CN101422977A - Filming material and preparation method thereof - Google Patents
Filming material and preparation method thereof Download PDFInfo
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- CN101422977A CN101422977A CNA2007101660564A CN200710166056A CN101422977A CN 101422977 A CN101422977 A CN 101422977A CN A2007101660564 A CNA2007101660564 A CN A2007101660564A CN 200710166056 A CN200710166056 A CN 200710166056A CN 101422977 A CN101422977 A CN 101422977A
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Abstract
The invention provides a coating material which comprises a substrate and a film plated on the surface of the substrate, the film comprises a bottom layer and a surface layer, the bottom layer includes one or a plurality of titanium, aluminum and magnesium, wherein, the film also comprises a middle layer which contains stainless steel and nonferrous metal, and the surface layer contains the carbide and/or nitride of the stainless steel and the carbide and/or nitride of the nonferrous metal. Compared with the existing coating material, the film of the coating material simultaneously has the advantages of smaller surface roughness, higher hardness and better wearing resistance.
Description
Technical field
The invention relates to a kind of Coating Materials and preparation method thereof.
Background technology
At present, Coating Materials such as titanium alloy obtain to use widely at industrial departments such as Aeronautics and Astronautics, chemical industry, shipbuilding, communications day by day, generally, Coating Materials comprises base material and is plated on the film of substrate surface, titanium carbide or the titanium nitride membrane of common film for being made of titanium layer and multilayer titanium carbide or titanium nitride layer.
In general, can use the arc ions electroplating method to prepare the film of above-mentioned Coating Materials.Though adopt the film of arc ions electroplating method preparation to have higher hardness and wearability preferably, the surface roughness of the film that this method makes is bigger, does not satisfy the demand of people to the best bright finish of the outward appearance of Related product.
So, people propose to adopt the method for magnetic controlled sputtering ion plating in the film forming method of substrate surface, the surface roughness of the film that this method makes is less, can reach the appearance requirement of Related product, but, the titanium carbide that existing employing magnetic controlled sputtering ion plating equipment makes or the hardness of titanium nitride membrane are lower, and wearability is relatively poor.
In sum, existing Coating Materials exists and can not possess simultaneously that roughness of film is less, hardness is higher and wearability defective preferably.
Summary of the invention
The objective of the invention is that surface roughness is less, hardness is higher and wear-resisting defective preferably for the film that overcomes existing Coating Materials can not possess simultaneously, provide a kind of and comprise that surface roughness is less, hardness is higher and the wearability Coating Materials and preparation method thereof of film preferably.
The invention provides a kind of Coating Materials, this material comprises base material and is plated on the film of substrate surface, described film comprises bottom and surface layer, described bottom contains one or more in titanium, aluminium and the magnesium, wherein, described film also comprises the intermediate layer, and stainless steel and nonferrous metal are contained in described intermediate layer, and described surface layer contains the carbide and/or the nitride of stainless steel and nonferrous metal.
The preparation method of Coating Materials provided by the invention is included under the sputtering condition, make the target material sputter on the magnetic control target and deposit on the base material applying power supply on the magnetic control target, film forming bottom of difference and surface layer, the target material of formation bottom contains one or more in titanium, aluminium and the magnesium, wherein, this method also is included in after the formation bottom and forms before the surface layer, forms the intermediate layer, and the target in formation intermediate layer comprises stainless target and nonferrous metal target; The target that forms surface layer comprises stainless target and nonferrous metal target.
The roughness result of the test shows, the surface roughness Ra value 0.06-0.07 of the film of the Coating Materials that obtains among the embodiment 1-4, the surface roughness Ra value 0.5 of the film that Comparative Examples 2 obtains, therefore, compare with the Coating Materials film that Comparative Examples 2 obtains, the surface roughness of the film of the Coating Materials that obtains among the embodiment 1-4 is less;
The case hardness experimental result shows, the hardness of the film of the Coating Materials that obtains among the embodiment 1-4 is 1000-1400HV, the hardness of the Coating Materials that Comparative Examples 1 obtains is 600HV, therefore, compare with the Coating Materials film that Comparative Examples 1 obtains, the hardness of the film of the Coating Materials that obtains among the embodiment 1-4 is obviously higher;
Abrasion test is the result show, the film corner angle of the Coating Materials that obtains among the embodiment 1-4 and surface are all without any coming off, the corner angle of the Coating Materials that Comparative Examples 1 obtains have slightly and come off, the surface does not come off, therefore, compare with the Coating Materials film that Comparative Examples 1 obtains, the wearability of the film of the Coating Materials that obtains among the embodiment 1-4 is better;
In sum, compare with the Coating Materials of Comparative Examples, the film of the Coating Materials that provides of the present invention has less surface roughness, higher hardness and wearability preferably simultaneously.
The specific embodiment
The invention provides a kind of Coating Materials, this material comprises base material and is plated on the film of substrate surface, described film comprises bottom and surface layer, described bottom contains one or more in titanium, aluminium and the magnesium, wherein, described film also comprises the intermediate layer, and stainless steel and nonferrous metal are contained in described intermediate layer, and described surface layer contains the carbide and/or the nitride of stainless carbide and/or nitride and nonferrous metal.
The thickness of the bottom of described film, intermediate layer and surface layer is respectively 0.1-1.0 micron, 0.1-1.0 micron and 2-7 micron.
The nonferrous metal of described surface layer and the nonferrous metal in intermediate layer are identical or different, be in vanadium, chromium, cobalt, nickel, copper and the zinc one or more, the nonferrous metal of preferred described surface layer is identical with the nonferrous metal in intermediate layer, be chromium, by this optimal way, can further improve the hardness and the wearability of film.
According to the present invention, described surface layer contains the carbide and/or the nitride of stainless carbide and/or nitride and nonferrous metal, and under the preferable case, described surface layer contains the carbide of stainless carbide and nonferrous metal, by this optimal way, can further improve the hardness of film.
Described base material is one or more in magnesium alloy, titanium alloy and the aluminium alloy.The bottom of described film contains one or more in titanium, aluminium and the magnesium, and under the preferable case, when described base material was magnesium alloy, described film bottom contained magnesium; When described base material was titanium alloy, described film bottom contained titanium; When described base material was aluminium alloy, described film bottom contained aluminium.
The present invention also provides a kind of preparation method of Coating Materials, this method is included under the sputtering condition, make the target material sputter on the magnetic control target and deposit on the base material applying power supply on the magnetic control target, film forming bottom of difference and surface layer, the target of formation bottom contains one or more in titanium, aluminium and the magnesium, and wherein, this method also is included in after the formation bottom and forms before the surface layer, form the intermediate layer, the target that forms the intermediate layer comprises stainless target and nonferrous metal target; The target that forms surface layer comprises stainless target and nonferrous metal target.
Described Coating Materials is to use the preparation of magnetic controlled sputtering ion plating equipment, and described magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest and magnetic control target, and described base material is placed on the work rest.
Described target contains target material, can be preferably the single element target for single element target (promptly only containing a kind of target material in a target) or multielement target (promptly containing multiple target material in a target), and the purity of target material is preferably more than 99.9%.Can select the kind of target material according to the composition of rete.For example, when titanizing on base material, target material is a titanium; When plating stainless steel on base material, target material is a stainless steel; When chromium plating on base material, target material is a chromium.
Described magnetic control target is preferably target structure, can use a pair of or several to magnetic control target as required; Every pair of magnetic control target is powered by a power supply, and two magnetic control targets extremely link to each other with one of power supply separately, and insulate mutually with whole vacuum chamber.Can be 10-25 centimetre to the distance between two magnetic control targets of target, be preferably 14-22 centimetre.Movements and postures of actors part can be around the central shaft of vacuum chamber clockwise or rotate counterclockwise, and its rotating speed can be 0.5-10 rev/min, is preferably 2-6 rev/min.
Described power supply can be preferably intermediate frequency power supply for the existing various power supplys that are used for magnetic controlled sputtering ion plating, and the frequency of intermediate frequency power supply is generally the 10-150 kilohertz, is preferably the 10-100 kilohertz.In the process of sputter, the power of described power supply is 8-20 kilowatt, is preferably 12-18 kilowatt.And the power when forming the intermediate layer is not higher than the power when forming bottom, and the power when forming surface layer is not higher than the power when forming the intermediate layer.
Described sputtering condition can be the sputtering condition of routine, and for example sputtering condition comprises that absolute pressure is the 0.1-1.0 handkerchief, is preferably the 0.3-0.8 handkerchief; Temperature is 20-200 ℃, is preferably 50-150 ℃.
The power of described sputtering time and power supply makes the thickness of described bottom, intermediate layer and surface layer be respectively 0.1-1.0 micron, 0.1-1.0 micron and 2-7 micron.
Described base material can be any base material that carries out magnetic controlled sputtering ion plating that is applicable to, for example, can be selected from magnesium alloy, titanium alloy and the aluminium alloy one or more.
According to the present invention, when forming bottom, when base material was magnesium alloy, described target material was preferably magnesium; When base material was titanium alloy, described target material was preferably titanium; When base material was aluminium alloy, described target material was preferably aluminium.Sputtering time is 2-15 minute, is preferably 5-10 minute, and the thickness of the bottom of formation is that 0.1-1.0 is little.
When forming the intermediate layer, described target material is stainless steel and nonferrous metal, and described nonferrous metal is one or more in vanadium, chromium, cobalt, nickel, copper and the zinc, is preferably chromium.The ratio that is applied to the power of the power supply on stainless steel magnetic control target and the nonferrous metal magnetic control target can be 1.1-1.6, is preferably 1.2-1.4; Sputtering time can be 2-15 minute, is preferably the 5-10 clock, and the thickness in the intermediate layer that bottom surface forms is the 0.1-1.0 micron.
When forming surface layer, described target material is stainless steel and nonferrous metal, and described nonferrous metal and intermediate layer nonferrous metal are identical or different, is in vanadium, chromium, cobalt, nickel, copper and the zinc one or more, preferred surface layer nonferrous metal is identical with the intermediate layer nonferrous metal, is chromium.The ratio that is applied to the power of the power supply on stainless steel magnetic control target and the nonferrous metal magnetic control target can be 1.1-1.6, is preferably 1.2-1.4.Sputtering time can be 60-240 minute, is preferably 80-200 minute, and the thickness of the surface layer that forms in interlayer surfaces is the 2-7 micron.
When described formation bottom and formation intermediate layer, described sputtering under the inert gas atmosphere carried out, and the pressure the when consumption of described inert gas makes sputter reaches the 0.1-1.5 handkerchief.Can for example can vacuumize earlier by in sputter procedure, in vacuum chamber, feeding inert gas realization inert gas atmosphere, make the absolute pressure in the vacuum chamber reach 2 * 10
-3Handkerchief to 6 * 10
-3In the scope of handkerchief, and then charge into inert gas, make the absolute pressure in the vacuum chamber reach the 0.1-1.5 handkerchief.Described inert gas for example can be helium and/or argon gas for not participating in the gas of sputter reaction;
During described formation surface layer, described sputtering under nitrogen and/or the gaseous hydrocarbon atmosphere carried out, and preferably carries out under gaseous hydrocarbon atmosphere, and the surface layer of Xing Chenging is the carbide that contains stainless steel and nonferrous metal like this, can further improve the hardness of film thus.Described gaseous hydrocarbon has been conventionally known to one of skill in the art, can be saturated hydrocarbons and/or the unsaturated hydrocarbons of 1-4 for carbon number, the example of gaseous hydrocarbon includes but not limited to one or more in methane, ethane, propane, normal butane, iso-butane, ethene, propylene, butylene, 2-butylene, butadiene, acetylene, propine, butine and the 2-butine.The consumption of described nitrogen and/or gaseous hydrocarbon can be preferably 20-500sccm, more preferably 50-300sccm for 10-800 standard ml/min (sccm).
In order in sputter procedure, the film that forms to be cleaned, improve adhesion of thin film, can on base material, apply grid bias power supply, the bias voltage of grid bias power supply can lie prostrate for 50-2000, is preferably the 100-1500 volt; Dutycycle is 15-90%, is preferably 30-80%.Described magnetic controlled sputtering ion plating equipment can also comprise biasing device, and biasing device can be grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Before carrying out sputter, can also clean magnetic control target.The method that magnetic control target is cleaned has been conventionally known to one of skill in the art, for example, can magnetic control target be cleaned by apply power supply on magnetic control target under the pressure of 0.5-1.5 handkerchief, the frequency of this power supply can be the 10-150 kilohertz, is preferably the 10-100 kilohertz; The power of this power supply can be 1-100 kilowatt, is preferably 2-60 kilowatt.Wherein, the step that magnetic control target is cleaned can be carried out in described magnetic controlled sputtering ion plating equipment.
Below by embodiment the present invention is described in more detail.
Embodiment 1
This embodiment is used to illustrate Coating Materials provided by the invention and preparation method thereof.
Adopt magnetic controlled sputtering ion plating equipment (magnetron sputtering ion plating machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is JP-700), this magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest, magnetic control target and biasing device, and heater, work rest and magnetic control target are arranged in vacuum chamber.Magnetic control target is to target structure, comprises a pair of chromium target, a pair of stainless steel target and a pair of titanium target.Distance between two targets of a pair of chromium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply; Distance between two targets of stainless steel target is 18 centimetres, and two targets and another frequency are that the both positive and negative polarity of 40 kilo hertzs power supply links to each other; Distance between two targets of titanium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply.Titanium alloy base material (TA2 model) is fixed on the work rest, and the titanium alloy base material equates with distance between two targets of a pair of target between to target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, charging into helium then in vacuum chamber, is 0.5 handkerchief until pressure, and temperature transfers to 150 ℃, start titanium target (promptly opening the power supply that is connected with the titanium target) and carry out magnetic controlled sputtering ion plating, the power of the power supply that is connected with the titanium target is 15 kilowatts, opens described grid bias power supply simultaneously, and the bias voltage of grid bias power supply is 200 volts, dutycycle is 55%, the rotating speed of work rest is 2 rev/mins, and the time is 5 minutes, forms the bottom titanium coating on titanium alloy base material surface.
Then, close the titanium target, start chromium target and stainless steel target (promptly opening the power supply that is connected with the stainless steel target with the chromium target), the power of the power supply that is connected with the chromium target is 12 kilowatts, the power of the power supply that is connected with the stainless steel target is 15 kilowatts, time is 10 minutes, forms the coating of intermediate layer stainless steel and chromium on bottom surface.
Feed acetylene gas again, the consumption of acetylene gas is 100sccm, bias voltage and dutycycle with described grid bias power supply is adjusted into 120 volts and 30% respectively simultaneously, and the time is 90 minutes, forms the carbide coating of stainless carbide of surface layer and chromium on interlayer surfaces.
At last, close stainless steel target, chromium target, grid bias power supply and stop to feed acetylene gas, when naturally cooling to 80 ℃, take out the titanium alloy base material, the thicknesses of layers that records bottom, intermediate layer and the surface layer on titanium alloy base material surface with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.2 micron, 0.8 micron and 3 microns, and note is made Coating Materials A1.
Embodiment 2
This embodiment is used to illustrate Coating Materials provided by the invention and preparation method thereof.
Adopt magnetic controlled sputtering ion plating equipment (magnetron sputtering ion plating machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is JP-700), this magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest, magnetic control target and biasing device, and heater, work rest and magnetic control target are arranged in vacuum chamber.Magnetic control target is to target structure, comprises a pair of cobalt target, a pair of stainless steel target and a pair of magnesium target.Distance between two targets of a pair of cobalt target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply; Distance between two targets of stainless steel target is 18 centimetres, and two targets and another frequency are that the both positive and negative polarity of 40 kilo hertzs power supply links to each other; Distance between two targets of magnesium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply.Magnesium alloy base material (AZ91 model) is fixed on the work rest, and the magnesium alloy base material equates with distance between two targets of a pair of target between to target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, charging into helium then in vacuum chamber, is 0.3 handkerchief until pressure, and temperature transfers to 50 ℃, start magnesium target (promptly opening the power supply that is connected with the magnesium target) and carry out magnetic controlled sputtering ion plating, the power of the power supply that is connected with the magnesium target is 15 kilowatts, opens described grid bias power supply simultaneously, and the bias voltage of grid bias power supply is 1000 volts, dutycycle is 15%, the rotating speed of work rest is 2 rev/mins, and the time is 10 minutes, forms bottom magnesium coating at the magnesium alloy substrate surface.
Then, close the titanium target, start cobalt target and stainless steel target (promptly opening the power supply that is connected with the stainless steel target with the chromium target), the power of the power supply that is connected with the cobalt target is 12 kilowatts, the power of the power supply that is connected with the stainless steel target is 15 kilowatts, time is 5 minutes, forms the coating of intermediate layer stainless steel and cobalt in bottom surface.
Feed acetylene gas again, the consumption of acetylene gas is 50sccm, and bias voltage and the dutycycle with described grid bias power supply is adjusted into 1500 volts and 80% respectively simultaneously, and the time is 200 minutes, forms the carbide coating of stainless carbide of surface layer and cobalt in interlayer surfaces.
At last, close stainless steel target, cobalt target, grid bias power supply and stop to feed acetylene gas, when naturally cooling to 80 ℃, take out the magnesium alloy base material, the thicknesses of layers that records bottom, intermediate layer and surface layer on the magnesium alloy substrate surface with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.8 micron, 0.2 micron and 6 microns, and note is made Coating Materials A2.
Embodiment 3
This embodiment is used to illustrate Coating Materials provided by the invention and preparation method thereof.
Adopt magnetic controlled sputtering ion plating equipment (magnetron sputtering ion plating machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is JP-700), this magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest, magnetic control target and biasing device, and heater, work rest and magnetic control target are arranged in vacuum chamber.Magnetic control target is to target structure, comprises a pair of chromium target, a pair of cobalt target, a pair of stainless steel target and pair of aluminum target.Distance between two targets of a pair of chromium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply; Distance between two targets of a pair of cobalt target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply; Distance between two targets of stainless steel target is 18 centimetres, and two targets and another frequency are that the both positive and negative polarity of 40 kilo hertzs power supply links to each other; Distance between two targets of aluminium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply.Aluminum alloy base material is fixed on the work rest, and aluminum alloy base material (6061 model) equates with distance between two targets of a pair of target between to target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, charging into helium then in vacuum chamber, is 1.0 handkerchiefs until pressure, and temperature transfers to 50 ℃, start aluminium target (promptly opening the power supply that is connected with the aluminium target) and carry out magnetic controlled sputtering ion plating, the power of the power supply that is connected with the aluminium target is 15 kilowatts, opens described grid bias power supply simultaneously, and the bias voltage of grid bias power supply is 700 volts, dutycycle is 50%, the rotating speed of work rest is 2 rev/mins, and the time is 8 minutes, forms the bottom aluminium coat on the aluminum alloy base material surface.
Then, close the titanium target, start chromium target and stainless steel target (promptly opening the power supply that is connected with the stainless steel target with the chromium target), the power of the power supply that is connected with the chromium target is 12 kilowatts, the power of the power supply that is connected with the stainless steel target is 15 kilowatts, time is 8 minutes, forms the coating of intermediate layer stainless steel and chromium in bottom surface.
Close the chromium target again, open the cobalt target, feed acetylene gas, the consumption of acetylene gas is 50sccm, bias voltage and dutycycle with described grid bias power supply is adjusted into 1500 volts and 80% respectively simultaneously, and the time is 140 minutes, forms the carbide coating of stainless carbide of surface layer and cobalt in interlayer surfaces.
At last, close stainless steel target, cobalt target, grid bias power supply and stop to feed nitrogen, when naturally cooling to 80 ℃, take out aluminum alloy base material, the thicknesses of layers that records the lip-deep bottom of aluminum alloy base material, intermediate layer and surface layer with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.6 micron, 0.5 micron and 4 microns, and note is made Coating Materials A3.
Embodiment 4
This embodiment is used to illustrate Coating Materials provided by the invention and preparation method thereof.
Adopt magnetic controlled sputtering ion plating equipment (magnetron sputtering ion plating machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is JP-700), this magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest, magnetic control target and biasing device, and heater, work rest and magnetic control target are arranged in vacuum chamber.Magnetic control target is to target structure, comprises a pair of chromium target, a pair of stainless steel target and a pair of titanium target.Distance between two targets of a pair of chromium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply; Distance between two targets of stainless steel target is 18 centimetres, and two targets and another frequency are that the both positive and negative polarity of 40 kilo hertzs power supply links to each other; Distance between two targets of titanium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply.Titanium alloy base material (TA2 model) is fixed on the work rest, and the titanium alloy base material equates with distance between two targets of a pair of target between to target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, charging into helium then in vacuum chamber, is 1.0 handkerchiefs until pressure, and temperature transfers to 50 ℃, start titanium target (promptly opening the power supply that is connected with the aluminium target) and carry out magnetic controlled sputtering ion plating, the power of the power supply that is connected with the titanium target is 15 kilowatts, opens described grid bias power supply simultaneously, and the bias voltage of grid bias power supply is 700 volts, dutycycle is 50%, the rotating speed of work rest is 2 rev/mins, and the time is 8 minutes, forms the bottom titanium coating on titanium alloy base material surface.
Then, close the titanium target, start chromium target and stainless steel target (promptly opening the power supply that is connected with the stainless steel target with the chromium target), the power of the power supply that is connected with the chromium target is 12 kilowatts, the power of the power supply that is connected with the stainless steel target is 15 kilowatts, time is 8 minutes, forms the coating of intermediate layer stainless steel and chromium in bottom surface.
Feed nitrogen again, the consumption of nitrogen is 300sccm, and bias voltage and the dutycycle with described grid bias power supply is adjusted into 1500 volts and 80% respectively simultaneously, and the time is 140 minutes, forms the nitride coating of stainless nitride of surface layer and chromium in interlayer surfaces.
At last, close stainless steel target, chromium target, grid bias power supply and stop to feed nitrogen, when naturally cooling to 80 ℃, take out the titanium alloy base material, the thicknesses of layers that records the lip-deep bottom of aluminum alloy base material, intermediate layer and surface layer with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.6 micron, 0.5 micron and 4 microns, and note is made Coating Materials A4.
Comparative Examples 1
This Comparative Examples is used to illustrate existing Coating Materials and preparation method thereof.
Adopt magnetic controlled sputtering ion plating equipment (magnetron sputtering ion plating machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is JP-700), this magnetic controlled sputtering ion plating equipment comprises vacuum chamber, heater, work rest, magnetic control target and biasing device, and heater, work rest and magnetic control target are arranged in vacuum chamber.Magnetic control target is to target structure, comprises a pair of titanium target.Distance between two targets of a pair of titanium target is 18 centimetres, and two targets link to each other with the both positive and negative polarity that a frequency is 40 kilo hertzs a power supply.Titanium alloy base material (TA2 model) is fixed on the work rest, and the titanium alloy base material equates with distance between two targets of a pair of target between to target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, charging into helium then in vacuum chamber, is 0.5 handkerchief until pressure, and temperature transfers to 150 ℃, start titanium target (promptly opening the power supply that is connected with the titanium target) and carry out magnetic controlled sputtering ion plating, the power of the power supply that is connected with the titanium target is 15 kilowatts, opens described grid bias power supply simultaneously, and the bias voltage of grid bias power supply is 200 volts, dutycycle is 55%, the rotating speed of work rest is 2 rev/mins, and the time is 5 minutes, forms titanium coating on titanium alloy base material surface.
Then, feed acetylene gas, the consumption of acetylene gas is 100sccm, and the time is 10 minutes, forms the coating of titanium carbide on the titanium coating surface.
Bias voltage and dutycycle with described grid bias power supply is adjusted into 120 volts and 30% respectively again, and the time is 90 minutes, forms the coating of titanium carbide on the titanium carbide surface.
At last, close titanium target, grid bias power supply and stop to feed acetylene gas, when naturally cooling to 80 ℃, take out the titanium alloy base material, the thicknesses of layers that records lip-deep titanium coating of titanium alloy base material and titanium carbide coating with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.2 micron and 3.8 microns, and note is made Coating Materials AC1.
Comparative Examples 2
This Comparative Examples is used to illustrate existing Coating Materials and preparation method thereof.
Adopt multi-arc ion plating equipment (multi-arc ion plating film machine, Beijing Beiyi Innovation Vacuum Technology Co., Ltd. makes, model is a LDH series, this multi-arc ion plating equipment comprises vacuum chamber, heater, work rest, multiple arc target and biasing device, and heater, work rest and multiple arc target are arranged in vacuum chamber.Multiple arc target is a titanium target.Titanium alloy base material (TA2 model) is fixed on the work rest, and the titanium alloy base material is over against target.Biasing device is a grid bias power supply, and the positive pole of grid bias power supply links to each other with the housing of vacuum chamber, and negative pole links to each other with work rest.
Earlier absolute pressure in the vacuum chamber is transferred to 4 * 10
-3Handkerchief, in vacuum chamber, charge into helium then, until pressure is 0.5 handkerchief, and temperature transfers to 150 ℃, starts titanium target (promptly opening the power supply that is connected with the titanium target) and carries out multi-arc ion coating, the electric current 70A that is connected with arc, open described grid bias power supply simultaneously, the bias voltage of grid bias power supply is 200 volts, and dutycycle is 55%, the rotating speed of work rest is 2 rev/mins, and the time is to form titanium coating in 5 minutes on titanium alloy base material surface.
Then, feed acetylene gas, the consumption of acetylene gas is 100sccm, and the time is 10 minutes, forms the coating of titanium carbide on the titanium coating surface.
Bias voltage and dutycycle with described grid bias power supply is adjusted into 120 volts and 30% respectively again, and the time is 90 minutes, forms the coating of titanium carbide at the titanium carbide coating surface.
At last, close titanium target, grid bias power supply and stop to feed acetylene gas, when naturally cooling to 80 ℃, take out titanium alloy product, the thicknesses of layers that records lip-deep titanium coating of titanium alloy base material and titanium carbide coating with the microscope of the Shanghai Cai Kang DMM-660D of Instr Ltd. model is respectively 0.2 micron and 3.8 microns, and note is made Coating Materials AC2.
Embodiment 5-8
This embodiment is used to measure the performance of the film of the Coating Materials that embodiment 1-4 makes.
Use following method to measure surface roughness, wearability and the hardness of film of the Coating Materials A1-A4 of embodiment 1-4 preparation.
Surface roughness: adopt the Shanghai Cai Kang optical instrument JB-3C of Co., Ltd model roughness tester to test.Scriber with instrument moves a segment distance at surface of the work, and the waveform of scriber being walked out by the computer processor that is connected with scriber amplifies and measures its crest and trough spacing, the surface roughness Ra value of being read workpiece by dial gauge.The Ra value is more little, illustrates that the roughness of film is more little.
Wearability is measured: the Coating Materials that respectively surface that obtains among the embodiment 1-4 is formed with rete is put into oscillating mill continuous shaking and is ground after 2 hours and take out product, and whether the rete of observing the corner angle of workpiece and surface (being non-property at parts of edges and corners) has comes off.
Hardness is measured: adopt the Shanghai HV-1000 of precision instrumentation Co., Ltd model micro Vickers to test, utilize the standard of instruments pressure head and add little load, be pressed into 1/3rd of thicknesses of layers, impression is measured, calculate the hardness of rete by MICROCOMPUTER PROCESSING.
Measurement result is as shown in table 1 below.
Comparative Examples 3-4
This Comparative Examples is used to measure the performance of the film of the Coating Materials that Comparative Examples 1-2 makes.
Adopt the method identical to measure surface roughness, wearability and the hardness of film of the Coating Materials AC1-AC2 of Comparative Examples 1-2 preparation with embodiment 5-8.
Measurement result is as shown in table 1 below.
Table 1
| The embodiment numbering | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative Examples 1 | Comparative Examples 2 |
| The Coating Materials numbering | A1 | A2 | A3 | A4 | ACl | AC2 |
| Surface roughness Ra | 0.06 | 0.07 | 0.07 | 0.06 | 0.08 | 0.5 |
| Wearability | Corner angle and surface are all without any coming off | Corner angle and surface are all without any coming off | Corner angle and surface are all without any coming off | Corner angle and surface are all without any coming off | Corner angle have slightly and come off, and the surface does not come off | Corner angle and surface are all without any coming off |
| Hardness (HV) | 1400 | 1000 | 1100 | 1000 | 600 | 1500 |
From the test result shown in the table 1 as can be seen, compare with the Coating Materials AC1 film that Comparative Examples 1 obtains, the hardness of the film of the Coating Materials that obtains among the embodiment 1-4 is obviously higher, and wearability is better; Compare with the film AC2 that Comparative Examples 2 obtains, the surface roughness of the film that obtains among the embodiment 1-4 is obviously less.Therefore, the film of the Coating Materials that obtains among the embodiment 1-4 has less surface roughness, higher hardness and wearability preferably simultaneously.
In addition, the nonferrous metal of using among the embodiment 1 is preferred chromium, and the nonferrous metal of using among the embodiment 2 is a cobalt, therefore, compares with embodiment 2, and the hardness of the film of the Coating Materials that embodiment 1 obtains is higher.
The nonferrous metal of intermediate layer and surface layer is identical among the embodiment 1, is chromium; And the nonferrous metal of the nonferrous metal in intermediate layer and surface layer is different among the embodiment 3, and the intermediate layer nonferrous metal is a chromium, and the nonferrous metal of surface layer is a cobalt, therefore, compares with the film AC3 that embodiment 3 obtains, and the hardness of the film AC1 that embodiment 1 obtains is higher.
Embodiment 1 carries out under acetylene gas atmosphere when forming surface layer, and the surface layer of the film that makes contains the carbide of stainless steel and chromium; And embodiment 4 carries out under nitrogen atmosphere when forming surface layers, and the surface layer of the film that makes contains the nitride of stainless steel and chromium, therefore, compares with the film AC4 that embodiment 4 obtains, and the hardness of the film AC1 that embodiment 1 obtains is higher.
Claims (12)
1, a kind of Coating Materials, this material comprises base material and is plated on the film of substrate surface, described film comprises bottom and surface layer, described bottom contains one or more in titanium, aluminium and the magnesium, it is characterized in that, described film also comprises the intermediate layer, and stainless steel and nonferrous metal are contained in described intermediate layer, and described surface layer contains the carbide and/or the nitride of stainless carbide and/or nitride and nonferrous metal.
2, Coating Materials according to claim 1, wherein, the thickness of described bottom, intermediate layer and surface layer is respectively 0.1-1.0 micron, 0.1-1.0 micron and 2-7 micron.
3, Coating Materials according to claim 1, wherein, the nonferrous metal of described surface layer and the nonferrous metal in intermediate layer are identical or different, are in vanadium, chromium, cobalt, nickel, copper and the zinc one or more.
4, Coating Materials according to claim 3, wherein, the nonferrous metal of described surface layer is identical with the nonferrous metal in intermediate layer, is chromium.
5, Coating Materials according to claim 1, wherein, described surface layer contains the carbide of stainless carbide and nonferrous metal.
6, Coating Materials according to claim 1, wherein, described base material is one or more in magnesium alloy, titanium alloy and the aluminium alloy.
7, the preparation method of the described Coating Materials of claim 1, this method is included under the sputtering condition, make the target material sputter on the magnetic control target and deposit on the base material applying power supply on the magnetic control target, film forming bottom of difference and surface layer, the target material of formation bottom contains one or more in titanium, aluminium and the magnesium, it is characterized in that, this method also is included in after the formation bottom and forms before the surface layer, form the intermediate layer, the target that forms the intermediate layer comprises stainless target and nonferrous metal target; The target that forms surface layer comprises stainless target and nonferrous metal target.
8, method according to claim 7, wherein, the power of described power supply is 8-20 kilowatt, and the power when forming the intermediate layer is not higher than the power when forming bottom, and the power when forming surface layer is not higher than the power when forming the intermediate layer; Described sputtering condition comprises that absolute pressure is the 0.1-1.0 handkerchief, and temperature is 20-200 ℃; The power of described sputtering time and power supply makes the thickness of described bottom, intermediate layer and surface layer be respectively 0.1-1.0 micron, 0.1-1.0 micron and 2-7 micron; All under inert gas shielding, carry out when described formation bottom and formation intermediate layer.
9, method according to claim 8, wherein, the sputtering time when forming bottom is 2-15 minute; Sputtering time when forming the intermediate layer is 2-15 minute; Sputtering time when forming surface layer is 60-240 minute.
10, method according to claim 8, wherein, described gaseous hydrocarbon is one or more in methane, ethane, propane, normal butane, iso-butane, ethene, propylene, butylene, 2-butylene, butadiene, acetylene, propine, butine and the 2-butine, described inert gas is helium and/or argon gas, during described formation surface layer nitrogen and/carry out under the gaseous hydrocarbon atmosphere.
11, method according to claim 7, wherein, the ratio of the power of the power supply that stainless target and nonferrous metal target are applied is 1.1-1.6.
12, method according to claim 7, wherein, the nonferrous metal of described surface layer and the nonferrous metal in intermediate layer are identical or different, are in vanadium, chromium, cobalt, nickel, copper and the zinc one or more; Described base material is one or more in magnesium alloy, titanium alloy and the aluminium alloy.
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