CN103894623B - A kind of preparation method of antioxidant ultrafine nickel powder - Google Patents
A kind of preparation method of antioxidant ultrafine nickel powder Download PDFInfo
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- CN103894623B CN103894623B CN201410102901.1A CN201410102901A CN103894623B CN 103894623 B CN103894623 B CN 103894623B CN 201410102901 A CN201410102901 A CN 201410102901A CN 103894623 B CN103894623 B CN 103894623B
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Abstract
The invention provides the preparation method of a kind of antioxidant ultrafine nickel powder.The method uses solution phase chemical reduction, using hydrazine hydrate with potassium borohydride as reducing agent, in the basic conditions extra-fine nickel powder is prepared in divalent nickel salt reduction, after reaction, separating, washing, vacuum drying, and pre-oxidation modification obtains the extra-fine nickel powder product of good in oxidation resistance at a certain temperature.Nickel powder product cut size prepared by the present invention is evenly distributed, initial oxidation temperature high, good dispersion, and preparation technology is simple, and production cost is low.
Description
Technical field
The present invention relates to 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.It prepares
Electrocondution slurry to have resistance weldering low, anti-good, without Ion transfer, linear, distinguishing and screen printability
Can well wait advantage.On the electronic devices and components that some use nickel metal conductive paste, its electrical property is the most excellent
In using precious metal material, such as:
(1) in multiple-layer sheet ceramic capacitor (MLCC), use sintrered nickel, copper slurry do interior electrode replace palladium and
Silver (Ag Pd) interior electrode, can make manufacturing cost decline about 70%, and improve the capacity of MLCC, reduces internal short
The occurrence probability on road, improves the reliability of product;
(2) in direct current plasma flat-panel monitor, silver electrode easily occurs sputtering to cause short circuit, and nickel is the most resistance to
The cathode material of Current Voltage bombardment, it will gradually replace silver electrode;
(3) in monocrystaline silicon solar cell, grid (sensitive surface) uses the silver electrode being doped with Ni powder, can make
Electrode forms Ohmic contact with silicon, improves the production efficiency of battery, and has good aging;
(4), after exothermic material Ni Cr slurry sintering, the resistance ratio non-operation of its operating conditions is the highest 1.5～2.0 times,
Favourable heater self controls power and increases, and extends the heater life-span.
Present in nickel based conductive slurry application at present, subject matter has:
1) point of incipient sintering of nickel powder is relatively low and non-oxidizability is poor；
2) in slurry sintering process, the shrinkage factor of nickel powder relatively ceramic medium material wants height, is susceptible to cracking.
By the Surface coating of nickel powder is processed, form protective cover layer, can effectively improve powder
Non-oxidizability and shrinkage, the most also make nickel powder in use keep good electric conductivity.Nickel powder
Cladding processes and generally can be divided into metallic cover and nonmetal-coated.Metallic cover mainly has silver cladding nickel powder, passes through
Electroplate process so that the non-oxidizability of nickel powder increases, be commonly used for conductive spacer, conducting filler and
Electrically-conducting paint etc..The method that nickel powder hydrolyzes has been obtained table in containing Ba Ti alkoxide by Hatano of Japan et al.
Bread covers the nickel powder of Ba Ti OH, is then passed through certain heat treatment, it is thus achieved that BaTiO3The nickel powder of cladding,
Making its oxidizing temperature improve nearly 200 DEG C, shrinkage temperature improves nearly 300 DEG C.
Nickel powder is first carried out oxidation processes and makes its surface contain layer oxide film by the old identical people of Central South University, then
Use NaBH4Reduction obtains Surface coating Ni2The powder of B, then through pre-oxidation treatment, it is thus achieved that non-oxidizability
Good NiBO system cladding nickel powder.But the initial oxidation temperature of its modified nickel powder improves 78 DEG C, and effect is not
Substantially, and complex process.
Summary of the invention
The preparation method of a kind of anti-oxidant nickel powder is the invention provides for above-mentioned deficiency.
The present invention uses hydrazine hydrate and NaBH4(or KBH4) complex reducing agent one step prepare the ultra-fine nickel of boracic
Powder, the more anti-oxidant nickel powder of Ni B O cladding is obtained through pre-oxidation treatment so that its initial oxidation temperature carries
High nearly 370 DEG C.The method comprises the steps:
1) prepare the divalent nickel salt aqueous solution, under stirring, add hydrazine hydrate, make divalent nickel salt and hydration
Hydrazine is complexed；
2) regulate above-mentioned 1 by NaOH or KOH solution) reaction solution pH to 11～13, add KBH4
Or NaBH4Solution makes nickelous by hydrazine hydrate and KBH4Or NaBH4Reduction generates Ni B powder；
3) separated by Ni B powder in reaction solution, be washed to neutrality, ethanol washes away moisture removal, and in vacuum
It is dried at 40～60 DEG C and processes；
4) dried Ni B powder is carried out pre-oxidation treatment and obtain the extra-fine nickel powder of Ni B O coating modification.
Wherein, divalent nickel salt described in step 1) is the one in nickel sulfate, nickel chloride, nickel nitrate, nickel acetate,
It is preferably nickel sulfate；Described, divalent nickel salt concentration in aqueous is 0.5～2.5mol/L；Described, water
The mass percent concentration closing hydrazine is preferably 80%；Hydrazine hydrate/nickel ion molar ratio is 2.5～10:1
Wherein, step 2) reaction temperature be 40～90 DEG C；Reaction time is 30～50min；Described NaOH
Or KOH solution mass percent concentration is 10%～50%, but it is not limited to this；Described KBH4Or NaBH4Molten
Liquid concentration is 0.1～2mol/L.
Wherein, described in step 4), Ni B powder pre-oxidation treatment temperature is 250 DEG C, preoxidation time be 30～
60min。
Specifically, the antioxidant ultrafine nickel powder preparation method of the present invention, its step is as follows:
1, compound concentration is the divalent nickel salt aqueous solution of 0.5～2.5mol/L, and nickel salt used is nickel sulfate, chlorination
One in nickel, nickel nitrate, nickel acetate, under stirring, adds the hydrazine hydrate that mass fraction is 80% molten
Liquid, hydrazine hydrate/nickel ion molar ratio is 2.5～10, complex reaction occurs, generates mauve nickel and hydration
The complex compound of hydrazine；
2, reaction solution is risen to 40～90 DEG C, with NaOH or KOH that mass percentage concentration is 10%～50%
Solution regulation pH value is to 11～13, and adds the KBH of 0.1～2mol/L4Or NaBH4Solution, nickel in solution
By hydrazine hydrate and KBH4Or NaBH4Reduction generates Ni B powder, stops after reaction 30～50min；
3, separated by Ni B powder in reaction solution, be washed to neutrality, ethanol washes away moisture removal, and in vacuum
It is dried at 40～60 DEG C and processes；
4, prepared ultra-fine Ni B powder pre-oxidation treatment 30～60min at 250 DEG C is obtained Ni B O
The extra-fine nickel powder product of coating modification.
Use merely NaBH4Doing nickel powder prepared by reducing agent is amorphous structure, and powder is easily reunited, no
Being suitable to the application in the fields such as electrocondution slurry, therefore, the present invention is preparing the reaction of nickel powder with hydrazine hydrate for reducing agent
On the basis of add boron hydride and do the Ni B cladding of nickel powder and process, and obtained by follow-up Technology for Heating Processing
The anti-oxidant nickel powder of boron cladding.
The technology of preparing of the anti-oxidant nickel powder that the present invention provides, boron-modified process, the initial oxidation temperature of nickel powder
Significantly improve, diameter of particle narrowly distributing, good dispersion, and use solution phase chemical reduction, it is easy to industrialization
Large-scale production.
Accompanying drawing explanation
Fig. 1 is prepared extra-fine nickel powder reference example sample thermal analysis curue in air atmosphere；
Fig. 2 is prepared boron modification antioxidant ultrafine nickel powder example 3 sample thermal analysis curue in air atmosphere；
Fig. 3 is the X-ray diffractogram of prepared antioxidant ultrafine nickel powder example 3 sample；
Fig. 4 is the scanning electron microscope (SEM) photograph of prepared antioxidant ultrafine nickel powder example 3 sample.
Detailed description of the invention
Following example further illustrate present disclosure, but should not be construed as limitation of the present invention.Not
In the case of deviating from present invention spirit and essence, the amendment that the inventive method, step or condition are made or replacement,
Belong to the scope of the present invention.
If not specializing, the conventional hand that technological means used in embodiment is well known to those skilled in the art
Section.
Embodiment 1
Weighing 42.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, makees in stirring
Under with, dropping 60g mass fraction is the hydrazine hydrate complexing of 80%, and temperature rises to 80 DEG C, and preparation quality is dense
Degree is the NaOH solution regulation pH to 11 of 30%, and drips the KBH that concentration is 0.8mol/L4Solution, instead
Answer and stop after 30min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 50 DEG C, be dried
After take synthesized Ni B powder and grind fully, ground nickel powder is pre-oxidized at 250 DEG C 40min and obtains boron
Modified anti-oxidant nickel powder.
After testing, in prepared nickel powder, boron mass fraction is 0.45%, hot analysis result display boron modification nickel powder
Initial oxidation temperature is 405 DEG C.
Embodiment 2
Weighing 63.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, makees in stirring
Under with, dropping 68g mass fraction is the hydrazine hydrate complexing of 80%, and temperature rises to 70 DEG C, and preparation quality is dense
Degree is the NaOH solution regulation pH to 12.5 of 10%, and drips the KBH that concentration is 0.9mol/L4Solution,
Stop after reaction 30min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 50 DEG C, dry
Take synthesized Ni B powder after dry to grind fully, ground nickel powder is pre-oxidized at 250 DEG C 40min
Obtain the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 0.7%, hot analysis result display boron modification nickel powder
Initial oxidation temperature is 530 DEG C.
Embodiment 3
Weighing 78.8g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, makees in stirring
Under with, dropping 76g mass fraction is the hydrazine hydrate complexing of 80%, and temperature rises to 60 DEG C, and preparation quality is dense
Degree is the NaOH solution regulation pH to 12 of 50%, and drips the KBH that concentration is 1.0mol/L4Solution, instead
Answer and stop after 40min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 50 DEG C, be dried
After take synthesized Ni B powder and grind fully, ground nickel powder is pre-oxidized at 250 DEG C 40min and obtains boron
Modified anti-oxidant nickel powder.
After testing, in prepared nickel powder, boron mass fraction is 1.2%, and heat is analyzed testing result and shown this boron modification
The initial oxidation temperature of nickel powder is 670 DEG C.
Embodiment 4
Weighing 105.1g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, in stirring
Under effect, dropping 76g mass fraction is the hydrazine hydrate complexing of 80%, temperature rises to 50 DEG C, prepares quality
Concentration is the NaOH solution regulation pH to 12 of 50%, and drips the KBH that concentration is 1.2mol/L4Solution,
Stop after reaction 40min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 60 DEG C, dry
Take synthesized Ni B powder after dry to grind fully, ground nickel powder is pre-oxidized at 250 DEG C 30min
Obtain the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.1%, and heat is analyzed test result and shown this boron modification
The initial oxidation temperature of nickel powder is 617 DEG C.
Embodiment 5
Weighing 120.9g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, in stirring
Under effect, dropping 87g mass fraction is the hydrazine hydrate complexing of 80%, temperature rises to 45 DEG C, prepares quality
Concentration is the NaOH solution regulation pH to 12.5 of 50%, and drips the KBH that concentration is 1.3mol/L4Solution,
Stop after reaction 40min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 60 DEG C, dry
Take synthesized Ni B powder after dry to grind fully, ground nickel powder is pre-oxidized at 250 DEG C 30min
Obtain the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.6%, and heat is analyzed test result and shown this boron modification
The initial oxidation temperature of nickel powder is 649 DEG C.
Embodiment 6
Weighing 71.3g Nickel dichloride hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, in stirring
Under effect, dropping 75g mass fraction is the hydrazine hydrate complexing of 80%, temperature rises to 60 DEG C, prepares quality
Concentration is the NaOH solution regulation pH to 12.5 of 50%, and drips the KBH that concentration is 1.3mol/L4Solution,
Stop after reaction 40min, separate, be washed to neutrality, ethanol is vacuum dried 12h after washing at 60 DEG C, dry
Take synthesized Ni B powder after dry to grind fully, ground nickel powder is pre-oxidized at 250 DEG C 30min
Obtain the anti-oxidant nickel powder of boron modification.
After testing, in prepared nickel powder, boron mass fraction is 1.2%, and heat is analyzed test result and shown this boron modification
The initial oxidation temperature of nickel powder is 641 DEG C.
Comparison example
Weighing 78.8g nickel sulfate hexahydrate, preparation 200ml nickel sulfate solution adds in there-necked flask, makees in stirring
Under with, dropping 76g mass fraction is the hydrazine hydrate complexing of 80%, and temperature rises to 60 DEG C, and preparation quality is dense
Degree be 50% NaOH solution regulation pH to 12, reaction 40min after stop, separating, be washed to neutrality,
Ethanol is vacuum dried 12h after washing at 50 DEG C, obtains pure nickel powder reference sample.
In comparison example in addition to adulterating without boron, other response parameter is identical with example 3, comparison example and example 3
The hot analysis result of nickel powder sample as shown in Figure 1 and Figure 2, is analyzed test result, comparison example institute from heat
The pure nickel powder sample initial oxidation temperature of preparation is about 297 DEG C, and terminating oxidizing temperature is 521 DEG C, and embodiment
The initial oxidation temperature of the anti-oxidant nickel powder sample of boron modification prepared by 3 is about 670 DEG C, terminates oxidizing temperature and is
947 DEG C, boron modification nickel powder relatively pure nickel powder non-oxidizability significantly improves.Fig. 3 is that the X-ray of example 3 sample is spread out
Penetrating collection of illustrative plates, contrast standard PDF card understands, the predominantly diffraction maximum of nickel, and crystallinity is good, also B2O3
Peak, there is no the peak of nickel oxide.Fig. 4 is the scanning electron microscope image of example 3 sample, contrasts several visual field
In boron modification nickel powder particle, particle size is uniform, and narrow distribution has good dispersiveness.
Claims (10)
1. a preparation method for antioxidant ultrafine nickel powder, it concretely comprises the following steps:
1) prepare the divalent nickel salt aqueous solution, under stirring, add hydrazine hydrate, make divalent nickel salt and hydrazine hydrate network
Close；
2) regulate above-mentioned 1 by NaOH or KOH solution) reaction solution pH to 12～13, add KBH4Or
NaBH4Solution makes nickelous by hydrazine hydrate and KBH4Or NaBH4Reduction generates Ni B powder；
3) separated by Ni B powder in reaction solution, be washed to neutrality, ethanol washes away moisture removal, and in vacuum 40～
It is dried at 60 DEG C and processes；
4) dried Ni B powder is carried out pre-oxidation treatment and obtain the extra-fine nickel powder of Ni B O coating modification.
Preparation method the most according to claim 1, it is characterised in that described divalent nickel salt is in aqueous
Concentration is 0.5～2.5mol/L.
Preparation method the most according to claim 1, described divalent nickel salt be nickel sulfate, nickel chloride, nickel nitrate,
One in nickel acetate.
Preparation method the most according to claim 1, it is characterised in that wherein step 1) hydrazine hydrate/nickel ion
Molar ratio is 2.5～10:1.
Preparation method the most according to claim 1, it is characterised in that wherein the mass percent of hydrazine hydrate is dense
Degree is 80%.
6. according to the preparation method described in any one of Claims 1 to 5, it is characterised in that wherein step 2) anti-
Answering temperature is 40～90 DEG C, and the reaction time is 30～50min.
7. according to the preparation method described in any one of Claims 1 to 5, it is characterised in that wherein step 2) described
NaOH or KOH solution mass percent concentration are 10%～50%.
8. according to the preparation method described in any one of Claims 1 to 5, it is characterised in that wherein step 2) described
KBH4Or NaBH4Solution concentration is 0.1～2mol/L.
9. according to the preparation method described in any one of Claims 1 to 5, it is characterised in that wherein step 4), described
Ni B powder pre-oxidation treatment temperature is 250 DEG C, and preoxidation time is 30～60min.
10. the antioxidant ultrafine nickel powder that prepared by method described in any one of claim 1～9.
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| CN104439278B (en) * | 2014-11-28 | 2017-03-15 | 深圳康特腾科技有限公司 | A kind of preparation method of nanometer spherical nikel powder |
| CN108311710B (en) * | 2018-02-28 | 2021-02-09 | 深圳市航天新材科技有限公司 | Preparation method of monodisperse antioxidant nano-scale nickel powder |
| CN110246605B (en) * | 2019-05-06 | 2021-01-12 | 深圳航天科技创新研究院 | Anti-oxidation conductive paste composition, conductive coating and preparation method of conductive coating |
| CN110340376B (en) * | 2019-07-16 | 2020-11-13 | 浙江大学 | Flower-shaped nickel wire wave-absorbing material and preparation method thereof |
| 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 |
| CN113270270B (en) * | 2021-05-27 | 2022-04-05 | 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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| US7648556B2 (en) * | 2006-04-11 | 2010-01-19 | Samsung Electro-Mechanics Co., Ltd. | Method for manufacturing nickel nanoparticles |
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| CN1426865A (en) * | 2001-12-19 | 2003-07-02 | 北京有色金属研究总院 | Method of preparing nano metal nickel powder |
| CN101041180A (en) * | 2007-04-28 | 2007-09-26 | 北京有色金属研究总院 | Nanometer Al contained Ni and the preparing method |
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