CN102294856A - Decoration material and preparation method thereof - Google Patents
Decoration material and preparation method thereof Download PDFInfo
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- CN102294856A CN102294856A CN2010102164474A CN201010216447A CN102294856A CN 102294856 A CN102294856 A CN 102294856A CN 2010102164474 A CN2010102164474 A CN 2010102164474A CN 201010216447 A CN201010216447 A CN 201010216447A CN 102294856 A CN102294856 A CN 102294856A
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- titanium
- magnetron sputtering
- metallized film
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- stainless steel
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0664—Carbonitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a decoration material. The material comprises a substrate and a film plated on the substrate; the film comprises a decoration film and a metallized film orderly plated on the substrate; the decoration film is one of titanium carbonitride, titanium aluminum nitride and tungsten nitride; and the metallized film is one of tungsten, aluminum, chromium, titanium and stainless steel. The invention further provides a preparation method of the decoration material. The method comprises orderly applying a power source on a magnetron target to sputter and deposit a target material on the magnetron target on the substrate in a magnetron sputtering condition for forming the decoration film and a magnetron sputtering condition for forming the metallized film, thereby, forming the decoration film and the metallized film orderly plated on the substrate, wherein the target material is at least one of titanium, aluminum, chromium, tungsten and stainless steel. The decoration material provided by the invention has abundant film colors and uniform colors; and the films have strong metal texture, good adhesion, good abrasive resistance and good corrosion resistance.
Description
Technical field
The present invention relates to a kind of ornament materials and preparation method thereof.
Background technology
At present, ornament materials is widely used in industrial circles such as Aeronautics and Astronautics, chemical industry, shipbuilding, communication, electronics, automobile making.When especially being applied to the decoration of electronic product, can make electronic product obtain decorative appearance attractive in appearance and better texture, thereby improve the value of product.
Common film plating process is to adopt physical vapour deposition (PVD), especially a kind of good film plating process of the method for magnetron sputtering wherein, the rete metal-like for preparing on base material is strong, adhesion is good, wearability and fine corrosion resistance, and the very thin thickness of rete, do not influence the function of high-end product or complicated shape product, be the environmental protection technology of generally acknowledging.As everyone knows, the method prepared membrane of employing magnetic controlled sputtering ion plating mainly comprises the titanium carbide layer of the chromium nitride layer of silver color, flavous titanium nitride layer, roseate titanium carbonitride layer and black.
But at present, the rete color that the method for employing magnetron sputtering obtains is fewer, can not satisfy people's demand.
Summary of the invention
The technical problem to be solved in the present invention is the single shortcoming of existing decoration coating color, thereby provides a kind of rich color, have ornament materials of metal-like and preparation method thereof.
The invention provides a kind of ornament materials, this material comprises base material and the rete that is plated on the described base material, and described rete comprises decoration coating and the layer of metallized film that is plated on successively on the described base material; Described decoration coating is a kind of in titanium carbonitride, TiAlN and the tungsten nitride; Described layer of metallized film is tungsten, aluminium, chromium, titanium and stainless a kind of.
The present invention also provides a kind of preparation method of ornament materials, this method is included in and applies power supply on the magnetic control target and make the target material sputter on the magnetic control target and be deposited on the described base material, forming decoration coating and the layer of metallized film be plated on successively on the described base material, described target is at least a in titanium, titanium aluminium, chromium, tungsten and the stainless steel.
Coating Materials provided by the invention, the rete color is abundant, and color is even, and the metal-like of rete is very strong, and adhesion is good, wearability and fine corrosion resistance.
The specific embodiment
The invention provides a kind of ornament materials, this material comprises base material and the rete that is plated on the described base material, and described rete comprises decoration coating and the layer of metallized film that is plated on successively on the described base material; Described decoration coating is a kind of in titanium carbonitride, TiAlN and the tungsten nitride; Described layer of metallized film is tungsten, aluminium, chromium, titanium and stainless a kind of.
According to ornament materials provided by the present invention, described decoration coating is a titanium carbonitride, and described layer of metallized film is a stainless steel.
According to ornament materials provided by the present invention, described decoration coating is a TiAlN, and described layer of metallized film is a stainless steel.
According to Coating Materials provided by the invention, the thickness of described decoration coating and the thickness of layer of metallized film are decided according to concrete color needs, in the preferred case, it is 0.8-2um that the magnetron sputtering condition of described formation decoration coating makes the thickness of described decoration coating, is preferably 1-1.5um; It is 2-8nm that the magnetron sputtering condition of described formation layer of metallized film makes the thickness of described layer of metallized film, is preferably 3-6nm.
According to Coating Materials provided by the invention, in order to increase the adhesion between decoration coating and the base material, in the preferred case, between base material and decoration coating, be provided with transition zone, described transition zone is at least a in tungsten, aluminium, chromium, titanium and the stainless steel.More preferably, described transition zone is the metal material identical with decorative layer.
According to Coating Materials provided by the invention, described base material can adopt the various base materials that can carry out magnetic controlled sputtering ion plating, for example can be stainless steel, titanium, chromium, aluminium, magnesium, zinc, titanium alloy, aluminium alloy or magnesium alloy.
The preparation method of ornament materials provided by the invention comprises, under the magnetron sputtering condition, on base material, form decoration coating and layer of metallized film successively, make the target material sputter on the magnetic control target and be deposited on the described base material applying power supply on the magnetic control target, forming decoration coating and the layer of metallized film be plated on successively on the described base material, described target is at least a in titanium, titanium aluminium, chromium, tungsten and the stainless steel.
Preparation method according to ornament materials of the present invention, described magnetic control target is preferably target structure, can use a pair of or severally to magnetic control target as required, and every pair of magnetic control target is powered by a power supply, two magnetic control targets extremely link to each other with one of power supply separately, and insulate with whole vacuum chamber.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.
According to preparation method provided by the invention, in the preferred case, the target that forms described decoration coating is a tabular, and the target that forms described layer of metallized film is cylindric.The purity of described target is preferred more than 99.9%, more preferably more than 99.99%.
According to preparation method provided by the invention, in the preferred case, in the process of described magnetron sputtering, bombard rete with grid bias power supply.Described grid bias power supply makes the ion of positively charged to film the bombardment effect be arranged off and on, has improved the adhesion and the density of rete effectively.
According to preparation method provided by the invention, in the preferred case, it is 0.8-2um that the magnetron sputtering condition of described formation decoration coating makes the thickness of described decoration coating, is preferably 1-1.5um; It is 2-8nm that the magnetron sputtering condition of described formation layer of metallized film makes the thickness of described layer of metallized film, is preferably 3-6nm.
According to preparation method provided by the invention, in the preferred case, the magnetron sputtering condition of described formation decoration coating comprises: the power of power supply is 5-10 kilowatt, more preferably 7-9 kilowatt; The vacuum of magnetron sputtering is the 0.3-0.8 handkerchief, more elects the 0.4-0.7 handkerchief as; Sputtering time is 35-120 minute, more preferably 40-70 minute; Working gas is an inert gas, and reacting gas is the mist of nitrogen or nitrogen and acetylene; Described flow rate of reactive gas is what increase progressively; When described reacting gas was nitrogen, the initial flow of nitrogen was 30-80 standard ml/min, more preferably 40-60 standard ml/min; Final flow is 90-260 standard ml/min, more preferably 100-150 standard ml/min; When described reacting gas was the mist of nitrogen and acetylene, the flow of acetylene was 1-20 standard ml/min or acetylene flow incremental variations, and its initial flow is a 8-20 standard ml/min, and final flow is a 20-60 standard ml/min; The initial flow of described nitrogen is 10-40 standard ml/min, more preferably 20-30 standard ml/min; Final flow is 50-100 standard ml/min, more preferably 50-80 standard ml/min; Bias voltage is the 150-200 volt; Dutycycle is 15%-75%, more preferably 30-50%.
According to preparation method provided by the invention, in the preferred case, the magnetron sputtering condition that forms described layer of metallized film comprises that the power of power supply is the permanent power in the 1-8 kilowatt of scope, more preferably the 2-4 kilowatt of permanent power that scope is interior; The vacuum of magnetron sputtering is the 0.1-1 handkerchief, more preferably the 0.4-0.7 handkerchief; Sputtering time is 1-6 minute, more preferably 3-5 minute; The atmosphere of magnetron sputtering is inert gas atmosphere; Bias voltage is the 100-200 volt, more preferably the 150-200 volt; Dutycycle is 15-50%, more preferably 30-50%.
According to preparation method provided by the invention, in the preferred case, described inert gas is preferably helium or argon gas, and the purity of helium or argon gas is preferably more than 99.9%, more preferably more than 99.99%.
According to preparation method provided by the invention, in the preferred case, in order to increase the adhesion between decoration coating and the base material, before forming decoration coating, form transition zone at substrate surface, the method of described formation transition zone is under the magnetron sputtering condition that forms the transition rete, make the target material sputter on the magnetic control target and be deposited on the described base material applying power supply on the magnetic control target, described target is at least a in titanium, titanium aluminium, chromium, tungsten and the stainless steel.The condition of described formation transition rete is that the power of power supply is the permanent power in the 8-10 kilowatt of scope, the vacuum of magnetron sputtering is the 0.4-0.7 handkerchief, and sputtering time is 5-15 minute, and the atmosphere of magnetron sputtering is inert gas atmosphere, bias voltage is the 150-200 volt, and dutycycle is 50-75%.
According to preparation method provided by the invention, in the preferred case, described base material is stainless steel, titanium, chromium, aluminium, magnesium, zinc, titanium alloy, aluminium alloy or magnesium alloy.
According to preparation method provided by the invention, in the preferred case, in order to improve the adhesion of rete and base material, the preparation method of described Coating Materials can also be included in and carry out before the magnetron sputtering base material being carried out the ion cleaning.The method that described ion cleans comprises, with the described base material of the positive ion bombardment in the glow discharge plasma, ion clean vacuum be the 0.8-1.2 handkerchief, the ion scavenging period is 25-30 minute, the atmosphere that ion cleans is inert gas atmosphere, bias voltage is the 900-1150 volt, and dutycycle is 50-75%.
According to preparation method provided by the invention, under normal conditions, the preparation method of described Coating Materials also is included in base material is carried out before ion cleans, base material is carried out pre-treatment, the method of this pre-treatment is well known to a person skilled in the art, for example, base material carried out machine glazed finish, frosted or wire drawing after, carry out ultrasonic wave and clean.
Can for the base material of the Coating Materials of expecting smooth touch, carry out carrying out the ultrasonic wave cleaning after the machine glazed finish as required; For the base material of the Coating Materials of expecting the frosted sense of touch, carry out carrying out the ultrasonic wave cleaning after the frosted; For the base material of the Coating Materials of expecting the strip sense of touch, carry out carrying out the ultrasonic wave cleaning after the wire drawing.The method that described machine glazed finish, frosted or wire drawing and ultrasonic wave clean has been conventionally known to one of skill in the art, no longer repeats at this.
Adopt specific embodiment that the present invention is further elaborated below.
Embodiment 1
Present embodiment illustrates ornament materials of the present invention and preparation method thereof.
Base material adopts stainless steel (model is 316L) workpiece
1, pre-treatment
(1) machine glazed finish
The polishing machine (JM-101 model) that adopts the close plant equipment of Dongguan City crystalline substance Co., Ltd to produce was slightly thrown 10 minutes stainless steel work-piece under 2840 rev/mins polishing wheel rotating speed with rough polishing ointment (SBT-600 model) in the yellow of Jiangmen outstanding profit letter rubbing down Materials Co., Ltd production, under 2840 rev/mins polishing wheel rotating speed this workpiece was carried out essence with white smart throwing ointment (SBW-804 model) again and threw 10 minutes.
(2) ultrasonic wave cleans
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.
2, preparation ornament materials
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of titanium target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area symmetrically and be 99.99% titanium metal planar magnetic control target.
(1) ion cleans
Workpiece after the above-mentioned cleaning is put on the work rest of vacuum chamber, work rest is with 3 rev/mins rotational speed, close the door, utilize thick pumped vacuum systems sliding vane rotary pump+lobe pump that equipped vacuum chamber is carried out just taking out, after vacuum reaches molecular pump startup pressure 5Pa, open high valve vacuum chamber is carefully taken out, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, when vacuum to 6 * 10
-3Behind the Pa, make vacuum reduce to 1Pa, open grid bias power supply this moment workpiece is carried out ion cleaning, dutycycle 75%, 1100 volts of bias voltages, scavenging period 30 minutes the vacuum chamber applying argon gas.
(2) form the transition rete
Open the titanium target power supply, operating air pressure is adjusted into 0.5Pa, power is 9 kilowatts, and bias voltage is 200 volts, and dutycycle is 75%, carries out magnetron sputtering, and the time of sputter is 10 minutes.
(3) form decoration coating
Adjusting power is 9 kilowatts, and bias voltage is 150 volts, and dutycycle is 50%, feeds acetylene and nitrogen, and the acetylene flow is 10sccm, and nitrogen flow is incremented to 50sccm from 20sccm, carries out magnetron sputtering, and the time of sputter is 40 minutes.Close the titanium target power supply, stop to feed gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 1.2um, this rete is golden yellow colour cast redness, and has metal-like.
(4) form layer of metallized film
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of stainless steel target is in this equipment: it is 99.99% stainless steel cylinder magnetic control target that two pairs of purity are arranged in the magnetron sputtering area.
Earlier vacuum chamber is slightly bled with the black vacuum extract system, after reaching molecular pump startup pressure, utilize high vacuum system that vacuum chamber is carefully taken out again, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, reach the base vacuum degree 6 * 10 of plated film at last
-3Pa.After reaching base vacuum, charge into the working gas argon gas, make operating air pressure at 0.5Pa, argon flow amount is 350sccm, opens the power supply of stainless steel target, carries out magnetron sputtering, power is 1.5KW, and grid bias power supply technology is 200 volts of dutycycle 50%, voltages, and the metallization time is 4min.
Close the stainless steel target power supply, close grid bias power supply, stop to feed argon gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 4nm, this rete is a pale pink, and has metal-like.
Embodiment 2
Present embodiment illustrates Coating Materials of the present invention and preparation method thereof.
Base material adopts titanium alloy (model is TA2) workpiece
1, pre-treatment
(1) machine glazed finish
The polishing machine (JM-101 model) that adopts the close plant equipment of Dongguan City crystalline substance Co., Ltd to produce was slightly thrown 10 minutes titanium alloy workpiece under 2840 rev/mins polishing wheel rotating speed with rough polishing ointment (SBT-600 model) in the yellow of Jiangmen outstanding profit letter rubbing down Materials Co., Ltd production, under 2840 rev/mins polishing wheel rotating speed this workpiece was carried out essence with white smart throwing ointment (SBW-804 model) again and threw 10 minutes.
(2) wire drawing
Adopt the polishing machine (JM-101 model) of the close plant equipment of Dongguan City crystalline substance Co., Ltd production under 1420 rev/mins pulling wheel rotating speed, titanium alloy workpiece to be carried out essence throwing 10 minutes with the red essence throwing ointment (555-10 model) that the grand side in Shenzhen is preced with the production of magnificent Science and Technology Ltd..
(3) ultrasonic wave cleans
Workpiece after the above-mentioned wire drawing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.
2, preparation ornament materials
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of titanium target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area symmetrically and be 99.99% titanium metal planar magnetic control target.
(1) ion cleans
Workpiece after the above-mentioned cleaning is put on the work rest of vacuum chamber, work rest is with 3 rev/mins rotational speed, close the door, utilize thick pumped vacuum systems sliding vane rotary pump+lobe pump that equipped vacuum chamber is carried out just taking out, after vacuum reaches molecular pump startup pressure 5Pa, open high valve vacuum chamber is carefully taken out, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, when vacuum to 6 * 10
-3Behind the Pa, make vacuum reduce to 1Pa, open grid bias power supply this moment workpiece is carried out ion cleaning, dutycycle 75%, 1100 volts of bias voltages, scavenging period 30 minutes the vacuum chamber applying argon gas.
(2) form the transition rete
Open the titanium target power supply, operating air pressure is adjusted into 0.5Pa, power is 9 kilowatts, and bias voltage is 200 volts, and dutycycle is 75%, carries out magnetron sputtering, and the time of sputter is 10 minutes.
(3) form decoration coating
Adjusting power is 7 kilowatts, and bias voltage is 170 volts, and dutycycle is 75%, feeds acetylene and nitrogen, and the acetylene flow is 20sccm, and nitrogen flow is incremented to 80sccm from 10sccm, carries out magnetron sputtering, and the time of sputter is 35 minutes.Close the titanium target power supply, stop to feed gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 1.2um, this rete is golden yellow colour cast redness, and has metal-like.
(4) form layer of metallized film
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of stainless steel target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area and be 99.99% stainless steel cylinder magnetic control target.
Earlier vacuum chamber is slightly bled with the black vacuum extract system, after reaching molecular pump startup pressure, utilize high vacuum system that vacuum chamber is carefully taken out again, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, reach the base vacuum degree 6 * 10 of plated film at last
-3Pa.After reaching vacuum, charge into the working gas argon gas, make operating air pressure at 0.5Pa, argon flow amount is 350sccm, opens the power supply of stainless steel target, carries out magnetron sputtering, power is 3KW, and grid bias power supply technology is 150 volts of dutycycle 30%, bias voltages, and the metallization time is 3min.
Close the stainless steel target power supply, close grid bias power supply, stop to feed argon gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 3nm, this rete is a pale pink, and has metal-like.
Embodiment 3
Present embodiment illustrates ornament materials of the present invention and preparation method thereof.
Base material adopts stainless steel (model is 316L) workpiece
1, pre-treatment
(1) machine glazed finish
The polishing machine (JM-101 model) that adopts the close plant equipment of Dongguan City crystalline substance Co., Ltd to produce was slightly thrown 10 minutes stainless steel work-piece under 2840 rev/mins polishing wheel rotating speed with rough polishing ointment (SBT-600 model) in the yellow of Jiangmen outstanding profit letter rubbing down Materials Co., Ltd production, under 2840 rev/mins polishing wheel rotating speed this workpiece was carried out essence with white smart throwing ointment (SBW-804 model) again and threw 10 minutes.
(2) ultrasonic wave cleans
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.
2, preparation ornament materials
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of titanium aluminium target is in this equipment: be provided with a pair of composition ratio in the magnetron sputtering area and be 5: 5 titanium-aluminium alloy planar targets.
(1) ion cleans
Workpiece after the above-mentioned cleaning is put on the work rest of vacuum chamber, work rest is with 3 rev/mins rotational speed, close the door, utilize thick pumped vacuum systems sliding vane rotary pump+lobe pump that equipped vacuum chamber is carried out just taking out, after vacuum reaches molecular pump startup pressure 5Pa, open high valve vacuum chamber is carefully taken out, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, when vacuum to 6 * 10
-3Behind the Pa, make vacuum reduce to 1Pa, open grid bias power supply this moment workpiece is carried out ion cleaning, dutycycle 75%, 1100 volts of bias voltages, scavenging period 30 minutes the vacuum chamber applying argon gas.
(2) form the transition rete
Operating air pressure is adjusted into 0.5Pa, opens the power supply of titanium-aluminum alloy target, power is 5 kilowatts, and bias voltage is 200 volts, and dutycycle is 75%, and argon flow amount is 280sccm, carries out magnetron sputtering, and the time of sputter is 10 minutes.
(3) form decoration coating
Power is 5 kilowatts, and it is 200 volts that bias voltage is set, and dutycycle is 30%, feeds nitrogen, and nitrogen flow is incremented to 150sccm from 40sccm, carries out magnetron sputtering, and the time of sputter is 50 minutes.Close target power supply, stop to feed gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 1.5um, this rete is a bluish violet, and has metal-like.
(4) form layer of metallized film
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of stainless steel target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area and be 99.99% stainless steel cylinder magnetic control target.
Earlier vacuum chamber is slightly bled with the black vacuum extract system, after reaching molecular pump startup pressure, utilize high vacuum system that vacuum chamber is carefully taken out again, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, reach the base vacuum degree 6 * 10 of plated film at last
-3Pa.After reaching base vacuum, charge into the working gas argon gas, make operating air pressure at 0.5Pa, argon flow amount is 280sccm, opens the power supply of stainless steel target, carries out magnetron sputtering, and power is 2KW, 100 volts of dutycycle 15%, bias voltages, and the metallization time is 4min.
Close the stainless steel target power supply, close grid bias power supply, stop to feed argon gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 5nm, this rete is light blue, and has metal-like.
Embodiment 4
Present embodiment illustrates ornament materials of the present invention and preparation method thereof.
Base material adopts stainless steel (model is 316L) workpiece
1, pre-treatment
(1) machine glazed finish
The polishing machine (JM-101 model) that adopts the close plant equipment of Dongguan City crystalline substance Co., Ltd to produce was slightly thrown 10 minutes stainless steel work-piece under 2840 rev/mins polishing wheel rotating speed with rough polishing ointment (SBT-600 model) in the yellow of Jiangmen outstanding profit letter rubbing down Materials Co., Ltd production, under 2840 rev/mins polishing wheel rotating speed this workpiece was carried out essence with white smart throwing ointment (SBW-804 model) again and threw 10 minutes.
(2) ultrasonic wave cleans
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.
2, preparation ornament materials
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of titanium aluminium target is in this equipment: be provided with a pair of composition ratio in the magnetron sputtering area and be 5: 5 titanium-aluminium alloy planar targets.
(1) ion cleans
Workpiece after the above-mentioned cleaning is put on the work rest of vacuum chamber, work rest is with 3 rev/mins rotational speed, close the door, utilize thick pumped vacuum systems sliding vane rotary pump+lobe pump that equipped vacuum chamber is carried out just taking out, after vacuum reaches molecular pump startup pressure 5Pa, open high valve vacuum chamber is carefully taken out, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, when vacuum to 6 * 10
-3Behind the Pa, make vacuum reduce to 1Pa, open grid bias power supply this moment workpiece is carried out ion cleaning, dutycycle 75%, 1100 volts of bias voltages, scavenging period 30 minutes the vacuum chamber applying argon gas.
(2) form decoration coating
Operating air pressure is adjusted into 0.5Pa, opens the power supply of titanium-aluminum alloy target, adjusting power is 5 kilowatts, it is 100 volts that bias voltage is set, and dutycycle is 15%, feeds nitrogen, nitrogen flow is incremented to 200sccm from 80sccm, carries out magnetron sputtering, and the time of sputter is 60 minutes.Close target power supply, stop to feed gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 1.6um, this rete is a blue-green, and has metal-like.
(3) form layer of metallized film
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of stainless steel target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area and be 99.99% stainless steel cylinder magnetic control target.
Earlier vacuum chamber is slightly bled with the black vacuum extract system, after reaching molecular pump startup pressure, utilize high vacuum system that vacuum chamber is carefully taken out again, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, reach the base vacuum degree 6 * 10 of plated film at last
-3Pa.After reaching base vacuum, charge into the working gas argon gas, make operating air pressure at 0.5Pa, argon flow amount is 280sccm, opens the power supply of stainless steel target, carries out magnetron sputtering, and power is 1KW, 100 volts of dutycycle 15%, bias voltages, and the metallization time is 4min.
Close the stainless steel target power supply, close grid bias power supply, stop to feed argon gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 3nm, this rete is light blue, and has metal-like.
Comparative Examples 1
Present embodiment illustrates ornament materials of the present invention and preparation method thereof.
Base material adopts stainless steel (model is 316L) workpiece
1, pre-treatment
(1) machine glazed finish
The polishing machine (JM-101 model) that adopts the close plant equipment of Dongguan City crystalline substance Co., Ltd to produce was slightly thrown 10 minutes stainless steel work-piece under 2840 rev/mins polishing wheel rotating speed with rough polishing ointment (SBT-600 model) in the yellow of Jiangmen outstanding profit letter rubbing down Materials Co., Ltd production, under 2840 rev/mins polishing wheel rotating speed this workpiece was carried out essence with white smart throwing ointment (SBW-804 model) again and threw 10 minutes.
(2) ultrasonic wave cleans
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.
2, preparation ornament materials
Adopt magnetron sputtering film device (strength source, Beijing Co., Ltd) to carry out plated film.
The structure of titanium target is in this equipment: be provided with two pairs of purity in the magnetron sputtering area symmetrically and be 99.99% titanium metal planar magnetic control target.
(1) ion cleans
Workpiece after the above-mentioned cleaning is put on the work rest of vacuum chamber, work rest is with 3 rev/mins rotational speed, close the door, utilize thick pumped vacuum systems sliding vane rotary pump+lobe pump that equipped vacuum chamber is carried out just taking out, after vacuum reaches molecular pump startup pressure 5Pa, open high valve vacuum chamber is carefully taken out, when 0.08Pa, vacuum chamber is heated the purpose that reduces the time of bleeding to reach, when vacuum to 6 * 10
-3Behind the Pa, make vacuum reduce to 1Pa, open grid bias power supply this moment workpiece is carried out ion cleaning, dutycycle 75%, 1100 volts of bias voltages, scavenging period 30 minutes the vacuum chamber applying argon gas.
(2) form the transition rete
Open the titanium target power supply, operating air pressure is adjusted into 0.5Pa, power is 9 kilowatts, and bias voltage is 200 volts, and dutycycle is 75%, and argon flow amount is 350sccm, carries out magnetron sputtering, and the time of sputter is 10 minutes.
(3) form decoration coating
Adjusting power is 9 kilowatts, and bias voltage is 150 volts, and dutycycle is 50%, feeds acetylene and nitrogen, and the acetylene flow is incremented to 22sccm from 10sccm, and nitrogen flow is incremented to 70sccm from 20sccm, carries out magnetron sputtering, and the time of sputter is 45 minutes.Close the titanium target power supply, stop to feed gas, cool off and came out of the stove in 10 minutes, obtain being formed with the workpiece that thickness is the rete of 1.1um, have metal-like.
Performance test
1, chromatic value is measured
Colourity output L, a, three groups of data of b with the chromascope specimen.Wherein, L represents lightness index, and a represents red green product index, and b represents champac chromaticity index.
2, adhesion is measured
Draw the square lattice of 100 1mm * 1mm in the coated surface of sample with drawing the lattice device, the model of producing with Minnesota Mining and Manufacturing Company is 600 smooth being bonded on the grid of adhesive tape, do not stay a space, vertically uncover adhesive tape then fast, the rete of observing cut edge has or not and comes off.Is 5B as the demoulding amount between 0-5 area %, is 4B between 5-10 area %, is 3B between 10-20 area %, is 2B between 20-30 area %, is 1B between 30-50 area %, is 0B more than 50 area %.
3, wearability is measured
The equipment that uses vibrates wear resistant instrument as Rosler, be furnished with the yellow circular cone that is used to wear and tear, green pyramid and FC120 cleaning agent, wearing-in period is set at 30 minutes, if judge eroded area area≤1 * 1mm, set wearing-in period once more and be 30 minutes and proceed wearability test, circulate till eroded area area＞1 * 1mm with this.It is qualified that general wearing and tearing accumulated time being judged to be of eroded area area＞1 * 1mm also do not occur in 2 hours.The time of eroded area area＞1 * 1mm appears in this wear-resisting test record.
4, corrosion resistance test
In salt fog cabinet, it is vaporific to cause the aqueous solution of an approximate seawater component that it is injected into, and is full of in the whole case, and cooperates the control of temperature humidity and air pressure, strengthens these factors, carries out accelerated test, thus the decay resistance of Rapid identification material.
Salt fog solution: Nacl 5%PH=3.1～3.3 (add glacial acetic acid and CuCl
2); Probe temperature: 50 ℃ of test cabinets, the temperature of saturation of the air bucket are 63 ℃; Testing time is 8 hours.
Test result assessment: press the evaluation of GB6461-86 outward appearance.
Adopt above-mentioned method of testing that embodiment 1-4 and the Comparative Examples 1 resulting workpiece that is formed with rete are carried out performance test, test result is as shown in table 1.
Table 1
As can be seen from Table 1, method of the present invention can obtain the abundant rete of color, and color is even, and adhesion is good, wearability and fine corrosion resistance.
Claims (12)
1. ornament materials, this material comprise base material and are plated on rete on the described base material, it is characterized in that described rete comprises decoration coating and the layer of metallized film that is plated on successively on the described base material; Described decoration coating is a kind of in titanium carbonitride, TiAlN and the tungsten nitride; Described layer of metallized film is a kind of in tungsten, aluminium, chromium, titanium and the stainless steel.
2. ornament materials according to claim 1, wherein, described decoration coating is a titanium carbonitride, described layer of metallized film is a stainless steel.
3. ornament materials according to claim 1, wherein, described decoration coating is a TiAlN, described layer of metallized film is a stainless steel.
4. according to any described ornament materials of claim 1-3, wherein, the thickness of described decoration coating is 0.8-2um, and the thickness of described layer of metallized film is 2-8nm.
5. ornament materials according to claim 4, wherein, described base material is stainless steel, titanium, chromium, aluminium, magnesium, zinc, titanium alloy, aluminium alloy or magnesium alloy.
6. the preparation method of the described ornament materials of claim 1, it is characterized in that, make the target material sputter on the magnetic control target and be deposited on the described base material applying power supply on the magnetic control target, forming decoration coating and the layer of metallized film be plated on successively on the described base material, described target is at least a in titanium, titanium aluminium, chromium, tungsten and the stainless steel.
7. method according to claim 6, wherein, the target that forms described decoration coating is a tabular, the target that forms described layer of metallized film is cylindric.
8. method according to claim 7 wherein, is bombarded rete with grid bias power supply in the process of described magnetron sputtering.
9. method according to claim 8, wherein, it is 0.8-2um that the magnetron sputtering condition of described formation decoration coating makes the thickness of described decoration coating, it is 2-8nm that the magnetron sputtering condition of described formation layer of metallized film makes the thickness of described layer of metallized film.
10. method according to claim 6, wherein, the magnetron sputtering condition of described formation decoration coating comprises, the power of power supply is 5-10 kilowatt, the vacuum of magnetron sputtering is the 0.3-0.8 handkerchief, sputtering time is 35-120 minute, working gas is an inert gas, reacting gas is the mist of nitrogen or nitrogen and acetylene, described flow rate of reactive gas is what increase progressively, when described reacting gas was nitrogen, the initial flow of nitrogen was that 30-80 standard ml/min, final flow are 90-260 standard ml/min when described reacting gas was nitrogen; When described reacting gas is the mist of nitrogen and acetylene, the flow of acetylene is 1-20 standard ml/min or acetylene flow incremental variations, its initial flow is a 8-20 standard ml/min, final flow is a 20-60 standard ml/min, and the initial flow of described nitrogen is that 10-40 standard ml/min, final flow are 50-100 standard ml/min; Bias voltage is the 50-200 volt, and dutycycle is 15%-75%.
11. method according to claim 6, wherein, the magnetron sputtering condition that forms described layer of metallized film comprises, the power of power supply is the permanent power in the 1-8 kilowatt of scope, the vacuum of magnetron sputtering is the 0.1-1 handkerchief, and sputtering time is 1-6 minute, and the atmosphere of magnetron sputtering is inert gas atmosphere, bias voltage is the 100-200 volt, and dutycycle is 15-50%.
12. method according to claim 6, wherein, described base material is stainless steel, titanium, chromium, aluminium, magnesium, zinc, titanium alloy, aluminium alloy or magnesium alloy.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102164474A CN102294856A (en) | 2010-06-28 | 2010-06-28 | Decoration material and preparation method thereof |
| PCT/CN2011/076164 WO2012000401A1 (en) | 2010-06-28 | 2011-06-22 | Composite structure and method of preparing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102164474A CN102294856A (en) | 2010-06-28 | 2010-06-28 | Decoration material and preparation method thereof |
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| CN103568391A (en) * | 2012-08-09 | 2014-02-12 | 精工爱普生株式会社 | Decorative article and timepiece |
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| WO2014166162A1 (en) * | 2013-04-11 | 2014-10-16 | 合肥京东方光电科技有限公司 | Thin film layer and manufacturing method therefor, substrate for display, and liquid crystal display |
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| CN103866322B (en) * | 2014-03-21 | 2016-09-07 | 恩平建高实业有限公司 | Aluminium technique for vacuum coating |
| CN105377193A (en) * | 2014-04-03 | 2016-03-02 | 爱德华兹生命科学公司 | High durability heart valve |
| CN105599384A (en) * | 2015-09-28 | 2016-05-25 | 无锡贺邦金属制品有限公司 | Simple metal product |
| CN107254662A (en) * | 2017-06-28 | 2017-10-17 | 维达力实业(深圳)有限公司 | Blue laminated film and preparation method thereof |
| CN108531869A (en) * | 2018-04-17 | 2018-09-14 | 广东正德材料表面科技有限公司 | A kind of coating processing method preparing superhard Cr-Al-N coatings |
| CN108728847A (en) * | 2018-06-28 | 2018-11-02 | 北京小米移动软件有限公司 | Film plating process, shell and equipment |
| CN110184566A (en) * | 2019-06-05 | 2019-08-30 | 广东省新材料研究所 | A kind of hard coat of Color tunable and preparation method thereof |
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| WO2012000401A1 (en) | 2012-01-05 |
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Application publication date: 20111228 |