WO2018107846A1 - 一种镀镍碳化硅颗粒及其制备方法 - Google Patents

一种镀镍碳化硅颗粒及其制备方法 Download PDF

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WO2018107846A1
WO2018107846A1 PCT/CN2017/102828 CN2017102828W WO2018107846A1 WO 2018107846 A1 WO2018107846 A1 WO 2018107846A1 CN 2017102828 W CN2017102828 W CN 2017102828W WO 2018107846 A1 WO2018107846 A1 WO 2018107846A1
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silicon carbide
nickel
carbide particles
mixture
plated
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French (fr)
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孙飞
赵勇
埃里克斯⋅高登
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苏州金仓合金新材料有限公司
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18Non-metallic particles coated with metal
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1635Composition of the substrate
    • C23C18/1639Substrates other than metallic, e.g. inorganic or organic or non-conductive
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18Pretreatment of the material to be coated
    • C23C18/1851Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1875Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
    • C23C18/1882Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers

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  • the invention relates to a method for preparing nickel-plated silicon carbide particles, in particular to a method for preparing nickel-plated silicon carbide particles for composite materials, and to nickel-plated silicon carbide particles prepared by the method.
  • Silicon carbide has the advantages of high purity, small particle size, uniform distribution, large specific surface area, high surface activity and low bulk density, and silicon carbide also has excellent mechanical, thermal, electrical and chemical properties, ie high hardness, High wear resistance and good self-lubrication, high thermal conductivity, low thermal expansion coefficient and high temperature strength make SiC ceramics widely used.
  • the friction coefficient is very small, and it has good self-lubricating properties, and is particularly suitable for making seals with airtight or dry friction conditions. Used in the process to improve the service life of the seal and the reliability of the work.
  • silicon carbide particles are difficult to uniformly disperse inside the metal material because of the low density (3.2 g/cm 3 ).
  • an object of the present invention is to provide a method for preparing nickel-plated silicon carbide particles, and nickel-plated silicon carbide particles prepared by the method.
  • Step one activating silicon carbide particles: adding silicon carbide particles to an alcohol solution of nickel acetate and sodium borohydride, adding a stabilizer NaOH solution, and stirring to form a mixture 1;
  • Step 2 The precipitate which is activated in the first step is allowed to stand for precipitation, and after filtration, the precipitate is washed with distilled water, and after washing, it is filtered and dried;
  • Step 3 Electroless nickel plating: adding the activated silicon carbide particles and the stabilizer thiourea dried in the second step to the main salt nickel sulfate hexahydrate, the reducing agent sodium phosphite monohydrate, the complexing agent citric acid and the buffer ammonium sulfate Forming a mixture 2 in the mixed solution, heating and stirring the mixture in a water bath, and adding a NaOH solution while heating and stirring to adjust the pH of the mixture 2 to be alkaline;
  • Step 4 The mixture obtained by electroless nickel plating in the third step is left to be precipitated, and after filtration, the precipitate is washed with distilled water. After the washing is completed, the mixture is filtered and dried to obtain nickel-plated silicon carbide particles.
  • the silicon carbide particles used in the first step have an average particle diameter of 5 ⁇ m.
  • the stirring time is 30 min, and the stirring speed is 400 r/min.
  • the pH of the mixture 2 in the third step is 9.
  • the water bath heating temperature is 40 ° C
  • the stirring speed is 400 r / min.
  • drying in the second step and the fourth step is performed at a temperature of 70-80 ° C.
  • a nickel-plated silicon carbide particle prepared by the preparation method as described above.
  • Nickel is attached to increase the degree of uniform fusion of silicon carbide and metal materials, avoiding segregation and cracking of composite materials, and improving the yield of composite materials.
  • 1 and 2 are scanning electron microscope (SEM) photographs of activated silicon carbide particles in the first step of the present invention
  • 3A and 3B are scanning electron microscope (SEM) photographs of nickel-plated silicon carbide particles prepared according to the present invention.
  • Fig. 5 is a comparison diagram of XRD spectra of nickel-plated silicon carbide particles after alkaline electroless nickel plating and nickel-plated silicon carbide particles after continuous annealing.
  • the preparation method of the nickel-plated silicon carbide particles of the invention comprises the following steps:
  • Step 1 Activate silicon carbide particles: According to the reaction formula and reaction conditions shown in Table 1, quantitative silicon carbide particles (average particle size 5 ⁇ m) were added to an alcohol solution of nickel acetate and sodium borohydride, and an appropriate amount of 10% was added dropwise. NaOH solution as a stabilizer, after stirring at room temperature for 30min, stirring speed of 400r / min, forming a mixture;
  • Step 2 The precipitated mixture in the first step is allowed to stand for precipitation, and the precipitate is washed with distilled water after filtration. After the washing is completed, it is filtered and dried at 70-80 ° C; as shown in FIGS. 1 and 2, the activated silicon carbide is shown. Particles, a small amount of particles are attached to the surface of the silicon carbide particles, and it can be seen from the results of the EDS spectrum (Fig. 1) that nickel is adhered to the surface of the silicon carbide particles, so that it can be concluded that after the above steps one and two, Nickel is adhered to the surface of the silicon carbide particles.
  • Step 3 electroless nickel plating: according to the reaction formula and reaction conditions shown in Table 2, the quantitative Nickel hexahydrate (main salt), sodium hypophosphite (reducing agent), citric acid (complexing agent) and ammonium sulfate (buffering agent) are added to the beaker, and distilled water is added until the solid matter is completely dissolved to form a plating solution. ;
  • the activated silicon carbide particles dried in the second step and the trace stabilizer thiourea are added to the above plating solution to form a mixture 2, and the mixture is heated in a water bath and stirred (heating temperature is 40 ° C, stirring speed is 400 r / min), and Adding NaOH solution while heating and stirring to adjust the pH of the mixture 2 to be alkaline;
  • Step 4 The mixture obtained by electroless nickel plating in the third step is left to be precipitated, and after filtration, the precipitate is washed with distilled water. After the washing is completed, it is filtered and dried at 70-80 ° C to obtain nickel-plated silicon carbide particles.
  • the preparation method of the nickel-plated silicon carbide particles of the invention comprises the following steps:
  • Step 1 Activate silicon carbide particles: 40 g of silicon carbide particles (average particle diameter of 5 ⁇ m) is added to an alcohol solution prepared by disposing 12 g of nickel acetate, sodium borohydride 4 g and 1 L of ethanol, and an appropriate amount of 10% NaOH solution is added as a stabilizer. After stirring at room temperature for 30 min, the stirring speed is 400 r / min, forming a mixture;
  • Step 2 The precipitate which is activated in the first step is allowed to stand for precipitation, and after filtration, the precipitate is washed with distilled water, and after washing, it is filtered and dried at 80 ° C;
  • Step 3 electroless nickel plating: According to the reaction formula and reaction conditions shown in Table 2, 26 g of nickel sulfate hexahydrate (main salt), 20 g of sodium hypophosphite (reducing agent), 44 g of citric acid (complexing agent) And 66g ammonium sulfate (buffering agent) is added to the beaker, and distilled water is added until the solid matter is completely dissolved to form a plating solution;
  • Step 4 The mixture obtained by electroless nickel plating in the third step is allowed to stand for precipitation, and after filtration, the precipitate is washed with distilled water. After the washing is completed, it is filtered and dried at 80 ° C to obtain nickel-plated silicon carbide particles.
  • the preparation method of the nickel-plated silicon carbide particles of the invention comprises the following steps:
  • Step 1 Activate silicon carbide particles: 20 g of silicon carbide particles (average particle diameter of 5 ⁇ m) is added to an alcohol solution of 6 g of nickel acetate, sodium borohydride 2 g and 500 mL of ethanol, and an appropriate amount of 10% NaOH solution is added as a stabilizer. After stirring at room temperature for 30 min, the stirring speed is 400 r / min, forming a mixture;
  • Step 2 The precipitate which is activated in the first step is allowed to stand for precipitation, and after filtration, the precipitate is washed with distilled water, and after washing, it is filtered and dried at 70 ° C;
  • Step 3 Electroless nickel plating: According to the reaction formula and reaction conditions shown in Table 2, 13 g of nickel sulfate hexahydrate (main salt), 10 g of sodium hypophosphite (reducing agent), and 22 g of citric acid (complexing agent) And 33 g of ammonium sulfate (buffer) is added to the beaker, and distilled water is added until the solid matter is completely dissolved to form a plating solution;
  • Step 4 The mixture obtained by electroless nickel plating in the third step is left to be precipitated, and after filtration, the precipitate is washed with distilled water. After the washing is completed, it is filtered and dried at 70 ° C to obtain nickel-plated silicon carbide particles.
  • Nickel is attached to increase the degree of uniform fusion of silicon carbide and metal materials, avoiding segregation and cracking of composite materials, and improving the yield of composite materials.

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

一种镀镍碳化硅颗粒的制备方法,其包括以下步骤:步骤一:活化碳化硅颗粒;步骤二:洗涤、过滤并烘干;步骤三:化学镀镍;步骤四:洗涤、过滤并烘干。选取一定粒径的碳化硅颗粒,通过清洗-活化处理-特定溶液镀镍的方法,将碳化硅颗粒表面进行涂层、镀镍,使碳化硅颗粒表面均匀附着镍,从而提高碳化硅与金属材料的均匀融合程度,避免出现复合材料的偏析与龟裂问题,提高复合材料的成材率。

Description

一种镀镍碳化硅颗粒及其制备方法 技术领域
本发明涉及一种镀镍碳化硅颗粒的制备方法,特别是一种复合材料用镀镍碳化硅颗粒的制备方法,本发明还涉及采用该方法所制备的镀镍碳化硅颗粒。
背景技术
碳化硅具有纯度高、粒径小、分布均匀、比表面积大、高表面活性、松装密度低的优点,并且碳化硅还具有极好的力学、热学、电学和化学性能,即具有高硬度、高耐磨性和良好的自润滑、高热传导率、低热膨胀系数及高温强度大等特点,这使得碳化硅陶瓷得到了广泛的应用。
由于在碳化硅基体中含有大量的弥散细小的石墨颗粒,与其它材料配对使用时,其摩擦系数非常小,具有良好的自润滑性能,特别适用于制作气密封或有干摩擦工况的密封件中使用,从而使密封件的使用寿命及工作的可靠性提高。但是,碳化硅颗粒由于密度较小(3.2g/cm3),很难在金属材料内部均匀的弥散。
发明内容
针对上述问题,本发明的目的是提供一种镀镍碳化硅颗粒的制备方法,以及采用该方法所制备的镀镍碳化硅颗粒。
为达到上述目的,本发明采用如下技术方案:
根据本发明,提供一种镀镍碳化硅颗粒的制备方法,包括以下步骤:
步骤一,活化碳化硅颗粒:将碳化硅颗粒加入乙酸镍和硼氢化钠的醇溶液中,滴加稳定剂NaOH溶液后进行搅拌,形成混合物一;
步骤二:将步骤一中活化完成的混合物一静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并烘干;
步骤三,化学镀镍:将步骤二中烘干的活化碳化硅颗粒和稳定剂硫脲加入主盐六水硫酸镍、还原剂一水次亚磷酸钠、络合剂柠檬酸和缓冲剂硫酸铵的混合溶液中形成混合物二,将混合物二水浴加热并搅拌,并在加热搅拌的同时加入NaOH溶液调节混合物二的pH值为碱性;
步骤四:将步骤三中化学镀镍完成的混合物二静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并烘干得到镀镍碳化硅颗粒。
进一步地,所述步骤一中使用的碳化硅颗粒平均粒径为5μm。
进一步地,所述步骤一中乙酸镍和硼氢化钠的质量比为乙酸镍∶硼氢化钠=3∶1。
进一步地,所述步骤一中碳化硅、乙酸镍和硼氢化钠的质量比为碳化硅∶乙酸镍∶硼氢化钠=10∶3∶1。
进一步地,所述步骤一中搅拌时间为30min,搅拌速度为400r/min。
进一步地,所述步骤三中六水硫酸镍、一水次亚磷酸钠、柠檬酸、硫酸铵的质量比为六水硫酸镍∶一水次亚磷酸钠∶柠檬酸∶硫酸铵=13∶10∶22∶33。
进一步地,所述步骤三中混合物二的pH值为9。
进一步地,所述步骤三中水浴加热温度为40℃,搅拌速度为400r/min。
进一步地,所述步骤二和所述步骤四中的所述烘干在70-80℃的温度下进行。
根据本发明,提供一种镀镍碳化硅颗粒,通过如上所述的制备方法制备而成。
本发明选取一定粒径(平均粒径R=5μm)的碳化硅颗粒,通过清洗-活化处理-特定溶液镀镍的方法,将碳化硅颗粒表面进行涂层、镀镍,使碳化硅颗粒表面均匀附着镍,从而提高碳化硅与金属材料的均匀融合程度,避免出现复合材料的偏析与龟裂问题,提高复合材料的成材率。
附图说明
图1和图2是本发明步骤一中活化后的碳化硅颗粒的扫描电子显微镜(SEM)照片;
图3A和3B为本发明所制备的镀镍碳化硅颗粒的扫描电子显微镜(SEM)照片;
图4为本发明所制备的镀镍碳化硅颗粒的EDS能谱图;
图5为在碱性化学镀镍后的镀镍碳化硅颗粒和继续退火处理后的镀镍碳化硅颗粒的XRD谱的对比图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,下面结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
本发明的镀镍碳化硅颗粒的制备方法,包括以下步骤:
步骤一:活化碳化硅颗粒:按照表1所示的反应配方和反应条件,将定量的碳化硅颗粒(平均粒径为5μm)加入乙酸镍和硼氢化钠的醇溶液中,滴加适量10%NaOH溶液作为稳定剂,之后常温搅拌30min,搅拌速度为400r/min,形成混合物一;
Figure PCTCN2017102828-appb-000001
表1
步骤二:将步骤一中活化完成的混合物一静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于70-80℃下烘干;如图1和2所示为活化后的碳化硅颗粒,该碳化硅颗粒表面附着有少量的颗粒,并且从EDS能谱(图1)测量的结果可以看出,碳化硅颗粒表面附着有镍,因此可以得出结论,经过上述步骤一和二,碳化硅颗粒表面附着有镍。
步骤三,化学镀镍:按照表2所示的反应配方和反应条件,将定量的 六水硫酸镍(主盐)、一水次亚磷酸钠(还原剂)、柠檬酸(络合剂)和硫酸铵(缓冲剂)加入烧杯中,并加入蒸馏水直至固体物质全部溶解,形成镀液;
Figure PCTCN2017102828-appb-000002
表2
将步骤二中烘干的活化碳化硅颗粒和痕量稳定剂硫脲加入上述镀液中形成混合物二,将混合物二水浴加热并搅拌(加热温度为40℃,搅拌速度为400r/min),并在加热搅拌的同时加入NaOH溶液调节混合物二的pH值为碱性;
步骤四:将步骤三中化学镀镍完成的混合物二静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于70-80℃下烘干得到镀镍碳化硅颗粒。
从图3A和3B的SEM结果看出,相比较活化后的碳化硅颗粒表面(图2所示),化学镀镍完成后的碳化硅颗粒表面基本实现了镍颗粒的全面包覆,从图4的EDS能谱结果看出,镍的质量比及原子比与活化后的碳化硅颗粒表面附着的镍相比均较高,说明经过上述步骤,镍已经完全包覆碳化硅。
为了进一步证明,如图5所示,将步骤四得到的镀镍碳化硅颗粒的XRD谱图与退火处理之后的镀镍碳化硅颗粒的XRD谱图进行比较,可以看出,镀镍碳化硅颗粒的XRD谱图有明显的镍元素的峰,而且经过退火处理的镀镍碳化硅颗粒表面包覆的镍晶粒由小变大,且有NiO生成。
实施例1
本发明的镀镍碳化硅颗粒的制备方法,包括以下步骤:
步骤一:活化碳化硅颗粒:将40g碳化硅颗粒(平均粒径为5μm)加入12g乙酸镍、硼氢化钠4g和1L乙醇配置成的醇溶液中,滴加适量10%NaOH溶液作为稳定剂,之后常温搅拌30min,搅拌速度为400r/min,形成混合物一;
步骤二:将步骤一中活化完成的混合物一静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于80℃下烘干;
步骤三,化学镀镍:按照表2所示的反应配方和反应条件,将26g六水硫酸镍(主盐)、20g一水次亚磷酸钠(还原剂)、44g柠檬酸(络合剂)和66g硫酸铵(缓冲剂)加入烧杯中,并加入蒸馏水直至固体物质全部溶解,形成镀液;
将步骤二中5g烘干的活化碳化硅颗粒和痕量稳定剂硫脲加入上述镀液中形成混合物二,将混合物二水浴加热并搅拌(加热温度为40℃,搅拌速度为400r/min),并在加热搅拌的同时加入NaOH溶液调节混合物二的pH值为9;
步骤四:将步骤三中化学镀镍完成的混合物二静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于80℃下烘干得到镀镍碳化硅颗粒。
实施例2
本发明的镀镍碳化硅颗粒的制备方法,包括以下步骤:
步骤一:活化碳化硅颗粒:将20g碳化硅颗粒(平均粒径为5μm)加入6g乙酸镍、硼氢化钠2g和500mL乙醇配置成的醇溶液中,滴加适量10%NaOH溶液作为稳定剂,之后常温搅拌30min,搅拌速度为400r/min,形成混合物一;
步骤二:将步骤一中活化完成的混合物一静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于70℃下烘干;
步骤三,化学镀镍:按照表2所示的反应配方和反应条件,将13g六水硫酸镍(主盐)、10g一水次亚磷酸钠(还原剂)、22g柠檬酸(络合剂)和33g硫酸铵(缓冲剂)加入烧杯中,并加入蒸馏水直至固体物质全部溶解,形成镀液;
将步骤二中2.5g烘干的活化碳化硅颗粒和痕量稳定剂硫脲加入上述镀液中形成混合物二,将混合物二水浴加热并搅拌(加热温度为40℃,搅拌速度为400r/min),并在加热搅拌的同时加入NaOH溶液调节混合物二 的pH值为9;
步骤四:将步骤三中化学镀镍完成的混合物二静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并于70℃下烘干得到镀镍碳化硅颗粒。
本发明选取一定粒径(平均粒径R=5μm)的碳化硅颗粒,通过清洗-活化处理-特定溶液镀镍的方法,将碳化硅颗粒表面进行涂层、镀镍,使碳化硅颗粒表面均匀附着镍,从而提高碳化硅与金属材料的均匀融合程度,避免出现复合材料的偏析与龟裂问题,提高复合材料的成材率。
以上所述仅为本发明的较佳实施例,并非用来限定本发明的实施范围;如果不脱离本发明的精神和范围,对本发明进行修改或者等同替换,均应涵盖在本发明权利要求的保护范围当中。

Claims (10)

  1. 一种镀镍碳化硅颗粒的制备方法,其特征在于,包括以下步骤:
    步骤一,活化碳化硅颗粒:将碳化硅颗粒加入乙酸镍和硼氢化钠的醇溶液中,滴加稳定剂NaOH溶液后进行搅拌,形成混合物一;
    步骤二:将步骤一中活化完成的混合物一静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并烘干;
    步骤三,化学镀镍:将步骤二中烘干的活化碳化硅颗粒和稳定剂硫脲加入主盐六水硫酸镍、还原剂一水次亚磷酸钠、络合剂柠檬酸和缓冲剂硫酸铵的混合溶液中形成混合物二,将混合物二水浴加热并搅拌,并在加热搅拌的同时加入NaOH溶液调节混合物二的pH值为碱性;
    步骤四:将步骤三中化学镀镍完成的混合物二静置沉淀,过滤后用蒸馏水洗涤沉淀,洗涤完成后过滤并烘干得到镀镍碳化硅颗粒。
  2. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤一中使用的碳化硅颗粒平均粒径为5μm。
  3. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤一中乙酸镍和硼氢化钠的质量比为乙酸镍∶硼氢化钠=3∶1。
  4. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤一中碳化硅、乙酸镍和硼氢化钠的质量比为碳化硅∶乙酸镍∶硼氢化钠=10∶3∶1。
  5. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤一中搅拌时间为30min,搅拌速度为400r/min。
  6. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤三中六水硫酸镍、一水次亚磷酸钠、柠檬酸、硫酸铵的质量比为六水硫酸镍∶一水次亚磷酸钠∶柠檬酸∶硫酸铵=13∶10∶22∶33。
  7. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤三中混合物二的pH值为9。
  8. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤三中水浴加热温度为40℃,搅拌速度为400r/min。
  9. 根据权利要求1所述的镀镍碳化硅颗粒的制备方法,其特征在于,所述步骤二和所述步骤四中的所述烘干在70-80℃的温度下进行。
  10. 一种镀镍碳化硅颗粒,其特征在于,通过权利要求1~9的任一项所述的制备方法制备而成。
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