CN101823353A - Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof - Google Patents
Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof Download PDFInfo
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- CN101823353A CN101823353A CN201010168336A CN201010168336A CN101823353A CN 101823353 A CN101823353 A CN 101823353A CN 201010168336 A CN201010168336 A CN 201010168336A CN 201010168336 A CN201010168336 A CN 201010168336A CN 101823353 A CN101823353 A CN 101823353A
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Abstract
The invention relates to a metal-diamond-like carbon nano composite membrane and is characterized in that the membrane is sequentially formed by a substrate (1), a metal transition layer (2), a metal nitride transition layer (3), a metal carbide transition layer (4) and a metal-doped diamond-like carbon layer (5). The preparation method is that a Ti, Cr or W target is used to sequentially bombard and clean the substrate, a deposited metal layer, the metal nitride layer, the metal carbide layer and a deposited metal-doped diamond-like carbon layer. The metal-diamond-like carbon nano composite membrane has the advantages of low friction factor, high wear resistance, high corrosion resistance, high biocompatibility and high color uniformity. The metal-diamond-like carbon nano composite membrane is suitable for surface coating of watch shells, ornaments, handicrafts and the like.
Description
Technical field
The present invention relates to a kind of coating for metal surfaces and preparation method thereof, particularly a kind of metal-DLC (Me-DLC) nano composite membrane and preparation method thereof.
Background technology
The face coat technology has been used for a long time on the five metals exterior trimming parts, mainly based on electroplating technology.But along with social development; the public strengthens gradually for the consciousness of environmental protection, energy conservation; high pollution, high energy consumption electroplating industry are in the stage that progressively is eliminated, and the vacuum ionic coating technology with energy-saving and environmental protection characteristics is that the advanced process for treating surface of representative replaces gradually.Utilize at present the various decoration functions films of vacuum ion plating preparation on the five metals exterior trimming parts, because rete approaches (0.2～1.0 μ m), its wearability and corrosion resistance are generally all bad.Utilize the diamond-film-like of vacuum ion plating preparation, have a series of excellent properties similar, particularly low coefficient of friction, high wearability, good anti-corrosion and biocompatibility and color uniformity consistency to diamond film.
China Patent No. ZL 200710028834.3 discloses the employing ion gun and has prepared metal carbides/DLC nanometer multilayer membrane material in conjunction with magnetron sputtering technique, and this multi-layer film material has higher microhardness, low coefficient of friction, firm performances such as adhesive force.But nano-multilayer film is to be made of two kinds of metaboly depositions, on the on-plane surface sample, because the sedimentation rate of different parts rete differs, positive slow at the backside deposition speed ratio of concrete workpiece, and the DLC layer is in certain thickness range and interferes coloredly, and it is inconsistent to have caused like this that metal carbides/the DLC nano-multilayer film is appearance color on target workpiece.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect that existing face coat technology exists; a kind of Me-DLC nano composite membrane is provided; this film material has high microhardness and wearability, low coefficient of friction, good film-substrate cohesion and the performances such as color of surperficial uniformity, to play protection exterior trimming parts surface anti scuffing, corrosion resistance and raising biocompatibility.
Another object of the present invention provides a kind of preparation method of Me-DLC nano composite membrane.
The present invention is achieved by the following technical solutions: described Me-DLC nano composite membrane belongs to DLC layer 5 by base material 1, intermediate metal 2, metal nitride transition zone 3, metal carbides transition zone 4 and gold doping successively and constitutes.
Described base material 1 is iron and steel, titanium alloy or carbide alloy.
The preparation method of described Me-DLC nano composite membrane adopts Ti, Cr or W to do target, is reaching base vacuum: 5.0 * 10
-3Pa, temperature: 150～350 ℃, work rest rotating speed: under 1～5rpm condition, may further comprise the steps successively:
1. ion beam cleans base material: pressure: 0.1～1.0Pa in the stove, Ar throughput: 100～300sccm, ion gun: 0.5～2.0kW, back bias voltage: 100～800V, time: 40～60min;
2. intermediate metal deposits: pressure: 0.2～0.5Pa in the stove, Ar throughput: 150～200sccm, non-balance magnetically controlled sputter Ti or Cr, target power output: 2.0～10kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
3. the metal nitride transition zone deposits: pressure: 0.3～0.6Pa in the stove, Ar throughput: 100～200sccm, N
2: 20～60sccm, non-balance magnetically controlled sputter Ti or Cr, target power output: 5.0～10kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
4. the metal carbides transition zone deposits: pressure: 0.3～0.6Pa in the stove, Ar throughput: 100～200sccm, CH
4Or C
2H
2Throughput: 20～100sccm, non-balance magnetically controlled sputter Ti, Cr or W, target power output: 3.0～8.0kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
5. gold doping belongs to DLC layer deposition: pressure: 0.3～0.55Pa in the stove, Ar throughput: 120～200sccm, CH
4Or C
2H
2Throughput: 160～250sccm, ion gun: 2.5～3.5kW, non-balance magnetically controlled sputter Ti, Cr or W, target power output: 0.5～1.0kW, back bias voltage: 20～100V, time: 60～120min.
Metal level transition zone of the present invention is Ti or Cr.Depositing metal layers Ti or Cr are that the thickness of this layer is 100～200nm because the adhesiveness of proper metal layer and materials such as iron and steel, titanium alloy or carbide alloy is good.
Metal nitride layer TiN of the present invention or CrN (1500-2500Hv) and metal carbide layer TiC, CrC or WC (Hv2000-3000), be in order between base material and Me-DLC nano composite membrane, to set up hardness thermal coefficient of expansion gradient transition, reduce the rete internal stress, improve the toughness of film/basic adhesion and rete, the thickness of this layer is respectively 100～200nm.
It is Ti-DLC, Cr-DLC or W-DLC that gold doping of the present invention belongs to the DLC layer, be to utilize anode layer flow pattern gas ion source ionization hydrocarbon methane, acetylene etc., open the non-balance magnetically controlled sputter metallic target simultaneously, be implemented in the preparation that the gold doping that mixes a small amount of nano-crystalline granule in the amorphous diamond-film-like belongs to DLC (Me-DLC) nanometer composite layer.Utilize the amorphous diamond-like carbon film to have excellent biological compatibility and corrosion resistance, when doing the jewelry use, wearer's skin is not easy to produce irritated.The oligometallic internal stress that can reduce significantly in the rete of mixing, and then improve film/film-substrate binding strength; On the basis of low coefficient of friction amorphous DLC, nano-crystalline granule also can further improve the wearability of rete.The thickness of this layer is 500～1000nm, and hardness is Hv2000～4000.Because this nano composite membrane is a spot of nano-crystalline granule of Mass in the amorphous DLC, though also existing in the sedimentation rate of target workpiece different parts rete differs, but because this layer is with a kind of material (Me-DLC), in the thickness range that is deposited, can not occur interfering colour, be the appearance color uniformity.
Description of drawings
Fig. 1 is a Me-DLC nano composite membrane structural representation of the present invention.
Among the figure: base material 1, intermediate metal 2, metal nitride transition zone 3, metal carbides transition zone 4, gold doping belong to diamond-film-like 5.
The specific embodiment
Embodiment 1,2,3 presses table 1,2,3 listed technological processes and parameter operation respectively.Method of testing is as follows:
1. thicknesses of layers adopts the cross section metallographic method to measure;
2. film hardness adopts micro Vickers to measure: load 10g, 15 seconds load times, survey three point hardnesses and average;
3. film/basic adhesion adopts film bond strength scratch test instrument to measure: loading velocity is 100N/min, and the speed of paddling is 5mm/min, and the time of paddling is 1 minute;
4. the rete coefficient of friction adopts ball-disc type friction wear testing machine to measure, and is GCr15 to mill part material, and linear velocity is 0.5m/s, and load is 0.98N;
5. back and forth friction of surface abrasion resistance employing and medium density fibre board (MDF) (roughness is 2.5～3.5 μ m), load is 2.45N;
6. surperficial corrosion resistance adopts artificial perspiration's corrosion resistance test, and testing liquid is NaCl:20g/L, NH
4Cl:17.5g/L, CH
4N
2O (concentration 〉=99.5%): 5g/L, CH
3COOH (concentration 〉=99%): 2.5g (2.4ml)/L, C
3H
6O
3(concentration 90%): 15g (12.4ml)/L, NaOH (concentration 80g/L) adjusts pH value of solution value to 4.7.Test temperature (40 ± 2) ℃, duration of test runs is not less than 24h.
Embodiment 1
Table 1 technological process table
Adopt the Ti target, gas is 99.99% Ar, N
2And CH
4, base material is the 316L stainless steel.The thickness of depositing Ti/TiN/TiC/Ti-DLC is respectively 100nm, 150nm, 150nm and 800nm successively.The rete gross thickness is 1200nm, the workpiece surface colour uniformity, and hardness number is Hv2100, and film/basic adhesion is 55N, and coefficient of friction is 0.110.Through back and forth rubbing after the 9000m test with medium density fibre board (MDF), the exemplar surface does not have show-through, no rete to come off; After the artificial perspiration tests 24 hours, acomia the changing of the integral color of rete, do not occur saltouing and corrosion.
Embodiment 2
Table 2 technological process table
Adopt the Cr target, gas is 99.99% Ar, N
2With 99.5% C
2H
2, base material is the Ti6Al4V titanium alloy.The thickness that deposits Cr/CrN/CrC/Cr-DLC successively is respectively 100nm, 150nm, 100nm and 750nm.The rete gross thickness is 1100nm, the workpiece surface colour uniformity, and hardness number is Hv2300, and film/basic adhesion is 70N, and coefficient of friction is 0.150.Through back and forth rubbing after the 7500m test with medium density fibre board (MDF), the exemplar surface does not have show-through, no rete to come off; After the artificial perspiration tests 24 hours, acomia the changing of the integral color of rete, do not occur saltouing and corrosion.
Embodiment 3
Table 3 technological process table
Adopt Cr and W target, gas is 99.99% Ar, N
2With 99.5% C
2H
2, base material is the TiC base cemented carbide.The thickness that deposits Cr/CrN/WC/W-DLC successively is respectively 100nm, 100nm, 100nm and 700nm.The rete gross thickness is 1000nm, the workpiece surface colour uniformity, and hardness number is Hv3100, and film/basic adhesion is 75N, and coefficient of friction is 0.135.Through back and forth rubbing after the 10000m test with medium density fibre board (MDF), the exemplar surface does not have show-through, no rete to come off; After the artificial perspiration tests 24 hours, acomia the changing of the integral color of rete, do not occur saltouing and corrosion.
Metal-DLC of the present invention (Me-DLC) nano composite membrane is suitable for the face coat of Wristwatch case, jewelry, handicraft etc.
Claims (4)
1. metal-diamond-like nanocomposite film is characterized in that belonging to DLC layer (5) by base material (1), intermediate metal (2), metal nitride transition zone (3), metal carbides transition zone (4) and gold doping successively constitutes.
2. metal according to claim 1-diamond-like nanocomposite film is characterized in that described base material is iron and steel, titanium alloy or carbide alloy.
3. metal according to claim 1-diamond-like nanocomposite film is characterized in that described metal is Ti, Cr or W.
4. the preparation method of the described metal of claim 1-diamond-like nanocomposite film is characterized in that adopting Ti, Cr or W to do target, is reaching base vacuum: 5.0 * 10
-3Pa, temperature: 150～350 ℃, work rest rotating speed: under 1～5rpm condition, may further comprise the steps successively:
1. ion beam cleans base material: pressure: 0.1～1.0Pa in the stove, Ar throughput: 100～300sccm, ion gun: 0.5～2.0kW, back bias voltage: 100～800V, time: 40～60min;
2. intermediate metal deposits: pressure: 0.2～0.5Pa in the stove, Ar throughput: 150～200sccm, non-balance magnetically controlled sputter Ti or Cr, target power output: 2.0～10kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
3. the metal nitride transition zone deposits: pressure: 0.3～0.6Pa in the stove, Ar throughput: 100～200sccm, N
2: 20～60sccm, non-balance magnetically controlled sputter Ti or Cr, target power output: 5.0～10kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
4. the metal carbides transition zone deposits: pressure: 0.3～0.6Pa in the stove, Ar throughput: 100～200sccm, CH
4Or C
2H
2Throughput: 20～100sccm, non-balance magnetically controlled sputter Ti, Cr or W, target power output: 3.0～8.0kW, ion gun: 0.5～1.0kW, back bias voltage: 50～200V, time: 5～15min;
5. gold doping belongs to DLC layer deposition: pressure: 0.3～0.55Pa in the stove, Ar throughput: 120～200sccm, CH
4Or C
2H
2Throughput: 160～250sccm, ion gun: 2.5～3.5kW, non-balance magnetically controlled sputter Ti, Cr or W, target power output: 0.5～1.0kW, back bias voltage: 20～100V, time: 60～120min.
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| CN102912298A (en) * | 2012-10-29 | 2013-02-06 | 西安浩元涂层技术有限公司 | Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method |
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