A kind of decorative material and preparation method thereof

[0015] The preparation method of the decorative material provided by the present invention comprises the steps of forming a decorative film layer and a metallized film layer on a base material in sequence under the condition of magnetron sputtering, and applying power on the magnetron target to sputter the target material on the magnetron target. The target material is at least one of titanium, titanium-aluminum, chromium, tungsten and stainless steel to form a decorative film layer and a metallized film layer plated on the substrate in turn. kind.

[0016] According to the preparation method of the decorative material of the present invention, the magnetron target is preferably a paired target structure, and one or several pairs of magnetron targets can be used as required. Each pair of magnetron targets is powered by one power supply and two magnetron targets. The targets are each connected to one pole of the power source and are insulated from the entire vacuum chamber. The workpiece can be rotated clockwise or counterclockwise around the central axis of the vacuum chamber, and its rotational speed can be 0.5-10 rpm, preferably 2-6 rpm.

[0017] According to the preparation method provided by the present invention, in a preferred case, the target for forming the decorative film layer is flat, and the target for forming the metallized film layer is cylindrical. The purity of the target material is preferably 99.9% or more, more preferably 99.99% or more.

[0018] According to the preparation method provided by the present invention, in a preferred case, the film layer is bombarded with a bias power supply during the magnetron sputtering process. The bias power supply causes positively charged ions to intermittently bombard the film, thereby effectively improving the bonding force and density of the film layer.

[0019] According to the preparation method provided by the present invention, in a preferred case, the magnetron sputtering conditions for forming the decorative film layer make the thickness of the decorative film layer 0.8-2um, preferably 1-1.5um; The magnetron sputtering conditions of the film layer are such that the thickness of the metallized film layer is 2-8 nm, preferably 3-6 nm.

[0020] According to the preparation method provided by the present invention, in a preferred case, the magnetron sputtering conditions for forming the decorative film layer include: the power of the power supply is 5-10 kilowatts, more preferably 7-9 kilowatts; the vacuum of the magnetron sputtering The temperature is 0.3-0.8 Pa, more preferably 0.4-0.7 Pa; the sputtering time is 35-120 minutes, more preferably 40-70 minutes; the working gas is an inert gas, and the reaction gas is nitrogen or a mixed gas of nitrogen and acetylene The flow rate of the reaction gas is incremental; when the reaction gas is nitrogen, the initial flow rate of nitrogen is 30-80 standard milliliters/min, more preferably 40-60 standard milliliters/min; the final flow is 90-260 standard milliliters/min ml/min, more preferably 100-150 standard ml/min; when the reaction gas is a mixed gas of nitrogen and acetylene, the flow rate of acetylene is 1-20 standard ml/min or the acetylene flow is incrementally changed, and its initial flow is 8-20 standard ml/min, the final flow is 20-60 standard ml/min; the initial flow rate of the nitrogen is 10-40 standard ml/min, more preferably 20-30 standard ml/min; the final flow is 50- 100 standard ml/min, more preferably 50-80 standard ml/min; bias voltage 150-200 volts; duty cycle 15%-75%, more preferably 30-50%.

[0021] According to the preparation method provided by the present invention, in a preferred case, the magnetron sputtering conditions for forming the metallized film layer include that the power of the power supply is constant power in the range of 1-8 kilowatts, more preferably in the range of 2-4 kilowatts The constant power inside; the vacuum degree of magnetron sputtering is 0.1-1 Pa, more preferably 0.4-0.7 Pa; the sputtering time is 1-6 minutes, more preferably 3-5 minutes; the atmosphere of magnetron sputtering is Inert gas atmosphere; bias voltage of 100-200 volts, more preferably 150-200 volts; duty cycle of 15-50%, more preferably 30-50%.

[0022] According to the preparation method provided by the present invention, in a preferred case, the inert gas is preferably helium or argon, and the purity of helium or argon is preferably 99.9% or more, more preferably 99.99% or more.

[0023] According to the preparation method provided by the present invention, in a preferred case, in order to increase the bonding force between the decorative film layer and the substrate, a transition layer is formed on the surface of the substrate before the decorative film layer is formed, and the method for forming the transition layer is: Under the condition of magnetron sputtering for forming the transition film layer, power is applied to the magnetron target to sputter and deposit the target material on the magnetron target on the substrate, and the target material is titanium, titanium aluminum, chromium , at least one of tungsten and stainless steel. The conditions for forming the transition film layer are that the power of the power supply is a constant power in the range of 8-10 kilowatts, the vacuum degree of the magnetron sputtering is 0.4-0.7 Pa, the sputtering time is 5-15 minutes, and the magnetron sputtering The atmosphere is an inert gas atmosphere, the bias voltage is 150-200 volts, and the duty cycle is 50-75%.

[0024] According to the preparation method provided by the present invention, in a preferred case, the substrate is stainless steel, titanium, chromium, aluminum, magnesium, zinc, titanium alloy, aluminum alloy or magnesium alloy.

[0025] According to the preparation method provided by the present invention, in a preferred case, in order to improve the bonding force between the film layer and the substrate, the preparation method of the coating material may further include ion cleaning the substrate before magnetron sputtering. The ion cleaning method includes bombarding the substrate with positive ions in the glow discharge plasma, the vacuum degree of the ion cleaning is 0.8-1.2 Pa, the ion cleaning time is 25-30 minutes, and the ion cleaning atmosphere is 0.8-1.2 Pa. Inert gas atmosphere, bias voltage 900-1150 volts, duty cycle 50-75%.

[0026] According to the preparation method provided by the present invention, under normal circumstances, the preparation method of the coating material further includes pre-treating the substrate before ion cleaning the substrate, and the pre-treatment method is well known to those skilled in the art , for example, ultrasonic cleaning after mechanical polishing, sanding or wire drawing of the substrate.

[0027] According to needs, for the substrate of the coating material that wants to get a smooth touch, ultrasonic cleaning is performed after mechanical polishing; for the substrate of the coating material that wants to get a matte touch, ultrasonic cleaning is performed after grinding; for the coating material that wants to get a strip-like touch The substrate is ultrasonically cleaned after wire drawing. The methods of mechanical polishing, sanding or wire drawing and ultrasonic cleaning are well known to those skilled in the art and will not be repeated here.

[0029] Example 1

[0030] This example illustrates the decorative material of the present invention and its preparation method.

[0031] The base material is stainless steel (model 316L) workpiece

[0032] 1. Pretreatment

[0033] (1) Mechanical polishing

[0034] Using the polishing machine (JM-101 model) produced by Dongguan Jingmi Machinery Equipment Co., Ltd. and the yellow medium-coarse polishing paste (SBT-600 model) produced by Jiangmen Jie Lixin Polishing Materials Co., Ltd. The polishing wheel at 2840 rpm The stainless steel workpiece was rough-polished for 10 minutes at the rotational speed, and then fine-polished for 10 minutes at a polishing wheel speed of 2840 rpm with a white fine-polishing ointment (model SBW-804).

[0035] (2) Ultrasonic cleaning

[0036] The above-mentioned polished workpiece was immersed in normal temperature dewaxing water, degreasing powder solution and deionized water at 70° C. for ultrasonic cleaning in sequence. Among them, dewaxing water and degreasing powder are all products of Mai Demei Fine Chemical Co., Ltd.

[0037] 2. Preparation of decorative materials

[0038] Coating was carried out using magnetron sputtering coating equipment (Beijing Strength Source Co., Ltd.).

[0039] The structure of the titanium target in the equipment is as follows: two pairs of titanium metal planar magnetron targets with a purity of 99.99% are symmetrically arranged in the magnetron sputtering area.

[0040] (1) Ion cleaning

[0041] Put the cleaned workpiece into the workpiece rack of the vacuum chamber, the workpiece rack rotates at 3 rpm, close the door, and use the rotary vane pump + Roots pump of the rough vacuum system to initially pump the vacuum chamber equipped with the equipment. , when the vacuum degree reaches the starting pressure of the molecular pump of 5Pa, open the high valve to perform fine pumping of the vacuum chamber, and heat the vacuum chamber at 0.08Pa to reduce the pumping time. When the vacuum degree reaches 6×10 -3 After Pa, the vacuum chamber was filled with argon gas to reduce the vacuum degree to 1Pa. At this time, the bias power supply was turned on to clean the workpiece with a duty ratio of 75%, a bias voltage of 1100 volts, and a cleaning time of 30 minutes.

[0042] (2) Forming a transition film layer

[0043] Turn on the titanium target power supply, adjust the working air pressure to 0.5Pa, the power supply power to 9kW, the bias voltage to 200V, the duty cycle to be 75%, and perform magnetron sputtering, and the sputtering time is 10 minutes.

[0044] (3) Forming a decorative film layer

[0045] Adjust the power supply to 9 kilowatts, the bias voltage to 150 volts, the duty cycle to be 50%, pass in acetylene and nitrogen, the acetylene flow is 10 sccm, the nitrogen flow is increased from 20 sccm to 50 sccm, and magnetron sputtering is performed, and the sputtering time is 40 minutes. The power of the titanium target was turned off, the gas was stopped, cooled for 10 minutes, and a workpiece was formed with a film layer with a thickness of 1.2um. The film layer was golden yellow and reddish, and had a metallic texture.

[0046] (4) Forming a metallized film layer

[0047] Coating was carried out using magnetron sputtering coating equipment (Beijing Strength Source Co., Ltd.).

[0048] The structure of the stainless steel target in the equipment is as follows: there are two pairs of stainless steel cylindrical magnetron targets with a purity of 99.99% in the magnetron sputtering zone.

[0049] The vacuum chamber is firstly pumped with the rough vacuum pumping system, and after reaching the starting pressure of the molecular pump, the vacuum chamber is finely pumped by the high vacuum system, and the vacuum chamber is heated at 0.08Pa to reduce the pumping time. , and finally the background vacuum of the coating is 6×10 -3 Pa. After reaching the background vacuum, fill in the working gas argon, so that the working pressure is 0.5Pa, the argon gas flow is 350sccm, the power of the stainless steel target is turned on, and the magnetron sputtering is carried out. The empty ratio is 50%, the voltage is 200V, and the metallization time is 4min.

[0050] Turn off the power supply of the stainless steel target, turn off the bias power supply, stop the supply of argon gas, cool for 10 minutes, and release the workpiece to obtain a workpiece with a film layer with a thickness of 4 nm. The film layer is pale pink and has a metallic texture.

[0051] Example 2

[0052] This embodiment illustrates the coating material of the present invention and its preparation method.

[0053] The base material is titanium alloy (type TA2) workpiece

[0054] 1. Pretreatment

[0055] (1) Mechanical polishing

[0056] Using the polishing machine (JM-101 model) produced by Dongguan Jingmi Machinery Equipment Co., Ltd. and the yellow medium-coarse polishing paste (SBT-600 model) produced by Jiangmen Jie Lixin Polishing Materials Co., Ltd. The polishing wheel at 2840 rpm The titanium alloy workpiece was rough-polished for 10 minutes at the rotational speed, and then fine-polished for 10 minutes at a polishing wheel speed of 2840 rpm with a white fine-polishing ointment (model SBW-804).

[0057] (2) Drawing

[0058] The polishing machine (JM-101 model) produced by Dongguan Jingmi Machinery Equipment Co., Ltd. was used, and the red fine throwing ointment (555-10 model) produced by Shenzhen Hongfang Guanhua Technology Co., Ltd. was used at the speed of 1420 rpm of the drawing wheel. Finish polishing the titanium alloy workpiece for 10 minutes.

[0059] (3) Ultrasonic cleaning

[0060] The above-mentioned wire-drawing workpieces were immersed in normal temperature dewaxing water, degreasing powder solution and deionized water at 70° C. for ultrasonic cleaning in sequence. Among them, dewaxing water and degreasing powder are all products of Mai Demei Fine Chemical Co., Ltd.

[0061] 2. Preparation of decorative materials

[0062] Coating was carried out using magnetron sputtering coating equipment (Beijing Strength Source Co., Ltd.).

[0063] The structure of the titanium target in the equipment is as follows: two pairs of titanium metal planar magnetron targets with a purity of 99.99% are symmetrically arranged in the magnetron sputtering area.

[0064] (1) Ion cleaning

[0065] Put the cleaned workpiece into the workpiece rack of the vacuum chamber, the workpiece rack rotates at 3 rpm, close the door, and use the rotary vane pump + Roots pump of the rough vacuum system to initially pump the vacuum chamber equipped with the equipment. , when the vacuum degree reaches the starting pressure of the molecular pump of 5Pa, open the high valve to perform fine pumping of the vacuum chamber, and heat the vacuum chamber at 0.08Pa to reduce the pumping time. When the vacuum degree reaches 6×10 -3 After Pa, the vacuum chamber was filled with argon gas to reduce the vacuum degree to 1Pa. At this time, the bias power supply was turned on to clean the workpiece with a duty ratio of 75%, a bias voltage of 1100 volts, and a cleaning time of 30 minutes.

[0066] (2) Forming a transition film layer

[0067] Turn on the titanium target power supply, adjust the working air pressure to 0.5Pa, the power supply power to 9kW, the bias voltage to 200V, the duty cycle to be 75%, and perform magnetron sputtering, and the sputtering time is 10 minutes.

[0068] (3) Forming a decorative film layer

[0069] Adjust the power supply to 7 kW, the bias voltage to 170 volts, the duty cycle to be 75%, pass in acetylene and nitrogen, the acetylene flow is 20 sccm, the nitrogen flow is increased from 10 sccm to 80 sccm, and magnetron sputtering is performed, and the sputtering time is 35 minutes. The power of the titanium target was turned off, the gas was stopped, cooled for 10 minutes, and a workpiece was formed with a film layer with a thickness of 1.2um. The film layer was golden yellow and reddish, and had a metallic texture.

[0070] (4) Forming a metallized film layer

[0071] Coating was carried out using magnetron sputtering coating equipment (Beijing Strength Source Co., Ltd.).

[0072] The structure of the stainless steel target in the equipment is as follows: two pairs of stainless steel cylindrical magnetron targets with a purity of 99.99% are arranged in the magnetron sputtering zone.

[0073] The vacuum chamber is firstly pumped with the rough vacuum pumping system, and after reaching the starting pressure of the molecular pump, the vacuum chamber is finely pumped by the high vacuum system, and the vacuum chamber is heated at 0.08Pa to reduce the pumping time. , and finally the background vacuum of the coating is 6×10 -3 Pa. After reaching the vacuum degree, fill in the working gas argon, so that the working pressure is 0.5Pa, the argon gas flow is 350sccm, the power supply of the stainless steel target is turned on, and magnetron sputtering is performed. The power supply power is 3KW, and the bias power supply process is the duty cycle. 30%, bias voltage 150V, metallization time 3min.

[0074] Turn off the power supply of the stainless steel target, turn off the bias power supply, stop the supply of argon gas, cool for 10 minutes, and release the workpiece to obtain a workpiece with a film layer with a thickness of 3 nm. The film layer is pale pink and has a metallic texture.