CN102787308A - Method for carrying out nickel plating coating on MWNT (multi-walled carbon nanotube) - Google Patents
Method for carrying out nickel plating coating on MWNT (multi-walled carbon nanotube) Download PDFInfo
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- CN102787308A CN102787308A CN201210282902XA CN201210282902A CN102787308A CN 102787308 A CN102787308 A CN 102787308A CN 201210282902X A CN201210282902X A CN 201210282902XA CN 201210282902 A CN201210282902 A CN 201210282902A CN 102787308 A CN102787308 A CN 102787308A
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- nickel plating
- mwnts
- walled carbon
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Abstract
The invention provides a method for carrying out nickel plating coating on a MWNT (multi-walled carbon nanotube), which comprises the following steps of: placing the MWNT in an acid solution containing Sn2+ to carry out sensitization; 2, activating in an acid solution containing Pd2+; and 3, carrying out nickel plating in an electroless plating solution containing a reducing agent and a nickel salt. The nickel-plated coated MWNT prepared by the method provided by the invention has excellent high temperature resistance; the ablation of wild-phase MWNTs, which is caused by thermal spraying high temperature, can be obviously reduced; the liquidity of a thermal spraying material added with the MWNTs is improved; and the nickel-plated coated spheroidized MWNTs with excellent high temperature resistance can be obtained by the method provided by the invention. The method has the advantages of simple process flow and low cost.
Description
Technical field
The invention belongs to the plating field of metallic substance, be specially a kind of method that nickel plating coats on multi-walled carbon nano-tubes material.
Background technology
Carbon nanotube is just found a kind of carbon structure in 1991, and it is one deck or the curling cage shape fiber that forms of several layers carbon atom in the graphite, and inside is empty, and outer dia has only a few to tens of nanometers.Number according to carbon atomic layer in the nanotube tube wall is divided into single wall and multi-walled carbon nano-tubes.(multi-walled carbon nanotubes MWNTs) contains the multi-layer graphene sheet to multi-walled carbon nano-tubes, and its number of plies does not wait from 2-50, and interlamellar spacing is 0.34 ± 0.01nm, and is suitable with the graphite layers distance.Multi-walled pipes when forming layer with layer between become trap center two easily and catch various defectives, thereby be covered with the defective of duck eye appearance usually on the tube wall of multi-walled pipes, have and SWCN different surface performance.
Multi-walled carbon nano-tubes has near perfect structure; Its average Young's modulus is up to 1.8TPa; Average flexural strength is up to 14.2GPa, and tensile strength is 100 times of steel and density is 1/6 of steel, is a kind of matrix material wild phase of excellent property; From since making discovery first, promptly having been paid close attention to, be widely used in material, microelectronics, catalyzer, medical science, biotechnology and aerospace field by the whole world.Because its excellent mechanical property, applied to play enhancement in the matrix material, as be added in rubber, plastics film, the low melting point metal matrix material and play toughening effect.But because its high thermal resistance (aerial ablation temperature is 500 ℃), mobile relatively poor, these defectives make its application in field of thermal spray seriously limited.
Therefore, be necessary to propose effective MWNTs treatment process, to improve resistance to elevated temperatures and the flowability of MWNTs.
Summary of the invention
To the weak point that prior art exists, the objective of the invention is to propose the method that a kind of multi-walled carbon nano-tubes nickel plating coats.
Another purpose of the present invention is the multi-walled carbon nano-tubes of the nickel plating coating that proposes to make with said method.
The technical scheme that realizes above-mentioned purpose of the present invention is:
The method that a kind of multi-walled carbon nano-tubes nickel plating coats comprises step:
1) multi-walled carbon nano-tubes is placed contains Sn
2+Acidic solution in sensitization;
2) containing Pd
2+Acidic solution in activation;
3) nickel plating in the chemical plating fluid that contains reductive agent and nickel salt.
Wherein, said step 1) also comprises the step with the multi-walled carbon nano-tubes ultra-sonic dispersion, is containing Sn then
2+With sensitization in the hydrochloric acid soln of 12 ~ 20g/L, the sensitization after-filtration is also used deionized water rinsing.MWNTs surface after the sensitization can obtain hydrolysis resultant Sn (OH) Cl and Sn (OH) through flushing
2, polymerization generates the spawn Sn that is slightly soluble in water then
2(OH)
3Cl.These hydrolysates and polymer deposition thereof form a layer thickness and reach the material that be similar to gel of several nanometers to the hundreds of nanometer thickness on the MWNTs surface.These jellies are attached to the MWNTs surface, can adsorb a large amount of nickel ions, play the effect of producer.
Wherein, contain Sn in the said step 1)
2+Acidic solution for containing the SnCl of 16 ~ 18g/L
2With the solution of the hydrochloric acid of 12 ~ 15g/L, the time of said sensitization is 25 ~ 35min.
Wherein, be to contain the PdCl of 0.4 ~ 0.8g/L said step 2)
2With activation in the hydrochloric acid soln of 12 ~ 15g/L, the activatory time is 25 ~ 35min, uses washed with de-ionized water after the activation.Pd in the activation solution
2+Diffuse into spawn Sn
2(OH)
3Among the Cl, and with wherein Sn
2+React, generate the Pd atom and be deposited on the ceramic coating surface with particulate state.Be equivalent in the MWNTs surface attachment the very thin catalyst film of one deck, this layer film plays the effect that causes the chemical nickel plating reaction when nickel plating begins.
Wherein, said step 3) is to contain tensio-active agent, complexing agent, reductive agent and NiSO
4Chemical plating fluid in nickel plating, after the nickel plating with washed with de-ionized water and drying; Said tensio-active agent is a kind of in sodium laurylsulfonate, sodium lauryl sulphate, the dioctyl sodium sulfosuccinate; The content of tensio-active agent is 1.3 ~ 1.7g/L; Said complexing agent is a kind of in Trisodium Citrate, EDTA disodium salt or the trolamine, and complexing agent content is 50 ~ 80g/L.Tensio-active agent can move by speeding-up ion in the electroless plating process, thereby improve electroless plating speed as a kind of AS; The effect of complexing agent is to prevent to generate the plating defect that alkali formula nickel salt deposition is caused, and in order to obtain fine and close more coating, must add an amount of complexing agent.
Wherein, the reductive agent in the said step 3) is NaH
2PO
2, its concentration is controlled to be 20 ~ 40g/L in the Ni-Speed; NiSO in the Ni-Speed
4Concentration is controlled to be 20 ~ 40g/L.NaH in chemical plating fluid
2PO
2And/or NiSO
4Density loss is then added chemical plating fluid during to 20g/L, keeps NaH
2PO
2And NiSO
4Concentration is 20 ~ 40g/L.Wherein, the temperature of said nickel plating is 40 ~ 60 ℃, preferred 48 ~ 52 ℃; The pH value of control chemical plating fluid is 8 ~ 9 in the Ni-Speed, and nickel plating consumes till 900 ~ 1000ml chemical plating fluid with the 1g multi-walled carbon nano-tubes.When reaction is accomplished, NiSO
4Concentration is below the 20g/L.
Wherein, also comprise the step of ball milling after the said step 3), ball-to-powder weight ratio is 1:8 ~ 11 in the ball-grinding machine.Ball-to-powder weight ratio is the weight ratio of grinding element and material.
The multi-walled carbon nano-tubes that the nickel plating that the method that the present invention proposes makes coats.
The application of multi-walled carbon nano-tubes in thermospray that the nickel plating that the present invention proposes coats.
Beneficial effect of the present invention is:
The nickel plating that method of the present invention makes coats multi-walled carbon nano-tubes and has good temperature resistance; Can obviously reduce the ablation that thermospray high temperature causes wild phase MWNTs; Improve the flowability of the thermospray material that has added MWNTs, method of the present invention can obtain the good nickel plating of resistance to elevated temperatures and coat nodularization MWNTs.This method technical process is simple, and cost is lower.
Description of drawings
Fig. 1 is operation technological process figure of the present invention;
Fig. 2 and 3 is that the MWNTs nickel plating of embodiment 1 coats cross-reference figure;
Fig. 2 is preceding photo for MWNTs nickel plating coats, and wherein a figure magnification is 10000 times, 20000 times of b figure magnifications;
Fig. 3 coats the back photo for MWNTs nickel plating, and wherein a figure magnification is 10000 times, 20000 times of b figure magnifications.
Embodiment
With following most preferred embodiment the present invention is described, but is not used for limiting scope of the present invention at present.Among the embodiment, like no specified otherwise, conventional equipment and the method in field under employed equipment and method are.
Employed processor for ultrasonic wave producer is that Kunshan Ultrasonic Instruments Co., Ltd. produces model: KQ100 in the instance of the present invention; Ball-grinding machine is the frequency conversion planetary ball mill, and producer is a Nanjing Da Ran Science and Technology Ltd., model: XQM-0.4L; Used multi-walled carbon nano-tubes is available from Sun Nantech company, purity>90%, caliber: 10 ~ 30nm.
Embodiment 1:
According to the process flow sheet of Fig. 1, concrete steps are:
Step 1: MWNTs is placed deionized water for ultrasonic concussion 30min, MWNTs is filtered out with filter paper.This moment is SEM pattern such as Fig. 2 of the NWNTs of nickel plating coating not;
Step 2: the MWNTs that filters out is placed the sensitizing solution for preparing in advance, and every separated 5min carries out magnetic agitation 5min to it, and stirring velocity 300r/min makes the abundant sensitization of MWNTs, and reduces the reunion of MWNTs.Sensitizing solution consist of SnCl
22H
2O:20g/L, (mass concentration is 20% to HCl, density 1.1g/cm
3): 65ml/L, sensitization time 30min.Sensitization finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 3: the MWNTs after the sensitization processing is placed the activation solution for preparing in advance, and whenever at a distance from 5min it is carried out magnetic agitation 5min, stirring velocity 300r/min makes the abundant activation of MWNTs, and reduces the reunion of MWNTs.Activation solution consists of PdCl
2: 0.5g/L, (mass concentration is 20% to HCl, density 1.1g/cm
3): 65ml/L, soak time 30min.Activation finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 4: the MWNTs after the activation treatment is placed every 1gMWNTs adding 1000ml plating bath in the chemical plating fluid for preparing in advance, and every separated 10min carries out magnetic agitation 10min to it, stirring velocity 300r/min, the reunion of reduction MWNTs.Chemical plating fluid consists of main salt NiSO
46H
2O:68g/L; Complexing agent Trisodium Citrate: 57g/L; Reductive agent NaH
2PO
2: 40g/L; And surfactant sodium laurylsulfonate: 1.5g/L; Constantly add ammoniacal liquor in the plating process and keep the pH value at 8-9; The electroless plating temperature remains on 50 ℃.NaH in chemical plating fluid
2PO
2And/or NiSO
4Density loss is then added chemical plating fluid during to 20g/L, keeps NaH
2PO
2And NiSO
4Concentration is 20 ~ 40g/L, and nickel plating consumes till the 1000ml chemical plating fluid with the 1g multi-walled carbon nano-tubes.The nickel plating reaction has great amount of bubbles to produce at first, and bubbles volume obviously reduced when reaction was accomplished, and the time of reaction is 20min.
When the chemical plating fluid consumption be 1gMWNTs to the 1000ml chemical plating fluid, then reaction finishes.This moment solution in NiSO
4Content is 20g/L.Use nickel plating MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7, place the interior 120 ℃ of oven dry of baking oven then;
Step 5: with planetary ball mill the MWNTs that nickel plating coats is carried out ball milling 1h, ball material mass ratio is 1:10.Revolution rotating speed 100r/min, rotation rotating speed 200r/min.The nickel plating that obtains coats SEM pattern such as Fig. 3 of MENTs.
The nickel plating that obtains with this method coats resistance to elevated temperatures and the flowability that nodularization MWNTs has effectively improved MWNTs; Metallic nickel is wrapped in MWNTs densely; It is significantly reduced with the contact area of oxygen in spraying process; The melting process of nickel has consumed most of spraying heat, makes the MWNTs that is wrapped in the inside be protected.Meanwhile the MWNTs after the nodularization can improve the flowability of powder, and the application in thermospray becomes possibility as wild phase to make MWNTs, and the thermal ablation rate that records pure MWNTs through overtesting is 2.700 * 10
-6G/s, the thermal ablation rate that nickel plating coats nodularization MWNTs is 0.935 * 10
-6G/s.
The MWNTs that present embodiment makes adds in the thermospray ceramic coating with 15% mass ratio, the coating good fluidity, and thermospray is in the reaction kettle inwall, and the coating even compact that obtains can anti-700 ℃ of high temperature.
Embodiment 2:
Step 1: MWNTs is placed deionized water for ultrasonic concussion 30min, MWNTs is filtered out with filter paper;
Step 2: the MWNTs that filters out is placed the sensitizing solution for preparing in advance, and every separated 5min carries out magnetic agitation 5min, stirring velocity 500r/min to it.Sensitizing solution consist of SnCl
216g/L, HCl (mass concentration is 20%): 60ml/L, sensitization time 25min.Sensitization finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 3: the MWNTs after the sensitization processing is placed the activation solution for preparing in advance, and whenever at a distance from 5min it is carried out magnetic agitation 5min, stirring velocity 500r/min makes the abundant activation of MWNTs, and reduces the reunion of MWNTs.Activation solution consists of PdCl
2: 0.4g/L, HCl (concentration is 20%): 60ml/L, soak time 25min.Activation finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 4: the MWNTs after the activation treatment is placed every 1gMWNTs adding 600ml plating bath in the chemical plating fluid for preparing in advance, and every separated 10min carries out magnetic agitation 10min to it, stirring velocity 500r/min, the reunion of reduction MWNTs.Chemical plating fluid consists of main salt NiSO
46H
2O:68g/L; Complexing agent EDTA disodium salt 50g/L; Reductive agent NaH
2PO
2: 40g/L; And surfactant sodium lauryl sulphate 1.3g/L; Constantly add ammoniacal liquor in the plating process and keep the pH value 9; The electroless plating temperature remains on 48 ℃.NaH in chemical plating fluid
2PO
2And/or NiSO
4Density loss is then added chemical plating fluid during to 30g/L, keeps NaH
2PO
2And NiSO
4Concentration is 30 ~ 40g/L.
When the chemical plating fluid consumption is that 1gMWNTs adds the 1000ml chemical plating fluid, then react and finish reaction times 15min.Use nickel plating MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7, place the interior 120 ℃ of oven dry of baking oven then;
Step 5: with planetary ball mill the MWNTs that nickel plating coats is carried out ball milling 1h, ball material mass ratio is 1:10.Revolution rotating speed 100r/min, rotation rotating speed 200r/min.
Embodiment 3:
Step 1: MWNTs is placed deionized water for ultrasonic concussion 30min, MWNTs is filtered out with filter paper;
Step 2: the MWNTs that filters out is placed the sensitizing solution for preparing in advance, every it is carried out magnetic agitation 5min at a distance from 5min, stirring velocity 500r/min, sensitizing solution consist of SnCl
218g/L, HCl (concentration is 20%): 75ml/L, sensitization time 35min.Sensitization finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 3: the MWNTs after the sensitization processing is placed the activation solution for preparing in advance, and every separated 5min carries out magnetic agitation 5min, stirring velocity 500r/min to it.Activation solution consists of PdCl
2: 0.5g/L, HCl (concentration is 20%): 70ml/L, soak time 30min.Activation finish the back use MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7;
Step 4: the MWNTs after the activation treatment is placed every 1gMWNTs adding 700ml plating bath in the chemical plating fluid for preparing in advance, and every separated 10min carries out magnetic agitation 10min, stirring velocity 500r/min to it.Chemical plating fluid consists of main salt NiSO
46H
2O:68g/L; Complexing agent trolamine 80g/L; Reductive agent NaH
2PO
2: 40g/L; And surfactant sodium laurylsulfonate: 1.7g/L; Constantly add ammoniacal liquor in the plating process and keep the pH value 8; The electroless plating temperature remains on 52 ℃.NaH in chemical plating fluid
2PO
2And/or NiSO
4Density loss is then added chemical plating fluid during to 20g/L, keeps NaH
2PO
2And NiSO
4Concentration is 20 ~ 30g/L.
When the plating bath consumption be 1gMWNTs to the 900ml plating bath, then reaction finishes.Reaction times 30min.Use nickel plating MWNTs that the deionized water washing and filtering comes out to wash-down water pH value be 7, place the interior 120 ℃ of oven dry of baking oven then;
Step 5: with planetary ball mill the MWNTs that nickel plating coats is carried out ball milling 1h, ball material mass ratio is 1:10.Revolution rotating speed 100r/min, rotation rotating speed 200r/min.
Above embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various modification and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (10)
1. the method that coats of a multi-walled carbon nano-tubes nickel plating comprises step:
1) multi-walled carbon nano-tubes is placed contains Sn
2+Acidic solution in sensitization;
2) containing Pd
2+Acidic solution in activation;
3) nickel plating in the chemical plating fluid that contains reductive agent and nickel salt.
2. the method for claim 1 is characterized in that, said step 1) also comprises the step with the multi-walled carbon nano-tubes ultra-sonic dispersion, is containing Sn then
2+With sensitization in the hydrochloric acid soln of 12 ~ 20g/L.
3. according to claim 1 or claim 2 method is characterized in that, contains Sn in the said step 1)
2+Acidic solution for containing the SnCl of 16 ~ 18g/L
2With the solution of the hydrochloric acid of 12 ~ 15g/L, the time of said sensitization is 25 ~ 35min.
4. according to claim 1 or claim 2 method is characterized in that said step 2) be to contain the PdCl of 0.4 ~ 0.8g/L
2With activation in the hydrochloric acid soln of 12 ~ 15g/L, the activatory time is 25 ~ 35min.
5. according to claim 1 or claim 2 method is characterized in that said step 3) is to contain tensio-active agent, complexing agent, reductive agent and NiSO
4Chemical plating fluid in nickel plating, after the nickel plating with washed with de-ionized water and drying; Said tensio-active agent is a kind of in sodium laurylsulfonate, sodium lauryl sulphate, the dioctyl sodium sulfosuccinate; The content of tensio-active agent is 1.3 ~ 1.7g/L; Said complexing agent is a kind of in Trisodium Citrate, EDTA disodium salt or the trolamine, and complexing agent content is 50 ~ 80g/L.
6. like claim 1 or 5 described methods, it is characterized in that the reductive agent in the said step 3) is NaH
2PO
2, its concentration is controlled to be 20 ~ 40g/L in the Ni-Speed; NiSO in the Ni-Speed
4Concentration is controlled to be 20 ~ 40g/L.
7. according to claim 1 or claim 2 method is characterized in that the temperature of said nickel plating is 40 ~ 60 ℃, preferred 48 ~ 52 ℃; The pH value of control chemical plating fluid is 8 ~ 9 in the Ni-Speed, and nickel plating finishes reaction when consuming 900 ~ 1000ml chemical plating fluid with every 1g multi-walled carbon nano-tubes.
8. the method for claim 1 is characterized in that, also comprises the step of ball milling after the said step 3), and ball-to-powder weight ratio is 1:8 ~ 11 in the ball-grinding machine.
9. the multi-walled carbon nano-tubes that coats of the nickel plating that makes of the arbitrary described method of claim 1 ~ 8.
10. the application of multi-walled carbon nano-tubes in thermospray of the described nickel plating coating of claim 9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978559A (en) * | 2012-11-30 | 2013-03-20 | 汕头大学 | Thermal spray coating for reinforcing carbon nanotube, as well as preparation method and application thereof |
| CN106905695A (en) * | 2017-03-02 | 2017-06-30 | 黄河科技学院 | A kind of carbon nano-tube modification carbon fibre composite for automotive hub and preparation method thereof |
| CN108546938A (en) * | 2018-04-28 | 2018-09-18 | 湖北理工学院 | A kind of preparation method of nickel coated carbon nano tube compound material |
| CN109338134A (en) * | 2018-09-08 | 2019-02-15 | 天津大学 | A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites |
| CN111020627A (en) * | 2019-12-18 | 2020-04-17 | 青岛大学 | Method for chemically plating NiP on surface of multi-wall carbon nano tube |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701334A (en) * | 2009-11-16 | 2010-05-05 | 哈尔滨工业大学 | Method for plating nickel layer on surface of multiwall carbon nanotube |
| CN101818337A (en) * | 2009-11-16 | 2010-09-01 | 兰州理工大学 | Coating method of high-density Ni layer of carbon nano tube |
-
2012
- 2012-08-09 CN CN201210282902XA patent/CN102787308A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701334A (en) * | 2009-11-16 | 2010-05-05 | 哈尔滨工业大学 | Method for plating nickel layer on surface of multiwall carbon nanotube |
| CN101818337A (en) * | 2009-11-16 | 2010-09-01 | 兰州理工大学 | Coating method of high-density Ni layer of carbon nano tube |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978559A (en) * | 2012-11-30 | 2013-03-20 | 汕头大学 | Thermal spray coating for reinforcing carbon nanotube, as well as preparation method and application thereof |
| CN102978559B (en) * | 2012-11-30 | 2015-02-11 | 汕头大学 | Thermal spray coating for reinforcing carbon nanotube, as well as preparation method and application thereof |
| CN106905695A (en) * | 2017-03-02 | 2017-06-30 | 黄河科技学院 | A kind of carbon nano-tube modification carbon fibre composite for automotive hub and preparation method thereof |
| CN108546938A (en) * | 2018-04-28 | 2018-09-18 | 湖北理工学院 | A kind of preparation method of nickel coated carbon nano tube compound material |
| CN109338134A (en) * | 2018-09-08 | 2019-02-15 | 天津大学 | A kind of preparation method of nickel-plating carbon nanotube reinforced aluminum matrix composites |
| CN111020627A (en) * | 2019-12-18 | 2020-04-17 | 青岛大学 | Method for chemically plating NiP on surface of multi-wall carbon nano tube |
| CN111020627B (en) * | 2019-12-18 | 2020-10-16 | 青岛大学 | Method for chemically plating NiP on surface of multi-wall carbon nano tube |
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Application publication date: 20121121 |