CN118703958B - Surface Treatment Technology of Stainless Steel Kitchenware - Google Patents
Surface Treatment Technology of Stainless Steel Kitchenware Download PDFInfo
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- CN118703958B CN118703958B CN202411190452.0A CN202411190452A CN118703958B CN 118703958 B CN118703958 B CN 118703958B CN 202411190452 A CN202411190452 A CN 202411190452A CN 118703958 B CN118703958 B CN 118703958B
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47J—KITCHEN EQUIPMENT; COFFEE MILLS; SPICE MILLS; APPARATUS FOR MAKING BEVERAGES
- A47J36/00—Parts, details or accessories of cooking-vessels
- A47J36/02—Selection of specific materials, e.g. heavy bottoms with copper inlay or with insulating inlay
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- 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
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- 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
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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
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- 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
- C23C14/0623—Sulfides, selenides or tellurides
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- 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
- C23C14/0635—Carbides
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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Abstract
Description
技术领域Technical Field
本发明涉及不锈钢处理领域,具体涉及不锈钢厨具的表面处理工艺。The invention relates to the field of stainless steel processing, in particular to a surface processing technology for stainless steel kitchenware.
背景技术Background Art
不锈钢具有独特的强度、耐磨性、防腐性及不易生锈,干净卫生等优良特性,被运用于各领域,如食品制造领域,生活制品领域,家用电器领域。不锈钢厨具更是被广泛应用于大家的日常生活中,包括但不限于:不锈钢餐具、不锈钢刀具、不锈钢烹饪器皿、不锈钢锅具、不锈钢漏铲。它们具有良好的导热性能,能够均匀加热食材,烹饪出美味佳肴,有独特的强度,能有效切割食物,是厨房中必不可少的利器。Stainless steel has unique strength, wear resistance, corrosion resistance, rust resistance, cleanliness and other excellent properties, and is used in various fields, such as food manufacturing, daily necessities, and household appliances. Stainless steel kitchenware is widely used in our daily lives, including but not limited to: stainless steel tableware, stainless steel knives, stainless steel cooking utensils, stainless steel pots, and stainless steel spatulas. They have good thermal conductivity, can evenly heat ingredients, cook delicious dishes, have unique strength, and can effectively cut food, making them an indispensable tool in the kitchen.
但市面上的不锈钢厨具由于工艺以及原料的问题,从而导致其强度、耐腐蚀度与耐磨损度略显不足,高温环境下容易变形,剐蹭中容易磨损,容易被其他材质腐蚀,因此需要频繁更换或磨削维护,增加了使用成本。However, due to problems with the craftsmanship and raw materials, the strength, corrosion resistance and wear resistance of stainless steel kitchen utensils on the market are slightly insufficient. They are easily deformed in high temperature environments, easily worn by scratches, and easily corroded by other materials. Therefore, they need to be frequently replaced or ground for maintenance, which increases the cost of use.
发明内容Summary of the invention
针对现有技术中存在的问题,本发明的目的是提供一种不锈钢厨具的表面处理工艺,适用的不锈钢厨具包括但不限于不锈钢餐具、不锈钢刀具、不锈钢烹饪器皿、不锈钢锅具、不锈钢漏铲。In view of the problems existing in the prior art, the purpose of the present invention is to provide a surface treatment process for stainless steel kitchenware, and applicable stainless steel kitchenware includes but is not limited to stainless steel tableware, stainless steel knives, stainless steel cooking utensils, stainless steel pots, and stainless steel spatulas.
本发明的目的采用以下技术方案来实现:The purpose of the present invention is achieved by the following technical solutions:
一种不锈钢厨具的表面处理工艺,包括以下步骤:A surface treatment process for stainless steel kitchenware comprises the following steps:
步骤1,将不锈钢基体浸泡至碱液内,超声处理,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第一处理物;Step 1, immersing the stainless steel substrate in an alkaline solution, ultrasonically treating it, taking it out and washing it in distilled water, and drying it to obtain a first treated stainless steel substrate;
步骤2,然后将不锈钢第一处理物置于混合酸液内,浸泡处理,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第二处理物;Step 2, then placing the first treated stainless steel object in a mixed acid solution, soaking it, taking it out, washing it in distilled water, and drying it to obtain a second treated stainless steel object;
步骤3,将不锈钢第二处理物以碳化锆@硒化铌微球作为靶材,使用磁控溅射的方法镀层,从而得到表面处理后的不锈钢厨具。Step 3: The second treated stainless steel object is coated with zirconium carbide @ niobium selenide microspheres as a target material by magnetron sputtering, thereby obtaining a surface-treated stainless steel kitchenware.
优选地,所述步骤1中,不锈钢基体的材质型号为304、304L、316、316L、1.4116中的一种。Preferably, in step 1, the material model of the stainless steel substrate is one of 304, 304L, 316, 316L, and 1.4116.
优选地,所述步骤1中,碱液为质量分数为5%-15%的氢氧化钠溶液,超声处理时间是超声处理10-20min。Preferably, in step 1, the alkali solution is a sodium hydroxide solution with a mass fraction of 5%-15%, and the ultrasonic treatment time is 10-20 minutes.
优选地,所述步骤2中,混合酸液为质量分数为5%氢氟酸和质量分数为20%硝酸的混合液,浸泡处理时间为20-30min。Preferably, in step 2, the mixed acid solution is a mixed solution of 5% by mass hydrofluoric acid and 20% by mass nitric acid, and the immersion treatment time is 20-30 minutes.
优选地,所述步骤3中,磁控溅射(Physical Vapor Deposition,PVD)的处理过程中,是使用高功率脉冲磁控溅射仪进行镀层处理,镀层的过程包括:Preferably, in the step 3, during the magnetron sputtering (Physical Vapor Deposition, PVD) treatment process, a high-power pulsed magnetron sputtering device is used for coating treatment, and the coating process includes:
(1)先将不锈钢第二处理物置于磁控溅射仪的腔体内,然后将腔体抽真空至压强为(3-5)×10-3Pa,升温至450-500℃处理30-50min;(1) First, place the second stainless steel treatment object in the chamber of the magnetron sputtering apparatus, then evacuate the chamber to a pressure of (3-5)×10 -3 Pa, raise the temperature to 450-500°C and treat for 30-50 minutes;
(2)向腔体内通入稀有气体作为保护气,稀有气体的流量为20-40mL/min,至压强为0.5-0.8Pa,设置偏压为0.6-1kV,进行辉光清洗处理15-20min;(2) Introduce rare gas into the chamber as protective gas, the flow rate of rare gas is 20-40mL/min, the pressure is 0.5-0.8Pa, the bias voltage is set to 0.6-1kV, and the glow cleaning process is performed for 15-20min;
(3)将腔体压强降至0.3-0.5Pa,温度为500-550℃,工架转速为3-6r/min,以碳化锆@硒化铌微球作为靶材,控制功率为3.2-5.8kW,峰值脉冲电压为0.5-0.8kV,以直流磁控溅射的方式进行镀层处理;(3) The chamber pressure is reduced to 0.3-0.5 Pa, the temperature is 500-550 ° C, the workpiece speed is 3-6 r/min, zirconium carbide @ niobium selenide microspheres are used as targets, the control power is 3.2-5.8 kW, the peak pulse voltage is 0.5-0.8 kV, and the coating is processed by DC magnetron sputtering;
(4)镀层完毕停止机器,并且降温至室温,得到表面处理后的不锈钢厨具。(4) After the coating is completed, stop the machine and cool it down to room temperature to obtain the surface-treated stainless steel kitchenware.
优选地,所述表面处理后的不锈钢厨具的表面镀层厚度为0.6-2.8μm。Preferably, the surface coating thickness of the surface treated stainless steel kitchenware is 0.6-2.8 μm.
优选地,所述碳化锆@硒化铌微球的制备方法包括:Preferably, the method for preparing the zirconium carbide@niobium selenide microspheres comprises:
S1、称取乙醇铌和去离子水混合在容器内,充分搅拌至均匀后,得到铌源溶液;称取亚硒酸钠和去离子水混合,充分搅拌至均匀后,得到硒源溶液;S1. Weigh ethanolic niobium and deionized water, mix them in a container, and stir them thoroughly to obtain a niobium source solution; weigh sodium selenite and deionized water, mix them, and stir them thoroughly to obtain a selenium source solution;
S2、将铌源溶液加入至硒源溶液内,再加入碳化锆颗粒,滴加水合肼,充分混合均匀之后,得到混合反应液;S2, adding the niobium source solution into the selenium source solution, then adding zirconium carbide particles, dropping hydrazine hydrate, and mixing thoroughly to obtain a mixed reaction solution;
S3、将混合反应液置于反应设备内,微波处理反应,反应结束后调节反应液的pH=7,然后过滤收集固体,依次经过洗涤和干燥后,得到碳化锆@硒化铌微球。S3. Place the mixed reaction liquid in a reaction device, and perform microwave treatment for reaction. After the reaction is completed, adjust the pH value of the reaction liquid to 7, and then filter and collect the solid. After washing and drying in sequence, zirconium carbide@niobium selenide microspheres are obtained.
优选地,所述S1中,铌源溶液中,乙醇铌和去离子水的质量比例为0.32-0.64:5-10;硒源溶液中,亚硒酸钠和去离子水的质量比例为0.36-0.72:5-10。Preferably, in S1, in the niobium source solution, the mass ratio of niobium ethanol to deionized water is 0.32-0.64:5-10; in the selenium source solution, the mass ratio of sodium selenite to deionized water is 0.36-0.72:5-10.
优选地,所述S2中,碳化锆颗粒、铌源溶液和硒源溶液的质量比例为1:5-10:5-10。Preferably, in S2, the mass ratio of zirconium carbide particles, niobium source solution and selenium source solution is 1:5-10:5-10.
优选地,所述S2中,水合肼的加入量是铌源溶液质量的5%-15%。Preferably, in S2, the amount of hydrazine hydrate added is 5%-15% of the mass of the niobium source solution.
优选地,所述S2中,碳化锆颗粒为球形,粒径为300-500nm。Preferably, in S2, the zirconium carbide particles are spherical and have a particle size of 300-500 nm.
优选地,所述S3中,微波处理的温度为80-120℃,功率为400-800W,处理时间是12-24h。Preferably, in S3, the temperature of the microwave treatment is 80-120° C., the power is 400-800 W, and the treatment time is 12-24 h.
优选地,所述S3中,调节反应液pH使用的是0.5-1mol/L的柠檬酸水溶液。Preferably, in S3, the pH of the reaction solution is adjusted using a 0.5-1 mol/L citric acid aqueous solution.
优选地,所述S3中,洗涤是依次经过醇洗和水洗,醇洗是使用无水乙醇洗涤至少三次,水洗是使用蒸馏水洗涤至少三次;干燥是真空干燥。Preferably, in S3, washing is performed sequentially by alcohol washing and water washing, the alcohol washing is performed at least three times using anhydrous ethanol, and the water washing is performed at least three times using distilled water; and drying is vacuum drying.
本发明的有益效果为:The beneficial effects of the present invention are:
1、本发明公开了一种新型的不锈钢厨具的表面处理工艺,处理后的不锈钢厨具相比较于目前市面上的产品具备更为优异的强度、韧性、耐磨性以及耐腐蚀性。1. The present invention discloses a new surface treatment process for stainless steel kitchenware. Compared with the products currently on the market, the treated stainless steel kitchenware has better strength, toughness, wear resistance and corrosion resistance.
2、本发明在镀层前对不锈钢基体依次进行碱液超声以及酸液浸泡处理,碱液超声的目的是除油,酸液浸泡的目的是粗化,目的是为了提高不锈钢基体材料的表面对后续镀层的附着力。2. The present invention sequentially performs alkaline solution ultrasonic treatment and acid solution immersion treatment on the stainless steel substrate before coating. The purpose of alkaline solution ultrasonic treatment is to remove oil, and the purpose of acid solution immersion is to roughen the surface of the stainless steel substrate material, so as to improve the adhesion of the surface of the subsequent coating.
3、本发明在不锈钢厨具的表面利用磁控溅射的方式镀层,镀层材质为碳化锆@硒化铌微球,该微球是以碳化锆颗粒作为基体,经过水热微波反应,在碳化锆的表面原位生成硒化铌,从而得到硒化铌包覆的碳化锆微球。3. The present invention utilizes magnetron sputtering to coat the surface of stainless steel kitchenware. The coating material is zirconium carbide @ niobium selenide microspheres. The microspheres use zirconium carbide particles as a matrix. Niobium selenide is generated in situ on the surface of zirconium carbide through a hydrothermal microwave reaction, thereby obtaining zirconium carbide microspheres coated with niobium selenide.
4、本发明将碳化锆@硒化铌微球磁控溅射至不锈钢厨具的表面,不仅增强了不锈钢厨具材料的硬度和韧性,而且增强了其耐腐蚀性和耐磨性,使得以此工艺制成的不锈钢厨具能够更加轻松地应付比较特殊的环境,比如可以应对酸碱性较强的材料,不锈钢刀具可用于砍切较硬的食物。4. The present invention magnetron sputters zirconium carbide @ niobium selenide microspheres onto the surface of stainless steel kitchenware, which not only enhances the hardness and toughness of the stainless steel kitchenware material, but also enhances its corrosion resistance and wear resistance, so that the stainless steel kitchenware made by this process can more easily cope with more special environments, such as materials with strong acidity and alkalinity, and stainless steel knives can be used to chop harder food.
具体实施方式DETAILED DESCRIPTION
以下通过特定的具体实例说明本发明的技术方案。应理解,本发明提到的一个或多个方法步骤并不排斥在所述组合步骤前后还存在其他方法步骤或在这些明确提到的步骤之间还可以插入其他方法步骤;还应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。而且,除非另有说明,各方法步骤的编号仅为鉴别各方法步骤的便利工具,而非为限制各方法步骤的排列次序或限定本发明可实施的范围,其相对关系的改变或调整,在无实质变更技术内容的情况下,当亦视为本发明可实施的范畴。The technical solution of the present invention is described below through specific examples. It should be understood that the one or more method steps mentioned in the present invention do not exclude the existence of other method steps before and after the combination step or the insertion of other method steps between these explicitly mentioned steps; it should also be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. Moreover, unless otherwise specified, the numbering of each method step is only a convenient tool for identifying each method step, and is not intended to limit the order of arrangement of each method step or to limit the scope of the present invention. The change or adjustment of the relative relationship thereof shall also be regarded as the scope of the present invention without substantially changing the technical content.
为了更好的理解上述技术方案,下面更详细地描述本发明的示例性实施例。虽然显示了本发明的示例性实施例,然而应当理解,可以以各种形式实现本发明而不应被这里阐述的实施例所限制。相反,提供这些实施例是为了能够更透彻地理解本发明,并且能够将本发明的范围完整的传达给本领域的技术人员。In order to better understand the above technical scheme, the exemplary embodiments of the present invention are described in more detail below. Although exemplary embodiments of the present invention are shown, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided in order to enable a more thorough understanding of the present invention and to enable the scope of the present invention to be fully communicated to those skilled in the art.
下面结合以下实施例对本发明作进一步描述。The present invention will be further described below in conjunction with the following examples.
实施例1Example 1
一种不锈钢厨具的表面处理工艺,包括以下步骤:A surface treatment process for stainless steel kitchenware comprises the following steps:
步骤1,将尺寸为10cm×8cm×0.2cm的不锈钢304L基体浸泡至质量分数为10%的氢氧化钠溶液内,超声处理15min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第一处理物;Step 1, immersing a stainless steel 304L substrate having a size of 10 cm×8 cm×0.2 cm in a sodium hydroxide solution having a mass fraction of 10%, ultrasonically treating the substrate for 15 minutes, taking the substrate out and washing it in distilled water, and drying the substrate to obtain a first treated stainless steel substrate;
步骤2,然后将不锈钢第一处理物置于质量分数为5%氢氟酸和质量分数为20%硝酸组成的混合液内,浸泡处理25min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第二处理物;Step 2, then placing the first treated stainless steel object in a mixed solution consisting of 5% by mass hydrofluoric acid and 20% by mass nitric acid, soaking for 25 minutes, taking it out and washing it in distilled water, and drying it to obtain the second treated stainless steel object;
步骤3,将不锈钢第二处理物以碳化锆@硒化铌微球作为靶材,使用高功率脉冲磁控溅射仪进行磁控溅射(PVD)镀层,镀层的过程包括:(1)先将不锈钢第二处理物置于磁控溅射仪的腔体内,然后将腔体抽真空至压强为4×10-3Pa,升温至500℃处理40min;(2)向腔体内通入氩气作为保护气,氩气的流量为30mL/min,至压强为0.6Pa,设置偏压为0.8kV,进行辉光清洗处理20min;(3)将腔体压强降至0.4Pa,温度为500℃,工架转速为5r/min,以碳化锆@硒化铌微球作为靶材,控制功率为4.6kW,峰值脉冲电压为0.6kV,以直流磁控溅射的方式进行镀层处理;(4)镀层完毕停止机器,并且降温至室温,得到表面镀层厚度为1.5μm的不锈钢厨具。Step 3: The stainless steel second treatment object is subjected to magnetron sputtering (PVD) coating using zirconium carbide @ niobium selenide microspheres as a target material using a high-power pulsed magnetron sputtering apparatus. The coating process includes: (1) first placing the stainless steel second treatment object in the chamber of the magnetron sputtering apparatus, and then evacuating the chamber to a pressure of 4×10 -3 Pa, and heat to 500℃ for 40min; (2) introduce argon as protective gas into the chamber, with a flow rate of 30mL/min, until the pressure reaches 0.6Pa, set the bias voltage to 0.8kV, and perform glow cleaning for 20min; (3) reduce the chamber pressure to 0.4Pa, the temperature to 500℃, the workbench speed to 5r/min, use zirconium carbide @ niobium selenide microspheres as the target material, control the power to 4.6kW, and the peak pulse voltage to 0.6kV, and perform coating by DC magnetron sputtering; (4) stop the machine after coating is completed, and cool to room temperature to obtain stainless steel kitchenware with a surface coating thickness of 1.5μm.
其中,碳化锆@硒化铌微球的制备方法包括:The preparation method of zirconium carbide@niobium selenide microspheres includes:
S1、称取乙醇铌和去离子水混合在容器内,乙醇铌和去离子水的质量比例为0.48:10,充分搅拌至均匀后,得到铌源溶液;称取亚硒酸钠和去离子水混合,亚硒酸钠和去离子水的质量比例为0.54:10,充分搅拌至均匀后,得到硒源溶液;S1. Weigh ethanolic niobium and deionized water, mix them in a container, the mass ratio of ethanolic niobium to deionized water is 0.48:10, and stir them thoroughly to obtain a niobium source solution; weigh sodium selenite and deionized water, mix them, the mass ratio of sodium selenite to deionized water is 0.54:10, and stir them thoroughly to obtain a selenium source solution;
S2、将铌源溶液加入至硒源溶液内,再加入粒径为300-500nm的碳化锆球形颗粒(纯度>99%),碳化锆颗粒、铌源溶液和硒源溶液的质量比例为1:6:6,滴加铌源溶液质量的10%的水合肼,充分混合均匀之后,得到混合反应液;S2, adding the niobium source solution to the selenium source solution, and then adding zirconium carbide spherical particles with a particle size of 300-500 nm (purity> 99%), the mass ratio of zirconium carbide particles, niobium source solution and selenium source solution is 1:6:6, and dropping hydrazine hydrate of 10% of the mass of the niobium source solution, after fully mixing, to obtain a mixed reaction solution;
S3、将混合反应液置于反应设备内,微波处理反应,温度为100℃,功率为600W,处理时间为18h,反应结束后使用0.5mol/L的柠檬酸水溶液调节反应液的pH=7,然后过滤收集固体,先使用无水乙醇洗涤至少三次,再使用蒸馏水洗涤至少三次,真空干燥,得到碳化锆@硒化铌微球。S3. Place the mixed reaction liquid in a reaction device and perform microwave treatment reaction at a temperature of 100°C, a power of 600 W, and a treatment time of 18 h. After the reaction, use 0.5 mol/L citric acid aqueous solution to adjust the pH of the reaction liquid to 7, and then filter and collect the solid, wash it with anhydrous ethanol for at least three times, and then wash it with distilled water for at least three times, and vacuum dry it to obtain zirconium carbide @ niobium selenide microspheres.
实施例2Example 2
一种不锈钢厨具的表面处理工艺,包括以下步骤:A surface treatment process for stainless steel kitchenware comprises the following steps:
步骤1,将不锈钢304L基体浸泡至质量分数为5%的氢氧化钠溶液内,超声处理20min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第一处理物;Step 1, immersing a stainless steel 304L substrate in a sodium hydroxide solution with a mass fraction of 5%, ultrasonically treating it for 20 minutes, taking it out and washing it in distilled water, and drying it to obtain a first treated stainless steel product;
步骤2,然后将不锈钢第一处理物置于质量分数为5%氢氟酸和质量分数为20%硝酸组成的混合液内,浸泡处理20min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第二处理物;Step 2, then placing the first treated stainless steel object in a mixed solution consisting of 5% by mass hydrofluoric acid and 20% by mass nitric acid, soaking for 20 minutes, taking it out and washing it in distilled water, and drying it to obtain the second treated stainless steel object;
步骤3,将不锈钢第二处理物以碳化锆@硒化铌微球(制备与实施例1相同)作为靶材,使用高功率脉冲磁控溅射仪进行磁控溅射(PVD)镀层,镀层的过程包括:(1)先将不锈钢第二处理物置于磁控溅射仪的腔体内,然后将腔体抽真空至压强为3×10-3Pa,升温至450℃处理50min;(2)向腔体内通入氦气作为保护气,氦气的流量为20mL/min,至压强为0.5Pa,设置偏压为0.6kV,进行辉光清洗处理15min;(3)将腔体压强降至0.3Pa,温度为500℃,工架转速为3r/min,以碳化锆@硒化铌微球作为靶材,控制功率为3.2kW,峰值脉冲电压为0.5kV,以直流磁控溅射的方式进行镀层处理;(4)镀层完毕停止机器,并且降温至室温,得到表面镀层厚度为0.6μm的不锈钢厨具。Step 3: The second stainless steel object is subjected to magnetron sputtering (PVD) coating using zirconium carbide @ niobium selenide microspheres (prepared in the same manner as in Example 1) as a target material using a high-power pulsed magnetron sputtering apparatus. The coating process includes: (1) first placing the second stainless steel object in a chamber of the magnetron sputtering apparatus, and then evacuating the chamber to a pressure of 3×10 -3 Pa, heat to 450℃ and treat for 50min; (2) introduce helium as protective gas into the chamber, the flow rate of helium is 20mL/min, until the pressure is 0.5Pa, set the bias voltage to 0.6kV, and perform glow cleaning for 15min; (3) reduce the chamber pressure to 0.3Pa, the temperature to 500℃, the workbench speed to 3r/min, use zirconium carbide @ niobium selenide microspheres as target materials, control power to 3.2kW, peak pulse voltage to 0.5kV, and perform coating by DC magnetron sputtering; (4) stop the machine after coating is completed, and cool to room temperature to obtain stainless steel kitchenware with a surface coating thickness of 0.6μm.
实施例3Example 3
一种不锈钢厨具的表面处理工艺,包括以下步骤:A surface treatment process for stainless steel kitchenware comprises the following steps:
步骤1,将不锈钢304L基体浸泡至质量分数为15%的氢氧化钠溶液内,超声处理10min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第一处理物;Step 1, immersing a stainless steel 304L substrate in a sodium hydroxide solution with a mass fraction of 15%, ultrasonically treating it for 10 minutes, taking it out and washing it in distilled water, and drying it to obtain a first treated stainless steel product;
步骤2,然后将不锈钢第一处理物置于质量分数为5%氢氟酸和质量分数为20%硝酸组成的混合液内,浸泡处理30min,取出后置于蒸馏水内清洗,干燥后,得到不锈钢第二处理物;Step 2, then placing the first treated stainless steel object in a mixed solution consisting of 5% by mass hydrofluoric acid and 20% by mass nitric acid, soaking for 30 minutes, taking it out and washing it in distilled water, and drying it to obtain the second treated stainless steel object;
步骤3,将不锈钢第二处理物以碳化锆@硒化铌微球(制备与实施例1相同)作为靶材,使用高功率脉冲磁控溅射仪进行磁控溅射(PVD)镀层,镀层的过程包括:(1)先将不锈钢第二处理物置于磁控溅射仪的腔体内,然后将腔体抽真空至压强为5×10-3Pa,升温至500℃处理30min;(2)向腔体内通入氖气作为保护气,氖气的流量为40mL/min,至压强为0.8Pa,设置偏压为1kV,进行辉光清洗处理20min;(3)将腔体压强降至0.5Pa,温度为550℃,工架转速为6r/min,以碳化锆@硒化铌微球作为靶材,控制功率为5.8kW,峰值脉冲电压为0.8kV,以直流磁控溅射的方式进行镀层处理;(4)镀层完毕停止机器,并且降温至室温,得到表面镀层厚度为2.8μm的不锈钢厨具。Step 3: The second stainless steel object is subjected to magnetron sputtering (PVD) coating using zirconium carbide @ niobium selenide microspheres (prepared in the same manner as in Example 1) as a target material using a high-power pulsed magnetron sputtering apparatus. The coating process includes: (1) first placing the second stainless steel object in a chamber of the magnetron sputtering apparatus, and then evacuating the chamber to a pressure of 5×10 -3 Pa, heat to 500℃ and treat for 30min; (2) introduce neon gas as protective gas into the chamber, the neon flow rate is 40mL/min, until the pressure is 0.8Pa, set the bias voltage to 1kV, and perform glow cleaning for 20min; (3) reduce the chamber pressure to 0.5Pa, the temperature to 550℃, the workbench speed to 6r/min, use zirconium carbide @ niobium selenide microspheres as target materials, control power to 5.8kW, peak pulse voltage to 0.8kV, and perform coating by DC magnetron sputtering; (4) stop the machine after coating is completed, and cool to room temperature to obtain stainless steel kitchenware with a surface coating thickness of 2.8μm.
实施例4Example 4
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,碳化锆@硒化铌微球的制备方法不相同。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the preparation method of zirconium carbide@niobium selenide microspheres is different.
碳化锆@硒化铌微球的制备方法包括:The preparation method of zirconium carbide@niobium selenide microspheres includes:
S1、称取乙醇铌和去离子水混合在容器内,乙醇铌和去离子水的质量比例为0.32:5,充分搅拌至均匀后,得到铌源溶液;称取亚硒酸钠和去离子水混合,亚硒酸钠和去离子水的质量比例为0.36:5,充分搅拌至均匀后,得到硒源溶液;S1. Weigh ethanolic niobium and deionized water, mix them in a container, the mass ratio of ethanolic niobium to deionized water is 0.32:5, and stir them thoroughly to obtain a niobium source solution; weigh sodium selenite and deionized water, mix them, the mass ratio of sodium selenite to deionized water is 0.36:5, and stir them thoroughly to obtain a selenium source solution;
S2、将铌源溶液加入至硒源溶液内,再加入粒径为300-500nm的碳化锆球形颗粒,碳化锆颗粒、铌源溶液和硒源溶液的质量比例为1:5:5,滴加铌源溶液质量的5%的水合肼,充分混合均匀之后,得到混合反应液;S2, adding the niobium source solution to the selenium source solution, and then adding spherical zirconium carbide particles with a particle size of 300-500 nm, the mass ratio of the zirconium carbide particles, the niobium source solution and the selenium source solution is 1:5:5, and dropping 5% of hydrazine hydrate by mass of the niobium source solution, after fully mixing, to obtain a mixed reaction solution;
S3、将混合反应液置于反应设备内,微波处理反应,温度为80℃,功率为400W,处理时间为24h,反应结束后使用0.5mol/L的柠檬酸水溶液调节反应液的pH=7,然后过滤收集固体,先使用无水乙醇洗涤至少三次,再使用蒸馏水洗涤至少三次,真空干燥,得到碳化锆@硒化铌微球。S3. Place the mixed reaction liquid in a reaction device and perform microwave treatment at 80°C, 400W, and 24h. After the reaction, adjust the pH value of the reaction liquid to 7 with 0.5mol/L citric acid aqueous solution. Then filter and collect the solid, wash it at least three times with anhydrous ethanol, and then wash it at least three times with distilled water, and dry it in vacuum to obtain zirconium carbide@niobium selenide microspheres.
实施例5Example 5
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,碳化锆@硒化铌微球的制备方法不相同。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the preparation method of zirconium carbide@niobium selenide microspheres is different.
碳化锆@硒化铌微球的制备方法包括:The preparation method of zirconium carbide@niobium selenide microspheres includes:
S1、称取乙醇铌和去离子水混合在容器内,乙醇铌和去离子水的质量比例为0.64:10,充分搅拌至均匀后,得到铌源溶液;称取亚硒酸钠和去离子水混合,亚硒酸钠和去离子水的质量比例为0.72:10,充分搅拌至均匀后,得到硒源溶液;S1. Weigh ethanolic niobium and deionized water, mix them in a container, the mass ratio of ethanolic niobium to deionized water is 0.64:10, and stir them thoroughly to obtain a niobium source solution; weigh sodium selenite and deionized water, mix them, the mass ratio of sodium selenite to deionized water is 0.72:10, and stir them thoroughly to obtain a selenium source solution;
S2、将铌源溶液加入至硒源溶液内,再加入粒径为300-500nm的碳化锆球形颗粒,碳化锆颗粒、铌源溶液和硒源溶液的质量比例为1:10:10,滴加铌源溶液质量的15%的水合肼,充分混合均匀之后,得到混合反应液;S2, adding the niobium source solution to the selenium source solution, and then adding spherical zirconium carbide particles with a particle size of 300-500 nm, the mass ratio of the zirconium carbide particles, the niobium source solution and the selenium source solution is 1:10:10, and dropping 15% of hydrazine hydrate by mass of the niobium source solution, after fully mixing, to obtain a mixed reaction solution;
S3、将混合反应液置于反应设备内,微波处理反应,温度为120℃,功率为800W,处理时间为12h,反应结束后使用1mol/L的柠檬酸水溶液调节反应液的pH=7,然后过滤收集固体,先使用无水乙醇洗涤至少三次,再使用蒸馏水洗涤至少三次,真空干燥,得到碳化锆@硒化铌微球。S3. Place the mixed reaction liquid in a reaction device and perform microwave treatment at a temperature of 120°C, a power of 800 W, and a treatment time of 12 h. After the reaction, adjust the pH value of the reaction liquid to 7 using a 1 mol/L citric acid aqueous solution. Then filter and collect the solid, wash it at least three times with anhydrous ethanol, then wash it at least three times with distilled water, and vacuum dry it to obtain zirconium carbide @ niobium selenide microspheres.
实施例6Example 6
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,不锈钢基体的型号为304。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the model of the stainless steel substrate is 304.
实施例7Example 7
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,不锈钢基体的型号为316。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the model of the stainless steel substrate is 316.
实施例8Example 8
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,不锈钢基体的型号为316L。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the model of the stainless steel substrate is 316L.
实施例9Example 9
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,不锈钢基体的型号为1.4116钢(德国DIN 17400标准)。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the model of the stainless steel substrate is 1.4116 steel (German DIN 17400 standard).
对比例1Comparative Example 1
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,所使用的碳化锆@硒化铌微球替换为市面购买的300-500nm的碳化锆颗粒(纯度>99%)。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the zirconium carbide@niobium selenide microspheres used are replaced with 300-500nm zirconium carbide particles (purity>99%) purchased from the market.
对比例2Comparative Example 2
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,所使用的碳化锆@硒化铌微球替换为市面购买的300-500nm的硒化铌(IV)颗粒(纯度>99%)。A surface treatment process for stainless steel kitchenware, which is different from Example 1 only in that the zirconium carbide@niobium selenide microspheres used are replaced with 300-500nm niobium (IV) selenide particles (purity> 99%) purchased from the market.
对比例3Comparative Example 3
一种不锈钢厨具的表面处理工艺,与实施例1的区别仅在于,所使用的碳化锆@硒化铌微球替换为市面购买的碳化锆颗粒(纯度>99%)和硒化铌(IV)颗粒(纯度>99%)的混合物,碳化锆颗粒和硒化铌(IV)颗粒的质量比为1:0.6。A surface treatment process for stainless steel kitchenware, which differs from Example 1 only in that the zirconium carbide@niobium selenide microspheres used are replaced by a mixture of zirconium carbide particles (purity>99%) and niobium (IV) selenide particles (purity>99%) purchased from the market, and the mass ratio of the zirconium carbide particles to the niobium (IV) selenide particles is 1:0.6.
检测实验Detection experiment
将实施例1、对比例1-3制备得到的表面镀层的不锈钢厨具的性能进行了检测,拉伸强度和屈服强度检测参考GB/T 228.1-2010,硬度检测参考GB/T 230.1-2018,冲击功检测参考GB/T 229-2007,耐酸碱腐蚀性检测参考GB/T19291-2003,结果如表1所示。The properties of the stainless steel kitchen utensils with surface coatings prepared in Example 1 and Comparative Examples 1-3 were tested. The tensile strength and yield strength tests were referred to GB/T 228.1-2010, the hardness test was referred to GB/T 230.1-2018, the impact energy test was referred to GB/T 229-2007, and the acid and alkali corrosion resistance test was referred to GB/T19291-2003. The results are shown in Table 1.
表1 不同镀层的不锈钢材料的性能表现Table 1 Performance of stainless steel materials with different coatings
表1中能够看出,实施例1所制备的不锈钢厨具材料具备更好的强度、韧性、硬度以及耐腐蚀性,说明其性能表现更佳,更适合用于对于性能要求更高的环境,特别是比较硬的材料和酸碱性强的环境等。It can be seen from Table 1 that the stainless steel kitchenware material prepared in Example 1 has better strength, toughness, hardness and corrosion resistance, indicating that its performance is better and is more suitable for use in environments with higher performance requirements, especially relatively hard materials and environments with strong acidity and alkalinity.
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、 “示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不应理解为必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。此外,本领域的技术人员可以将本说明书中描述的不同实施例或示例进行接合和组合。In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms should not be understood as necessarily being directed to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification.
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.
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CN108752845A (en) * | 2018-06-20 | 2018-11-06 | 安徽江淮汽车集团股份有限公司 | A kind of wear-resisting ABS composite material of antibacterial and preparation method thereof |
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CN108752845A (en) * | 2018-06-20 | 2018-11-06 | 安徽江淮汽车集团股份有限公司 | A kind of wear-resisting ABS composite material of antibacterial and preparation method thereof |
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