CN101670743B - Bicolor basal plate and method for preparing same - Google Patents
Bicolor basal plate and method for preparing sameDownload PDFInfo
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Abstract
Translated fromChineseDescription
Translated fromChinese技术领域technical field
本发明涉及本发明属于表面处理技术领域，主要涉及一种双色基板及其制备方法。The invention relates to the technical field of surface treatment, and mainly relates to a two-color substrate and a preparation method thereof.
背景技术Background technique
商标、按键等是手机、数码相机、电脑等电子产品的表面配件之一，起到了重要的装饰作用。目前往往在电子产品的表面增加薄膜达到表面装饰的目的，现有技术中采用多层镀层如在基材表面溅射金属与金属氧化物层，根据光的干涉原理，控制金属氧化物层的厚度，制备了多种颜色的金属化基材。但是这种方法某个金属氧化物层的厚度只能对应一种颜色，无法一次得到表面为双色(两种颜色)的基材。Trademarks, buttons, etc. are one of the surface accessories of electronic products such as mobile phones, digital cameras, and computers, and play an important decorative role. At present, thin films are often added on the surface of electronic products to achieve the purpose of surface decoration. In the prior art, multi-layer coatings are used, such as sputtering metal and metal oxide layers on the surface of the substrate, and the thickness of the metal oxide layer is controlled according to the principle of light interference. , prepared metallized substrates of various colors. However, in this method, the thickness of a certain metal oxide layer can only correspond to one color, and it is impossible to obtain a substrate with a double-color (two-color) surface at one time.
为了在电子产品的表面达到双色(两种颜色)效果，一般先采用真空电镀处理，得到第一种颜色镀层，通过帖胶纸、喷漆或印刷对相应的图形进行覆盖保护，对基材进行退镀处理，使没有覆盖保护的区域的褪去第一种颜色镀层，再对基材进行不同颜色即第二种颜色的电镀，这样在已经褪去镀层露出基材的区域得到第二种颜色镀层，除去帖胶纸、喷漆或印刷对相应的图形得到带有第一种颜色镀层的区域，这样就得到了双色基板。但该方法需要退镀、两次镀膜、覆盖保护，工艺烦琐，而且也造成成本的增加。同时产品的耐磨性、两种颜色交界处与基材的结合力较差。In order to achieve a two-color (two-color) effect on the surface of electronic products, vacuum electroplating is generally used first to obtain the first color coating, and the corresponding graphics are covered and protected by adhesive paper, spray paint or printing, and the substrate is retreated. Plating treatment, so that the first color coating is removed from the area that is not covered and protected, and then the substrate is electroplated with a different color, that is, the second color, so that the second color coating is obtained in the area where the coating has been removed and the substrate is exposed. Paste gummed paper, spray paint or print the corresponding graphics to get the area with the first color coating, so that a two-color substrate is obtained. However, this method requires deplating, two coatings, and covering protection, and the process is cumbersome, and it also causes an increase in cost. At the same time, the wear resistance of the product and the bonding force between the junction of the two colors and the substrate are poor.
发明内容Contents of the invention
本发明的目的在于提供一种双色基板及其制备方法，该双色基板的颜色选择丰富，同时该基材的颜色膜层的耐磨性、颜色膜层与基材的结合力较好，同时该基板的制备方法简单。The object of the present invention is to provide a two-color substrate and a preparation method thereof. The two-color substrate has rich color options, and the wear resistance of the color film layer of the substrate and the bonding force between the color film layer and the substrate are good. The preparation method of the substrate is simple.
本发明提供一种双色基板，包括基材及覆盖在基材上的膜层，所述基材上有凸出区和非凸出区，所述膜层至少为一层膜，所述凸出区的膜层厚度与非凸出区的膜层厚度差异使凸出区与非凸出区呈现不同的颜色，所述覆盖在凸出区与覆盖在非凸出区的膜层材料相同。The invention provides a two-color substrate, comprising a base material and a film layer covering the base material, the base material has a protruding area and a non-protruding area, the film layer is at least one film, and the protruding The difference between the thickness of the film layer in the area and the thickness of the film layer in the non-extruded area makes the area in the embossed area and the area in the non-extruded area present different colors, and the material of the film covering the area in the embossed area is the same as that in the area covered in the non-extruded area.
本发明采用了本领域公知的光的干涉原理，即当光照射到基板上时，基材或者膜层材料的反射率或者光的吸收率不同，导致光的干涉发生，从而使基板上呈现出彩色，控制膜层的厚度可以得到不同的颜色。The present invention adopts the principle of light interference known in the art, that is, when light is irradiated on the substrate, the reflectivity of the substrate or the film layer material or the light absorption rate are different, resulting in light interference, so that the substrate appears Color, different colors can be obtained by controlling the thickness of the film layer.
上述双色基板的制备方法，对基材采用化学蚀刻、冲压、压铸成型中的一种处理方法进行处理，使基材表面形成凸出区和非凸出区，对含有凸出区和非凸出区的基材表面进行至少一次溅射处理，溅射处理使凸出区的膜层厚度与非凸出区的膜层厚度不同，凸出区的膜层厚度与非凸出区的膜层厚度差异使凸出区与非凸出区呈现不同的颜色，所述覆盖在凸出区与覆盖在非凸出区的膜层材料相同。In the preparation method of the above-mentioned two-color substrate, the base material is treated by one of the treatment methods of chemical etching, stamping, and die-casting, so that the surface of the base material forms a raised area and a non-bulged area. The substrate surface of the region is sputtered at least once, and the sputtering treatment makes the film thickness of the raised region different from the film thickness of the non-raised region, and the film thickness of the raised region is different from the film thickness of the non-raised region. The difference makes the protruding area and the non-protruding area present different colors, and the material of the film layer covering the protruding area and the non-protruding area is the same.
本发明的发明人将双色基板分为凸出区和非凸出区，进行溅射处理时，凸出区与非凸出区距离溅射所用的靶的距离即靶基距的不同，从而导致溅射材料在凸出区与非凸出区的沉积速率不同，从而凸出区的溅射膜层厚度与非凸出区的溅射膜层厚度不同，因此，凸出区的膜层厚度与非凸出区的膜层厚度不同。The inventor of the present invention divides the two-color substrate into a protruding area and a non-protruding area. When performing sputtering treatment, the distance between the protruding area and the non-protruding area from the target used for sputtering, that is, the target base distance, is different, resulting in The deposition rate of the sputtered material is different in the protruding area and the non-protruding area, so that the thickness of the sputtered film in the protruding area is different from the thickness of the sputtering film in the non-protruding area. Therefore, the thickness of the film in the protruding area is different from The thickness of the film layer in the non-protruding area is different.
本发明的产品颜色选择丰富，产品颜色膜层的耐磨性、颜色膜层与基材的结合力好，且该基板的制备方法简单，一次溅射即可形成双色，制造成本大大降低。The product color of the present invention is rich in choice, the wear resistance of the color film layer of the product, and the bonding force between the color film layer and the substrate are good, and the preparation method of the substrate is simple, and two colors can be formed by one sputtering, and the manufacturing cost is greatly reduced.
具体实施方式Detailed ways
本发明提供一种双色基板，包括基材及覆盖在基材上的膜层，所述基材上有凸出区和非凸出区，所述膜层至少为一层膜，所述凸出区的膜层厚度与非凸出区的膜层厚度差异使凸出区与非凸出区呈现不同的颜色，所述覆盖在凸出区与覆盖在非凸出区的膜层材料相同。The invention provides a two-color substrate, comprising a base material and a film layer covering the base material, the base material has a protruding area and a non-protruding area, the film layer is at least one film, and the protruding The difference between the thickness of the film layer in the area and the thickness of the film layer in the non-extruded area makes the area in the embossed area and the area in the non-extruded area present different colors, and the material of the film covering the area in the embossed area is the same as that in the area covered in the non-extruded area.
本发明的发明人经过大量实验发现，凸出区与非凸出区距离溅射所用的靶的距离即靶基距的差距越大，导致的溅射膜层的厚度差越大，两种颜色的差别越明显，越能区分出该两种颜色，当凸出区比非凸出区的凸出厚度为大于1mm时，产品表面的凹凸过于明显，不适合对表面外观要求较高的产品。当凸出区比非凸出区的凸出厚度为小于0.1mm时，导致的溅射膜层的厚度差过小，两种颜色的差别较小，不能明显区分出该两种颜色。因此，优选地，在制备该双色基板时，采用一次溅射得到凸出区与非凸出区的膜层，凸出区的膜层厚度与非凸出区的膜层厚度差异使凸出区与非凸出区呈现不同的颜色，所述凸出区比非凸出区凸出的厚度为0.1-1mm。The inventors of the present invention have found through a large number of experiments that the greater the distance between the protruding area and the non-protruding area from the target used for sputtering, that is, the distance between the target and the base distance, the greater the thickness difference of the sputtered film layer, and the two colors The more obvious the difference is, the more the two colors can be distinguished. When the thickness of the protruding area is greater than 1 mm than that of the non-protruding area, the unevenness of the product surface is too obvious, which is not suitable for products with high requirements on surface appearance. When the protruding thickness of the protruding area is less than 0.1 mm than that of the non-protruding area, the thickness difference of the resulting sputtered film layer is too small, the difference between the two colors is small, and the two colors cannot be clearly distinguished. Therefore, preferably, when preparing the two-color substrate, a sputtering is used to obtain the film layers of the protruding area and the non-protruding area, and the difference between the film thickness of the protruding area and the film thickness of the non-protruding area makes the protruding area The non-protruding area presents a different color, and the thickness of the protruding area protruding from the non-protruding area is 0.1-1 mm.
当所述膜层为一层膜，所述基材为消光材料，才能使基材与膜层之间产生光的干涉，从而得到双色基材。When the film layer is a film and the substrate is a matting material, light interference can be generated between the substrate and the film layer, thereby obtaining a two-color substrate.
当所述膜层至少为二层膜，相邻二层膜的材料的折射率不同，当控制膜层厚度与折射率，使光在整个膜层上下表面的光程差为某个颜色的波长的整数倍时，膜层即显示为该颜色。除了溅射得到的膜层，其它层的膜层可以为溅射或者电镀等常见的镀膜方法得到的膜层。When the film layer is at least two layers of film, the refractive index of the materials of adjacent two layers of film is different, when the thickness and refractive index of the film layer are controlled, the optical path difference of the light on the upper and lower surfaces of the entire film layer is the wavelength of a certain color When it is an integer multiple of , the film layer is displayed in this color. In addition to the film layer obtained by sputtering, the film layers of other layers may be film layers obtained by common coating methods such as sputtering or electroplating.
所述膜层为二层膜，该二层膜为金属层与金属氧化层、金属层与非金属氧化物层中的一种。The film layer is a two-layer film, and the two-layer film is one of a metal layer and a metal oxide layer, or a metal layer and a non-metal oxide layer.
所述金属为钛、铝、硅、铬、不锈钢中的一种，所述金属氧化物为二氧化钛、三氧化二铝中的一种，非金属氧化物为二氧化硅。The metal is one of titanium, aluminum, silicon, chromium and stainless steel, the metal oxide is one of titanium dioxide and aluminum oxide, and the non-metal oxide is silicon dioxide.
所述基材为塑料或金属，当所述基材采用塑料时，所述塑料是本领域常见的各种塑料，如PC、ABS。当所述基材采用金属时，所用金属为本领域常见的各种金属，如铝合金、镁合金、不锈钢等。The base material is plastic or metal, and when the base material is plastic, the plastic is various plastics common in the field, such as PC and ABS. When the base material is metal, the metal used is various metals commonly used in this field, such as aluminum alloy, magnesium alloy, stainless steel and the like.
一种双色基板的制备方法，对基材采用化学蚀刻、冲压、压铸成型中的一种处理方法进行处理，使基材表面形成凸出区和非凸出区，对含有凸出区和非凸出区的基材进行表面镀覆处理，在基材上形成膜层，含有膜层的基材的凸出区比非凸出区的凸出厚度使凸出区与非凸出区呈现不同的颜色。A method for preparing a two-color substrate. The base material is treated with one of the treatment methods of chemical etching, stamping, and die-casting, so that the surface of the base material forms a raised area and a non-raised area. The base material in the protruding area is subjected to surface plating treatment to form a film layer on the base material. The protruding thickness of the protruding area of the substrate containing the film layer is different from that of the non-protruding area, so that the protruding area and the non-protruding area present different differences. color.
所述化学蚀刻、冲压、压铸成型为本领域常见的化学蚀刻、冲压、压铸成型，只要能形成边界清晰的凸出区和非凸出区即可。The chemical etching, stamping, and die-casting molding are common chemical etching, stamping, and die-casting moldings in the field, as long as they can form a protruding area and a non-protruding area with clear boundaries.
本发明中仅采用本领域常见的磁控溅射作为实例对本发明的发明内容进行说明。In the present invention, only common magnetron sputtering in the field is used as an example to illustrate the content of the present invention.
采用中频磁控溅射离子镀设备(深圳振恒昌实业有限公司800型)实现镀覆膜层。The intermediate frequency magnetron sputtering ion plating equipment (Shenzhen Zhenhengchang Industrial Co., Ltd. 800 type) is used to realize the coating film layer.
根据本发明提供的制备方法，在优选情况下，为了提高膜层与基材的结合力，所述镀膜材料的制备方法还可以包括对基材进行磁控溅射离子镀之前对进行清洗和清洁活化，所述清晰为本领域公知的超声波清洗处理；所述清洗活化的方法包括，在清洗活化的条件下，用惰性气体的离子轰击所述基材。According to the preparation method provided by the present invention, in preferred cases, in order to improve the bonding force between the film layer and the substrate, the preparation method of the coating material can also include cleaning and cleaning the substrate before magnetron sputtering ion plating Activation, the cleaning is ultrasonic cleaning treatment well known in the art; the method of cleaning and activation includes bombarding the substrate with ions of an inert gas under the conditions of cleaning and activation.
所述镀膜工艺步骤气压为1×10-1-2.0帕，优选为2×10-1-1.0帕。The gas pressure in the coating process step is 1×10-1 -2.0 Pa, preferably 2×10-1 -1.0 Pa.
所述镀膜工艺采用恒功率模式，所述中频电源的功率为1-50千瓦范围内的恒定值，优选为5-30千瓦范围内的恒定值，更优选为10-20千瓦范围内的恒定值。The coating process adopts a constant power mode, and the power of the intermediate frequency power supply is a constant value within the range of 1-50 kilowatts, preferably a constant value within the range of 5-30 kilowatts, more preferably a constant value within the range of 10-20 kilowatts .
所述靶材可以为钛、铝、硅、铬、不锈钢等；所述氧化物可以为金属氧化物和非金属氧化物，金属氧化物可以为二氧化钛、三氧化二铝，非金属氧化物为二氧化硅。The target material can be titanium, aluminum, silicon, chromium, stainless steel, etc.; the oxide can be metal oxide and non-metal oxide, the metal oxide can be titanium dioxide, aluminum oxide, and the non-metal oxide is di silicon oxide.
当镀覆金属氧化物膜层时，在磁控溅射设备中通入反应气体，所述反应气体为氧气，所述氧气的流量为100-800sccm，优选为200-600sccm。When the metal oxide film layer is plated, a reaction gas is introduced into the magnetron sputtering device, the reaction gas is oxygen, and the flow rate of the oxygen is 100-800 sccm, preferably 200-600 sccm.
所述镀膜时间为本领域常见的镀膜时间，一般为1-100分钟；The coating time is a common coating time in the art, generally 1-100 minutes;
该工艺可以根据不同金属层和金属氧化物层或者非金属氧化物层的搭配，得到多种颜色搭配的双色效果，色彩绚丽，金属质感强，结合力好。According to the matching of different metal layers and metal oxide layers or non-metal oxide layers, the process can obtain a double-color effect with various colors, gorgeous colors, strong metal texture, and good bonding force.
以金属层为钛和金属氧化物层为二氧化钛为例，得到一系列颜色，如表1所示：Taking the metal layer as titanium and the metal oxide layer as titanium dioxide as an example, a series of colors are obtained, as shown in Table 1:
表1Table 1
下面通过具体实施例来对本发明进一步详细说明The present invention will be described in further detail below by specific examples
实施例1Example 1
采用经过化学刻蚀并清洗过的不锈钢基材B1进行中频磁控溅射离子镀来说明本发明。The present invention is illustrated by using the stainless steel substrate B1 that has been chemically etched and cleaned to carry out intermediate frequency magnetron sputtering ion plating.
所述不锈钢基材B1的基材的凸出区比非凸出区凸出的厚度为0.7mm。所述膜层为二层膜，金属钛层和二氧化钛层。所选靶材为纯度99.99％的钛靶。The thickness of the protruding area of the base material of the stainless steel substrate B1 protruding from the non-protruding area is 0.7 mm. The film layer is a two-layer film, a metal titanium layer and a titanium dioxide layer. The selected target material is a titanium target with a purity of 99.99%.
将B1放入真空炉，关炉门，开启真空泵进行抽空，抽空至3.0×10-2帕，通入氩气调整真空度为2.0帕，偏压为600伏，占空比50％，进行等离子体轰击清洗活化，时间为10分钟。Put B1 into the vacuum furnace, close the furnace door, turn on the vacuum pump to evacuate to 3.0×10-2 Pa, pass in argon gas to adjust the vacuum degree to 2.0 Pa, the bias voltage is 600 volts, and the duty cycle is 50%, and the plasma is carried out Body bombardment cleaning activation, the time is 10 minutes.
通入工作气体氩气，使真空度为3.5×10-1帕，开启钛靶电源，电源功率为16kW，偏压为200V，占空比为50％，时间为6分钟；得到金属钛层。Introduce the working gas argon to make the vacuum degree 3.5×10-1 Pa, turn on the titanium target power supply, the power supply is 16kW, the bias voltage is 200V, the duty cycle is 50%, and the time is 6 minutes; the metal titanium layer is obtained.
通入反应气体氧气，使氩气和氧气比例为1：2.5，调整钛靶电源功率为14kW，偏压为150V，占空比为40％，时间为18分钟，得到二氧化钛层。Feed the reaction gas oxygen to make the ratio of argon and oxygen 1:2.5, adjust the titanium target power to 14kW, the bias voltage to 150V, the duty cycle to 40%, and the time to 18 minutes to obtain a titanium dioxide layer.
金属钛层在这里的作用是和二氧化硅层组成一个膜系，其主要起到消光和反射的作用。The role of the metal titanium layer here is to form a film system with the silicon dioxide layer, which mainly plays the role of extinction and reflection.
关闭钛靶电源，关闭偏压电源，停止通入氩气和氧气，冷却10分钟出炉，产品非凸出区和凸出区颜色分别为黄色和橙色，采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区二氧化钛膜层的厚度分别为116.8nm和128.2nm，记为D1。Turn off the titanium target power supply, turn off the bias power supply, stop feeding argon and oxygen, cool for 10 minutes and leave the furnace. The color of the non-protruding area and the protruding area of the product are yellow and orange respectively, and the Alpha step meter produced by Tencor Corporation of the United States is used for measurement. , the thicknesses of the titanium dioxide film layer in the non-protruding area and the protruding area are 116.8nm and 128.2nm respectively, which are denoted as D1.
实施例2Example 2
采用经过刻蚀并清洗过的铝合金基材B2进行中频磁控溅射离子镀来说明本发明。The present invention is illustrated by using the etched and cleaned aluminum alloy substrate B2 for ion plating by intermediate frequency magnetron sputtering.
所述铝合金基材B2的凸出区比非凸出区凸出的厚度为0.8mm。所述膜层为二层膜，金属钛层和二氧化硅层。所选靶材为纯度99.99％的钛靶和硅靶。The protruding area of the aluminum alloy substrate B2 is 0.8 mm thicker than the non-protruding area. The film layer is a two-layer film, a metal titanium layer and a silicon dioxide layer. The selected target materials are titanium targets and silicon targets with a purity of 99.99%.
将B2放入真空炉，关炉门，开启真空泵进行抽空，抽空至3.0×10-2帕，通入氩气调整真空度为2.0帕，偏压为600伏，占空比50％，进行等离子体轰击清洗活化，时间为10分钟。Put B2 into the vacuum furnace, close the furnace door, turn on the vacuum pump to evacuate to 3.0×10-2 Pa, pass in argon gas to adjust the vacuum degree to 2.0 Pa, the bias voltage is 600 volts, and the duty cycle is 50%, and the plasma is carried out Body bombardment cleaning activation, the time is 10 minutes.
通入工作气体氩气，使真空度为3.2×10-1帕，开启钛靶电源，电源功率为14kW，偏压为200V，占空比为50％，时间为7分钟；得到金属钛层。Introduce the working gas argon to make the vacuum degree 3.2×10-1 Pa, turn on the titanium target power supply, the power supply is 14kW, the bias voltage is 200V, the duty cycle is 50%, and the time is 7 minutes; the metal titanium layer is obtained.
关闭钛靶电源，通入反应气体氧气，使氩气和氧气比例为1：2，开启硅靶电源，氧气和硅靶反应形成二氧化硅，功率为12kW，偏压为150V，占空比为40％，时间为44分钟，形成二氧化硅层。Turn off the power supply of the titanium target, feed in the reaction gas oxygen, so that the ratio of argon and oxygen is 1:2, turn on the power supply of the silicon target, the oxygen and the silicon target react to form silicon dioxide, the power is 12kW, the bias voltage is 150V, and the duty cycle is 40% for 44 minutes to form a silicon dioxide layer.
关闭硅靶电源，关闭偏压电源，停止通入氩气和氧气，冷却10分钟出炉，产品非凸出区和凸出区颜色分别为橙色和紫红，采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区二氧化硅膜层的厚度分别为198.3nm和219.5nm，记为D2。Turn off the power supply of the silicon target, turn off the bias power supply, stop feeding argon and oxygen, cool for 10 minutes and leave the furnace. The color of the non-protruding area and the protruding area of the product are orange and purple respectively, and the Alpha profilometer produced by Tencor Company of the United States is used for measurement. , the thickness of the silicon dioxide film layer in the non-protruding area and the protruding area is 198.3nm and 219.5nm respectively, which is recorded as D2.
实施例3Example 3
采用经过冲压并清洗过的塑料基材B3进行中频磁控溅射离子镀来说明本发明。The present invention is illustrated by using the punched and cleaned plastic substrate B3 to carry out intermediate frequency magnetron sputtering ion plating.
所述塑料基材B3的凸出区比非凸出区凸出的厚度为0.7mm，所述膜系为三氧化二铝和钛的组合。所选靶材为纯度99.99％的钛靶和铝靶。The protruding area of the plastic substrate B3 is 0.7 mm thicker than the non-protruding area, and the film system is a combination of aluminum oxide and titanium. The selected target materials are titanium targets and aluminum targets with a purity of 99.99%.
将B3放入真空炉，关炉门，开启真空泵进行抽空，抽空至3.0×10-2帕，通入氩气调整真空度为2.0帕，偏压为600伏，占空比50％，进行等离子体轰击清洗活化，时间为10分钟。Put B3 into the vacuum furnace, close the furnace door, turn on the vacuum pump to evacuate to 3.0×10-2 Pa, pass in argon to adjust the vacuum degree to 2.0 Pa, the bias voltage is 600 volts, the duty cycle is 50%, and the plasma is carried out Body bombardment cleaning activation, the time is 10 minutes.
通入工作气体氩气，使真空度为3.5×10-1帕，开启钛靶电源，电源功率为12kW，偏压为200V，占空比为40％，时间为8分钟；得到金属钛层。Introduce the working gas argon to make the vacuum degree 3.5×10-1 Pa, turn on the titanium target power supply, the power supply is 12kW, the bias voltage is 200V, the duty cycle is 40%, and the time is 8 minutes; the metal titanium layer is obtained.
关闭钛靶电源，通入反应气体氧气，使氩气和氧气比例为1：3，开启铝靶电源，氧气和铝靶反应形成三氧化二铝，功率为10kW，偏压为150V，占空比为30％，时间为21分钟，生成三氧化二铝层。Turn off the titanium target power supply, feed in the reaction gas oxygen, so that the ratio of argon to oxygen is 1:3, turn on the aluminum target power supply, the oxygen and aluminum target react to form aluminum oxide, the power is 10kW, the bias voltage is 150V, and the duty cycle is 30%, and the time is 21 minutes, a layer of aluminum oxide is formed.
关闭铝靶电源，关闭偏压电源，停止通入氩气和氧气，冷却10分钟出炉，产品非凸出区和凸出区颜色分别为粉红和紫红，采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区三氧化二铝层的厚度分别为199.6nm和210.2nm，记为D3。Turn off the aluminum target power supply, turn off the bias power supply, stop feeding argon and oxygen, cool for 10 minutes and leave the furnace. The color of the non-protruding area and the protruding area of the product are pink and purple respectively, and the Alpha profilometer produced by Tencor Company of the United States is used for measurement. , the thicknesses of the Al2O3 layer in the non-protruding area and the protruding area are 199.6nm and 210.2nm, respectively, denoted as D3.
实施例4Example 4
实施例4为实施例1中工艺基础上仅改变二氧化钛镀膜时间为28分钟，较实施例1的反应时间18分钟时间要久，镀膜厚的基材非凸出区和凸出区颜色分别为蓝色和绿色，采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区二氧化钛层的厚度分别为176.7nm和191.8nm，记为D4。In embodiment 4, on the basis of the process in embodiment 1, only the coating time of titanium dioxide is changed to 28 minutes, which is longer than the reaction time of 18 minutes in embodiment 1, and the colors of the non-protruding area and the protruding area of the base material with thick coating film are blue respectively. The color and green are measured by the Alpha step meter produced by Tencor Corporation of the United States. The thicknesses of the titanium dioxide layer in the non-protruding area and the protruding area are 176.7nm and 191.8nm, respectively, which are recorded as D4.
实施例5Example 5
实施例5为实施例1中工艺基础上改变基材的凸出区比非凸出区的凸出厚度为1.05mm。采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区二氧化钛层的厚度分别为107.6nm和127.3nm，记为D5。Example 5 is based on the process in Example 1, changing the protruding thickness of the protruding area of the substrate to 1.05 mm compared to the non-protruding area. The Alpha profilometer produced by Tencor Corporation of the United States was used to measure the thickness of the titanium dioxide layer in the non-protruding area and the protruding area were 107.6nm and 127.3nm, which were recorded as D5.
实施例6Example 6
实施例6为实施例1中工艺相同，不同之处在于溅射的膜层为一层膜，该层膜的成分为二氧化钛，所述的基材为钛合金。采用美国Tencor公司生产的Alpha台阶仪进行测量，非凸出区和凸出区二氧化钛层的厚度分别为118.4nm和128.1nm，记为D6。Embodiment 6 is the same process as in Embodiment 1, except that the sputtered film layer is a film, the composition of the film layer is titanium dioxide, and the substrate is titanium alloy. The Alpha profilometer produced by Tencor Corporation of the United States was used to measure the thickness of the titanium dioxide layer in the non-protruding area and the protruding area were 118.4nm and 128.1nm, which were recorded as D6.
对比例1Comparative example 1
采用目前主要的双色装饰方法进行镀膜。The current main two-color decoration method is used for coating.
1)将清洗过的不锈钢基材进行真空电镀处理，膜层材料为碳化钛，电镀后的基材呈现黑色。1) Vacuum electroplating treatment is carried out on the cleaned stainless steel base material, the material of the film layer is titanium carbide, and the base material after electroplating appears black.
所述真空电镀黑色薄膜采用中频磁控溅射离子镀沉积碳化钛的方法实现，所选靶材为纯度99.99％的钛靶。The vacuum electroplating black film is realized by the method of intermediate frequency magnetron sputtering ion plating and depositing titanium carbide, and the selected target material is a titanium target with a purity of 99.99%.
将金属制品放入真空炉，关炉门，开启真空泵进行抽空，抽空至3.0×10-2帕，通入氩气调整真空度为2.0帕，偏压为600伏，占空比50％，进行等离子体轰击清洗活化，时间为10分钟。Put the metal product into the vacuum furnace, close the furnace door, turn on the vacuum pump to evacuate to 3.0×10-2 Pa, pass in argon to adjust the vacuum degree to 2.0 Pa, the bias voltage is 600 volts, and the duty cycle is 50%. Plasma bombardment cleaning and activation takes 10 minutes.
调整氩气流量，使真空度为4.0×10-1帕，通入反应气体乙炔，乙炔气体的初始流量为20标准毫升/分钟，开启钛靶电源，电源功率为13kW，偏压为200V，占空比为40％，采用递增方式逐步增大乙炔流量，乙炔最终流量为100标准毫升/分钟，时间为20分钟。关闭钛靶，关闭偏压，停止通入氩气和乙炔，冷却10分钟后出炉，即可得到黑色，即得到第一种颜色镀层的基材。Adjust the flow rate of argon gas to make the vacuum degree 4.0×10-1 Pa, pass the reaction gas acetylene, the initial flow rate of acetylene gas is 20 standard ml/min, turn on the titanium target power supply, the power supply is 13kW, the bias voltage is 200V, accounting for The empty ratio is 40%, and the flow rate of acetylene is gradually increased in an incremental manner, the final flow rate of acetylene is 100 standard ml/min, and the time is 20 minutes. Turn off the titanium target, turn off the bias voltage, stop feeding argon and acetylene, cool for 10 minutes, and then take it out of the furnace, and you can get black, that is, the substrate of the first color coating.
2)根据需要的图案对上述黑色基材的一部分通过丝网印刷分色电镀保护油墨(深圳市嘉美德表面技术有限公司)，对相应的图案部分进行保护。2) According to the required pattern, a part of the above-mentioned black substrate is screen-printed with color-separated electroplating protection ink (Shenzhen Jiameide Surface Technology Co., Ltd.) to protect the corresponding pattern part.
3)将上述处理的基材浸入本领域公知的退镀液中，所述退渡液只要能退除掉碳化钛即可，使未保护部分的褪去碳化钛镀层，并进行清洗。3) immerse the substrate treated above into a deplating solution known in the art, as long as the deplating solution can remove the titanium carbide, the unprotected part of the titanium carbide coating can be removed and cleaned.
4)将基材进行不同于步骤1)颜色的真空电镀处理，使未保护部分的金属表面呈现第二种颜色镀层，第二种颜色镀层为氮化钛。4) The base material is subjected to a vacuum electroplating treatment with a color different from step 1), so that the metal surface of the unprotected part presents a second color coating, and the second color coating is titanium nitride.
将基材放入炉内，关炉门，开启真空泵进行抽空，抽真空至5.0×10-3帕，通入氩气，使真空度为3.0×10-1帕，通入反应气体氮气，流量为60标准毫升/分钟，开启钛靶电源，电源功率为16kW，偏压为150V，占空比为30％，时间为25分钟。关闭钛靶，关闭偏压，停止通入氩气和氮气，冷却10分钟后出炉，即可使未保护部分呈现黄色。Put the base material into the furnace, close the furnace door, turn on the vacuum pump to evacuate, evacuate to 5.0×10-3 Pa, pass in argon to make the vacuum degree 3.0×10-1 Pa, pass in the reaction gas nitrogen, the flow rate Turn on the titanium target power supply, the power supply is 16kW, the bias voltage is 150V, the duty cycle is 30%, and the time is 25 minutes. Turn off the titanium target, turn off the bias voltage, stop feeding argon and nitrogen, cool it for 10 minutes and take it out of the furnace, so that the unprotected part will appear yellow.
5)清洗掉被保护部分表面的保护油墨，由此基材表面形成具有黑色和黄色两种不同颜色的表面镀层。5) The protective ink on the surface of the protected part is washed away, so that two different-color surface coatings of black and yellow are formed on the surface of the substrate.
从上述实施例和对比例中可以看出，本发明的实施例所得到的产品工序很简单，镀膜工艺简单，而且通过一次镀膜就能达到两种不同颜色的效果。较现有技术中通过两次成色得到双色基板的方法，不但工艺烦琐，而且对比例1在二次镀膜时为了保护前一膜层的性能，不能采用离子轰击活化表面，导致两膜层与基材的结合力较差，同时膜层的耐磨性也较实施例膜层的耐磨性较差。相比而言，本发明所得的产品工艺简单，颜色组合丰富，色彩艳丽，性能更稳定。It can be seen from the above examples and comparative examples that the product process obtained in the examples of the present invention is very simple, the coating process is simple, and the effect of two different colors can be achieved by one coating. Compared with the method of obtaining a two-color substrate through two color formations in the prior art, not only the process is cumbersome, but also in Comparative Example 1, in order to protect the performance of the previous film layer during the second coating, the surface cannot be activated by ion bombardment, resulting in the two film layers being separated from the substrate. The binding force of the materials is poor, and the wear resistance of the film layer is also poorer than that of the embodiment film layer. In comparison, the product obtained by the present invention has simple process, rich color combinations, bright colors and more stable performance.
性能测试Performance Testing
1、色度值测定：1. Chromaticity value measurement:
采用SP60系列积分球式分光光度仪测试产品的色度，得到L、a、b数据。其中，L为照度分量，也可称为亮度。a、b为色度分量。Use SP60 series integrating sphere spectrophotometer to test the chromaticity of the product, and obtain L, a, b data. Among them, L is the illuminance component, which can also be called brightness. a and b are chrominance components.
2、耐磨性测试：2. Wear resistance test:
使用型号为F350008的RCA纸带耐磨仪，在175克力下磨擦上述具有颜色装饰的表面至露出基体材料为止，记录橡胶轮转动的圈数。Use the RCA tape abrasion tester model F350008 to rub the above-mentioned surface with color decoration under 175 grams of force until the base material is exposed, and record the number of turns of the rubber wheel.
3、结合力测定3. Determination of binding force
用划格器在镀膜材料表面的镀膜上划100个1毫米×1毫米的正方形格，用美国3M公司生产的型号为600的透明胶带平整粘结在这些方格上，不留一丝空隙，然后以快速将该胶带垂直揭起，观察划痕边缘处的膜层是否有脱落。测试标准为，脱膜量在0-5％之间为5B，在5-10％之间为4B，在10-20％之间为3B，在20-30％之间为2B，在30-50％之间为1B，在50％以上为0B。Use a scribe to draw 100 square grids of 1mm x 1mm on the coating on the surface of the coating material, and use 600 scotch tape produced by 3M Company of the United States to evenly bond these grids without leaving any gaps, and then Quickly peel off the tape vertically and observe whether the film layer at the edge of the scratch has fallen off. The test standard is that the release amount is 5B between 0-5%, 4B between 5-10%, 3B between 10-20%, 2B between 20-30%, 2B between 30- 1B between 50% and 0B above 50%.
将实施例1-8所得到的镀膜材料按照上述方法进行测试，所得结果列于表2中。The coating materials obtained in Examples 1-8 were tested according to the above method, and the obtained results are listed in Table 2.
表2Table 2
从表2的测试结果可以看出，根据本发明的基材产品通过不同金属和不同氧化物的组合，可以得到更多不同颜色的双色装饰组合，色彩绚丽，同时耐磨性、膜层与基材的结合力均有所提高，可广泛用于电子产品的装饰件。As can be seen from the test results in Table 2, the substrate product according to the present invention can obtain more two-color decoration combinations of different colors through the combination of different metals and different oxides, and the color is gorgeous, and at the same time, the abrasion resistance, film layer and substrate The binding force of materials has been improved, and can be widely used in decorative parts of electronic products.
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