CN1730440A - Process method for full coating of micron and nanometer (SiC) p surfaces - Google Patents
Process method for full coating of micron and nanometer (SiC) p surfaces Download PDFInfo
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- 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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- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000008569 process Effects 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 14
- 239000011248 coating agent Substances 0.000 title claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000004913 activation Effects 0.000 claims abstract description 6
- 238000009776 industrial production Methods 0.000 claims abstract 2
- 230000003647 oxidation Effects 0.000 claims abstract 2
- 238000007254 oxidation reaction Methods 0.000 claims abstract 2
- 239000002699 waste material Substances 0.000 claims abstract 2
- 206010070834 Sensitisation Diseases 0.000 claims description 5
- 230000008313 sensitization Effects 0.000 claims description 5
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- 238000007772 electroless plating Methods 0.000 claims description 4
- 238000007747 plating Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000001235 sensitizing effect Effects 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000002203 pretreatment Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 229910018104 Ni-P Inorganic materials 0.000 description 1
- 229910018536 Ni—P Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000012669 liquid formulation Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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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
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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510010144 CN1730440A (en) | 2005-07-01 | 2005-07-01 | Process method for full coating of micron and nanometer (SiC) p surfaces |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510010144 CN1730440A (en) | 2005-07-01 | 2005-07-01 | Process method for full coating of micron and nanometer (SiC) p surfaces |
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| Publication Number | Publication Date |
|---|---|
| CN1730440A true CN1730440A (en) | 2006-02-08 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510010144 Pending CN1730440A (en) | 2005-07-01 | 2005-07-01 | Process method for full coating of micron and nanometer (SiC) p surfaces |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906625A (en) * | 2010-08-16 | 2010-12-08 | 宿辉 | Method for Reinforcing Nickel-Phosphorus Composite Coating by 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 strengthening 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 | A magnetic metal@SiC wave-absorbing powder and its preparation method |
-
2005
- 2005-07-01 CN CN 200510010144 patent/CN1730440A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906625B (en) * | 2010-08-16 | 2012-05-23 | 宿辉 | Method for Reinforcing Nickel-Phosphorus Composite Coating by Modified Nano-Silicon Dioxide Particles |
| CN101906625A (en) * | 2010-08-16 | 2010-12-08 | 宿辉 | Method for Reinforcing Nickel-Phosphorus Composite Coating by 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 strengthening 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 | A magnetic metal@SiC wave-absorbing powder and its preparation method |
| 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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