning in petroleum ether and absolute ethyl alcohol, drying, and putting into a vacuum chamber of a multi-arc vacuum ion plating machine for deposition;
(3) starting a multi-arc vacuum ion plating machine, wherein the target material selected by the multi-arc vacuum ion plating machine is a titanium target, vacuumizing, heating, filling argon, controlling the flow of the argon, maintaining the stability of air pressure, starting bias bombardment, and performing glow cleaning until a bias gauge pointer is stable;
(4) arc cleaning is carried out, bias voltage is maintained, and the current of the titanium target is adjusted;
(5) adjusting the bias voltage, passing C2H2And plating a Ti-containing diamond-like film on the punching needle substrate sample.
Preferably, in the step (1), the surfaces of the punched needle base samples are polished step by using water-milled sandpaper of 240#, 320#, 600#, 800#, 1000#, and 2000#, so as to remove oxide layers, burrs and the like on the surfaces of the needles, thereby ensuring good film-forming quality.
Preferably, in the step (2), ultrasonic cleaning is respectively carried out in petroleum ether and absolute ethyl alcohol for 30min, the petroleum ether and the absolute ethyl alcohol are both analytically pure, and the ultrasonic cleaning power is 500W; ultrasonic cleaning is carried out to remove various dust, grease, sweat stains, adsorbed gas and the like adhered to the surface of the substrate so as to ensure strong film-substrate binding force.
Preferably, in step (3), vacuum is applied to 5X 10-3Pa, heating to 200 deg.C after 50-80min, introducing 99.99% high purity argon gas, controlling the flow of argon gas to gradually decrease from 80sccm to 50sccm, and maintaining the pressure at 5 × 10- 2Pa; when the glow cleaning is carried out, the duty ratio is adjusted to be 60%, the bias voltage is gradually increased to-600V from-400V, and the cleaning time is 5-8min until the pointer of the bias voltage meter is stable. The surface of the workpiece after chemical cleaning still leaves very thin residual substances, and in addition, the vacuum chamber is not clean at all, and the dirty parts can generate abnormal discharge phenomena to generate stains in the vacuum ion discharge process, so the workpiece needs to be cleaned by glow ion bombardment to obtain high-quality coating. The main function of the device is to collide the gas adsorbed on the surface of the workpiece, impurity atoms and atoms on the surface layer of the workpiece, namely to activate the metal surface so as to improve the binding force and the film forming quality of the coating. In addition, when the ions with high energy bombard the workpiece, the energy is transferred to the workpiece, so that the temperature of the workpiece is raised, and the function of pre-bombardment heating is achieved.
Preferably, in step (4), the bias voltage is maintained between-400V and-500V, the titanium target current is adjusted to be 115A, and the cleaning time is 4 min. The arc cleaning purpose is as follows: further bombarding, sputtering and cleaning the surface of the activated matrix; coarsening the surface of the matrix to generate defects and improving the film-substrate binding force; the temperature of the matrix is raised, and an additional heating source is not needed; the bombarding ions can generate non-diffusion type mixing on the surface area of the sample to form a co-permeation layer, and the film/base binding force is greatly improved.
Preferably, in step (5), the bias voltage is adjusted to-250V, C2H2The flow rate of (2) is controlled to be 300sccm, and the time for plating the Ti-containing diamond-like film is controlledIt is 45 min.
Preferably, in the step (5), the alloying element comprises one of W, Mo, Cr, V, Co or Ti, and the alloying element is dissolved, so that the material has good high-temperature strength, and the softening degree of steel is reduced, so that the intrinsic hardness of the steel can be maintained in the spinneret punch hole after high-temperature deposition.
The invention has the advantages that: the invention has simple manufacturing process, greatly improves the punching performance compared with the non-film-coated punching needle, thereby prolonging the service life of the punching needle of the spinning nozzle, has good high-temperature strength of the material and reduced softening degree of steel along with the fusion of alloy elements, and can keep the intrinsic hardness in the punching needle of the spinning nozzle after the high-temperature film coating.
Drawings
FIG. 1 is a physical diagram of a high-speed steel punch needle tip under a 100-fold microscope used in the present invention;
FIG. 2 is an optical micrograph of Ti-doped DLC deposited by multi-arc ion plating at different bias voltages, wherein (a) to 150V; (b) -200V; - (c) 250V;
FIG. 3 is a photomicrograph of an in situ punch through Ti-doped DLC coated needle prepared in example 1, where (a) the holes are punched 2900 times; (b) punching 4900 times.
Detailed Description
The invention will be further described with reference to the accompanying drawings in which:
example 1
In this example, the chemical compositions of high-speed steel and punch pin provided by Beijing Huayu Innovation Korea company are shown in Table 1.
TABLE 1 high speed steel punch needle chemical composition
The whole length of the needle is 36mm, the diameter is 1.0mm, the diameter of the needle point is about 0.06mm, and the length is about 0.4 mm. And (3) depositing the DLC film by using a multi-arc vacuum ion plating machine, wherein the target material selected by the multi-arc vacuum ion plating machine is a titanium target.
Firstly, the surface of a carbon steel needle head substrate sample is gradually ground by using water abrasive paperGrade sanding (240# -320 # -600 # -800 # -1000 # -2000 #), and using Al2O3And (4) polishing the powder to a mirror surface state until no obvious scratch is formed on the surface of the substrate. And then, ultrasonically cleaning the sample by using an ultrasonic cleaning machine with the power of 500W, sequentially cleaning the sample in petroleum ether (analytically pure) and absolute ethyl alcohol (analytically pure) for 30min, drying the sample by using a blower, and putting the dried sample into a vacuum chamber of a multi-arc vacuum ion plating machine for deposition.
Adjusting parameters of multi-arc vacuum ion plating machine, firstly vacuumizing to 5 × 10-3Heating to 200 deg.C after Pa and 60min, introducing 99.99% high purity argon gas, controlling flow gradually from 80sccm to 50sccm, and maintaining gas pressure at 5 × 10-2Pa, starting bias voltage bombardment, and performing glow cleaning, wherein the duty ratio is adjusted to be 60%, the bias voltage is gradually increased to-600V from-400V, and the cleaning time is controlled to be about 6min until the pointer of the bias voltage meter is stable. Then arc cleaning is carried out, the bias voltage is maintained between-400V and-500V, the current of the titanium target is 115A, and cleaning is carried out for 4 min. Adjust bias to-250V and then let in C2H2The flow rate was controlled at 300sccm, and a DLC film containing Ti was plated on the substrate. And repeating the steps to perform multi-period compounding operation on the high-speed steel matrix.
Example 2
Based on example 1, in this example, only in the last step of example 1, the bias voltage was adjusted to-150V, and then C was introduced2H2The flow rate was controlled at 300sccm, and a DLC film containing Ti was plated on the substrate. The rest of the process was identical to example 1.
Example 3
Based on example 1, in this example, only in the last step of example 1, the bias voltage was adjusted to-200V, and then C was introduced2H2The flow rate was controlled at 300sccm, and a DLC film containing Ti was plated on the substrate. The rest of the process was identical to example 1.
Sample detection and analysis:
optical micrographs of Ti-doped DLC deposited at different biases for examples 1, 2, 3 are shown in FIG. 2, where (a) -150V; (b) -200V; (c) -250V; the results show that the bias voltage is-150V, the surface appearance of the film layer is rough, the number of liquid drops is large and the size is large. The bias voltage is-200V, the number of surface liquid drops is gradually reduced, the compactness of the film layer is improved, the surface roughness is reduced, the film layer is compact, and the particle size is refined. The bias voltage is-250V, the surface of the film layer is flat and further smooth and compact, and the quantity of liquid drops is almost zero. Due to the fact that the bias voltage is increased, the ion energy for bombarding the thin film is increased, the diffusion activity is high, large particles are not prone to being gathered, and in addition, the bombardment of high-energy ions is also beneficial to smashing the large particles in the thin film, so that the quantity and the size of liquid drops are reduced. It can be seen that the bias has a significant effect on the roughness of the film surface. The increase in bias voltage can appropriately suppress large particles from reaching the substrate surface. The smaller the particle size, the more pronounced the electric field force contrast advantage, i.e. the more sensitive the bias is to small-scale particle purification. On the other hand, under bias voltage, the high-energy ion bombardment can refine macro particles, and the macro particles are eliminated through sputtering stripping, so that the surface purification effect is achieved. But when the bias voltage value increases again, the surface may exhibit dishing. This is because the combination of the droplets and the film is poor, the bias voltage is increased, the bombardment effect of the ions on the deposited film is enhanced, and some defects such as large droplet particles are easily sputtered off.
As shown in fig. 3, which is a microphotograph of in-situ punching of Ti-doped DLC coated needles prepared in example 1, wherein (a) the punching is 2900 times; (b) punching 4900 times. Fig. 3(a) shows a photomicrograph after punch 2900, with the film layer ground thin; fig. 3(b) shows a photomicrograph after punching 4900, where the film begins to peel off in the workplace region. Compared with the practical 2100 holes punched by the high-speed steel needle without the film coating, the number of holes punched by the DLC film-coated needle is doubled, and the punching performance of the punching needle is greatly improved.
Finally, it should be noted that: it should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (1)
1. A method for multi-arc ion plating of a titanium-doped diamond-like film on the surface of a punching needle head is characterized by comprising the following steps:
(1) polishing the surface of the punching needle head substrate sample step by using water abrasive paper, and using Al2O3Polishing the powder to a mirror surface state until no obvious scratch is formed on the surface of the substrate;
(2) putting a punching needle head substrate sample into an ultrasonic cleaning machine, sequentially carrying out ultrasonic cleaning in petroleum ether and absolute ethyl alcohol, drying, and putting into a vacuum chamber of a multi-arc vacuum ion plating machine for deposition;
(3) starting a multi-arc vacuum ion plating machine, wherein a target material selected by the multi-arc vacuum ion plating machine is a titanium target, vacuumizing, heating, filling argon, controlling the flow of the argon, maintaining the stability of air pressure, starting bias bombardment, and performing glow cleaning until a bias gauge pointer is stable;
(4) arc cleaning is carried out, bias voltage is maintained, and the current of the titanium target is adjusted;
(5) adjusting the bias voltage, passing C2H2Plating a diamond-like film containing alloy elements on a punching needle substrate sample;
wherein:
in the step (1), the surfaces of the punching needle head base body samples are sequentially polished step by using water grinding sand paper of 240#, 320#, 600#, 800#, 1000#, and 2000 #;
in the step (2), ultrasonic cleaning is respectively carried out in petroleum ether and absolute ethyl alcohol for 30min, the petroleum ether and the absolute ethyl alcohol are both analytically pure, and the power of an ultrasonic cleaning machine is 500W;
in the step (3), vacuum-pumping is carried out to 5X 10-3Pa, heating to 200 deg.C after 50-80min, introducing 99.99% high purity argon gas, controlling the flow of argon gas to gradually decrease from 80sccm to 50sccm, and maintaining the pressure at 5 × 10-2Pa; when glow cleaning is carried out, the duty ratio is adjusted to be 60%, the bias voltage is gradually increased to-600V from-400V, and the cleaning time is 5-8min until the pointer of the bias voltage meter is stable;
in the step (4), the bias voltage is maintained between minus 400V and minus 500V, the titanium target current is adjusted to be 115A, and the cleaning time is 4 min;
in the step (5), the step (c),
adjusting the bias voltage to-250V, C2H2The flow rate of the alloy element is controlled to be 300sccm, and the time for plating the diamond-like film containing the alloy element is 45 min;
the alloy element is Ti.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
| CN101792898A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院宁波材料技术与工程研究所 | Carbon film for improving abrasion resistance of magnesium alloy and preparation method thereof |
| CN102817008A (en) * | 2012-08-01 | 2012-12-12 | 南京航空航天大学 | Preparation method of Ag-Ti-codoped diamond like carbon (DLC) film |
| CN104141109A (en) * | 2014-06-19 | 2014-11-12 | 武汉大学 | Method for in-situ synthesis of composite TiC-DLC coating on surface of titanium |
| CN107338414A (en) * | 2016-05-03 | 2017-11-10 | 大连金泰表面工程科技有限公司 | Conduction, anticorrosive, wear-resistant, the preparation method of high-hardness diamond-like coating |
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| CN102092166A (en) * | 2009-12-09 | 2011-06-15 | 中国科学院兰州化学物理研究所 | Multilayered gradient diamond like nano composite coating for aluminum alloy piston and preparation method thereof |
| CN103920185B (en) * | 2014-04-25 | 2017-10-31 | 岭南师范学院 | A kind of metal-doped composite diamond coating titanium alloy artificial Bones and joints of Mo and preparation method thereof |
| CN106637207B (en) * | 2016-12-30 | 2019-08-23 | 纳峰真空镀膜（上海）有限公司 | A kind of high temperature resistant diamond-like coating method in graphite substrate |
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| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
| CN101792898A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院宁波材料技术与工程研究所 | Carbon film for improving abrasion resistance of magnesium alloy and preparation method thereof |
| CN102817008A (en) * | 2012-08-01 | 2012-12-12 | 南京航空航天大学 | Preparation method of Ag-Ti-codoped diamond like carbon (DLC) film |
| CN104141109A (en) * | 2014-06-19 | 2014-11-12 | 武汉大学 | Method for in-situ synthesis of composite TiC-DLC coating on surface of titanium |
| CN107338414A (en) * | 2016-05-03 | 2017-11-10 | 大连金泰表面工程科技有限公司 | Conduction, anticorrosive, wear-resistant, the preparation method of high-hardness diamond-like coating |
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