CN102327806A - 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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- CN102327806A CN102327806A CN201110165976A CN201110165976A CN102327806A CN 102327806 A CN102327806 A CN 102327806A CN 201110165976 A CN201110165976 A CN 201110165976A CN 201110165976 A CN201110165976 A CN 201110165976A CN 102327806 A CN102327806 A CN 102327806A
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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 be medium with the organic solvent, utilize the method for hydroclone classification MLCC (chip multilayer ceramic capacitor) with nano-nickel powder.
Background technology
Traditional M LCC inner electrode is Pd/Ag alloy or pure Pd electrode; But because of its cost height; Adopting low-cost metal material to replace the Pd/Ag electrode is the important trend of MLCC development; In order to take into account the requirement of big capacity and low-cost aspect simultaneously, metal Ni (low price) electrode is a kind of good selection, and at present the Ni electrode has become that degree of being practical is the highest, the most a kind of low price metal electrode of research.Be used for that the nickel powder raw material of electrode production should possess following performance in the MLCC: spherical, evenly, high-purity, high crystallization.
PVD (physical vapour deposition (PVD)) method is to be used to prepare the comparatively ripe a kind of physical method of metal nano powder at present.It is to utilize methods such as vacuum evaporation, heating, high-frequency induction to make copper raw material gasification form plasma that PVD prepares copper nanoparticle, and quenching then forms the superfine powder of good dispersion at last.High, good, the controllable granularity of crystalline structure of the metal nano powder purity of this method preparation.
But, wide through the metal nano powder particle diameter distribution that the PVD method is produced, must carry out the instructions for use that certain hierarchical processing just can reach the raw material of MLCC.Hydrocyclone is a kind of purposes wet type mechanical separation classifying equipoment very widely, and its operation principle is to rely on the centrifugal force in the conical vessel that the particle of different-grain diameter size is separated from current.
When utilizing the hydroclone classification nano-nickel powder for the classification medium with water; Because the nano-nickel powder particle diameter is little; Specific area and surface can be big, and the new surface texture Ni-O-H of chemical reaction generation also takes place with it powder surface very easily adsorbed water, and this type of mechanism will further form hydrogen bond; And cause the reunion of nickel powder, finally influence the classification efficiency of hydrocyclone.Simultaneously, 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 the MLCC field.
Summary of the invention
The present invention is directed to the deficiency of prior art, a kind of cyclone classification efficient that both guaranteed be provided, do not influence again powder configuration of surface be the method for medium classification MLCC with the organic solvent with nano-nickel powder.
In order to solve the problems of the technologies described above, technical scheme of the present invention is: a kind of method that with the organic solvent is medium classification MLCC with nano-nickel powder, and the step of this method comprises:
(1) be that metal nickel powder below the 1000nm is a raw material with the average grain diameter, it is joined concentration (mass concentration) is to mix in 90 ~ 99.9% the organic solvent to obtain the 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 mechanical dispersion and handle, the temperature of solid-liquid system was controlled at 10 ~ 50 ℃ of score bulk cargo slurries when jitter time was controlled at 10min ~ 60min, mechanical dispersion;
(3) the dispersion slip of step (2) gained is sent in the cyclone through 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 the cyclone outlet at bottom is the underflow slurry outlet) flow-control is at 2 ~ 20 L/min;
(4) time with hydroclone classification is controlled at 5min ~ 60min, and the slip that step (3) cyclone overfall overflow (outlet of cyclone top just is overfall) goes out is collected, and obtains the nickel powder that required particle diameter distributes.
The nano-nickel powder that the used feed metal nickel powder of the present invention prepares for the PVD method.
Raw material below the average grain diameter 1000nm described in the step of the present invention (1), the metal nickel powder of preferable particle size scope 100nm ~ 400nm.
Organic solvent described in the step of the present invention (1) is a kind of of absolute ethyl alcohol, isopropyl alcohol or propyl alcohol.
Solid content described in the step of the present invention (1) preferably is controlled at 10% ~ 30%.
Mechanical dispersion described in the step of the present invention (2) is treated to ultrasonic dispersing, and mulser disperses, any during high speed disintegrator disperses.
Slurry temperature described in the step of the present invention (2) is controlled at 10 ~ 50 ℃; The height of temperature influences physical parameter; The particularly viscosity of fluid, surface tension etc.; These variations of physical parameters will directly change the stickiness power and the centrifugal force of fluid in the flow field, the too high volatilization that will will speed up organic solvent of simultaneous temperature, so slurry temperature of the present invention is preferably 20 ~ 40 ℃.
Booster pump described in the step of the present invention (3) is a centrifugal pump of horizontal axis, vertical centrifugal pump, vertical multi-stage centrifugal pump, a kind of in the screw pump.
Advantage of the present invention and beneficial effect
1. the present invention selects for use organic solvent that certain concentration (90 ~ 99.9%) requires as the classification medium; Compare for the classification medium with utilizing water, the dispersiveness of nano-nickel powder in organic solvent is better, through the solid content of control solid-liquid system; The grading effect of cyclone is better, and classification efficiency is higher.
The present invention select concentration requirement for use organic solvent as the classification medium; Compare for the classification medium with utilizing water,, can avoid powder surface to receive the erosion of classification medium through the temperature of control organic solvent; Influence the specific area of powder, thereby the extensive use of nickel powder is not exerted an influence.
The present invention select concentration requirement for use organic solvent as decentralized medium; Pressure through control cyclone inlets place slip; And cyclone imports and exports the flow of slip, can obtain the nano-nickel powder of different-grain diameter scope, compares with the moisture level; The particle diameter of classification gained powder distributes narrower, and the macroparticle numerical control makes better.
The specific embodiment
Through embodiment the present invention is described in further detail below, the present invention not only is confined to following examples.
The equipment that present embodiment adopts is the industry conventional equipment.
Embodiment 1:
(1) with the average grain diameter of PVD method preparation be the nano-nickel powder of 380nm as raw material, it is joined concentration is that solid content is controlled at 20% in 99.9% the absolute ethyl alcohol;
(2) utilize mulser emulsification to disperse above-mentioned solid-liquid system, jitter time is kept 30min, and slurry temperature is controlled at 30 ℃ ~ 35 ℃;
(3) utilize centrifugal pump will disperse slip to send 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) that the overflow slip is detected; According to testing result the cyclone classification time is controlled at 60min; It is even that classification obtains particle diameter; Bulky grain few (>=0.8um), the qualified nickel powder slip about average grain diameter 300nm.
Table 1: respectively with absolute ethyl alcohol, deionized water is the detection data of classification medium products obtained therefrom under the same process parameter condition
Embodiment 2:
(1) with the average grain diameter of PVD method preparation be the nano-nickel powder of 300nm as raw material, it is joined concentration is that solid content is controlled at 20% in 99.9% the isopropyl alcohol;
(2) utilize mulser emulsification to disperse above-mentioned solid-liquid system, jitter time is kept 30min, and slurry temperature is controlled at 30 ℃ ~ 35 ℃;
(3) utilize centrifugal pump will disperse slip to send 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 that the overflow slip is detected, according to testing result grading time is controlled at 15min, it is even that classification obtains particle diameter, bulky grain few (>=0.6um), the qualified nickel powder slip about average grain diameter 200nm.
Table 2: respectively with isopropyl alcohol, deionized water is the detection data of classification medium products obtained therefrom under the same process parameter condition
Can find out from above-mentioned two groups (table 1-2) results; Under the same process condition; The BET (specific area) of moisture level product wants big than organic solvent, explains that in the process of utilizing the deionized water classification, powder surface receives the erosion of water; The surface has formed the Ni-O-H structure, and this point has also been verified in the increase of moisture level product oxygen content.Simultaneously; Because form hydrogen bond between the Ni-O-H; Cause the dispersed variation of nickel powder, influenced the classification efficiency and the grading effect of cyclone, it is big that the PSD data of moisture level product become; The product yield reduces, and adopts organic solvent of the present invention then to have bigger advantage as the classification medium than deionized water.
Claims (8)
1. one kind is the method for medium classification MLCC with nano-nickel powder with the organic solvent, and it is characterized in that: the step of this method comprises:
(1) be that metal nickel powder below the 1000nm is a raw material with the average grain diameter, it is joined concentration is to mix in 90 ~ 99.9% the organic solvent to obtain the 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 mechanical dispersion and handle, the temperature of solid-liquid system was controlled at 10 ~ 50 ℃ of score bulk cargo slurries when jitter time was controlled at 10min ~ 60min, mechanical dispersion;
(3) the dispersion slip of step (2) gained is sent in the cyclone through 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 ~ 20 L/min;
(4) time with hydroclone classification is controlled at 5min ~ 60min, and the slip that overflow goes out to step (3) cyclone overfall is collected, and obtains the nickel powder that required particle diameter distributes.
2. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1 is characterized in that: described metal nickel powder is the nano-nickel powder by the preparation of PVD method.
3. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1, it is characterized in that: the average grain diameter of the metal nickel powder described in the step (1) is 100nm ~ 400nm.
4. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1, it is characterized in that: the organic solvent described in the step (1) is a kind of of absolute ethyl alcohol, isopropyl alcohol or propyl alcohol.
5. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1, it is characterized in that: the solid content described in the step (1) is controlled at 10% ~ 30%.
6. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1 is characterized in that: the mechanical dispersion described in the step (2) is treated to ultrasonic dispersing, mulser disperses or high speed disintegrator disperses.
7. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1, it is characterized in that: the slurry temperature described in the step (2) is controlled at 20 ~ 40 ℃.
8. the method that with the organic solvent is medium classification MLCC with nano-nickel powder according to claim 1, it is characterized in that: the booster pump described in the step (3) is a centrifugal pump of horizontal axis, vertical centrifugal pump, vertical multi-stage centrifugal pump, a kind of in the screw pump.
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| CN102676813A (en) * | 2012-04-18 | 2012-09-19 | 赣州腾远钴业有限公司 | New process for treating interphase dirt produced by P204 extraction system |
| CN102974833A (en) * | 2012-11-20 | 2013-03-20 | 宁波广博纳米新材料股份有限公司 | Method for preparing flake silver powder |
| CN103691931A (en) * | 2013-12-16 | 2014-04-02 | 宁波广博纳米新材料股份有限公司 | Antioxidant method for grading treatment of metal nickel powder by water |
| CN103706462A (en) * | 2013-12-16 | 2014-04-09 | 宁波广博纳米新材料股份有限公司 | Classification processing method for micron size copper 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 |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through 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 |
| CN114694898A (en) * | 2022-06-01 | 2022-07-01 | 西北工业大学 | Preparation method of MLCC nickel inner electrode slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102676813A (en) * | 2012-04-18 | 2012-09-19 | 赣州腾远钴业有限公司 | New process for treating interphase dirt produced by P204 extraction system |
| CN102974833A (en) * | 2012-11-20 | 2013-03-20 | 宁波广博纳米新材料股份有限公司 | Method for preparing flake silver powder |
| 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 |
| CN103691931A (en) * | 2013-12-16 | 2014-04-02 | 宁波广博纳米新材料股份有限公司 | Antioxidant method for grading treatment of metal nickel powder by water |
| CN103706462A (en) * | 2013-12-16 | 2014-04-09 | 宁波广博纳米新材料股份有限公司 | Classification processing method for micron size copper 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 |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through 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 |
| CN114694898A (en) * | 2022-06-01 | 2022-07-01 | 西北工业大学 | Preparation method of MLCC nickel inner electrode slurry |
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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. |