CN102327806B - Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) - Google Patents
Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) Download PDFInfo
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- CN102327806B CN102327806B CN201110165976.0A CN201110165976A CN102327806B CN 102327806 B CN102327806 B CN 102327806B CN 201110165976 A CN201110165976 A CN 201110165976A CN 102327806 B CN102327806 B CN 102327806B
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Abstract
The invention discloses a method taking an organic solvent as a medium for grading nano-nickel powder for an MLCC (multilayer ceramic capacitor), which comprises the following steps of: taking metal nickel powder in the average particle size of below 1000nm as raw materials, adding into the organic solvent and mixing so as to get a solid-liquid system; then performing mechanical dispersion treatment to get slurry; sending the slurry into a cyclone through a booster pump, controlling the pressure of the slurry at an inlet of the cyclone at 0.1-2.0Mpa, controlling the flow rate at a material inlet of the cyclone at 10-200L/min, and controlling the flow rate at an underflow port of the cyclone at 2-20L/min; and collecting the slurry overflowed from an overflow port of the cyclone to get the nickel powder with the required particle size distribution. The method has the advantages of not only ensuring the grading efficiency of the cyclone, but also preventing affecting the surface morphology of the powder.
Description
Technical field
The present invention relates to nano-nickel powder classification technique field, be specifically related to a kind of take organic solvent as medium, utilize hydroclone classification MLCC(chip multilayer ceramic capacitor) by the method for nano-nickel powder.
Background technology
Traditional MLCC inner electrode is Pd/Ag alloy or pure Pd electrode, but because of its cost high, adopting low-cost metal material to replace Pd/Ag electrode is the important trend of MLCC development, in order to take into account the requirement of large capacity and low-cost aspect simultaneously, metal Ni(low price) electrode is a kind of good selection, at present Ni electrode become that degree of being practical is the highest, research the most a kind of low price metal electrode.Nickel powder raw material for electrode production in MLCC should possess following performance: spherical, even, high-purity, high crystallization.
PVD(physical vapour deposition (PVD)) method is at present for the preparation of the comparatively ripe a kind of physical method of metal nano powder.It is to utilize the methods such as vacuum evaporation, heating, high-frequency induction to make copper raw material gasification form plasma that PVD prepares copper nanoparticle, and then quenching finally forms the superfine powder of good dispersion.Metal nano powder purity prepared by the method is high, crystalline structure good, granularity is controlled.
But the metal nano powder particle diameter of producing by PVD method distributes wide, must carry out certain classification processing and just can reach the instructions for use of the raw material of MLCC.Hydrocyclone is a kind of purposes separated classifying equipoment of wet type machinery very widely, and its operation principle is to rely on the centrifugal force in conical vessel that the particle of different-grain diameter size is separated from current.
?take water when classification medium utilizes hydroclone classification nano-nickel powder, because nano-nickel powder particle diameter is little, specific area and surface can be large, powder surface is adsorbed water chemical reaction occurs with it generate new surface texture Ni-O-H very easily, this type of mechanism will further form hydrogen bond, and cause the reunion of nickel powder, finally affect the classification efficiency of hydrocyclone.Meanwhile, the existence of Ni-O-H structure will change nickel powder surface texture form, impel the long-pending roughness of powder surface to increase, and the specific area that shows as powder increases, and this will have a strong impact on the application of nano-nickel powder in MLCC field.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of cyclone classification efficiency that both guaranteed be provided, do not affect again powder configuration of surface take organic solvent as the method for nano-nickel powder for medium classification MLCC.
In order to solve the problems of the technologies described above, technical scheme of the present invention is: a kind ofly take organic solvent and be the method for nano-nickel powder for medium classification MLCC, the step of the method comprises:
(1) take the metal nickel powder of average grain diameter below 1000nm is raw material, is joined concentration (mass concentration) and be in 90 ~ 99.9% organic solvent to be mixed to get solid-liquid system, and the solid content of solid-liquid system is controlled at 5% ~ 50%;
(2) above-mentioned solid-liquid system is carried out to mechanical dispersion processing, when jitter time is controlled at 10min ~ 60min, mechanical dispersion, the temperature of solid-liquid system is controlled at 10 ~ 50 ℃ and obtains disperse materials slurry;
(3) the dispersion slip of step (2) gained is sent in cyclone by booster pump, the pressure of cyclone inlets place slip is controlled at 0.1 ~ 2.0Mpa, the flow-control of cyclone charging aperture is at 10 ~ 200L/min, and cyclone underflow opening (underflow opening is that cyclone outlet at bottom is underflow slurry outlet) flow-control is at 2 ~ 20 L/min;
(4) time of hydroclone classification is controlled to 5min ~ 60min, the slip that step (3) cyclone overfall overflow (outlet of cyclone top is just overfall) is gone out is collected, and obtains the nickel powder that required particle diameter distributes.
The present invention's feed metal nickel powder used is the standby nano-nickel powder of PVD legal system.
Raw material below average grain diameter 1000nm described in step of the present invention (1), the metal nickel powder of preferable particle size scope 100nm ~ 400nm.
Organic solvent described in step of the present invention (1) is a kind of of absolute ethyl alcohol, isopropyl alcohol or propyl alcohol.
Solid content described in step of the present invention (1) is preferably controlled at 10% ~ 30%.
Mechanical dispersion described in step of the present invention (2) is treated to ultrasonic wave disperses, and mulser disperses, any during high speed disintegrator disperses.
Slurry temperature described in step of the present invention (2) is controlled at 10 ~ 50 ℃, the height of temperature affects physical parameter, the particularly viscosity of fluid, surface tension etc., the variation of these physical parameters will directly change stickiness power and the centrifugal force of fluid in flow field, simultaneous temperature is too high will will speed up the volatilization of organic solvent, so slurry temperature of the present invention is preferably 20 ~ 40 ℃.
Booster pump described in step of the present invention (3) is centrifugal pump of horizontal axis, vertical centrifugal pump, vertical multi-stage centrifugal pump, a kind of in screw pump.
Advantage of the present invention and beneficial effect
1. the present invention selects the organic solvent of certain concentration (90 ~ 99.9%) requirement as classification medium, compare for classification medium with utilizing water, the dispersiveness of nano-nickel powder in organic solvent is better, by controlling the solid content of solid-liquid system, the grading effect of cyclone is better, and classification efficiency is higher.
2. the present invention selects the organic solvent of concentration requirement as classification medium, compare for classification medium with utilizing water, by controlling the temperature of organic solvent, can avoid powder surface to be subject to the erosion of classification medium, affect the specific area of powder, thereby the extensive use of nickel powder is not exerted an influence.
3. the present invention selects the organic solvent of concentration requirement as decentralized medium, by controlling the pressure of cyclone inlets place slip, and cyclone is imported and exported the flow of slip, can obtain the nano-nickel powder of different-grain diameter scope, compare with moisture level, the particle diameter of classification gained powder distributes narrower, and macroparticle numerical control makes better.
The specific embodiment
Below by embodiment, the present invention is described in further detail, the present invention is not only confined to following examples.
The equipment that the present embodiment adopts is industry conventional equipment.
Embodiment 1:
(1) using nano-nickel powder that the standby average grain diameter of PVD legal system is 380nm as raw material, joined concentration and be in 99.9% absolute ethyl alcohol, solid content is controlled at 20%;
(2) utilize the above-mentioned solid-liquid system of mulser emulsion dispersion, jitter time maintains 30min, and slurry temperature is controlled at 30 ℃ ~ 35 ℃;
(3) utilize centrifugal pump that dispersion slip is sent into hydrocyclone, cyclone inlets pressure is controlled at 0.8Mpa, and cyclone inlets slip flow is controlled at 200L/min, and cyclone underflow outlet slip flow is controlled at 20L/min;
(4) utilize SEM/BET/PSD(SEM/specific area detection/laser particle size analysis) overflow slip is detected, according to testing result, the cyclone classification time is controlled to 60min, it is even that classification obtains particle diameter, bulky grain few (>=0.8um), the qualified nickel powder slip of average grain diameter 300nm left and right.
Table 1: under same process Parameter Conditions,, respectively with absolute ethyl alcohol, deionized water is the detection data of classification medium products obtained therefrom
Embodiment 2:
(1) using nano-nickel powder that the standby average grain diameter of PVD legal system is 300nm as raw material, joined concentration and be in 99.9% isopropyl alcohol, solid content is controlled at 20%;
(2) utilize the above-mentioned solid-liquid system of mulser emulsion dispersion, jitter time maintains 30min, and slurry temperature is controlled at 30 ℃ ~ 35 ℃;
(3) utilize centrifugal pump that dispersion slip is sent into hydrocyclone, cyclone inlets pressure is controlled at 1.5Mpa, and cyclone inlets slip flow is controlled at 70L/min, and cyclone underflow outlet slip flow is controlled at 17L/min.
(4) utilize SEM/BET/PSD to detect overflow slip, according to testing result, grading time is controlled to 15min, it is even that classification obtains particle diameter, bulky grain few (>=0.6um), the qualified nickel powder slip of average grain diameter 200nm left and right.
Table 2: under same process Parameter Conditions,, respectively with isopropyl alcohol, deionized water is the detection data of classification medium products obtained therefrom
From above-mentioned two groups (table 1-2) results, can find out, under same process condition, the BET(specific area of water graded product) compared with organic solvent, want large, explanation is in utilizing the process of deionized water classification, powder surface is subject to the erosion of water, surface has formed Ni-O-H structure, and this point has also been verified in the increase of water graded product oxygen content.Simultaneously, because form hydrogen bond between Ni-O-H, cause the dispersed variation of nickel powder, classification efficiency and the grading effect of cyclone have been affected, it is large that the PSD data of water graded product become, product yield reduces, and adopts organic solvent of the present invention than deionized water, to have larger advantage as classification medium.
Claims (6)
1. take organic solvent as the method for medium classification MLCC with nano-nickel powder, it is characterized in that: the step of the method comprises:
(1) take the metal nickel powder of average grain diameter below 1000nm is raw material, joined concentration and be in 90～99.9% organic solvent and be mixed to get solid-liquid system, the solid content of solid-liquid system is controlled at 20%～50%, and described organic solvent is a kind of of absolute ethyl alcohol, isopropyl alcohol or normal propyl alcohol;
(2) above-mentioned solid-liquid system is carried out to mechanical dispersion processing, when jitter time is controlled at 10min～60min, mechanical dispersion, the temperature of solid-liquid system is controlled at 10～50 ℃ and obtains disperse materials slurry;
(3) the dispersion slip of step (2) gained is sent in cyclone by booster pump, the pressure of cyclone inlets place slip is controlled at 0.1～2.0Mpa, the flow-control of cyclone charging aperture is at 10～200L/min, and the flow-control of cyclone underflow opening is at 2～20L/min;
(4) time of hydroclone classification is controlled to 5min～60min, the slip that step (3) cyclone overfall is overflowed is collected, and obtains the nickel powder that required particle diameter distributes, and described metal nickel powder is by the standby nano-nickel powder of PVD legal system.
2. according to claim 1ly take the agent of organic road and be the method for nano-nickel powder for medium classification MLCC, it is characterized in that: the average grain diameter of the metal nickel powder described in step (1) is 100nm～400nm.
3. according to the organic solvent of take described in claim l, be the method for nano-nickel powder for medium classification MLCC, it is characterized in that: the solid content described in step (1) is controlled at 20%～30%.
4. according to claim 1ly take organic solvent and be the method for nano-nickel powder for medium classification MLCC, it is characterized in that: the mechanical dispersion described in step (2) is treated to that ultrasonic wave disperses, mulser disperses or high speed disintegrator disperses.
5. according to claim 1ly take organic solvent and be the method for nano-nickel powder for medium classification MLCC, it is characterized in that: the slurry temperature described in step (2) is controlled at 20～40 ℃.
6. according to claim 1ly take organic solvent and be the method for nano-nickel powder for medium classification MLCC, it is characterized in that: the booster pump described in step (3) is centrifugal pump of horizontal axis, vertical centrifugal pump, a kind of in screw pump.
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| CN102676813B (en) * | 2012-04-18 | 2014-05-07 | 赣州腾远钴业有限公司 | New process for treating interphase dirt produced by P204 extraction system |
| CN102974833B (en) * | 2012-11-20 | 2015-03-18 | 宁波广博纳米新材料股份有限公司 | Method for preparing flake silver powder |
| CN103706462B (en) * | 2013-12-16 | 2015-11-18 | 宁波广博纳米新材料股份有限公司 | The hierarchical processing method of Micron-Sized Copper Powders Coated |
| CN103691931B (en) * | 2013-12-16 | 2015-12-02 | 宁波广博纳米新材料股份有限公司 | The anti-oxidation method of moisture level process metal 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 |
| CN104998746B (en) * | 2015-07-31 | 2018-04-10 | 合肥银派科技有限公司 | A kind of method that nano silver wire is separated by hydrocyclone |
| CN105834436A (en) * | 2016-04-13 | 2016-08-10 | 江苏博迁新材料有限公司 | Production method for sheet modified conductive nickel powder |
| CN114694898B (en) * | 2022-06-01 | 2022-10-14 | 西北工业大学 | Preparation method of MLCC nickel inner electrode slurry |
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| CN1778497A (en) * | 2004-11-24 | 2006-05-31 | 三星电机株式会社 | Method for surface treatment of nano nickel particles with organic solvent |
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| KR100682884B1 (en) * | 2003-04-08 | 2007-02-15 | 삼성전자주식회사 | Metallic nickel powder and preparing method thereof |
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| CN1657204A (en) * | 2004-02-19 | 2005-08-24 | 西北师范大学 | Technological method for preparating ultrafine nickel powder |
| CN1778497A (en) * | 2004-11-24 | 2006-05-31 | 三星电机株式会社 | Method for surface treatment of nano nickel particles with organic solvent |
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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 Shiqi car 315153 Zhejiang city in Ningbo province where extensive science and Technology Park Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |