CN106756903A - A kind of Nickel-plated carbon silicon grain and preparation method thereof - Google Patents
A kind of Nickel-plated carbon silicon grain and preparation method thereof Download PDFInfo
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- CN106756903A CN106756903A CN201611149319.6A CN201611149319A CN106756903A CN 106756903 A CN106756903 A CN 106756903A CN 201611149319 A CN201611149319 A CN 201611149319A CN 106756903 A CN106756903 A CN 106756903A
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- nickel
- plated carbon
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- carbon silicon
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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
- C23C18/00—Chemical 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
- C23C18/16—Chemical 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
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- 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
- C23C18/00—Chemical 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
- C23C18/16—Chemical 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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- 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
- C23C18/00—Chemical 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
- C23C18/16—Chemical 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1882—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
Abstract
The present invention relates to a kind of preparation method of Nickel-plated carbon silicon grain, it is comprised the following steps：Step one：Activation silicon-carbide particle；Step 2：Wash, filter and dry；Step 3：Chemical nickel plating；Step 4：Wash, filter and dry.The present invention chooses the silicon-carbide particle of certain particle diameter, method by cleaning activation process particular solution nickel plating, silicon-carbide particle surface is carried out into coating, nickel plating, silicon-carbide particle surface is set uniformly to adhere to nickel, so as to improve the uniform fusion degree of carborundum and metal material, segregation and the cracking problem of composite are avoided the occurrence of, the lumber recovery of composite is improved.
Description
Technical field
The present invention relates to a kind of preparation method of Nickel-plated carbon silicon grain, particularly a kind of composite nickel-plated carbon SiClx
The preparation method of particle, the invention further relates to using the Nickel-plated carbon silicon grain prepared by the method.
Background technology
It is excellent that carborundum has that purity is high, particle diameter is small, is evenly distributed, specific surface area is big, high surface, apparent density are low
Point, and carborundum also has fabulous mechanics, calorifics, electricity and chemical property, i.e., with high rigidity, high-wearing feature and good
Self-lubricating, high thermoconductivity, low thermal coefficient of expansion and the features such as big elevated temperature strength, this causes that silicon carbide ceramics has been obtained extensively
Application.
When being used due to, containing the graphite particle that substantial amounts of disperse is tiny, being matched with other materials in silicon carbide substrate,
Its coefficient of friction is very small, with good self-lubricating property, is particularly well-suited to make hermetic seal or has the close of dry friction operating mode
Used in sealing, so that the service life of seal and the reliability of work are improved.But, silicon-carbide particle due to density compared with
Small (3.2g/cm3), it is difficult in the disperse of metal material inner homogeneous.
The content of the invention
Regarding to the issue above, it is an object of the invention to provide a kind of preparation method of Nickel-plated carbon silicon grain, and use
Nickel-plated carbon silicon grain prepared by the method.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
According to the present invention, there is provided a kind of preparation method of Nickel-plated carbon silicon grain, comprise the following steps：
Step one, activates silicon-carbide particle：By in the alcoholic solution of silicon-carbide particle addition nickel acetate and sodium borohydride, it is added dropwise
It is stirred after stabilizer NaOH solution, forms mixture one；
Step 2：The mixture one that completion will be activated in step one is staticly settled, and is precipitated with distillation water washing after filtering, is washed
Filtered after the completion of washing and dried；
Step 3, chemical nickel plating：The activation silicon-carbide particle and stabilizer thiocarbamide that will be dried in step 2 add main salt six
Mixing is formed in the mixed solution of water nickel sulfate, the waterside sodium phosphite of reducing agent one, complexing agent citric acid and buffer ammonium sulfate
Thing two, by the heating water bath of mixture two and stirs, and adds NaOH solution to adjust the pH of mixture two while heating stirring
It is alkalescence to be worth；
Step 4：The mixture two that chemical nickel plating in step 3 is completed is staticly settled, is sunk with distillation water washing after filtering
Form sediment, filtered after the completion of washing and dried and obtain Nickel-plated carbon silicon grain.
Further, the silicon-carbide particle average grain diameter for being used in the step one is 5 μm.
Further, the mass ratio of nickel acetate and sodium borohydride is nickel acetate: sodium borohydride=3: 1 in the step one.
Further, the mass ratio of carborundum, nickel acetate and sodium borohydride is carborundum: nickel acetate in the step one:
Sodium borohydride=10: 3: 1.
Further, mixing time is 30min in the step one, and mixing speed is 400r/min.
Further, nickel sulfate hexahydrate, a waterside sodium phosphite, citric acid, the mass ratio of ammonium sulfate in the step 3
It is nickel sulfate hexahydrate: a waterside sodium phosphite: citric acid: ammonium sulfate=13: 10: 22: 33.
Further, the pH value of mixture two is 9 in the step 3.
Further, water bath heating temperature is 40 DEG C in the step 3, and mixing speed is 400r/min.
Further, the drying in the step 2 and the step 4 is carried out at a temperature of 70-80 DEG C.
According to the present invention, there is provided a kind of Nickel-plated carbon silicon grain, it is prepared from by preparation method as described above.
The present invention chooses the silicon-carbide particle of certain particle diameter (R=5 μm of average grain diameter), by cleaning-activation process-specific
The method of solution nickel plating, coating, nickel plating are carried out by silicon-carbide particle surface, silicon-carbide particle surface is uniformly adhered to nickel, so that
Improve the uniform fusion degree of carborundum and metal material, it is to avoid the segregation of composite and cracking problem occur, improve compound
The lumber recovery of material.
Brief description of the drawings
Fig. 1 and Fig. 2 are SEM (SEM) photos of the silicon-carbide particle after activating in step one of the present invention；
Fig. 3 A and 3B are SEM (SEM) photo of the Nickel-plated carbon silicon grain prepared by the present invention；
Fig. 4 is the EDS energy spectrum diagrams of the Nickel-plated carbon silicon grain prepared by the present invention；
Fig. 5 is the Nickel-plated carbon silicon grain after Nickel-plated carbon silicon grain and continuation annealing after alkaline chemical nickel-plating
XRD spectrum comparison diagram.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings and embodiment, it is right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain the present invention, not
For limiting the present invention.
The preparation method of Nickel-plated carbon silicon grain of the invention, comprises the following steps：
Step one：Activation silicon-carbide particle：According to reaction formula and reaction condition shown in table 1, by quantitative carborundum
Particle (average grain diameter is 5 μm) is added in the alcoholic solution of nickel acetate and sodium borohydride, and appropriate 10%NaOH solution is added dropwise as steady
Determine agent, afterwards stirring at normal temperature 30min, mixing speed is 400r/min, form mixture one；
Table 1
Step 2：The mixture one that completion will be activated in step one is staticly settled, and is precipitated with distillation water washing after filtering, is washed
Filtered after the completion of washing and in drying at 70-80 DEG C；It is as illustrated in fig. 1 and 2 the silicon-carbide particle after activation, the silicon-carbide particle table
Face is attached with a small amount of particle, and the result measured from EDS power spectrums (Fig. 1) can be seen that silicon-carbide particle surface attachment and have
Nickel, therefore it may be concluded that by above-mentioned steps one and two, silicon-carbide particle surface attachment has nickel.
Step 3, chemical nickel plating：It is according to reaction formula and reaction condition shown in table 2, quantitative nickel sulfate hexahydrate is (main
Salt), during a waterside sodium phosphite (reducing agent), citric acid (complexing agent) and ammonium sulfate (buffer) adds beaker, and add steaming
Distilled water is until solid matter all dissolvings, form plating solution；
Table 2
The activation silicon-carbide particle and trace stabilizer thiocarbamide that will be dried in step 2 form mixing in adding above-mentioned plating solution
Thing two, by the heating water bath of mixture two and stirs (heating-up temperature be 40 DEG C, mixing speed is 400r/min), and in heating stirring
While add NaOH solution regulation mixture two pH value for alkalescence；
Step 4：The mixture two that chemical nickel plating in step 3 is completed is staticly settled, is sunk with distillation water washing after filtering
Form sediment, filtered after the completion of washing and obtain Nickel-plated carbon silicon grain in drying at 70-80 DEG C.
Find out from the SEM results of Fig. 3 A and 3B, the silicon-carbide particle surface (shown in Fig. 2) after the activation that compares, chemical plating
Silicon-carbide particle surface after the completion of nickel realizes comprehensive cladding of nickel particle substantially, finds out from the EDS power spectrum results of Fig. 4, nickel
Quality when atomic ratio is higher compared with the nickel of the silicon-carbide particle surface attachment after activation, illustrate by above-mentioned steps,
Nickel coats carborundum completely.
In order to further prove, as shown in figure 5, the XRD spectra of the Nickel-plated carbon silicon grain that step 4 is obtained and annealing
The XRD spectra of the Nickel-plated carbon silicon grain after treatment is compared, it can be seen that the XRD spectra of Nickel-plated carbon silicon grain has
The peak of obvious nickel element, and change from small to big by the surface coated nickel crystallite of Nickel-plated carbon silicon grain for making annealing treatment, and
There is NiO to generate.
Embodiment 1
The preparation method of Nickel-plated carbon silicon grain of the invention, comprises the following steps：
Step one：Activation silicon-carbide particle：40g silicon-carbide particles (average grain diameter is 5 μm) are added into 12g nickel acetates, boron
In the alcoholic solution that sodium hydride 4g and 1L ethanol is configured to, appropriate 10%NaOH solution is added dropwise as stabilizer, afterwards stirring at normal temperature
30min, mixing speed is 400r/min, forms mixture one；
Step 2：The mixture one that completion will be activated in step one is staticly settled, and is precipitated with distillation water washing after filtering, is washed
Filtered after the completion of washing and in drying at 80 DEG C；
Step 3, chemical nickel plating：It is according to reaction formula and reaction condition shown in table 2,26g nickel sulfate hexahydrates is (main
Salt), during the waterside sodium phosphites (reducing agent) of 20g mono-, 44g citric acids (complexing agent) and 66g ammonium sulfate (buffer) adds beaker,
And distilled water is added until solid matter all dissolvings, form plating solution；
Form mixed during the activation silicon-carbide particle and trace stabilizer thiocarbamide of 5g drying in step 2 are added into above-mentioned plating solution
Compound two, by the heating water bath of mixture two and stirs (heating-up temperature be 40 DEG C, mixing speed is 400r/min), and is stirred in heating
The pH value that NaOH solution regulation mixture two is added while mixing is 9；
Step 4：The mixture two that chemical nickel plating in step 3 is completed is staticly settled, is sunk with distillation water washing after filtering
Form sediment, filtered after the completion of washing and obtain Nickel-plated carbon silicon grain in drying at 80 DEG C.
Embodiment 2
The preparation method of Nickel-plated carbon silicon grain of the invention, comprises the following steps：
Step one：Activation silicon-carbide particle：20g silicon-carbide particles (average grain diameter is 5 μm) are added into 6g nickel acetates, boron hydrogen
In changing the alcoholic solution that is configured to of sodium 2g and 500mL ethanol, appropriate 10%NaOH solution is added dropwise as stabilizer, afterwards stirring at normal temperature
30min, mixing speed is 400r/min, forms mixture one；
Step 2：The mixture one that completion will be activated in step one is staticly settled, and is precipitated with distillation water washing after filtering, is washed
Filtered after the completion of washing and in drying at 70 DEG C；
Step 3, chemical nickel plating：It is according to reaction formula and reaction condition shown in table 2,13g nickel sulfate hexahydrates is (main
Salt), during the waterside sodium phosphites (reducing agent) of 10g mono-, 22g citric acids (complexing agent) and 33g ammonium sulfate (buffer) adds beaker,
And distilled water is added until solid matter all dissolvings, form plating solution；
Formed during the activation silicon-carbide particle and trace stabilizer thiocarbamide of 2.5g drying in step 2 are added into above-mentioned plating solution
Mixture two, by the heating water bath of mixture two and stirs (heating-up temperature be 40 DEG C, mixing speed is 400r/min), and in heating
The pH value that NaOH solution regulation mixture two is added while stirring is 9；
Step 4：The mixture two that chemical nickel plating in step 3 is completed is staticly settled, is sunk with distillation water washing after filtering
Form sediment, filtered after the completion of washing and obtain Nickel-plated carbon silicon grain in drying at 70 DEG C.
The present invention chooses the silicon-carbide particle of certain particle diameter (R=5 μm of average grain diameter), by cleaning-activation process-specific
The method of solution nickel plating, coating, nickel plating are carried out by silicon-carbide particle surface, silicon-carbide particle surface is uniformly adhered to nickel, so that
Improve the uniform fusion degree of carborundum and metal material, it is to avoid the segregation of composite and cracking problem occur, improve compound
The lumber recovery of material.
Presently preferred embodiments of the present invention is the foregoing is only, not for limiting practical range of the invention；If do not taken off
From the spirit and scope of the present invention, the present invention is modified or equivalent, all should covered in the claims in the present invention
In the middle of protection domain.
Claims (10)
1. a kind of preparation method of Nickel-plated carbon silicon grain, it is characterised in that comprise the following steps：
Step one, activates silicon-carbide particle：By in the alcoholic solution of silicon-carbide particle addition nickel acetate and sodium borohydride, stabilization is added dropwise
It is stirred after agent NaOH solution, forms mixture one；
Step 2：The mixture one that completion will be activated in step one is staticly settled, and is precipitated with distillation water washing after filtering, has been washed
Into rear filtering and dry；
Step 3, chemical nickel plating：The activation silicon-carbide particle and stabilizer thiocarbamide that will be dried in step 2 add the main water sulphur of salt six
Mixture two is formed in the mixed solution of sour nickel, the waterside sodium phosphite of reducing agent one, complexing agent citric acid and buffer ammonium sulfate,
By the heating water bath of mixture two and stir, and it is alkali that the pH value of NaOH solution regulation mixture two is added while heating stirring
Property；
Step 4：The mixture two that chemical nickel plating in step 3 is completed is staticly settled, is precipitated with distillation water washing after filtering, washed
Filtered after the completion of washing and dried and obtain Nickel-plated carbon silicon grain.
2. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that used in the step one
Silicon-carbide particle average grain diameter be 5 μm.
3. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that acetic acid in the step one
The mass ratio of nickel and sodium borohydride is nickel acetate: sodium borohydride=3: 1.
4. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that be carbonized in the step one
The mass ratio of silicon, nickel acetate and sodium borohydride is carborundum: nickel acetate: sodium borohydride=10: 3: 1.
5. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that stirred in the step one
Time is 30min, and mixing speed is 400r/min.
6. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that six water in the step 3
Nickel sulfate, a waterside sodium phosphite, citric acid, the mass ratio of ammonium sulfate are nickel sulfate hexahydrate：One waterside sodium phosphite: citric acid
: ammonium sulfate=13: 10: 22: 33.
7. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that mix in the step 3
The pH value of thing two is 9.
8. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that water-bath in the step 3
Heating-up temperature is 40 DEG C, and mixing speed is 400r/min.
9. the preparation method of Nickel-plated carbon silicon grain according to claim 1, it is characterised in that the step 2 and described
The drying in step 4 is carried out at a temperature of 70-80 DEG C.
10. a kind of Nickel-plated carbon silicon grain, it is characterised in that by the preparation method system described in any one of claim 1~9
It is standby to form.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611149319.6A CN106756903A (en) | 2016-12-14 | 2016-12-14 | A kind of Nickel-plated carbon silicon grain and preparation method thereof |
| PCT/CN2017/102828 WO2018107846A1 (en) | 2016-12-14 | 2017-09-22 | Nickel-plated silicon carbide particles and preparation method therefor |
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| CN201611149319.6A CN106756903A (en) | 2016-12-14 | 2016-12-14 | A kind of Nickel-plated carbon silicon grain and preparation method thereof |
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| WO (1) | WO2018107846A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018107846A1 (en) * | 2016-12-14 | 2018-06-21 | 苏州金仓合金新材料有限公司 | Nickel-plated silicon carbide particles and preparation method therefor |
| US20190264330A1 (en) * | 2018-02-24 | 2019-08-29 | Tangshan Normal University | Method of electroless nickle plating on surface of silicon carbide powder |
| CN114433846A (en) * | 2021-12-22 | 2022-05-06 | 南京泉峰汽车精密技术股份有限公司 | Fin-type heat dissipation plate and forming process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201614008D0 (en) * | 2016-08-16 | 2016-09-28 | Seram Coatings As | Thermal spraying of ceramic materials |
| CN112695353A (en) * | 2020-12-11 | 2021-04-23 | 四川渝邻汽车零部件有限公司 | Preparation method of aluminum cylinder body composite electroplating |
| 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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| CN106756903A (en) * | 2016-12-14 | 2017-05-31 | 苏州金仓合金新材料有限公司 | A kind of Nickel-plated carbon silicon grain and preparation method thereof |
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- 2017-09-22 WO PCT/CN2017/102828 patent/WO2018107846A1/en active Application Filing
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| CN103451634A (en) * | 2013-07-29 | 2013-12-18 | 洛阳德欣石化科技有限公司 | Method for chemical nickel plating on surface of micron silicon carbide powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018107846A1 (en) * | 2016-12-14 | 2018-06-21 | 苏州金仓合金新材料有限公司 | Nickel-plated silicon carbide particles and preparation method therefor |
| 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 |
| CN114433846A (en) * | 2021-12-22 | 2022-05-06 | 南京泉峰汽车精密技术股份有限公司 | Fin-type heat dissipation plate and forming process thereof |
| CN114433846B (en) * | 2021-12-22 | 2024-03-29 | 南京泉峰汽车精密技术股份有限公司 | Fin-column type heat radiation plate and forming process thereof |
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| Publication number | Publication date |
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| WO2018107846A1 (en) | 2018-06-21 |
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