CN103691931B - The anti-oxidation method of moisture level process metal nickel powder - Google Patents
The anti-oxidation method of moisture level process metal nickel powder Download PDFInfo
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- CN103691931B CN103691931B CN201310690780.2A CN201310690780A CN103691931B CN 103691931 B CN103691931 B CN 103691931B CN 201310690780 A CN201310690780 A CN 201310690780A CN 103691931 B CN103691931 B CN 103691931B
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Abstract
The present invention discloses a kind of anti-oxidation method of moisture level process metal nickel powder, step comprises: add antioxidant TX-02 in deionized water, be stirred to antioxidant to dissolve completely, being mixed with antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.1-2%, controls this corrosion inhibiting solution pH within the scope of 7-8; Above-mentioned antioxidant TX-02 by carbohydrazide and citric acid according to weight ratio for (1-3:1) mixes and obtains; Unassorted metal nickel powder is added to fill mass concentration prepared by step (1) be in the emulsifying device of the corrosion inhibiting solution of 0.1-2%, be mixed with the nickel powder slip that solid content is 10-25%; Start emulsifying device, emulsification nickel powder slip 20-50min, the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed; After emulsification, nickel powder slip after filtering, sends into hierarchy system classification.Method of the present invention has the advantage that in water classification process, metal-powder is not easily corroded, is oxidized.
Description
Technical field:
The present invention is a kind of metal powder moisture level anti-oxidation tech field, is specifically related to a kind of anti-oxidation method of moisture level process metal nickel powder.
Background technology:
The sub-micron-sized metal nickel powder that PVD method is produced, diameter of particle size is uneven, can not directly be used in MLCC industry, needs, through classification process, to obtain the powder of even particle size distribution.In known sub-micron-sized metal nickel powder grading technology, in liquid phase stage division, be medium mainly with alcohols, conventional solvent medium has the alcohols such as ethanol, propyl alcohol.Such as ethanol other organic solvents relatively, light specific gravity, viscosity is also little, and classification was imitated good, and raw material is easy to get.Classification processing procedure powder surface is long-pending, oxygen content change is little, stable performance.But ethanol belongs to volatile product, classification process, ethanol is under the high speed machine motion of centrifugal pump impeller, and produce a large amount of heat, the mutual collision of metal nickel powder particle also produces a large amount of heat energy, ethanol temperature is raised, accelerates ethanol evaporation.Because ethanol is expensive, a large amount of ethanol of classification process consumption, increases nickel powder classification cost.Through statistics, in nickel powder classification production process, ethanol consumption accounts for more than 50% of classification cost.
Ethanol is again inflammable thing simultaneously, and classification process, under the mechanical movement of water pump, producing a large amount of heat energy makes ethanol temperature raise, and ethanol evaporates in a large number, and in working environment, ethanol vapor concentration is too high, close to combustion explosion easy during the limit, there is great potential safety hazard as nickel powder classification medium in ethanol.
Adopt water consumption substitution ethanol as nickel powder classification medium, be not only economical and but also one of the production method of safety, but what adopt in moisture level method is industrial deionized water, in classification process, metal-powder soaks for a long time in water, with the dissolved oxygen generation oxidation reaction in water, causes the metal nickel powder oxidized corrosion in surface, form small scraggly surface, metal nickel powder surface area is increased.When detecting specific area calculating nickel powder particle diameter by BET method, larger with actual particle size sheet difference.Nickel powder surface relief is uneven, and between particle, frictional force is large, causes nickel powder to increase in pulping process viscosity, affects slurrying and produces.Metal-powder soaks in water, and nickel powder is oxidized, and oxygen content increases.Nickel powder also can occur and manufacturing capacitor sintering process generation cracking phenomena, therefore, the problem solving metal-powder burn into oxidation in liquid phase water stage division is crucial.
Summary of the invention:
The present invention is directed to the above-mentioned deficiency of prior art, the anti-oxidation method of the moisture level process metal nickel powder provide metal-powder in a kind of water classification process to be not easily corroded, being oxidized.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of anti-oxidation method of moisture level process metal nickel powder, and step comprises:
(1) add antioxidant TX-02 in deionized water, be stirred to antioxidant and dissolve completely, being mixed with antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.1-2%, controls this corrosion inhibiting solution pH within the scope of 7-8; Above-mentioned antioxidant TX-02 by carbohydrazide and citric acid according to weight ratio for (1-3:1) mixes and obtains;
(2) unassorted metal nickel powder is added to fill mass concentration prepared by step (1) be in the emulsifying device of the corrosion inhibiting solution of 0.1-2%, be mixed with the nickel powder slip that solid content is 10-25%;
(3) emulsifying device is started, the nickel powder slip 20-50min of emulsifying step (2), the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip after filtering, sends into hierarchy system classification.
Unassorted metal nickel powder described in step of the present invention (2) is the standby submicron particle of PVD legal system.
As preferably, the corrosion inhibiting solution described in step of the present invention (1) is antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.2%.
As preferably, the solid content being mixed with nickel powder slip described in step of the present invention (2) is 20%.
As preferably, the emulsification nickel powder slip emulsification times described in step of the present invention (3) is 30min.
Classification metal nickel powder of the present invention adopts liquid phase wet classification, is specially described hierarchy system by surge tank, centrifugal pump, cyclone hydraulic separators, and receiving vat forms; Classification process is: by step (4) emulsification, sieve after solid content be that the nickel powder slip of 10-25% delivers to surge tank, by centrifugal pump under 1.0-1.5MPa pressure, squeeze in cyclone hydraulic separators and carry out centrifugal classification, remove super large particle, from the overfall of cyclone hydraulic separators, obtain the powder of even particle size distribution, the temperature of institute of the present invention classification processing procedure is carried out at normal temperature condition.Above-mentioned hierarchy system classification process is industry conventional hierarchical processing procedure.
Advantage of the present invention and beneficial effect:
1. superfine metal nickel powder of the present invention is in moisture level processing procedure, adds composite antioxidant TX-02(carbohydrazide, the citric acid of preparation in classification deionized water used), be mixed with certain proportion corrosion inhibiting solution.This composite antioxidant TX-02 has strong reducing property, with the dissolved oxygen generation redox reaction in the aqueous solution, consumes the oxygen in water, and reaction generates nitrogen and carbon dioxide is discharged, and reduces the dissolved oxygen content in solution; On the other hand corrosion inhibiting solution can form passivating film on metal nickel powder surface, and the dissolved oxygen in isolated solution to the oxidation of metal nickel powder, thus reaches the oxidation that slows down metal nickel powder and plays the effect on protection metal nickel powder surface.Therefore, method of the present invention solves industrial deionized water classification nickel powder and is corroded, and surface relief is uneven, and surface area becomes large, and between particle, frictional force is large, and pulping process viscosity increases problem; Also solve nickel powder classification process oxidized, oxygen content increases, and nickel powder occurs in the phenomenon manufacturing capacitor sintering process generation cracking.
2. antioxidant TX-02 raw material of the present invention is easy to get, safety non-toxic, and stage solution is antioxidant TX-02(carbohydrazide, citric acid) corrosion inhibiting solution that is mixed with, adopt deionized water preparation, raw material is easy to get, price is low, and production process is safe, pollution-free; Composite antioxidant TX-02(carbohydrazide used, citric acid) be organic compound, not metal ion, classification processing procedure, can not generate metal salt compound, therefore not consume metal nickel powder; Composite antioxidant TX-02(carbohydrazide used, citric acid) react with oxygen in water, consume oxygen in water, classification processing procedure, does not produce insoluble precipitate, has deaerating effect good, metallic nickel powder good in oxidation resistance, oxygen content change is little, and metallic nickel powder corrosion resistance is good, and nickel powder surface is round and smooth, surface area change is little, avoids nickel powder in the advantage manufacturing capacitor sintering process generation cracking phenomena.
3. the present invention carries out classification after nickel powder slurry is carried out emulsification treatment again, and nickel powder is fully uniformly dispersed in the slurry, do not reunite, do not unite, be therefore more easily separated in follow-up classification process, grading effect is good; And in the corrosion inhibiting solution that is mixed with at antioxidant TX-02 of abundant scattered nickel powder, each dispersion nickel powder particle all fully can be contacted with antioxidant TX-02, therefore, antioxidant effect is better.After emulsification, nickel powder slip after filtration, to remove the nickel powder of larger particles, makes subsequent hierarchical process more smooth.
Detailed description of the invention:
Below in conjunction with example, the present invention is further described.
Embodiment
(1) preparation of corrosion inhibiting solution: add carbohydrazide that weight ratio is 3:1 in deionized water, antioxidant TX-02 that citric acid mixture is formed, be stirred to antioxidant TX-02 to dissolve completely, being mixed with antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.2%, controls this corrosion inhibiting solution pH within the scope of 7-8;
(2) mass concentration prepared by step (1) is in the emulsifying device of the corrosion inhibiting solution of 0.2% to utilize conveyer to be added by unassorted metal nickel powder, and the volume of emulsifying device is 250L, is mixed with the nickel powder slip that solid content is 25%;
(3) start emulsifying device, emulsifying device power is 15kw, and rotating speed is 2900rpm, emulsification nickel powder slip 30min, the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip filters through 600 order vibratory sieves, removes in raw material slurry the agglomerate, foreign matter etc. that are greater than more than 30 microns, avoids blocking cyclone hydraulic separators during classification;
(5) hierarchy system is by surge tank (600L), centrifugal pump (15KW), cyclone hydraulic separators, and receiving vat (100L) forms, and is industry conventional equipment;
(6) emulsification, sieve after solid content be 20% nickel powder slip deliver to surge tank, by centrifugal pump under 1.0-1.5MPa pressure, squeeze in cyclone hydraulic separators and carry out centrifugal classification, remove super large particle, from overflow, obtain the powder of even particle size distribution.
Nickel powder slip carries out classification in the corrosion inhibiting solution adding composite antioxidant, and classification process temperature is carried out at normal temperatures.
Nickel powder slip is classified as the slip of different grain size distribution in hierarchy system, and the overflow slurry after classification, after SEM/BET/PSD etc. detects requirement up to specification mutually, enters in drying system and carries out drying.
Table 1:
| Grading technology | BET(m2/g) | Particle diameter (nm) | Oxygen (ppm) | Oxygen rate of change % |
| Before the non-classification of nickel powder | 2.46 | 274 | 5719 | |
| After the classification of nickel powder pure water | 2.49 | 271 | 8131 | 42.1 |
| After the classification of nickel powder oxidation resistance liquid | 2.24 | 301 | 5991 | 4.7 |
By the nickel powder Data Detection to above-mentioned distinct methods, as can be seen from upper table 1, after metal nickel powder emulsification, classification, storing process all complete in the corrosion inhibiting solution adding composite antioxidant TX-02, oxygen content amplification 4.7%, and after using pure water classification, oxygen content increases floating 42.1%.Therefore, foregoing invention metallic nickel powder moisture level anti-oxidation method effectively reduces the oxide etch effect of oxygen in water to metal nickel powder, and compare classification metal nickel powder in pure water, extent of corrosion is little, and surface area variable quantity is little, and oxygen content amplification is little.
Superfine metal nickel powder moisture level processing procedure antioxygen method of the present invention, classification cost comparatively uses ethanol low, production process safety, and the change of product oxygen content is little, and product is stablized.
Claims (4)
1. an anti-oxidation method for moisture level process metal nickel powder, is characterized in that: step comprises:
(1) add antioxidant TX-02 in deionized water, be stirred to antioxidant and dissolve completely, being mixed with antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.1-2%, controls this corrosion inhibiting solution pH within the scope of 7-8; Above-mentioned antioxidant TX-02 is (1-3) by carbohydrazide and citric acid according to weight ratio: 1 mixes and obtains;
(2) unassorted metal nickel powder is added to fill mass concentration prepared by step (1) be in the emulsifying device of the corrosion inhibiting solution of 0.1-2%, be mixed with the nickel powder slip that solid content is 10-25%;
(3) emulsifying device is started, emulsification nickel powder slip 20-50min, the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip, after sieving, sends into hierarchy system classification; Hierarchy system described in step (4) is by surge tank, centrifugal pump, cyclone hydraulic separators, and receiving vat forms; Classification process is: by step (4) emulsification, sieve after solid content be that the nickel powder slip of 10-25% delivers to surge tank, by centrifugal pump under 1.0-1.5MPa pressure, squeeze in cyclone hydraulic separators and carry out centrifugal classification, from the overfall of cyclone hydraulic separators, obtain the powder of even particle size distribution.
2. the anti-oxidation method of moisture level process metal nickel powder according to claim 1, is characterized in that: the corrosion inhibiting solution described in step (1) is antioxidant TX-02 mass concentration is the corrosion inhibiting solution of 0.2%.
3. the anti-oxidation method of moisture level process metal nickel powder according to claim 1, is characterized in that: the solid content being mixed with nickel powder slip described in step (2) is 20%.
4. the anti-oxidation method of moisture level process metal nickel powder according to claim 1, is characterized in that: the emulsification nickel powder slip emulsification times described in step (3) is 30min.
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| CN103962251A (en) * | 2014-04-18 | 2014-08-06 | 松阳县中奇环境工程有限公司 | Shearing emulsifying smashing device for processing materials containing ferrites |
| CN104399975A (en) * | 2014-12-18 | 2015-03-11 | 江苏博迁新材料有限公司 | Method for fully dispersing nanoscale nickel powder |
| CN104785354A (en) * | 2015-04-07 | 2015-07-22 | 台州市金博超导纳米材料科技有限公司 | Method for grading nano-sized metal powder with low-temperature high purity water as medium |
| CN105127412B (en) * | 2015-09-14 | 2018-09-18 | 江苏博迁新材料股份有限公司 | The preparation method of low-oxygen content submicron cupromanganese powder |
| CN112893830A (en) * | 2020-12-29 | 2021-06-04 | 宁波广新纳米材料有限公司 | Liquid phase grading method for magnetic metal powder |
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Effective date of registration: 20161028 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Zhejiang city in Ningbo province where 315153 broad industrial park spring news site Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |