CN105951044A - Preparation method of modified acetylene gas graphite carbon film - Google Patents

Preparation method of modified acetylene gas graphite carbon film Download PDF

Info

Publication number
CN105951044A
CN105951044A CN201610291946.7A CN201610291946A CN105951044A CN 105951044 A CN105951044 A CN 105951044A CN 201610291946 A CN201610291946 A CN 201610291946A CN 105951044 A CN105951044 A CN 105951044A
Authority
CN
China
Prior art keywords
preparation
matrix
amorphous carbon
acetylene
chromium
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
Application number
CN201610291946.7A
Other languages
Chinese (zh)
Inventor
宋福田
王忠平
张政民
李世涛
王泰吉
徐鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CRRC Qingdao Sifang Co Ltd
Original Assignee
CRRC Qingdao Sifang Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by CRRC Qingdao Sifang Co Ltd filed Critical CRRC Qingdao Sifang Co Ltd
Priority to CN201610291946.7A priority Critical patent/CN105951044A/en
Publication of CN105951044A publication Critical patent/CN105951044A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605Carbon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only

Abstract

The invention relates to the technical field of abrasion-resistant protective coatings, in particular to a preparation method of a modified acetylene gas graphite carbon film. The preparation method comprises the steps that S1, the surface of a matrix is pretreated; S2, the matrix subjected to surface pretreatment is placed in a vacuum cavity of non-balanced magnetron sputtering ion plating equipment; S3, the vacuum cavity is vacuumized; S4, carbon target currents are started; and S5, the gas mixture of argon and acetylene is guided into the vacuum cavity, and biasing is conducted on the matrix, so that the modified graphite carbon film is formed on the surface of the matrix. According to the modified graphite carbon film, the good bonding performance can be reserved while the hardness of the modified graphite carbon film is improved, and the friction coefficient and the abrasion rate are both decreased, so that the modified graphite carbon film has excellent performance and long service life. The ratio of sp3 to sp2 in the modified graphite carbon film can be regulated and controlled within a wide range by adjusting the proportion between acetylene and argon, and thus the tribology performance of the modified graphite carbon film is optimized.

Description

The preparation method of acetylene gas modification amorphous carbon coating
Technical field
The present invention relates to wear Protection coating technology field, particularly relate to a kind of acetylene gas modified The preparation method of amorphous carbon coating.
Background technology
Along with the development of modern Computerized Numerical Control processing technology, the production requirement of high-efficiency environment friendly day by day improves, The material of various extreme working conditions and difficult cutting also gets more and more, particularly high-speed cutting, DRY CUTTING and the appearance of micro-profit Cutting Process, propose the strictest wanting to cutting tool Ask.Hard films coating can reduce the friction and wear of workpiece, be effectively improved case hardness, toughness, Wearability and high-temperature stability, increase substantially the service life of coating product.Hard coat skill The appearance of art has adapted to the modern manufacturing industry high-tech requirement for metal cutting tool, is considered It it is the technical revolution of metal cutting tool.Before carbon film has development and application as one very much The hard friction coat material of scape, is paid close attention to the most widely, is had been applied to industry In production.
Rely on sputtering graphite target, the amorphous carbon-film prepared by ion plating based on sp2 structure, Its optics, electricity are similar to graphite with character such as tribology, generally known as amorphous carbon coating (Graphite-Like Carbon, GLC).Utilize the chemical gaseous phase deposition that Hydrocarbon decomposes The amorphous carbon-film that method (CVD) is prepared often contains higher sp3C-C linkage content, and its character is more Add close to diamond, and be referred to as diamond-like carbon film (Diamond-Like Carbon, DLC).Though carbon film prepared by two kinds of methods is all hard friction coat, but character is different. Under hydrogeneous DLC smooth surface prepared by CVD, DRY SLIDING, coefficient of friction is low;And GLC Then bearing capacity is good, good environmental adaptability.Owing to deposition principle is different with technological parameter, typically Do not co-deposit under same process conditions.Up to now, there is no one by compound DLC And GLC, obtain a kind of while retaining the feature that GLC bond strength is high, bearing capacity is good, Reduce the process of its coefficient of friction.
Summary of the invention
(1) to solve the technical problem that
The technical problem to be solved in the present invention is to provide a kind of acetylene gas modification amorphous carbon coating Preparation method, forms modified amorphous carbon coating layer, it is possible to realize reduction and rub on workpiece substrate surface Wipe coefficient and wear rate.
(2) technical scheme
In order to solve above-mentioned technical problem, the invention provides a kind of acetylene gas modification class graphite The preparation method of carbon film, including: step S1, carries out surface preparation to matrix;Step S2, Matrix after surface preparation being completed puts into the vacuum chamber of non-balance magnetically controlled sputter ion plating equipment In;Step S3, vacuum chamber is carried out evacuation;Step S4, unlatching carbon target current;Step S5, in vacuum chamber, it is passed through the mixed gas of argon and acetylene, to matrix biasing, with at base Surface forms modified amorphous carbon coating layer.
According to the present invention, in step s 5, the air inflow of acetylene is less than the air inflow of argon.
According to the present invention, in step s 5, the air inflow of acetylene is 5-15sccm, entering of argon Tolerance is 15-20sccm.
According to the present invention, in step s 5, substrate bias is 55-100V.
According to the present invention, after performing step S3, before execution step S4, perform step S31, unlatching chromium target current, be passed through argon, to matrix biasing, with to matrix in vacuum chamber Surface is carried out.
According to the present invention, after performing step S31, before execution step S4, perform step S32, it is gradually increased chromium target current, is gradually lowered substrate bias, to form matrix at matrix surface Blended layer with chromium.
According to the present invention, after performing step S32, before execution step S4, perform step S33, it is gradually increased chromium target current, forms pure chromium transition zone with deposition chromium in matrix blended layer.
According to the present invention, in step s 4, it is gradually lowered chromium target current, is gradually increased carbon target electricity Stream, forms compound transition zone with deposition chromium and carbon on pure chromium transition zone.
According to the present invention, in step s 5, chromium target current is 0.2-0.5A.
According to the present invention, in step s 2, the matrix after surface preparation being completed puts into three axles In rotation cage, then three axles rotation cages are put in vacuum chamber.
(3) beneficial effect
The technique scheme of the present invention has the advantage that
The preparation method of the acetylene gas modification amorphous carbon coating of the present invention, by matrix In vacuum chamber, it is passed through the mixed gas of acetylene and argon while sputtered carbon, utilizes sputtering method multiple Conjunction chemical vapour deposition technique acts on jointly prepares modified amorphous carbon coating layer, this modification class graphite Carbon film layer can retain good binding ability while hardness improves, and coefficient of friction and mill Loss rate all lowers, thus has the performance of excellence and longer service life.Further, by adjusting The ratio of modified amorphous carbon coating layer inside sp3 with sp2 can be entered by the ratio of joint acetylene and argon The regulation and control that row is interior in a big way, to optimize its tribological property, reach to improve modified class graphitic carbon Film performance adapts it in the purpose of different operating modes.
Accompanying drawing explanation
Fig. 1 is the flow process of the preparation method of embodiment of the present invention acetylene gas modification amorphous carbon coating Schematic diagram;
Fig. 2 is that the preparation method of embodiment of the present invention acetylene gas modification amorphous carbon coating uses The structural scheme of mechanism of equipment;
Fig. 3 is modified GLC and the XRD figure spectrum of common sputtering GLC adding acetylene;
Fig. 4 is the modified GLC adding acetylene recorded by XPS and common sputtering GLC C1 peak figure;
Fig. 5 is the modified GLC adding acetylene recorded by friction wear testing machine and commonly spatters Penetrate the coefficient of friction figure of GLC;
Fig. 6 is the modified GLC and common sputtering GLC being recorded by contourograph and adding acetylene After wear extent, the specific wear rate figure obtained.
In figure: 101: revolution pivoted frame;102: rotation pivoted frame;103: third level rotating cage;201、 202: chromium target;301,302: carbon target.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below will knot Close the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, It is fully described by, it is clear that described embodiment is a part of embodiment of the present invention, and not It it is whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having There is on the premise of making creative work the every other embodiment obtained, broadly fall into the present invention The scope of protection.
Embodiment one
As depicted in figs. 1 and 2, the preparation method of acetylene gas modification amorphous carbon coating of the present invention A kind of embodiment one.As it is shown in figure 1, the acetylene gas modification class graphitic carbon of the present embodiment one The preparation method of film specifically includes following steps:
Step S1: matrix is carried out surface preparation, matrix refers to pending surface Hardening Treatment Workpiece.In the present embodiment one, utilize supersonic flow waterline that the surface of this matrix is carried out clearly Wash.
Step S2: the matrix after surface preparation being completed is put into three axles and rotated cage, then by three Axle rotates cage and puts into the vacuum chamber of non-balance magnetically controlled sputter ion plating equipment.As in figure 2 it is shown, this Three axles that embodiment one uses rotate cage and include revolve round the sun pivoted frame 101, rotation pivoted frame 102 and the third level Rotating cage 103, rotation pivoted frame 102 is provided with moving tooth, and this moving tooth coordinates with third level rotating cage 103, When rotation pivoted frame 102 rotates, it is possible to stir third level rotating cage 103 rotation by moving tooth.Base Body is fixed in third level rotating cage 103, can be with third level rotating cage 103 from transferring in vacuum chamber Rotate.Thus, the uniformity of the coating composition formed at matrix surface can be improved, and permissible In third level rotating cage 103, place multiple matrixes, it is achieved the multiple matrixes of disposable process simultaneously, Ensure the coating of the surface forming component uniformity of multiple matrix simultaneously, thus be greatly improved work Industry efficiency.It is provided with two in the vacuum chamber of the non-balance magnetically controlled sputter ion plating equipment of the present embodiment one Individual chromium target and two carbon targets, as in figure 2 it is shown, chromium target 201 and chromium target 202 are for matrix Sputtering chromium, carbon target 301 and carbon target 302 are for sputtered carbon on matrix.
Step S3: vacuum chamber is carried out evacuation, makes the vacuum in vacuum chamber reach 3 × 10-5torr Below.
Step S31: matrix surface is carried out plasma cleaning.Open two chromium target currents, Xiang Zhen It is passed through argon in cavity, to matrix biasing, starts matrix surface is carried out plasma cleaning. Specifically, during matrix surface is carried out plasma cleaning, the electric current of two chromium targets is equal For 0.3-0.6A, substrate bias is 400-600V, and the air inflow of argon is 10-30sccm, cleans Time is 20-40min.Preferably, in the present embodiment one, the electric current of two chromium targets is 0.5A, Substrate bias is 500V, and the air inflow of argon is 20sccm, and scavenging period is 30min.
Step S32: prepare the blended layer of matrix and chromium.After plasma cleaning terminates, gradually increase Add chromium target current, be gradually lowered substrate bias, to form being blended of matrix and chromium at matrix surface Layer.Specifically, in the 60-180s after plasma cleaning terminates, by equal for the electric current of two chromium targets Be gradually increased to 1-3A, substrate bias be gradually decreased to 100-150V, with start to prepare matrix with The blended layer of chromium, preparation time is 20-30min.Preferably, in the present embodiment one, waiting Ion Cleaning terminate after 120s in, the electric current of two chromium targets is increased to 2A by 0.5A, By 500V, substrate bias is down to 120V, and the time preparing matrix and the blended layer of chromium is 25min。
Step S33: prepare pure chromium transition zone.After prepared by blended layer, it is gradually increased two Chromium target current, forms pure chromium transition zone with deposition chromium in matrix blended layer.Specifically, altogether In 1-3min after mixed layer preparation, the electric current of two chromium targets is all gradually increased to 6-8A, Substrate bias is gradually decreased to 60-80V, utilizes sputtering method deposition chromium, form pure chromium transition zone, Sedimentation time is 15-25min.Preferably, in the present embodiment one, prepare complete in blended layer After 2min in, the electric current of two chromium targets is gradually increased to 7A by 2A, by substrate bias Being gradually decreased to 70V by 120V, the chromium deposition time is 20min, and the thickness of pure chromium transition zone is 200-800nm。
Step S4: the compound transition zone of preparation.Pure chromium transition zone prepare complete after, gradually drop Low chromium target current, opens carbon target current, and is gradually increased carbon target current, with at pure chromium transition zone Upper deposition chromium and carbon form compound transition zone.Specifically, pure chromium transition zone prepare complete after 20-40min in, the electric current of two chromium targets is all gradually decrease to 0.2-0.4A, by two carbon The electric current of target is all gradually increased to 7-9A, completes the deposition of the compound transition zone of chromium and carbon.Preferably Ground, in the present embodiment one, pure chromium transition zone prepare complete after 30min in, by two The electric current of individual chromium target is gradually decrease to 0.3A by 7A, by the electric current of two carbon targets by 0A by Cumulative add to 8A.Thus complete the preparation of compound transition zone.
Step S5: the modified amorphous carbon coating layer of preparation.After prepared by compound transition zone, to The mixed gas of argon and acetylene, and the air inflow of acetylene entering less than argon it is passed through in vacuum chamber Tolerance, to form modified amorphous carbon coating layer at matrix surface.Specifically, the air inflow of acetylene For 5-15sccm, the air inflow of argon is that 15-20sccm, acetylene and argon are sufficiently mixed and are passed through In vacuum chamber.The electric current of two one of them chromium targets 201 of chromium target is disconnected, i.e. chromium target 201 Electric current be 0A, the electric current of another chromium target 202 is 0.2-0.5A, preferably 0.25A.Matrix Bias is 55-100V, and the electric current of two carbon targets is 7-8A.Utilize sputtering method composite chemical gas Phase sedimentation acts on jointly prepares modified amorphous carbon coating layer.Sedimentation time is 5-7 hour, excellent Electing 6 hours as, the thickness of the modified amorphous carbon coating layer of preparation is 2-3.5 μm.
The preparation method of the acetylene gas modification amorphous carbon coating of the present embodiment one, in preparation modification During amorphous carbon coating layer, can be according to the reality requirement to surface of the work performance, by changing argon The ratio of gas and acetylene changes the structure of modified amorphous carbon coating layer, the modified class graphitic carbon of regulation The ratio of internal sp3 Yu sp2 of film layer, to reach to improve the purpose of modified amorphous carbon coating layer performance. Specifically, can regulate according to the requirement of surface of the work performance, if requiring preferably to combine Intensity and bearing capacity, then can reduce the ratio of acetylene;If improving modified class graphitic carbon Dry friction performance under the hardness of film layer and atmospheric condition, then increase acetylene gas that can be suitable Ratio.In general, modified amorphous carbon coating layer is based on sputtered carbon, and acetylene gas leads to The carbon crossing chemical gaseous phase deposition decomposition plays regulation modified amorphous carbon coating layer internal structure, improvement The effect of performance.Between matrix and modified amorphous carbon coating layer, deposit pure chromium transition zone, be for Directly by modification class stone when preventing that between matrix and modified amorphous carbon coating layer, performance difference is the biggest Ink carbon film layer is plated on matrix and modified amorphous carbon coating pull-up can be caused to fall, by pure chromium transition zone The bond strength of modified amorphous carbon coating layer and collective can be improved.According to matrix and modified class stone The thickness of pure chromium transition zone can be adjusted by the size of ink carbon film layer performance difference, works as matrix And performance difference can suitably increase pure chromium transition zone time excessive between modified amorphous carbon coating layer Thickness, improves the bond strength of modified amorphous carbon coating layer and matrix.
The preparation method of the acetylene gas modification amorphous carbon coating of the present embodiment one, by base In vacuum chamber, it is passed through the mixed gas of acetylene and argon on body while sputtered carbon, utilizes sputtering Method composite chemical vapour deposition process acts on jointly prepares modified amorphous carbon coating layer, this modification class Graphite carbon film layer can retain good binding ability, and coefficient of friction while hardness improves All lower with wear rate, thus there is the performance of excellence and longer service life.Further, logical The ratio overregulating acetylene and argon can be to the ratio of modified amorphous carbon coating layer inside sp3 and sp2 Value carries out the regulation and control in a big way, to optimize its tribological property, reaches to improve modified class stone Ink carbon film layer performance adapts it in the purpose of different operating modes.
Embodiment two
Embodiment two provides one and commonly sputters the system of amorphous carbon coating (hereinafter referred GLC) The acetylene gas modification class stone of Preparation Method, the preparation method of the GLC of embodiment two and embodiment one The preparation method of ink carbon film (hereinafter referred modification GLC) is essentially identical, and something in common is the most superfluous Stating, difference is, in an embodiment, in step s 5, is only passed through argon in vacuum chamber Gas, and it is not passed through acetylene.
Thus, the modified LGC prepared by the method using embodiment one and employing embodiment two Performance and the structure of LGC prepared by method compare:
(1) with XRD-7000 type X-ray diffractometer, the phase composition of coating is analyzed, adopts With Cu K α as radiographic source, tube voltage is 40kV, and tube current is 40mA, and scanning speed is 8deg/min.Grazing angle is 0.5deg.It is illustrated in figure 3 the XRD figure spectrum of two kinds of coatings, Figure can be seen that in addition to corresponding to the polycrystalline state Cr diffraction maximum of transition Cr thin layer, do not occur Other crystal diffraction peaks, this shows that in GLC, carbon exists with non crystalline structure.Deposition process adds Acetylene gas, does not find that other crystal occurs mutually, modified GLC prepared after adding acetylene Coating is still non crystalline structure.
(2) utilize K-Alpha type x-ray photoelectron spectroscopy (XPS) to the composition of element and The chemical state of element is analyzed, and measures after using Ar ion gun etching 30s.Such as figure Shown in 4, contrast be passed through acetylene after modified GLC coating and the GLC for preparing of simple sputtered carbon target The C1s of the XPS of coating finely composes, and finds that modified GLC collection of illustrative plates C1s peak moves to right, bond energy liter High.If Fig. 4 is in terms of swarming result, after showing to introduce acetylene, in carbon film, sp3 key C content improves.
(3) use HT-500 type high temperature friction and wear testing machine to the coefficient of friction of sample and ratio Wear extent measures.Test environment is in atmosphere at room temperature, Si3N4Ball, as to mill material, carries Lotus is 225g, and sample rotation rate is 168rpm, utilizes contourograph to measure abrasion area of section, calculates Total wear extent and specific wear amount.The change in time of two kinds of coating coefficient of frictions as it is shown in figure 5, Being found by contrast, the modified GLC coefficient of friction adding acetylene is substantially reduced.In stable friction In the stage, the coefficient of friction of common sputtering GLC is 0.21, adds the modified GLC after acetylene and rubs Wipe coefficient and be reduced to 0.13.From Fig. 6 block diagram it can be seen that under 225g load, add Modified GLC specific wear rate after acetylene is by 1.08 × 10-15m3/ N m drops to 7.3 × 10-16m3/N·m。
(4) use JS-QHY-2 type ball trace instrument, utilize ball hole method that the thickness of coating is surveyed Amount.Use the orchidization institute automatic scratching instrument of WS-2005 coating adhesion strong to the combination of two kinds of coatings Degree is evaluated, and on scratching instrument, load is from 0 to 100N, and loading speed is 60N/min, at light The dropping situations of coating at Microscopic observation cut.Result shows commonly to sputter GLC and modified GLC The thickness of coating is about 2 μm.And it is loaded into 100N, does not occurs film phenomenon.
(5) painting is calculated with HXD-1000TMC/LCD microhardness testers and area equivalent model Layer hardness.Adopting 50g-1kg load on microscope to load, guarantor's load time is 15s, utilizes Jonsson-Hogmark formula calculates the Composite hardness of GLC from film base composite hardness.Survey Amount result shows, the microhardness adding the modified GLC after acetylene gas is increased by 3290HV To 3500HV, in conjunction with XPS analysis, show that sp3 hydridization C element content increase causes coating Hardness is significantly improved.
To sum up, the modified LGC using the method for embodiment one to prepare and the side using embodiment two LGC prepared by method compares, and hardness raising, coefficient of friction and wear rate all lower, and have More excellent performance.
Last it is noted that above example is only in order to illustrate technical scheme, and Non-to its restriction;Although the present invention being described in detail with reference to previous embodiment, ability The those of ordinary skill in territory is it is understood that it still can be to the skill described in foregoing embodiments Art scheme is modified, or wherein portion of techniques feature is carried out equivalent;And these are repaiied Change or replace, not making the essence of appropriate technical solution depart from various embodiments of the present invention technical side The spirit and scope of case.

Claims (10)

1. the preparation method of an acetylene gas modification amorphous carbon coating, it is characterised in that including:
Step S1, matrix is carried out surface preparation;
Step S2, surface preparation is completed after matrix put into non-balance magnetically controlled sputter ion plating In the vacuum chamber of equipment;
Step S3, vacuum chamber is carried out evacuation;
Step S4, unlatching carbon target current;
Step S5, in vacuum chamber, it is passed through the mixed gas of argon and acetylene, to matrix biasing, To form modified amorphous carbon coating layer at matrix surface.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 1, It is characterized in that, in described step S5, the air inflow of acetylene is less than the air inflow of argon.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 1, It is characterized in that, in described step S5, the air inflow of acetylene is 5-15sccm, entering of argon Tolerance is 15-20sccm.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 1, It is characterized in that, in described step S5, substrate bias is 55-100V.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 1, It is characterized in that, before performing after described step S3, performing described step S4, perform Step S31, unlatching chromium target current, be passed through argon, to matrix biasing, with right in vacuum chamber Matrix surface is carried out.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 5, It is characterized in that, before performing after described step S31, performing described step S4, perform Step S32, it is gradually increased chromium target current, is gradually lowered substrate bias, to be formed at matrix surface Matrix and the blended layer of chromium.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 6, It is characterized in that, before performing after described step S32, performing described step S4, perform Step S33, it is gradually increased chromium target current, forms pure chromium transition with deposition chromium in matrix blended layer Layer.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 7, It is characterized in that, in described step S4, be gradually lowered chromium target current, be gradually increased carbon target electricity Stream, forms compound transition zone with deposition chromium and carbon on pure chromium transition zone.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 5, It is characterized in that, in described step S5, chromium target current is 0.2-0.5A.
The preparation method of acetylene gas modification amorphous carbon coating the most according to claim 1, It is characterized in that, in described step S2, the matrix after surface preparation being completed puts into three axles In rotation cage, more described three axles rotation cages are put in vacuum chamber.
CN201610291946.7A 2016-05-05 2016-05-05 Preparation method of modified acetylene gas graphite carbon film Pending CN105951044A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610291946.7A CN105951044A (en) 2016-05-05 2016-05-05 Preparation method of modified acetylene gas graphite carbon film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610291946.7A CN105951044A (en) 2016-05-05 2016-05-05 Preparation method of modified acetylene gas graphite carbon film

Publications (1)

Publication Number Publication Date
CN105951044A true CN105951044A (en) 2016-09-21

Family

ID=56913760

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610291946.7A Pending CN105951044A (en) 2016-05-05 2016-05-05 Preparation method of modified acetylene gas graphite carbon film

Country Status (1)

Country Link
CN (1) CN105951044A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109728307A (en) * 2017-10-27 2019-05-07 中国科学院大连化学物理研究所 A kind of preparation and bipolar plates and application of the metal double polar plates based on carbon film modification
CN109913798A (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
CN110863188A (en) * 2019-12-03 2020-03-06 中国建筑材料科学研究总院有限公司 Graphite-like hydrogen-containing carbon film, preparation method and optical film
CN111485208A (en) * 2020-03-20 2020-08-04 北京师范大学 Preparation method of lubricating coating of air-floating motor
CN112267100A (en) * 2020-09-30 2021-01-26 大连交通大学 Preparation method of carbon membrane material with high carrier concentration

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002161352A (en) * 2000-11-07 2002-06-04 Teer Coatings Ltd Carbon coating, method and apparatus for coating carbon, and article having such coating
CN101209606A (en) * 2007-12-25 2008-07-02 浙江大学 Self-lubricating abrasion-proof graphite//TiC gradient composite thin film
CN101818330A (en) * 2010-05-27 2010-09-01 中国船舶重工集团公司第十二研究所 Unbalanced magnetron sputtering C/Ta graphite-like carbon film and preparation method thereof
CN102230153A (en) * 2011-06-22 2011-11-02 西安理工大学 Method for self-lubricating steel balls for precision bearing by ion-plating GLC (graphite-like carbon) coating

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002161352A (en) * 2000-11-07 2002-06-04 Teer Coatings Ltd Carbon coating, method and apparatus for coating carbon, and article having such coating
CN101209606A (en) * 2007-12-25 2008-07-02 浙江大学 Self-lubricating abrasion-proof graphite//TiC gradient composite thin film
CN101818330A (en) * 2010-05-27 2010-09-01 中国船舶重工集团公司第十二研究所 Unbalanced magnetron sputtering C/Ta graphite-like carbon film and preparation method thereof
CN102230153A (en) * 2011-06-22 2011-11-02 西安理工大学 Method for self-lubricating steel balls for precision bearing by ion-plating GLC (graphite-like carbon) coating

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
宋福田等: "乙炔气改性类石墨涂层结构和性能研究", 《铸造技术》 *
王福贞等: "《气相沉积应用技术》", 31 January 2007 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109728307A (en) * 2017-10-27 2019-05-07 中国科学院大连化学物理研究所 A kind of preparation and bipolar plates and application of the metal double polar plates based on carbon film modification
CN109913798A (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
CN110863188A (en) * 2019-12-03 2020-03-06 中国建筑材料科学研究总院有限公司 Graphite-like hydrogen-containing carbon film, preparation method and optical film
CN111485208A (en) * 2020-03-20 2020-08-04 北京师范大学 Preparation method of lubricating coating of air-floating motor
CN111485208B (en) * 2020-03-20 2021-07-13 北京师范大学 Preparation method of lubricating coating of air-floating motor
CN112267100A (en) * 2020-09-30 2021-01-26 大连交通大学 Preparation method of carbon membrane material with high carrier concentration
CN112267100B (en) * 2020-09-30 2022-11-18 大连交通大学 Preparation method of carbon membrane material with high carrier concentration

Similar Documents

Publication Publication Date Title
CN105951044A (en) Preparation method of modified acetylene gas graphite carbon film
CN101444985B (en) Amorphous carbon coating and preparation method and application thereof
Sánchez-López et al. Doping and alloying effects on DLC coatings
CN104508171B (en) Coat system, the matrix of coating and the method with coat system coating matrix surface
CN106244986B (en) Diamond-like carbon film of functionally gradient and preparation method thereof and product
CN108690956A (en) Arc ion plating-magnetron sputtering composite deposition high-temperature wearable antifriction AlTiN nano laminated coatings and its preparation method and application
CN101712215B (en) TiCN series nanometer gradient compound multi-layer coating and method for preparing same
EP1900844B1 (en) Article with high-hardness carbon coating
CN106086806A (en) A kind of AlTiCrN high-temperature wear resistant coating and preparation method thereof
CN109504945A (en) A kind of space environment long acting antibiotic solid lubricating film and preparation method thereof
CN106811725A (en) Temperature range self adaptation lubricant coating wide and preparation method and application
CN110453190B (en) Composite magnetron sputtering preparation method of AlCrSiN/Mo self-lubricating film
CN106191794A (en) The coating method of titanium alloy surface superhard anti-friction wear-resistant composite film and titanium alloy material
CN106119783B (en) Diamond-like carbon film of functionally gradient and preparation method thereof and product
CN110438442A (en) A kind of nano silicon nitride niobium aluminium yttrium/amorphous silicon nitride two-phase superhard coating and its deposition method
CN107058949B (en) A kind of preparation method of wear-resisting tungsten disulfide film
CN114703454A (en) Wide-temperature-range wear-resistant self-lubricating CrVN/Ag composite coating and preparation method thereof
CN115287592A (en) High-temperature wear-resistant self-lubricating coating for fingertip sealing and preparation method thereof
CN108977775A (en) A kind of TiAlSiN coated cutting tool preparation process
CN108624881B (en) A kind of dry cutting cutter and preparation method thereof
Weise et al. Influence of magnetron sputtering process parameters on wear properties of steel/Cr3Si or Cr/MoSx
CN105779937A (en) Method for depositing amorphous diamond thick film on steel substrate by using multi-energy ion beams
CN113046703B (en) High-hardness nano composite coating and preparation method and application thereof
CN104372299B (en) Sandwich construction hard, wear-resisting, lubricant coating and preparation method thereof
CN107130223A (en) A kind of new super lubricating solid coating production

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160921