CN101358374A - Method for preparing functional gradient composite materials - Google Patents
Method for preparing functional gradient composite materials Download PDFInfo
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- CN101358374A CN101358374A CNA2008102230854A CN200810223085A CN101358374A CN 101358374 A CN101358374 A CN 101358374A CN A2008102230854 A CNA2008102230854 A CN A2008102230854A CN 200810223085 A CN200810223085 A CN 200810223085A CN 101358374 A CN101358374 A CN 101358374A
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Abstract
The invention provides a preparation method of function gradient composite material, which is only a method for obtaining an Ni/SiC function composite gradient cladding layer with cyclic reversing pulse power supply through changing the pulse frequency and duty ratio of the power supply under the conditions of constant current and not changing the components of the plating bath. The material can be widely used in aeronautics and space, medicine, electronics, nuclear energy and other fields, such as anti-oxidation, wear resistant, anti-corrosion and heat barrier coatings.
Description
Technical field
The invention belongs to the functional gradient composite materials preparing technical field, a kind of preparation method of ceramics particle strengthened metal-based gradient composite material particularly is provided.That this material can be used as is anti-oxidant, wear-resisting, etch-resistant coating and thermal barrier coating are widely used in fields such as aerospace, medical science, electronics, nuclear energy.
Background technology
Called function gradient material (Functionally Gradient Materials, be called for short FGM), be according to service requirements, select the material of two kinds of different performances, adopt advanced material compounding technology, it is formed continuously change in gradient, thereby make the character of material and the class advanced composite material that function also changes in gradient along thickness direction.The distinguishing feature of this class matrix material is to have overcome two kinds of problems that the different material interface branch performance of performance is easily suddenlyd change.
The proposition of functional gradient composite materials notion is based on the heat protection problem that solves space shuttle.As everyone knows, with hypervelocity flight, shell and atmosphere friction produce high temperature to space shuttle when passing through atmosphere.The heat-stable material that the space shuttle shell covers generally is a carbon-fibre composite.Because this matrix material is different with the aluminum alloy casing thermal expansivity, paste interface at it under the high temperature and can produce huge thermal stresses, cause refractory layer to peel off even come off, to the consequence of the bringing on a disaster property of flight of space shuttle.Therefore, the research and development of Functionally Graded Materials cause material supplier author's common concern.
In recent years, people have carried out deep research to the preparation method of Functionally Graded Materials.Usually, divide, the preparation method of Functionally Graded Materials can be divided into vapour deposition process, solid phase method and liquid phase method according to the state of material.Require when utilizing vapour deposition process to prepare Functionally Graded Materials under vacuum condition, to carry out; Adopt high-temperature operation when solid phase method prepares Functionally Graded Materials mostly, production process is numerous and diverse, and the porosity of material is bigger; Electrodip process is as a kind of low temperature liquid phase technology of preparing, can obtain the settled layer of metal, alloy or pottery on the surface of solid material, improves that it is wear-resisting, solidity to corrosion or make material surface have special function solenoid, optical function, heat physical properties etc.Electrodip process has been widely used in the Functionally Graded Materials of preparation film-type at present because equipment is simple, easy to operate.Usually adopt the MULTILAYER COMPOSITE coating technology when utilizing electrodip process to prepare the film-type Functionally Graded Materials, promptly on the basis of composite plating, wait and obtain the gradient function matrix material by repeatedly changing disperse particles type, solution composition in the plating bath.For example, people such as Wang (Hongzhi Wang, Suwei Yao, et.Electrochemical preparationand characterizationof Ni/SiC gradient deposit, Journal of MaterialsProcessing Technology 145 (2004) 299-302) made the Ni/SiC gradient coating by the fraction of particle in the control plating bath.But this method trivial operations, SiC content is wayward, just can obtain needed gradient composition and is difficult to grasp because how many particles reusable plating bath adds.In order to promote galvanic deposit Functionally Graded Materials Development of Preparation Technology, press for a kind of operability of exploitation is stronger, prepare material tissue and the more stable electro-deposition method of performance.
In recent years, some scholars attempt only changing the pulse plating parameter to obtain the coating material of superperformance.(M.E.Bahrololoom such as Bahrololoom, R.Sani, The influence ofpulse plating parameters on the hardness and wear resistance ofnickel-alumina composite coatings, Surface ﹠amp; Coatings Technology 192 (2005) 154-163) pulse-repetition and dutycycle have been studied to deposit N i-Al
2O
3The influence of coating hardness finds that under low duty ratio (0.1-0.2) condition, the hardness of composite deposite reduces with the increase of pulse-repetition and dutycycle at low frequency (10-20Hz).People such as Guo (Chao Guo, Yu Zuo, et.The effects of pulse reverse parameters on the properties of Nicarbon nanotubes composite coatings, Surface ﹠amp; Coatings Technology201 (2007) 9,491 9496) the reverse pulse electric current of frequency of utilization below 1KHz prepared Ni-CNTs (carbon nanotube), and finding increases with pulse-repetition and dutycycle, and content of carbon nanotubes increases in the composite deposite.But pulse-repetition by changing pulse-repetition and dutycycle, is not appeared in the newspapers with the graded composite coating material for preparing premium properties more than 1KHz.
Summary of the invention
The objective of the invention is to: provide a kind of reverse pulse power supply that only utilizes, by changing the pulse-repetition and the dutycycle of power supply, at continuous current, do not change the method that obtains Ni/SiC function complex gradient coating under the solution composition condition
Formation of the present invention: master metal salt is formulated as nickel plating solution with deionized water.The SiC ceramic particle that adds 1-3g/L selects positive primary alconol sulfuric ester and cetyl trimethylammonium bromide as dispersion agent as strengthening phase, and cooperates ultrasonic dispersing to prevent the reunion of SiC ceramic particle.Life cycle commutating pulse power supply fixed current density, according to required gradient and thickness of coating, regularly different dutycycle and the pulse-repetitioies of conversion electroplated.Concrete grammar is as follows:
1) takes by weighing 120-240g/L NiSO
46H
2O, 22.5-45g/L NiCl
26H
2O, 20-40g/L H
3BO
4, be made into nickel plating solution with deionized water;
2) take by weighing 1-3g/L SiC ceramic particle, put into the described nickel plating solution of 50-100mL, add the positive primary alconol sulfuric ester of 0.2-1.5mL/L, 0.1-1.2g/L cetyl trimethylammonium bromide simultaneously.Ultrasonic dispersing 45-60min; Add the whole nickel plating solutions of residue, ultrasonic dispersing 10-20min obtains the homodisperse plating bath of SiC ceramic particle again;
3) selecting part to be plated is negative electrode, and pure nickel, graphite or platinum electrode are anode, makes negative electrode and the anode keeping parallelism of trying one's best; Negative electrode, anode are placed the homodisperse plating bath of described SiC ceramic particle; Coating bath is placed water bath, be heated to 40-60 ℃, keep constant temperature, and carry out induction stirring with the speed of 200-600r/min; The setting range of the pulse-repetition of reverse pulse power supply, dutycycle and current density is respectively 1-50KHz, 0.5-0.9 and 3-6A/dm2; According to thickness of coating and the requirement of SiC granule content, change needed dutycycle and reverse impulse frequency, timed interval 5-30min.
Another technical scheme of the present invention is that above-mentioned part to be plated can be a copper sheet.
Advantage applies of the present invention is simple to operate, and is with low cost, is fit to produce in enormous quantities.
Description of drawings
Fig. 1 is a Ni-SiC composite deposite cross section SEM picture;
Fig. 2 is Ni-SiC composite deposite cross section EDS figure;
Fig. 3 is a Ni-SiC composite deposite cross section SEM picture
Fig. 4 is a Ni-SiC composite deposite cross section SEM picture
Embodiment
Embodiment 1
Take by weighing 18g NiSO
46H
2O, 3.375g NiCl
26H
2O, 3g H
3BO
4, be modulated into nickel plating solution with the 150mL deionized water.Taking by weighing the 0.15g median size is the β type SiC particle of 50nm, and load weighted SiC particle is placed the 50mL nickel plating solution.Add 0.02g cetyl trimethylammonium bromide and the positive primary alconol sulfuric ester of 0.05mL as dispersion agent, use ultrasonic dispersing 45min, add residue nickel plating solution redispersion 10min.NiSO in the final Ni-SiC plating bath
46H
2O concentration is 120g/L, NiCl
26H
2O concentration is 22.5g/L, H
3BO
4Concentration is 20g/L, and the SiC granule density is 1g/L, and positive primary alconol sulfuric ester concentration is that 0.33mL/L, cetyl trimethylammonium bromide concentration are 0.13g/L.
The selection copper sheet is that negative electrode, nickel plate are anode.The beaker of the plating bath that modulates is placed 50 ℃ water bath, carry out induction stirring with the speed of 200r/min.Open the reverse pulse power switch, depositing current density is adjusted to 3A/dm
2, pulse-repetition is adjusted to 1KHz, and dutycycle is adjusted to 0.5, and every ten minutes change pulse frequencies and dutycycle, order change is as shown in table 1, and deposition total time is 50min.
Table 1 pulse parameter changes sequence list
Deposition finishes back taking-up negative electrode to be cleaned, dries up, and sample preparation is also analyzed.Coating cross section pattern as shown in Figure 1.Fig. 2 is the EDS analytical results of position Ni shown in Fig. 1 arrow and Si element.The result shows, reduces gradually to copper base SiC content from coating surface.
Embodiment 2
Take by weighing 36g NiSO46H2O, 6.7g NiCl26H2O, 6g H3BO4 is modulated into nickel plating solution with the 200mL deionized water; Taking by weighing the 0.45g median size is the β type SiC particle of 50nm, and load weighted SiC particle placed the 100mL nickel-plating liquid, add 0.12g cetyl trimethylammonium bromide and the positive primary alconol sulfuric ester of 0.2mL as dispersion agent, use ultrasonic dispersing 50min, add residue plating bath redispersion 20min.NiSO in the final Ni-SiC plating bath
46H
2O concentration is 180g/L, NiCl
26H
2O concentration is 33.5g/L, H
3BO
4Concentration is 30g/L, and the SiC granule density is 2.25g/L, and positive primary alconol sulfuric ester concentration is that 1mL/L, cetyl trimethylammonium bromide concentration are 0.6g/L.
The selection copper sheet is that negative electrode, nickel plate are anode, and the beaker of the plating bath that modulates is placed 40 ℃ water bath, carries out induction stirring with the speed of 400r/min.Open the reverse pulse power switch, depositing current density is fixed as 5A/dm2, and dutycycle is 0.7, and the reverse impulse frequency is respectively 50KHz, 20KHz, 5KHz, 10KHz, and order changes, and be 20min pitch time.Deposition finishes the back and takes out negative electrode and clean, dry up and carry out the sample preparation analysis.Coating cross section back scattering (BSD) photo as shown in Figure 3, black particle wherein is the SiC particle.As seen from the figure, the SiC granule content reduces from the coating surface to the copper base gradually.
Take by weighing 48g NiSO46H2O, 9g NiCl26H2O, 8g H3BO4 is modulated into homogeneous solution with the 200mL deionized water; Taking by weighing the 0.6g median size is the β type SiC particle of 50nm, and load weighted SiC particle placed the 100mL plating bath, add 0.24g cetyl trimethylammonium bromide and the positive primary alconol sulfuric ester of 0.3mL as dispersion agent, use ultrasonic dispersing 60min, add residue plating bath redispersion 20min.NiSO in the final Ni-SiC plating bath
46H
2O concentration is 240g/L, NiCl
26H
2O concentration is 45g/L, H
3BO
4Concentration is 40g/L, and the SiC granule density is 3g/L, and positive primary alconol sulfuric ester concentration is that 1.5mL/L, cetyl trimethylammonium bromide concentration are 1.2g/L.
The selection copper sheet is that negative electrode, graphite are anode, and the beaker of the plating bath that modulates is placed 60 ℃ water bath, carries out induction stirring with the speed of 600r/min.Open the reverse pulse power switch, depositing current density is fixed as 6A/dm2, and reverse impulse frequency and dutycycle are respectively 50KHz, 0.8,20KHz, 0.8, and 10KHz, 0.7, order changes, and is respectively 5min, 15min, 30min pitch time.Deposition finishes the back and takes out negative electrode and clean, dry up and carry out the sample preparation analysis.Coating cross section back scattering (BSD) photo as shown in Figure 4, black particle wherein is the SiC particle.As seen from the figure, the SiC granule content reduces from the coating surface to the copper base gradually.
Claims (2)
1, a kind of preparation method of functional gradient composite materials is characterized in that:
1) takes by weighing 120-240g/L NiSO
46H
2O, 22.5-45g/L NiCl
26H
2O, 20-40g/L H
3BO
4, be made into nickel plating solution with deionized water;
2) take by weighing 1-3g/L SiC ceramic particle, put into the described nickel plating solution of 50-100mL, add the positive primary alconol sulfuric ester of 0.2-1.5mL/L, 0.1-1.2g/L cetyl trimethylammonium bromide simultaneously, ultrasonic dispersing 45-60min; Add the whole nickel plating solutions of residue, ultrasonic dispersing 10-20min obtains the homodisperse plating bath of SiC ceramic particle again;
3) selecting part to be plated is negative electrode, and pure nickel, graphite or platinum electrode are anode, makes negative electrode and the anode keeping parallelism of trying one's best; Negative electrode, anode are placed the homodisperse plating bath of described SiC ceramic particle; Coating bath is placed water bath, be heated to 40-60 ℃, keep constant temperature, and carry out induction stirring with the speed of 200-600r/min; The setting range of the pulse-repetition of reverse pulse power supply, dutycycle and current density is respectively 1-50KHz, 0.5-0.9 and 3-6A/dm
2According to thickness of coating and the requirement of SiC granule content, change needed dutycycle and reverse impulse frequency, timed interval 5-30min.
2, the preparation method of a kind of functional gradient composite materials as claimed in claim 1 is characterized in that: described part to be plated can be a copper sheet.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979997A (en) * | 2010-09-09 | 2011-02-23 | 北京理工大学 | System for testing damage to gradient composite under thermal/electric/magnetic/coupling action |
| CN102443829A (en) * | 2011-12-08 | 2012-05-09 | 天津大学 | Surface plating of Ag-Ni electric contact and preparation process thereof |
| CN103668370A (en) * | 2013-12-19 | 2014-03-26 | 潮州市连思科技发展有限公司 | Method for pulse plating of disk |
| CN105177645A (en) * | 2015-07-27 | 2015-12-23 | 昆明理工大学 | Preparation method of multi-layer composite gradient nano pure copper materials |
| CN107419319A (en) * | 2016-05-23 | 2017-12-01 | 云南民族大学 | A kind of method of micron SiC granule content in raising nickel-base composite coat |
| CN110129864A (en) * | 2019-05-30 | 2019-08-16 | 中国石油大学(华东) | A kind of Ni-based gradient coating of redox graphene-and preparation method thereof |
| CN110938850A (en) * | 2019-12-16 | 2020-03-31 | 南京信息职业技术学院 | Composite nickel electroplating solution, nickel-based nano composite coating and preparation method |
| CN111411377A (en) * | 2020-05-07 | 2020-07-14 | 广东省焊接技术研究所（广东省中乌研究院） | Novel nickel-phosphorus alloy with gradient structure and preparation method thereof |
| CN111607816A (en) * | 2020-06-03 | 2020-09-01 | 暨南大学 | Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy |
| CN116352233A (en) * | 2023-05-30 | 2023-06-30 | 中镱新材料智能制造研究院(山西)有限公司 | Manufacturing method for fused accumulation additive of ejection type ceramic particle reinforced composite material |
-
2008
- 2008-09-26 CN CNA2008102230854A patent/CN101358374A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979997A (en) * | 2010-09-09 | 2011-02-23 | 北京理工大学 | System for testing damage to gradient composite under thermal/electric/magnetic/coupling action |
| CN102443829A (en) * | 2011-12-08 | 2012-05-09 | 天津大学 | Surface plating of Ag-Ni electric contact and preparation process thereof |
| CN102443829B (en) * | 2011-12-08 | 2014-07-16 | 天津大学 | Surface plating of Ag-Ni electric contact and preparation process thereof |
| CN103668370A (en) * | 2013-12-19 | 2014-03-26 | 潮州市连思科技发展有限公司 | Method for pulse plating of disk |
| CN105177645A (en) * | 2015-07-27 | 2015-12-23 | 昆明理工大学 | Preparation method of multi-layer composite gradient nano pure copper materials |
| CN107419319B (en) * | 2016-05-23 | 2019-08-02 | 云南民族大学 | A kind of method of micron SiC granule content in raising nickel-base composite coat |
| CN107419319A (en) * | 2016-05-23 | 2017-12-01 | 云南民族大学 | A kind of method of micron SiC granule content in raising nickel-base composite coat |
| CN110129864A (en) * | 2019-05-30 | 2019-08-16 | 中国石油大学(华东) | A kind of Ni-based gradient coating of redox graphene-and preparation method thereof |
| CN110129864B (en) * | 2019-05-30 | 2020-04-28 | 中国石油大学(华东) | Reduced graphene oxide-nickel-based gradient coating and preparation method thereof |
| CN110938850A (en) * | 2019-12-16 | 2020-03-31 | 南京信息职业技术学院 | Composite nickel electroplating solution, nickel-based nano composite coating and preparation method |
| CN111411377A (en) * | 2020-05-07 | 2020-07-14 | 广东省焊接技术研究所（广东省中乌研究院） | Novel nickel-phosphorus alloy with gradient structure and preparation method thereof |
| CN111607816A (en) * | 2020-06-03 | 2020-09-01 | 暨南大学 | Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy |
| CN116352233A (en) * | 2023-05-30 | 2023-06-30 | 中镱新材料智能制造研究院(山西)有限公司 | Manufacturing method for fused accumulation additive of ejection type ceramic particle reinforced composite material |
| CN116352233B (en) * | 2023-05-30 | 2023-08-22 | 中镱新材料智能制造研究院(山西)有限公司 | Manufacturing method for fused accumulation additive of ejection type ceramic particle reinforced composite material |
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