CN106544653A - A kind of SiC powder surface chemical plating copper method - Google Patents
A kind of SiC powder surface chemical plating copper method Download PDFInfo
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- CN106544653A CN106544653A CN201710040802.9A CN201710040802A CN106544653A CN 106544653 A CN106544653 A CN 106544653A CN 201710040802 A CN201710040802 A CN 201710040802A CN 106544653 A CN106544653 A CN 106544653A
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- sic powder
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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
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
-
- 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
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention belongs to ceramic powders surface metalation field, and in particular to a kind of SiC powder surface chemical plating copper method, its processing step is：SiC powder is carried out cleaning, surface coarsening process, surface active sensitized treatment, the preparation of chemical plating fluid, electroless copper is implemented to SiC powder.The present invention with advantages below and salience effect：1st, technical scheme has the advantages that copper-plating technique is easy, coating speed is fast, uniform coating thickness and substrate are well combined, coating surface is highly polished, it is adaptable to SiC powder particle surface electroless copper, also can be in SiC ceramic block surface plating；2nd, electroplate liquid formulation used does not contain any poisonous and harmful substance, and the harmful substances such as gaseous state, liquid or solid-state are not discharged during plating yet；3rd, the plating copper thickness of technical solution of the present invention can be controlled as needed, and control method is simple.
Description
Technical field
The invention belongs to ceramic powders surface metalation field, and in particular to a kind of SiC powder surface chemical plating copper method.
Background technology
SiC particulate has the advantages that density is low, hardness is high, elastic modelling quantity is high, wear-resisting, corrosion-resistant, be in metal material often
With reinforcement, the SiC reinforcement metallic composite of various function admirables can be prepared.At some in particular cases, liquid gold
Category is not good enough to SiC particulate wettability；Or liquid metal can be reacted with SiC, harmful interface phase material is generated；Or base
Body is relatively low with the interface bond strength of SiC reinforcements；Or matrix is excessive with the coefficient of thermal expansion differences of SiC reinforcements, need to draw
Enter transition zone and alleviate interfacial stress.Above major part problem, generally can be by doing in SiC powder surface-coated layer of metal
Method, is addressed.
The method of ceramic surface metallization has a lot, such as chemical vapor deposition, physical vapour deposition (PVD), vacuum sputtering,
Chemical oxidization method, sol-gel process, galvanoplastic etc..Chemical oxidization method, sol-gel process are generally used for preparing ceramic coating, right
Formed metal coating layer for and do not apply to.Chemical vapor deposition, physical vapour deposition (PVD), vacuum sputtering, galvanoplastic, although energy
Metal coating is enough prepared, but the coating one by one of the ceramic particle to size micro/nano level cannot be realized.Only electroless plating method, can
By ceramic particle dispersion in the solution, the uniform metal coating of formation, and equipment needed thereby is few, production efficiency is high, is best suitable for pottery
The batch production of porcelain powder surface modifications.
The metal level applied in ceramic surface using electroless plating method, more with low-cost nickel, copper, cobalt and nickel-phosphor coating
Based on, coated ceramic matrix has ceramic bulk material, fiber, also has powder.Obviously, which kind of metal ceramic surface applies, and needs
Determined according to the species and specific use condition of ceramics.Specific in SiC particles reinforced metallic composite, SiC powder
One layer of copper of last surface-coated is than applying other metals, the advantage for more having technology simple and with low cost.
Report dedicated for SiC powder Electroless copper is also rare.Such as Chinese patent CN104561955A "
The metallization process of kind ceramic substrate chemical copper plating solution and ceramic substrate ", CN104561944A " a kind of glass, ceramic substrate
Electroless copper plating method ", a kind of CN103319208A " Al2O3Ceramic substrate metallization process ", a kind of CN104651815A " systems
Standby ZrB2Method of-Cu composite powders " etc., majority are to carry out electroless copper on ceramic block surface, remaining or be not related to powder
End, or it is inapplicable to SiC powder.
Chinese patent CN87100186 " method of adhesion metal deposition layer on the ceramic material " is proposed, in ceramic table
Before the metallization of face, needs first carry out roughening, drying and heating to ceramic.Chinese patent CN101486594 " ceramic whiskers
The method of surface chemical plating " proposition, ceramic whisker plating under the conditions of sonic oscillation.Chinese patent CN103334093A is " a kind of
The activating process of ceramic material electroless copper " proposes, surface-treated ceramic surface completes to activate by reduction reaction.
Document disclosed above is primarily present complex process, thickness of coating and the defect such as is difficult to control to.
The content of the invention
It is an object of the invention to provide a kind of process is simple, thickness of coating are uniform, thickness of coating is controllable, coating and substrate are tied
Close a kind of highly polished SiC powder surface chemical plating copper method of good, coating surface.
Technical scheme is as follows：A kind of SiC powder surface chemical plating copper method, its processing step is：
Step 1：SiC powder is cleaned：It is 0.1-100 microns by particle mean size, optimum grain-diameter is 0.6-4 microns
SiC powder enter in being put into acetone ultrasound carry out clean 5-60 minutes after, by SiC powder filter, be dried, then filter, cleaning, dry
It is dry；
Step 2：Surface coarsening process；Above-mentioned steps dried SiC particulate is put in the HF solution of 20ml/L, ultrasound
Vibration 5-25min, then filters, cleans, dries；
Step 3：Surface active sensitized treatment：The SiC powder after above-mentioned roughening treatment is put in sensitization activating solution, plus
Heat sensitization activating solution to after 20-40 DEG C ultrasonic 5-120 minutes, is then filtered, cleans, is dried；Above-mentioned sensitization activating solution is with dense
Spend the PdCl for 0.1-1g/L2, concentration for 5-30g/L SnCl2·2H2O, concentration for the NaCl and concentration of 20-150mL/L are
The hydrochloric acid HCl deionized waters configuration of 20-150mL/L is formed；The consumption of above-mentioned sensitization activating solution is to use per 100 grams of SiC powders
Sensitization activating solution 300-500 milliliters；
Step 4：The preparation of chemical plating fluid：Deionized water is by CuSO4·5H2It is molten that O is configured to the A that concentration is 10-30g/L
Liquid, then adjusts the PH of above-mentioned solution to 10-14 with NaOH solution, and optimal pH value is 13；
Sodium potassium tartrate tetrahydrate, HCHO and EDTA-Na are configured to mix B solution, wherein sodium potassium tartrate tetrahydrate by deionized water
Concentration is 20-60g/L for the concentration of 5-100mL/L, LEDTA-Na for the concentration of 5-40g/L, HCHO；
Above-mentioned solution A is slowly added in B solution under stirring, while adjusting mixed solution with NaOH solution
PH value be maintained at 10-14 after, clarified, without precipitation chemical plating fluid；
Step 5：Electroless copper is implemented to SiC powder：Will be the SiC powder after above-mentioned chemical plating fluid and activation sensitized treatment pre-
To 30-50 DEG C, then the SiC powder after preheating is added in chemical plating fluid under stirring carries out copper facing, thickness of coating to heat
Thicken speed for micro- m/h of 0.01-10.
Cleaning in above-mentioned steps is to adopt deionized water to clean pH to cleanout fluid for 7 or so.
Drying in above-mentioned steps is natural air drying or dries in an oven that temperature when drying in an oven is 80-120
DEG C, the time is 5-10 minutes.
During the above-mentioned enforcement electroless copper to SiC powder, the consumption of chemical plating fluid is to add per 100 grams of SiC powders
500-1000 milliliter chemical plating fluids.
The present invention with advantages below and salience effect：1st, technical scheme have copper-plating technique it is easy,
Coating speed is fast, uniform coating thickness and the advantages of substrate is well combined, coating surface is highly polished, it is adaptable to SiC powder
Grain Electroless copper, also can be in SiC ceramic block surface plating；2nd, electroplate liquid formulation used does not contain any poisonous and harmful substance,
The harmful substances such as gaseous state, liquid or solid-state are not discharged during plating yet；3rd, the plating copper thickness of technical solution of the present invention can basis
Needs are controlled, and control method is simple.
Description of the drawings
Accompanying drawing 1 is the XRD spectrum for not covering copper SiC powder；
Accompanying drawing 2 is the XRD spectrum for covering copper SiC powder；
Accompanying drawing 3 is the SEM photograph for not covering copper SiC powder pattern；
Accompanying drawing 4 is to cover the SEM photograph that copper SiC powder sends out last pattern；
Accompanying drawing 5 is the bond strength qualitative test of coating and SiC matrix.
Specific embodiment
By taking 100 grams of SiC powders as an example, the implementation process of the technical program is illustrated.
Embodiment 1：
A kind of new technology in SiC powder Electroless copper, comprises the following steps that：
Step 1：SiC powder is cleaned, its objective is to wash away the greasy dirt on SiC particulate surface, specific embodiment is：
The SiC powder that 100 grams of mean diameters are 4 microns is put into after being cleaned by ultrasonic 10 minutes in the acetone of 200mL, filters, cleaning, dry
It is dry；
Above-mentioned cleaning is that deionized water is cleaned repeatedly, till the PH of cleanout fluid is 7, its objective is to wash away SiC powder
Remaining acetone on end.
Above-mentioned drying is dried using baking oven, and drying temperature is dried to SiC powder moisture content and is less than at 80 DEG C or so
0.01% weight ratio.
Step 2：Surface coarsening process：SiC powder after above-mentioned steps are dried is put into the HF that 100mL concentration is 20ml/L
In aqueous solution, then sonic oscillation 5min filters, cleans, dries.
Step 3：Surface active sensitized treatment：By the SiC powder after the process of above-mentioned surface coarsening, it is put into 300mL sensitizations and lives
Change in liquid, heating sensitization activating solution is to after 20 DEG C, ultrasonic 120 minutes, then filtration, cleaning, drying；
Above-mentioned sensitization activating solution is by the PdCl that concentration is 0.1g/L2, concentration for 30g/L SnCl2·2H2O, concentration are
The NaCl and concentration of 100g/L is formed for the hydrochloric acid deionized water configuration of 20mL/L.
It is cleaning in above-mentioned steps 2,3, the condition of drying and step 1,2 identical.
Step 4：The preparation of chemical plating fluid；Deionized water is by CuSO4·5H2O is configured to the solution that concentration is 10g/L, so
Adjust the solution A of the pH to 13 of above-mentioned solution or so afterwards with NaOH solution；
The B solution that sodium potassium tartrate tetrahydrate, HCHO and EDTA-Na are configured to mix by deionized water, wherein sodium potassium tartrate tetrahydrate
Concentration for 5g/L, HCHO concentration for 100mL/L, LEDTA-Na concentration be 60g/L；
Above-mentioned solution A is slowly added in the B solution of mixing under stirring, while adjusted with NaOH solution mixing
After the pH value of solution is maintained at 10, clarified, without precipitation chemical plating fluid；
Step 5：Electroless copper is implemented to the SiC powder after above-mentioned process；30 DEG C will be preheated to after activation sensitized treatment
100 grams of SiC powders, during the above-mentioned chemical plating fluids of 500mL are added under stirring, according to the need of SiC powder overlay coating thickness
Will, it is determined that when chemical copper-plated time, such as thickness of coating require 0.1 microns, the time for implementing electroless copper is 12 minutes
Left and right.
The XRD things of SiC powder are mutually constituted as shown in Figure 1, are mutually mainly 6H phases SiC, containing a small amount of other multiform body phases；
Cover copper SiC powder XRD thing mutually to constitute as shown in Figure 2 after the completion of electroless copper, in addition to SiC phases, it was found that elemental copper is spread out
Peak is penetrated, illustrates that the powder after copper plating treatment is made up of SiC and elemental copper；The SEM photograph for not covering copper SiC powder granule-morphology is for example attached
Shown in Fig. 3, the SEM photograph of copper SiC powder granule-morphology is covered as shown in Figure 4, as can be seen from Figure, cover copper SiC powder table
Face is highly polished, uniform coating thickness, has Fig. 5 to can be seen that copper coating is well combined with SiC matrix.
Embodiment 2-6：
On the basis of embodiment 1, change SiC powder mean diameter, cleaning, drying time and sensitization activation liquor
Concentration, embodiment such as following table.
Cover copper SiC powder XRD thing mutually to constitute as shown in Figure 2 after the completion of electroless copper, in addition to SiC phases, it was found that single
The diffraction maximum of matter copper, illustrates that the powder after copper plating treatment is made up of SiC and elemental copper；The SEM for covering copper SiC powder granule-morphology shines
As shown in Figure 4, as can be seen from Figure, it is high to cover copper SiC powder surface smoothness, uniform coating thickness for piece, can be with by Fig. 5
Find out that copper coating is well combined with SiC matrix.
Embodiment 6-10：
On the basis of above-described embodiment, change and SiC powder is implemented in electroless copper step, chemical plating fluid and activation are quick
The proportion relation and its consumption of each material of SiC powder preheating temperature and chemical plating fluid after change process, embodiment such as following table.
Embodiment 11：
On the basis of embodiment 1, SiC raw materials are the full ceramic of compact block that a block size is 25mm × 25mm × 5mm, right
Which carries out Electroless copper.After polishing is ground to each face of SiC ceramic first, the HF solution that concentration is 20ml/L is put into
In, ceramic block is totally submerged in solution, sonic oscillation 10 minutes, then deionized water is clean by its surface washing, natural
After drying, place in 30 DEG C of sensitization activating solution, ultrasound 20 minutes or so, after taking-up, its surface washing is done by deionized water
Only, dry naturally, be then placed in the chemical plating fluid of 500mL, stir chemical plating fluid 30 minutes or so, so that it may in fine and close SiC
Ceramic block surface forms the electroless copper that thickness is 0.3 microns, and copper-plated coating speed is fast, uniform coating thickness and base
Bottom is well combined, coating surface is highly polished.
Electroplate liquid formulation used does not contain any poisonous and harmful substance in the above-described embodiments, and gas is not discharged during plating yet
State, liquid or solid-state harmful substance.According to GB GB/T5270-200X, bond strength of the coating with SiC ceramic matrix is carried out
Qualitative evaluation.Specific practice is：Knife is drawn with hard the parallel lines that two at a distance of 2 millimeters are carved on coating, depth of score is saturating to draw
Coating is defined to ceramic matrix.The good criterion of adhesion, is that the coating between line is not separated with matrix.Test knot
Fruit is as shown in Figure 5：It was found that coating comes off, it was demonstrated that copper coating is well combined with SiC matrix.
Claims (4)
1. a kind of SiC powder surface chemical plating copper method, its processing step is：
Step 1：SiC powder is cleaned：It is 0.1-100 microns by particle mean size, optimum grain-diameter is the SiC of 0.6-4 microns
Powder enter in being put into acetone ultrasound carry out clean 5-60 minutes after, by SiC powder filter, be dried, then filter, cleaning, drying；
Wherein acetone consumption is 2-3 times of SiC powder apparent volume；
Step 2：Surface coarsening process；Above-mentioned steps dried SiC particulate is put in the HF solution of 20ml/L, sonic oscillation
5-25min, then filters, cleans, dries；
Step 3：Surface active sensitized treatment：By the SiC powder after above-mentioned roughening treatment, it is put in sensitization activating solution, heats quick
Change activating solution to after 20-40 DEG C, ultrasonic 5-120 minutes, then filter, clean, dry；Above-mentioned sensitization activating solution is to be with concentration
The PdCl of 0.1-1g/L2, concentration for 5-30g/L SnCl2·2H2O, concentration are 20- for the NaCl and concentration of 20-150mL/L
The hydrochloric acid HCl deionized waters configuration of 150mL/L is formed；The consumption of above-mentioned sensitization activating solution is to be sensitized per 100 grams of SiC powders
Activating solution 300-500 milliliters；
Step 4：The preparation of chemical plating fluid：Deionized water is by CuSO4·5H2O is configured to the solution A that concentration is 10-30g/L, so
The PH of above-mentioned solution is adjusted to 10-14 with NaOH solution afterwards, optimal pH value is 13；
Sodium potassium tartrate tetrahydrate, HCHO and EDTA-Na are configured to mix B solution, the wherein concentration of sodium potassium tartrate tetrahydrate by deionized water
Concentration for 5-40g/L, HCHO is 20-60g/L for the concentration of 5-100mL/L, LEDTA-Na；
Above-mentioned solution A is slowly added in B solution under stirring, while the PH of mixed solution is adjusted with NaOH solution
After value is maintained at 10-14, clarified, without precipitation chemical plating fluid；
Step 5：Electroless copper is implemented to SiC powder：SiC powder after above-mentioned chemical plating fluid and activation sensitized treatment is preheated to
30-50 DEG C, then the SiC powder after preheating is added under stirring carries out copper facing, the increasing of thickness of coating in chemical plating fluid
Thick speed is micro- m/h of 0.01-10.
2. a kind of SiC powder surface chemical plating copper method according to claim 1, it is characterised in that clear in above-mentioned steps
Wash is to adopt deionized water to clean pH to cleanout fluid for 7 or so.
3. a kind of SiC powder surface chemical plating copper method according to claim 2, it is characterised in that the baking in above-mentioned steps
Do as natural air drying or dry in an oven, at 80-120 DEG C, the time is 5-10 minutes to temperature control when drying in an oven.
4. a kind of SiC powder surface chemical plating copper method according to claim 3, it is characterised in that above-mentioned to SiC powder
During implementing electroless copper, the consumption of chemical plating fluid is to add 500-1000 milliliter chemical plating fluids per 100 grams of SiC powders.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739870A (en) * | 2017-09-11 | 2018-02-27 | 北方民族大学 | A kind of preparation method of SiC reinforcement high Al-Zn base composite |
| CN108034934A (en) * | 2017-12-05 | 2018-05-15 | 山东电盾科技股份有限公司 | The method that electroless copper method prepares silicon oxide powder conductive filler |
| CN108441728A (en) * | 2018-04-18 | 2018-08-24 | 明光市天淼新能源科技有限公司 | A kind of enhancing magnesium alloy materials |
| CN114315368A (en) * | 2022-01-05 | 2022-04-12 | 河南科技大学 | Composite material of metal copper and MoAlB ceramic and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739870A (en) * | 2017-09-11 | 2018-02-27 | 北方民族大学 | A kind of preparation method of SiC reinforcement high Al-Zn base composite |
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| CN108441728A (en) * | 2018-04-18 | 2018-08-24 | 明光市天淼新能源科技有限公司 | A kind of enhancing magnesium alloy materials |
| CN114315368A (en) * | 2022-01-05 | 2022-04-12 | 河南科技大学 | Composite material of metal copper and MoAlB ceramic and preparation method and application thereof |
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