CN103894623A - Preparing method of antioxidant super-fine nickel powder - Google Patents
Preparing method of antioxidant super-fine nickel powder Download PDFInfo
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Abstract
The invention provides a preparing method of antioxidant super-fine nickel powder. In the method, the liquid phase chemical reduction method is adopted, hydrazine hydrate and potassium borohydride are used as reducing agents, nickelous salt is reduced under the alkaline condition to prepare the super-fine nickel powder, separation, washing and vacuum drying are conducted after reaction, and pre-oxidation and modification processing are conducted so as to obtain the super-fine nickel powder which is good in inoxidizability under a certain temperature. The particle diameters of the prepared nickel powder are even, primary oxidizing temperature is high, dispersibility is good, a preparing technology is simple, and production cost is low.
Description
Technical field
What the present invention relates to is extra-fine nickel powder preparing technical field, particularly antioxidant ultrafine nickel powder preparation method.
Background technology
In base metal, metallic nickel possesses good electric conductivity, chemical stability, solderability and soldering resistance.Its electrocondution slurry making have low, the anti-weldering of resistance good, without advantages such as ion migration, linear, distinguishing and serigraphy are functional.Use on the electronic devices and components of nickel metal conductive paste at some, its electrical property will obviously be better than using precious metal material, as:
(1) in multiple-layer sheet ceramic capacitor (MLCC); use sintrered nickel, copper slurry to do interior electrode and replace the interior electrode of palladium and silver (Ag ?Pd), can make manufacturing cost decline approximately 70%, and improve the capacity of MLCC; reduce the occurrence probability of internal short-circuit, improve the reliability of product;
(2) in direct current plasma flat-panel monitor, easily there is sputter and cause short circuit in silver electrode, and nickel is the cathode material of strong resistance to current/voltage bombardment, and it will replace silver electrode gradually;
(3) in monocrystaline silicon solar cell, grid (sensitive surface) adopts the silver electrode of the Ni powder that adulterated, and can make electrode and silicon form Ohmic contact, improves the production efficiency of battery, and has good aging;
(4) exothermic material Ni ?after Cr slurry sintering, the resistance ratio non-operation of its operating conditions is approximately high 1.5～2.0 times, favourable heater self power ratio control increases, and extends the heater life-span.
The subject matter existing in nickel based conductive slurry application at present has:
1) point of incipient sintering of nickel powder is lower poor with non-oxidizability;
2), in slurry sintering process, the shrinkage factor of nickel powder wants high compared with ceramic medium material, easily ftractures.
By processing the surface of nickel powder is coated, form protective cover layer, can effectively improve non-oxidizability and the shrinkage of powder, also make nickel powder in use keep good electric conductivity simultaneously.The coated processing of nickel powder generally can be divided into metallic cover and nonmetal-coated.Metallic cover mainly contains the coated nickel powder of silver, by electroplate processing, the non-oxidizability of nickel powder is increased, and is commonly used for conductive spacer, conducting filler and electrically-conducting paint etc.The people such as Hatano of Japan by nickel powder by the method for hydrolysis containing the nickel powder that has obtained surperficial coated Ba ?Ti ?OH in Ba ?Ti alkoxide, then pass through certain heat treatment, obtained BaTiO
3coated nickel powder, makes its oxidizing temperature improve nearly 200 ℃, and shrinkage temperature has improved nearly 300 ℃.
The old identical people of Central South University first carries out nickel powder oxidation processes and makes its surface contain layer oxide film, then adopts NaBH
4reduction obtains the coated Ni in surface
2the powder of B, then through pre-oxidation treatment, obtains the coated nickel powder of NiBO system of good in oxidation resistance.But after its modification, the initial oxidation temperature of nickel powder has improved 78 ℃, DeGrain, and complex process.
Summary of the invention
The invention provides a kind of preparation method of anti-oxidant nickel powder for above-mentioned deficiency.
The present invention adopts hydrazine hydrate and NaBH
4(or KBH
4) complex reducing agent one step prepare boracic extra-fine nickel powder, then through pre-oxidation treatment obtain Ni ?B ?the coated anti-oxidant nickel powder of O, make its initial oxidation temperature improve nearly 370 ℃.The method comprises the steps:
1) prepare the divalent nickel salt aqueous solution, under stirring action, add hydrazine hydrate, make divalent nickel salt and hydrazine hydrate complexing;
2) regulate above-mentioned 1 with NaOH or KOH solution) reaction solution pH to 11～13, add KBH
4or NaBH
4solution makes nickelous be hydrated hydrazine and KBH
4or NaBH
4reduction generate Ni ?B powder;
3) Ni ?B powder in reaction solution separated, be washed to neutrality, ethanol washes away except moisture, and at 40～60 ℃, vacuum dry processing;
4) by dried Ni ?B powder carry out pre-oxidation treatment obtain Ni ?B ?the extra-fine nickel powder of the coated modification of O.
Wherein, divalent nickel salt is the one in nickelous sulfate, nickel chloride, nickel nitrate, nickel acetate described in step 1), is preferably nickelous sulfate; Described, the concentration of divalent nickel salt in the aqueous solution is 0.5～2.5mol/L; Described, the mass percent concentration of hydrazine hydrate is preferably 80%; Hydrazine hydrate/nickel ion molar ratio is 2.5～10:1
Wherein, step 2) reaction temperature be 40～90 ℃; Reaction time is 30～50min; Described NaOH or KOH solution quality percent concentration are 10%～50%, but are not limited to this; Described KBH
4or NaBH
4solution concentration is 0.1～2mol/L.
Wherein, described in step 4) Ni ?B powder pre-oxidation treatment temperature be 250 ℃, preoxidation time is 30～60min.
Particularly, antioxidant ultrafine nickel powder preparation method of the present invention, its step is as follows:
1, the divalent nickel salt aqueous solution that compound concentration is 0.5～2.5mol/L, nickel salt used is the one in nickelous sulfate, nickel chloride, nickel nitrate, nickel acetate, under stirring action, adding mass fraction is 80% hydrazine hydrate solution, hydrazine hydrate/nickel ion molar ratio is 2.5～10, there is complex reaction, generate the complex compound of mauve nickel and hydrazine hydrate;
2, reaction solution is risen to 40～90 ℃, the NaOH that is 10%～50% by mass percentage concentration or KOH solution regulate pH value to 11～13, and add the KBH of 0.1～2mol/L
4or NaBH
4solution, in solution, nickel is hydrated hydrazine and KBH
4or NaBH
4reduction generate Ni ?B powder, reaction stops after 30～50min;
3, Ni ?B powder in reaction solution separated, be washed to neutrality, ethanol washes away except moisture, and at 40～60 ℃, vacuum dry processing;
4, by prepared ultra-fine Ni ?B powder pre-oxidation treatment 30～60min at 250 ℃ obtain Ni ?B ?the extra-fine nickel powder product of the coated modification of O.
The simple NaBH that adopts
4doing nickel powder prepared by reducing agent is amorphous structure, and powder is easily reunited, be unsuitable for the application in the fields such as electrocondution slurry, therefore, the present invention adds boron hydride and does coated processing of Ni ?B of nickel powder on the reaction basis of preparing nickel powder take hydrazine hydrate as reducing agent, and obtains the coated anti-oxidant nickel powder of boron by follow-up Technology for Heating Processing.
The technology of preparing of anti-oxidant nickel powder provided by the invention, through boron modification, the initial oxidation temperature of nickel powder obviously improves, diameter of particle narrowly distributing, good dispersion, and adopt liquid phase chemical reduction method, be easy to large-scale industrialization and produce.
Accompanying drawing explanation
Fig. 1 is the thermal analysis curue of prepared extra-fine nickel powder reference example sample under air atmosphere;
Fig. 2 is the thermal analysis curues of prepared boron modification antioxidant ultrafine nickel powder example 3 samples under air atmosphere;
Fig. 3 is the X-ray diffractogram of prepared antioxidant ultrafine nickel powder example 3 samples;
Fig. 4 is the scanning electron microscope (SEM) photograph of prepared antioxidant ultrafine nickel powder example 3 samples.
The specific embodiment
Following examples further illustrate content of the present invention, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, the modification that the inventive method, step or condition are done or replacement, all belong to scope of the present invention.
If do not specialize, the conventional means that in embodiment, technological means used is well known to those skilled in the art.
Embodiment 1
Take 42.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 60g mass fraction is 80%, temperature is risen to 80 ℃, and the NaOH solution that preparation mass concentration is 30% regulates pH to 11, and drips the KBH that concentration is 0.8mol/L
4solution, reaction stops after 30min, after separating, be washed to neutrality, ethanol and washing at 50 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 40min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 0.45%, and hot analysis result shows that the initial oxidation temperature of boron modification nickel powder is 405 ℃.
Embodiment 2
Take 63.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 68g mass fraction is 80%, temperature is risen to 70 ℃, the NaOH solution that preparation mass concentration is 10% regulates pH to 12.5, and drips the KBH that concentration is 0.9mol/L
4solution, reaction stops after 30min, after separating, be washed to neutrality, ethanol and washing at 50 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 40min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 0.7%, and hot analysis result shows that the initial oxidation temperature of boron modification nickel powder is 530 ℃.
Embodiment 3
Take 78.8g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 76g mass fraction is 80%, temperature is risen to 60 ℃, and the NaOH solution that preparation mass concentration is 50% regulates pH to 12, and drips the KBH that concentration is 1.0mol/L
4solution, reaction stops after 40min, after separating, be washed to neutrality, ethanol and washing at 50 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 40min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.2%, and hot analyzing and testing result shows that the initial oxidation temperature of this boron modification nickel powder is 670 ℃.
Embodiment 4
Take 105.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 76g mass fraction is 80%, temperature is risen to 50 ℃, and the NaOH solution that preparation mass concentration is 50% regulates pH to 12, and drips the KBH that concentration is 1.2mol/L
4solution, reaction stops after 40min, after separating, be washed to neutrality, ethanol and washing at 60 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 30min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.1%, and hot analytical test result shows that the initial oxidation temperature of this boron modification nickel powder is 617 ℃.
Embodiment 5
Take 120.9g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 87g mass fraction is 80%, temperature is risen to 45 ℃, the NaOH solution that preparation mass concentration is 50% regulates pH to 12.5, and drips the KBH that concentration is 1.3mol/L
4solution, reaction stops after 40min, after separating, be washed to neutrality, ethanol and washing at 60 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 30min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.6%, and hot analytical test result shows that the initial oxidation temperature of this boron modification nickel powder is 649 ℃.
Embodiment 6
Take 71.3g Nickel dichloride hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 75g mass fraction is 80%, temperature is risen to 60 ℃, the NaOH solution that preparation mass concentration is 50% regulates pH to 12.5, and drips the KBH that concentration is 1.3mol/L
4solution, reaction stops after 40min, after separating, be washed to neutrality, ethanol and washing at 60 ℃ vacuum drying 12h, get after dry synthesized Ni ?B powder grind fully, ground nickel powder pre-oxidation 30min at 250 ℃ is obtained to the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.2%, and hot analytical test result shows that the initial oxidation temperature of this boron modification nickel powder is 641 ℃.
Comparison example
Take 78.8g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, under stirring action, drip the hydrazine hydrate complexing that 76g mass fraction is 80%, temperature is risen to 60 ℃, and the NaOH solution that preparation mass concentration is 50% regulates pH to 12, after reaction 40min, stops, after separating, being washed to neutrality, ethanol and washing at 50 ℃ vacuum drying 12h, obtain pure nickel powder reference sample.
In comparison example except without boron doping, other response parameter is identical with example 3, the hot analysis result of comparison example and example 3 nickel powder samples as shown in Figure 1 and Figure 2, from hot analytical test result, the prepared pure nickel powder sample initial oxidation temperature of comparison example is about 297 ℃, stopping oxidizing temperature is 521 ℃, and the initial oxidation temperature of the anti-oxidant nickel powder sample of the prepared boron modification of embodiment 3 is about 670 ℃, stopping oxidizing temperature is 947 ℃, and boron modification nickel powder obviously improves compared with pure nickel powder non-oxidizability.Fig. 3 is the X ray diffracting spectrum of example 3 samples, and contrast standard PDF card is known, is mainly the diffraction maximum of nickel, and crystallinity is good, also has B
2o
3peak, there is no the peak of nickel oxide.Fig. 4 is the scanning electron microscope image of example 3 samples, contrasts the boron Modified Nickel powder particles in several visuals field, and particle size is even, and narrow distribution has good dispersiveness.
Claims (10)
1. a preparation method for antioxidant ultrafine nickel powder, its concrete steps are:
1) prepare the divalent nickel salt aqueous solution, under stirring action, add hydrazine hydrate, make divalent nickel salt and hydrazine hydrate complexing;
2) regulate above-mentioned 1 with NaOH or KOH solution) reaction solution pH to 11～13, add KBH
4or NaBH
4solution make nickelous be hydrated hydrazine and KBH4 or NaBH4 reduction generate Ni ?B powder;
3) Ni ?B powder in reaction solution separated, be washed to neutrality, ethanol washes away except moisture, and at 40～60 ℃, vacuum dry processing;
4) by dried Ni ?B powder carry out pre-oxidation treatment obtain Ni ?B ?the extra-fine nickel powder of the coated modification of O.
2. preparation method according to claim 1, is characterized in that, the concentration of described divalent nickel salt in the aqueous solution is 0.5～2.5mol/L.
3. preparation method according to claim 1, described divalent nickel salt is the one in nickelous sulfate, nickel chloride, nickel nitrate, nickel acetate.
4. preparation method according to claim 1, is characterized in that, wherein step 1) hydrazine hydrate/nickel ion molar ratio is 2.5～10:1.
5. preparation method according to claim 1, is characterized in that, wherein the mass percent concentration of hydrazine hydrate is 80%.
6. according to the preparation method described in claim 1～5 any one, it is characterized in that, wherein step 2) reaction temperature be 40～90 ℃, the reaction time is 30～50min.
7. according to the preparation method described in claim 1～5 any one, it is characterized in that, wherein step 2) described NaOH or KOH solution quality percent concentration be 10%～50%.
8. according to the preparation method described in claim 1～5 any one, it is characterized in that, wherein step 2) described KBH
4or NaBH
4solution concentration is 0.1～2mol/L.
9. according to the preparation method described in claim 1～5 any one, it is characterized in that, wherein step 4), described Ni ?B powder pre-oxidation treatment temperature be 250 ℃, preoxidation time is 30～60min.
10. the antioxidant ultrafine nickel powder that described in claim 1～9 any one prepared by method.
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Cited By (7)
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|---|---|---|---|---|
| CN104439278A (en) * | 2014-11-28 | 2015-03-25 | 深圳康特腾科技有限公司 | Method for preparing nanometer spherical nickel powder |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110246605A (en) * | 2019-05-06 | 2019-09-17 | 深圳航天科技创新研究院 | A kind of anti-oxidative conductive paste composition and conductive coating and preparation method thereof |
| CN110340376A (en) * | 2019-07-16 | 2019-10-18 | 浙江大学 | A kind of flower-shaped nickel wire absorbing material and preparation method thereof |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN113270270A (en) * | 2021-05-27 | 2021-08-17 | 广东省先进陶瓷材料科技有限公司 | Anti-oxidation nickel slurry and preparation method and application thereof |
| WO2022137691A1 (en) * | 2020-12-23 | 2022-06-30 | 三井金属鉱業株式会社 | Nickel powder, method for producing same, conductive composition, and conductive film |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104439278A (en) * | 2014-11-28 | 2015-03-25 | 深圳康特腾科技有限公司 | Method for preparing nanometer spherical nickel powder |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110246605A (en) * | 2019-05-06 | 2019-09-17 | 深圳航天科技创新研究院 | A kind of anti-oxidative conductive paste composition and conductive coating and preparation method thereof |
| CN110340376A (en) * | 2019-07-16 | 2019-10-18 | 浙江大学 | A kind of flower-shaped nickel wire absorbing material and preparation method thereof |
| CN110340376B (en) * | 2019-07-16 | 2020-11-13 | 浙江大学 | Flower-shaped nickel wire wave-absorbing material and preparation method thereof |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN111653768B (en) * | 2020-05-25 | 2023-03-24 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| WO2022137691A1 (en) * | 2020-12-23 | 2022-06-30 | 三井金属鉱業株式会社 | Nickel powder, method for producing same, conductive composition, and conductive film |
| CN113270270A (en) * | 2021-05-27 | 2021-08-17 | 广东省先进陶瓷材料科技有限公司 | Anti-oxidation nickel slurry and preparation method and application thereof |
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