CN1730440A - Micrometer, nanometer (SiC)P surface entirely-cladding technology - Google Patents

Micrometer, nanometer (SiC)P surface entirely-cladding technology Download PDF

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Publication number
CN1730440A
CN1730440A CN 200510010144 CN200510010144A CN1730440A CN 1730440 A CN1730440 A CN 1730440A CN 200510010144 CN200510010144 CN 200510010144 CN 200510010144 A CN200510010144 A CN 200510010144A CN 1730440 A CN1730440 A CN 1730440A
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sic
nanometer
coats
treatment
micron
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宿辉
曹茂盛
王正平
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Harbin Engineering University
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Harbin Engineering University
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Abstract

The invention discloses a process for realizing micron and nano (SiC)P surface total coating under normal atmosphere and low temperature, wherein (SiC)P waste in industrial production is used as raw material, and a simple chemical plating method is employed for low cost (SiC)P surface coating and modifying. In order to achieve good coating effect, (SiC)P is subject to a pretreatment procedure which comprises oxidation treatment, hydrophilic treatment, sensitizing treatment and activation processing.

Description

Micron, nanometer (SiC) PThe full processing method that coats in surface
Technical field
The present invention is a kind of realization micron, nanometer (SiC) PThe full processing method that coats in surface belongs to stupalith modification field.
Background technology
Synthesize the another research focus that the material with higher hardness and wear resistance is current material field with low-cost raw material.(SiC) PHaving hardness height, advantage such as wear-resisting, high temperature resistant, be widely used as reinforced particulate and prepare metal-base composites, also is the basic raw material of preparation engineering material, functional materials simultaneously.But (SiC) PWhen directly using, also exist some critical technical problems to need to solve, for example: as (SiC) PWhen strengthening metal-base composites, (SiC) PCovalent linkage and the essential distinction between the metallic bond of metallic matrix, make the interface wet ability can be very poor; (SiC) PWhen contacting with metallic matrix, significant solid phase interface reaction can take place under the high temperature, change the microstructure and the performance of metallic matrix, make its hardness and wear resistance reduction etc.For performance (SiC) more fully PExcellent properties, need carry out the surface to it and be coated with modification.
At present, micron, nanometer (SiC) PSurface coated method has following several: 1. electrodip process, with electrochemical method at (SiC) PSurface deposition goes out the process of skim metal or alloy, gained compound (SiC) PTack is good, but can be because of contraction cracks when dry, and it is prefabricated to relate to electrode, and the frock investment is relatively large.2. sol-gel method is utilized diffluent metallic compound, reacts with water in certain solvent, and through hydrolysis and polycondensation gelation gradually, the drying sintering is to realize micron and nanometer (SiC) again PFinishing.Product purity height, good uniformity, but in conjunction with not firm, easily peel off and organic raw material cost height.3. electroless plating method is modified micron, nanometer (SiC) with this method P, the process controllability is strong, becomes originally with technology from process unit, very likely takes the lead in being generalized to micron, nanometer (SiC) PAmong the production of mass-producing finishing, coat (SiC) with this method P, Chinese scholars research is more.
But from the resulting test result analysis of present employing chemical plating method, technical elements await further perfect, improve.As employed technology or need microwave wet the very high nanometer of etching, high pressure, hot conditions and rule, purity, micron (SiC) POr modification effect is inhomogeneous, continuous, and quality product is not good.So reduce to the requirement of processing condition and raw material, a striving direction of ensuring the quality of products and to be following technological development.
The article " Simple and fast ion sediment microwave-enhanced wetetching of SiC particles for electroless Ni-P plating " that the people such as Min Kang that delivered in 2002 as " Surface and Coatings Technology " magazine write.
Summary of the invention
The purpose of this invention is to provide a kind of easy and simple to handle, low, (SiC) that the products obtained therefrom quality is high to processing condition and ingredient requirement PThe full technological method that coats in surface.
We propose the mentality of designing of normal pressure, low temperature, accelerated surface modification on experiment that has accumulated and theoretical empirical basis, select for use and produce 1200 #In the process of silicon single crystal, pulverize the industrial waste (SiC) that produces by Raymond machine and supersonic airstream PBe raw material, adopt electroless plating technology, (SiC) PCarry out finishing cheaply, it is continuous to obtain coating, no smooth (SiC) PExposed high-quality modification (SiC) P[be abbreviated as (Ni/SiC) p].Test results such as SEM, EDS, XRD, TEM show: (Ni/SiC) after the modification P(SiC) before modifying PElectroconductibility obviously improves, and pattern, composition, structure change.
For achieving the above object, the technical solution used in the present invention is:
In order to reach covered effect preferably, (SiC) PMust carry out pre-treatment, this process comprises: utilize the oxide treatment of carrying out in the resistance furnace; The wetting ability of carrying out in HF, HCl solution is handled; SnCl 2, the sensitization carried out in the HCl solution handles and PdCl 2, the activation treatment of carrying out in the HCl solution.
Take by weighing (SiC) after the pre-treatment of certain mass P, under normal pressure (1 standard atmospheric pressure), low temperature (35-45 ℃) condition, join in the nickel-phosphorus chemistry plating bath that has prepared, after ultrasonic dispersing number, the mechanical stirring, filter this plating bath, till being washed till filtrate and being neutrality with distilled water.Plating time is about 2.0h, and pH is 8.5-9.5.
In the coating process, can also reach controlled to covered effect, improve the repeatability and the controllability of technology, and intend to large-scale development by regulating electroplate liquid formulation, processing parameter, pre-treatment condition etc.Realize making low cost, industrial scaleization.(SiC) after the surface coats PReduced intergranular absorption, reunion, improved (SiC) PWith the wettability at metallic matrix interface, reduced the solid phase interface reaction has taken place under the high temperature, change the microstructure of metallic matrix and the possibility of performance, for the low-cost matrix material of research preparation provides a kind of new method.
Description of drawings
Fig. 1 is (SiC) before coating PX-ray diffraction pattern
Fig. 2 is for coating back (SiC) PX-ray diffraction pattern
Embodiment
Provide the specific embodiment of the present invention below.
Embodiment 1
With micron order naked (SiC) PPut into resistance furnace, under the situation of unprotect gas, be heated to 1100 ℃, be incubated about 1 hour after, get and carry out wetting ability in the HF that handles back sample 2g and join 100ml, the HCl solution and handle.Again with (SiC) after the hydrophilic treatment PThe SnCl that adds 100ml respectively 2, HCl and PdCl 2, HCl is to carrying out sensitization and activation treatment.
Get (SiC) after the pre-treatment of 2g P, join in the chemical plating fluid that 100ml prepared, detect the pH value of solution, after the conformance with standard, the about 10min of ultrasonic dispersing again, the about 40min of mechanical stirring.At last, filter this plating bath, till being washed till filtrate and becoming neutrality with distilled water.Plating temperature is controlled at 35-45 ℃.
Embodiment 2
With nano level naked (SiC) PPut into resistance furnace, under the situation of unprotect gas, be heated to 1000 ℃, be incubated about 1 hour after, get and carry out wetting ability in the HF that handles back sample 2g and join 100ml, the HCl solution and handle.Again with (SiC) after the hydrophilic treatment PThe SnCl that adds 100ml respectively 2, HCl and PdCl 2, HCl is to carrying out sensitization and activation treatment.
Get (SiC) after the pre-treatment of 2g P, ultra-sonic dispersion 10min joins in the chemical plating fluid that 100ml prepared, detects the pH value of solution, after the conformance with standard, and the about 20min of ultrasonic dispersing again, the about 30min of mechanical stirring.At last, filter this plating bath, till being washed till filtrate and becoming neutrality with distilled water.Plating temperature is controlled at 35-45 ℃.
Former powder before coating is (SiC) PA series of crystal, only contain the characteristic peak of Si in the x-ray diffraction pattern (XRD), the content of Ni is zero (see figure 1); (SiC) after the coating PThe surface has plated more metallic nickel, has occurred more characteristic peak (see figure 2) among the XRD.By Fig. 1,2 as seen, the electroconductibility after the coating obviously improves, and this result also can pass through the specific conductivity testing authentication; Scanning electronic microscope (SEM) test can be observed, and depositing after the coating be intensive, coating layer uniformly.

Claims (6)

1. a micron, nanometer (SiC) PThe full processing method that coats in surface is characterized in that: under normal pressure and lower temperature, utilize conventional chemical plating method, realized (SiC) PThe full coating on surface, (SiC) PPre-treatment must be carried out to it before coating in the surface, and this process comprises: oxide treatment, wetting ability processing, sensitization processing, activation treatment.
2. micron according to claim 1, nanometer (SiC) PThe full processing method that coats in surface is characterized in that: wetting ability is handled and is carried out in HF, HCl solution.
3. micron according to claim 1, nanometer (SiC) PThe full processing method that coats in surface, it is characterized in that: it is at SnCl that sensitization is handled 2, carry out in the HCl solution.
4. micron according to claim 1, nanometer (SiC) PThe full processing method that coats in surface, it is characterized in that: activation treatment is at PdCl 2, carry out in the HCl solution.
5. micron according to claim 1, nanometer (SiC) PThe full processing method that coats in surface, it is characterized in that: the processing parameter of its electroless plating is: temperature is controlled at 35-45 ℃, and pH is 8.5-9.5.
6. micron according to claim 1, nanometer (SiC) PThe full processing method that coats in surface is characterized in that: the raw material that is adopted (SiC) PBe the processing waste in the industry.
CN 200510010144 2005-07-01 2005-07-01 Micrometer, nanometer (SiC)P surface entirely-cladding technology Pending CN1730440A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101906625A (en) * 2010-08-16 2010-12-08 宿辉 Method for enhancing nickel-phosphorus composite deposit by using modified nano silicon dioxide particles
CN102400121A (en) * 2011-11-05 2012-04-04 上海上大瑞沪微系统集成技术有限公司 Preparation process of nano ceramic particles for reinforcing composite lead-free solder
CN102642025A (en) * 2012-04-26 2012-08-22 上海交通大学 Method for plating tungsten on surface of SiC particle
CN105195737A (en) * 2015-10-14 2015-12-30 东南大学 Method for covering surfaces of SiC particles with nickel
CN106946244A (en) * 2017-03-22 2017-07-14 西京学院 A kind of method that graphene and carbon nanotube mixture are prepared based on electroless copper SiC particulate
CN108118315A (en) * 2018-02-24 2018-06-05 唐山师范学院 A kind of method of the uniform and stable silicon carbide powder chemical nickel plating on surface of coating
CN115505910A (en) * 2022-10-25 2022-12-23 北京航空航天大学 Magnetic metal @ SiC wave-absorbing powder and preparation method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101906625B (en) * 2010-08-16 2012-05-23 宿辉 Method for enhancing nickel-phosphorus composite deposit by using modified nano silicon dioxide particles
CN101906625A (en) * 2010-08-16 2010-12-08 宿辉 Method for enhancing nickel-phosphorus composite deposit by using modified nano silicon dioxide particles
CN102400121A (en) * 2011-11-05 2012-04-04 上海上大瑞沪微系统集成技术有限公司 Preparation process of nano ceramic particles for reinforcing composite lead-free solder
CN102400121B (en) * 2011-11-05 2014-07-02 上海上大瑞沪微系统集成技术有限公司 Preparation process of nano ceramic particles for reinforcing composite lead-free solder
CN102642025A (en) * 2012-04-26 2012-08-22 上海交通大学 Method for plating tungsten on surface of SiC particle
CN105195737B (en) * 2015-10-14 2017-07-18 东南大学 A kind of method of SiC particulate surface cladded with nickel
CN105195737A (en) * 2015-10-14 2015-12-30 东南大学 Method for covering surfaces of SiC particles with nickel
CN106946244A (en) * 2017-03-22 2017-07-14 西京学院 A kind of method that graphene and carbon nanotube mixture are prepared based on electroless copper SiC particulate
CN108118315A (en) * 2018-02-24 2018-06-05 唐山师范学院 A kind of method of the uniform and stable silicon carbide powder chemical nickel plating on surface of coating
US20190264330A1 (en) * 2018-02-24 2019-08-29 Tangshan Normal University Method of electroless nickle plating on surface of silicon carbide powder
US10995408B2 (en) * 2018-02-24 2021-05-04 Tangshan Normal University Method of electroless nickle plating on surface of silicon carbide powder
CN115505910A (en) * 2022-10-25 2022-12-23 北京航空航天大学 Magnetic metal @ SiC wave-absorbing powder and preparation method thereof
CN115505910B (en) * 2022-10-25 2023-10-27 北京航空航天大学 Magnetic metal @ SiC wave-absorbing powder and preparation method thereof

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