CN1821443A - Method and device for preparing hollow nickel, cobalt, nickel-cobalt fiber and hollow ball - Google Patents
Method and device for preparing hollow nickel, cobalt, nickel-cobalt fiber and hollow ball Download PDFInfo
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- CN1821443A CN1821443A CN 200610011542 CN200610011542A CN1821443A CN 1821443 A CN1821443 A CN 1821443A CN 200610011542 CN200610011542 CN 200610011542 CN 200610011542 A CN200610011542 A CN 200610011542A CN 1821443 A CN1821443 A CN 1821443A
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Abstract
The method and apparatus for preparing hollow nickel, cobalt, nickel-cobalt fiber and ball belongs to the field of metal material preparing technology. The present invention features that the nanometer hollow nickel, cobalt, nickel-cobalt fiber and ball is prepared through chemical metal film coating with viscose and carbon fiber or spherical viscose and carbon material as inducing agent, solution of soluble noble metal compound as activator, the salt of nickel, cobalt, nickel-cobalt salt as main salt, hydrazine as reductant, ammonia water as compounding agent and ammonium salt of the same anion as the main salt as the buffering agent; the subsequent carbon oxidation and gasification or carbonization, hydrogen treatment and other steps. The process is superior to available hydrogen reducing process, and has no need of pressure apparatus and simple operation.
Description
Technical field
The invention belongs to metal material field, particularly a kind of method and apparatus for preparing hollow nickel, cobalt, nickel-cobalt fiber and hollow ball.
Background technology
The traditional chemical depositing process is the chemical nickel plating reaction of reductive agent with hypophosphite and borane derivative promptly, generates in the nickel layer and unavoidably brings phosphorus (P) and boron (B) element impurity problem into, at high temperature can produce Ni
3P and Ni
3Intermediate phase such as B.
The hollow nickel fiber is widely used in nickel metal hydride battery, has improved the performance of battery, for the Application and Development of large-sized power power supply provides essential condition.Hollow nickel, nickel cobalt (alloy) fiber and ball can be used as electromagnetic shielding material, absorbing material and be used for stealth material in the national defense industry.
Yet the method that present employing prepares the hollow nickel fiber is carried out the high temperature depoling and is handled after mostly being the synthetic conjugated fibre of methods such as vapour deposition process, high pressure water thermal synthesis method, and flow process is higher to equipment requirements, complicated operation, and cost is also higher; Do not appear in the newspapers as yet as for Metal Ball such as hollow Nano nickel.
Summary of the invention:
The object of the invention is to overcome the traditional chemical depositing process, at high temperature can produce Ni
3P and Ni
3Intermediate phase problems such as B have enlarged the use range of hollow nickel fiber or hollow nickel ball; Solving the adding hydroxycarboxylate simultaneously can not the recycle problem as complexing (cooperation) agent.
A kind of method for preparing hollow nickel, cobalt, nickel-cobalt fiber and hollow ball, it is characterized in that the sphere material with viscose and carbon fiber or viscose and carbon is that organic carrier is induced realization chemical plating metal film, surface at the organic carrier of plating at first makes its surface-coated activator with the method for homogeneous immersion, activator is for containing Pt, Pd, Au, the soluble compound solution (H of precious metals such as Ag
3PtCl
6, PdCl
2, H
3AuCl
6, AuCl
3, Ag (NO
3)
2Deng), the consumption of activator is 0.02～0.2% of a carrier amount.Pt, Pd, Au, precious metal ions such as Ag are spontaneous evenly is adsorbed on organic carrier (plating piece) surface, uses hydrazine (hydrazine N again
2H
4) class, as the sulfuric acid hydrazine, chlorination hydrazine, reductive agent such as water and hydrazine or stannous chloride solution dip in the plating sensitization and handle, reductant solution concentration is greater than activator concentration, but is lower than saturation concentration, makes the organic carrier natural air drying then.Chemical nickel plating, cobalt, nickel cobalt metallic membrane in the middle of the organic carrier after overactivation and the sensitization processing sinks to plating bath again.Plating bath is made up of main salt, reductive agent, Synergist S-421 95, buffer reagent.With the salt that contains nickel, cobalt, nickel cobalt metal lining is main salt, comprises rose vitriol or single nickel salt, Xiao Suangu or nickelous nitrate, Cobaltous diacetate or nickel acetate, salt such as cobalt chloride or nickelous chloride; Reductive agent is hydrazine (hydrazine N
2H
4) class, as the sulfuric acid hydrazine, chlorination hydrazine, water and hydrazine etc.; Synergist S-421 95 is an ammoniacal liquor; Buffer reagent be by with have identical anionic ammonium salt to constitute with main salt.Main salt concentration scope 0.05～1.0mol/L; Reductant concentration is 4～8 times of the main salt stoichiometric concentration of reduction, i.e. 0.1～8.0mol/L; The minimum amount of ammoniacal liquor is 2 times of all main salt amount of metal ion, i.e. 0.1～0.5mol/L; The minimum add-on of ammonium salt is 0.1～0.6mol/L; Add reductive agent and ammoniacal liquor, can not have precipitation to separate out; The overall pH value of reaction process system remains between 8～12.The chemical equation of plating reaction process is:
Or
。
For preventing to produce insoluble complex-precipitation, the present invention adopts the measure that adds or drip continuously in batches reductive agent.In the aqueous solution, add earlier and become owner of salt and buffer reagent, after treating that the solution dissolving is limpid, add reduction dosage (half amount of promptly main salt concentration of metal ions of calculating by above-mentioned chemical equation earlier, all the other reductive agents are added at subsequent step), reduction dosage can produce insoluble complex too much, reduction dosage can produce infusible precipitate very little after Synergist S-421 95 adds.After solution dissolves clarification once more, once add whole Synergist S-421 95s.Remaining reductive agent divides the adding of three minor ticks or reacts dropping continuously with plating in the plating reaction process.Can guarantee like this, the plating bath clarification, even everywhere, the coating even compact that institute's plating goes out.
For guaranteeing the plating effect, the present invention has designed special-purpose electroless plating equipment, and this equipment is made of agitator 1, thermometer 2, water bath with thermostatic control function unit 3, temperature-control heat couple 4, heater block 5, stirring in water bath device 6, plating bath device 7, funnel 8.
Metal coating technological operation step is
1) enough water of in water bath, packing into, water bath with thermostatic control function unit 3 in the setting device, by well heater 5 with water-bath and be immersed between plating bath device 7 pre-heating temperature elevations to 60 in the water-bath～95 ℃, make equalizing temperature in the whole water-bath by stirring in water bath device 6, stirring in water bath device 6 rotating speeds are 400～1500 rev/mins.Measure bath temperature by temperature-control heat couple 4, make bath temperature be stabilized in design temperature, error is in ± 1 ℃; But since the reaction vessel size, material, and there is about 1～5 ℃ temperature difference in the wall thickness difference between thermometer 2 observed values and temperature-control heat couple observed value, when design temperature, should consider this temperature difference.When temperature reaches assigned temperature, and after constant, activatory plating piece (being the plating thing) joins in the plating bath device 7, and stirs by agitator 1, makes plating liquid phase concentration homogenizing, and agitator 1 rotating speed is 400～1200 rev/mins.Whole plating process need tracking observation drips reductive agent by 8 continuous supplementation of the feed hopper among Fig. 4, (also can adopt to be interrupted to add and replenish reductive agent.Because the plating reaction produces with a large amount of nitrogen bubble, when plating bath stops to produce bubble, promptly need to replenish reductive agent, replenish the reductive agent of fixed amount at every turn, generally divide to have added for three times and be advisable.) after having added all reductive agents, observe with suction pipe sucking-off part plating bath.Blueness in plating bath (the nickel ammino closes the ionic color) is taken off, and becomes colorless, and plating bath stops to produce bubble fully simultaneously, is the plating reaction end.The plating reaction finishes, and whole plating time is about 15～80 minutes.
Plating staticly settles and makes solid-liquid separation after finishing, and washes with water, removes the foreign ion of absorption.Then, carry out drying treatment.
2). oxidation of coal gasification or the carbonization product after with plating, put into 300～500 ℃ retort furnace after ℃ oven dry of room temperature～100, oxidation in 30 minutes, partial combustion are removed by the plating carrier.
3). hydrogen is handled
Through the product of oxide treatment, enter the furnace reduction of hydrogen (or ammonia pyrolysis gas) protection, reduction temperature is 600～1000 ℃, residual carbon is removed by the metal catalytic hydrogasification.
If when preparation nano particle balls or fiber, grow up for preventing sintering, this step also can be carried out in fluidised hydrogen reduction furnace.
Synergist S-421 95 is to be made of ammoniacal liquor and identical anionic ammonium salt with main salt with buffer reagent, in addition, can be according to the system difference, strength of solution is regulated ammoniacal liquor and ammonium salt amount, sees table 1 for details.
Table 1 plating bath is formed
| No. | Main salt, mol/L | Reductive agent, mol/L | Synergist S-421 95, mol/L | Buffer reagent, mol/L | pH |
| 1 | Vitriol 0.05～1.0 | Sulfuric acid hydrazine 0.1～8.0 | Ammoniacal liquor 0.1～0.5 | Ammonium sulfate 0.1～0.6 | 8～12 |
| 2 | Nitrate 0.05～1.0 | Water and hydrazine 0.1～8.0 | Ammoniacal liquor 0.1～0.5 | Ammonium nitrate 0.1～0.6 | 8～12 |
| 3 | Acetate 0.05～1.0 | Water and hydrazine 0.1～8.0 | Ammoniacal liquor 0.1～0.5 | Ammonium acetate 0.1～0.6 | 8～12 |
| 4 | Villaumite 0.05～1.0 | Chlorination hydrazine 0.1 ∽ 8.0 | Ammoniacal liquor 0.1～0.5 | Ammonium chloride 0.1～0.6 | 8～12 |
| 5 | Other is 0.05～1.0 years old | Water and hydrazine 0.1 ∽ 8.0 | Ammoniacal liquor 0.1～0.5 | Ammonium salt 0.1～0.6 | 8～12 |
Plating bath thermostability, chemical, stabilization of industry that the present invention adopts are good, are easy to industrialization, and can recycle.Compare with hydrogen reduction technology, do not need press device, simple to operation.Technology of the present invention is simple, coating is even, product performance are stable, applied widely, and cost is low.
Description of drawings:
Fig. 1 is the micron order metallic graphite carbon compound ball pattern that utilizes the inventive method to prepare.
Fig. 2 is the nano metal viscose conjugated fibre pattern that utilizes the inventive method to prepare.
Fig. 3 utilizes the metallic nickel of present method preparation and the x ray diffraction result of viscose conjugated fibre.
Fig. 4 is the special-purpose electroless plating equipment synoptic diagram of the present invention.
Fig. 5 is the pattern of the tubular fibre nickel section after handling.
Fig. 6 is the pattern of nanometer nickel-cobalt alloy fiber.
Embodiment:
Table 2 is specific embodiments of the invention
| Numbering | Activator species, PdCl 2， g/L | Organic fiber value, g/L | Additive, (NH 4) 2S O 4， mol/L | NH 4OH， mol/L | Bath temperature, ℃ | Main salt concentration, NiS O 4·6H 2 O，mol/ L | Reductive agent, N 2H 4· H 2O， mol/L | Plating time, min | Carbonization temperature, ℃ | The hydrogen treatment temp, ℃ |
| 1 | 0.01 | 1.0 | 0.01 | 0.4 | 70 | 0.05 | 0.2 | 80 | 300 | 600 |
| 2 | 0.01 | 1.0 | 0.012 | 0.5 | 72 | 0.06 | 0.25 | 40 | 350 | 700 |
| 3 | 0.01 | 1.0 | 0.014 | 0.6 | 75 | 0.07 | 0.3 | 30 | 400 | 750 |
| 4 | 0.01 | 1.0 | 0.016 | 0.7 | 76 | 0.08 | 0.35 | 15 | 500 | 800 |
Wherein: NiSO
46H
2O is 15.8g; (NH
4)
2SO
4Be 3.0g; NH
3H
2O is 25ml; Organic fibre is 1.0g; N
2H
4H
2O is 12ml.
The influence of the different main salt pair coating of table 3
| Main salt system | Chloride system (NiCl 2·6H 2O) | Nitrate system (Ni (NO 3) 2·6H 2O) | Sulfate system (NiSO 4·6H 2O) |
| The median size of nano metal, nm | 12 | 10.0 | 9.0 |
Claims (6)
1. method for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball, it is characterized in that the sphere material with viscose and carbon fiber or viscose and carbon is that organic carrier is induced realization chemical plating metal film, surface at the organic carrier of plating at first makes organic carrier surface-coated activator with the method for homogeneous immersion, activator is the soluble compound solution that contains Pt, Pd, Au, Ag precious metal, and the consumption of activator is 0.02～0.2% of an organic carrier amount; Pt, Pd, Au, Ag precious metal ion are spontaneous evenly is adsorbed on the organic carrier surface, uses hydrazine again--hydrazine N
2H
4Class reductive agent or stannous chloride solution dip in the plating sensitization and handle, and reductant solution concentration is greater than activator concentration, but are lower than saturation concentration, make the organic carrier natural air drying then; Chemical nickel plating, cobalt, nickel cobalt metallic membrane in the middle of the organic carrier after overactivation and the sensitization processing sinks to plating bath again; Plating bath is made up of main salt, reductive agent, Synergist S-421 95, buffer reagent; With the salt that contains nickel, cobalt, nickel cobalt metal lining is main salt, and reductive agent is a hydrazine--hydrazine N
2The Hx class; Synergist S-421 95 is an ammoniacal liquor; Buffer reagent is by having identical anionic ammonium salt to constitute with main salt; Main salt concentration scope 0.05～1.0mol/L; Reductant concentration is 4～8 times of the main salt stoichiometric concentration of reduction, i.e. 0.1～8.0mol/L; The minimum amount of ammoniacal liquor is 2 times of all main salt amount of metal ion, i.e. 0.1～0.5mol/L; The minimum add-on of ammonium salt is 0.1～0.6mol/L; Add reductive agent and ammoniacal liquor, can not have precipitation to separate out; The overall pH value of reaction process system remains between 8～12; The chemical equation of plating reaction process is:
Or
。
2. a kind of method for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball as claimed in claim 1 is characterized in that containing Pt, Pd, and Au, the soluble compound solution of Ag precious metal is H
3PtCl
6, PdCl
2, H
3AuCl
6, AuCl
3, Ag (NO
3)
2, the main salt that contains nickel, cobalt, nickel cobalt metal lining is rose vitriol or single nickel salt, Xiao Suangu or nickelous nitrate, Cobaltous diacetate or acetic acid nickel salt, cobalt chloride or nickelous chloride; Reductive agent is the sulfuric acid hydrazine, chlorination hydrazine, water and hydrazine.
3. a kind of method for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball as claimed in claim 1 or 2, it is characterized in that adopting the measure that adds or drip continuously in batches reductive agent, in the aqueous solution, add earlier and become owner of salt and buffer reagent, treat that solution dissolving is limpid after, add earlier and press
Or
Half amount of the promptly main salt concentration of metal ions of reduction dosage that chemical equation calculates, all the other reductive agents are added at subsequent step, after solution dissolves clarification once more, once add whole Synergist S-421 95s, remaining reductive agent divides the adding of three minor ticks or reacts dropping continuously with plating in the plating reaction process.
4. a kind of method for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball as claimed in claim 3 is characterized in that metal coating technological operation step is:
1) plating temperature is between 60～95 ℃, and plating bath carries out under water bath condition, and temperature is wanted evenly in the whole water-bath, and bath temperature is stabilized in design temperature, and error is in ± 1 ℃; Plating liquid concentration is wanted evenly; After adding reductive agent for the last time, to observe with suction pipe sucking-off part plating bath, the blue nickel ammino in plating bath closes the ion color fade, becomes colorless, and plating bath stops to produce bubble fully simultaneously, is the plating reaction end, and the plating reaction finishes; Whole plating time is 15～80 minutes; Plating staticly settles and makes solid-liquid separation after finishing, and washes with water, behind the foreign ion of removal absorption, carries out drying treatment;
2) oxidation of coal gasification or carbonization
With the product after the plating, put into 300～500 ℃ retort furnace after 15～100 ℃ of oven dry, oxidation in 30 minutes, partial combustion is removed;
3) hydrogen is handled
Through the product of oxide treatment, enter the furnace reduction of hydrogen or ammonia pyrolysis gas protection, 600～1000 ℃ of reduction temperatures.
5. a kind of method for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball as claimed in claim 4 is characterized in that when the plating material was nanoparticle or fiber, the hydrogen treatment step carried out in fluidised hydrogen reduction furnace.
6. equipment for preparing hollow nanometer nickel, cobalt, nickel-cobalt fiber and hollow ball, it is characterized in that this equipment is made of agitator (1), thermometer (2), water bath with thermostatic control function unit (3), temperature-control heat couple (4), heater block (5), stirring in water bath device (6), plating bath device (7), funnel (8), water bath with thermostatic control function unit (3) by well heater (5) with water-bath and be immersed in plating bath device (7) pre-heating temperature elevation in the water-bath; Stirring in water bath device (6) makes equalizing temperature in the whole water-bath; Stirring in water bath device (6) rotating speed is 400～1500 rev/mins; Temperature-control heat couple (4) is measured bath temperature and bath temperature is stabilized on the design temperature point, and error is in ± 1 ℃; When temperature reach assigned temperature and constant after, will be the activatory plating piece be that the plating material joins in the plating bath device (7), stir by agitator (1), make plating liquid concentration homogenizing, agitator (1) rotating speed is 400～1200 rev/mins; The uninterrupted dropping of feed hopper (8) replenished reductive agent or pressed the additional reductive agent that adds of reaction requirement gradation.
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|---|---|---|---|
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|---|---|---|---|
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| CN101214444B (en) * | 2007-01-04 | 2010-04-21 | 北京有色金属研究总院 | Catalyst for sodium borohydride catalyzing hydrolyzation hydrogen supplying method and preparation thereof |
| CN101767205B (en) * | 2008-12-29 | 2011-06-08 | 宁波大学 | Preparation method of hollow nickel nanosphere |
| CN102309950A (en) * | 2010-07-01 | 2012-01-11 | 通用汽车环球科技运作有限责任公司 | Preparation has the nanostructured porous hollow ball of adjustable structure |
| CN102345232A (en) * | 2011-07-14 | 2012-02-08 | 北京工业大学 | Ferronickel alloy magnetic wood fiber and preparation method thereof |
| CN102983312A (en) * | 2012-11-28 | 2013-03-20 | 武汉工程大学 | Preparation method of composite fiber anode material of lithium-sulfur battery |
| CN104129818A (en) * | 2014-07-09 | 2014-11-05 | 奇瑞汽车股份有限公司 | Nickel-cobalt oxide material and preparation method thereof |
| CN105504276A (en) * | 2015-12-30 | 2016-04-20 | 西北工业大学 | Preparation method of polyaniline/nickel-coated carbon fiber composite wave absorbing material |
| CN110734116A (en) * | 2019-11-06 | 2020-01-31 | 中国天辰工程有限公司 | method for treating high-salt organic wastewater by electrodialysis |
| WO2020078302A1 (en) * | 2018-10-19 | 2020-04-23 | 洛阳尖端技术研究院 | Wave-absorbing material and preparation method therefor |
| CN114378291A (en) * | 2022-01-11 | 2022-04-22 | 金华职业技术学院 | Multi-cladding cobalt-coated carbon nanotube composite powder and preparation method thereof |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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| CN101214444B (en) * | 2007-01-04 | 2010-04-21 | 北京有色金属研究总院 | Catalyst for sodium borohydride catalyzing hydrolyzation hydrogen supplying method and preparation thereof |
| CN101767205B (en) * | 2008-12-29 | 2011-06-08 | 宁波大学 | Preparation method of hollow nickel nanosphere |
| CN102309950B (en) * | 2010-07-01 | 2014-09-17 | 通用汽车环球科技运作有限责任公司 | Making nanostructured porous hollow spheres with tunable structure |
| CN102309950A (en) * | 2010-07-01 | 2012-01-11 | 通用汽车环球科技运作有限责任公司 | Preparation has the nanostructured porous hollow ball of adjustable structure |
| CN102345232A (en) * | 2011-07-14 | 2012-02-08 | 北京工业大学 | Ferronickel alloy magnetic wood fiber and preparation method thereof |
| CN102345232B (en) * | 2011-07-14 | 2013-06-05 | 北京工业大学 | Ferronickel alloy magnetic wood fiber and preparation method thereof |
| CN102983312A (en) * | 2012-11-28 | 2013-03-20 | 武汉工程大学 | Preparation method of composite fiber anode material of lithium-sulfur battery |
| CN104129818A (en) * | 2014-07-09 | 2014-11-05 | 奇瑞汽车股份有限公司 | Nickel-cobalt oxide material and preparation method thereof |
| CN105504276A (en) * | 2015-12-30 | 2016-04-20 | 西北工业大学 | Preparation method of polyaniline/nickel-coated carbon fiber composite wave absorbing material |
| WO2020078302A1 (en) * | 2018-10-19 | 2020-04-23 | 洛阳尖端技术研究院 | Wave-absorbing material and preparation method therefor |
| CN110734116A (en) * | 2019-11-06 | 2020-01-31 | 中国天辰工程有限公司 | method for treating high-salt organic wastewater by electrodialysis |
| CN110734116B (en) * | 2019-11-06 | 2022-03-04 | 中国天辰工程有限公司 | Method for treating high-salinity organic wastewater through electrodialysis |
| CN114378291A (en) * | 2022-01-11 | 2022-04-22 | 金华职业技术学院 | Multi-cladding cobalt-coated carbon nanotube composite powder and preparation method thereof |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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