CN111918724A - Method for producing metal powder - Google Patents
Method for producing metal powder Download PDFInfo
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- CN111918724A CN111918724A CN201980023373.1A CN201980023373A CN111918724A CN 111918724 A CN111918724 A CN 111918724A CN 201980023373 A CN201980023373 A CN 201980023373A CN 111918724 A CN111918724 A CN 111918724A
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- metal powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B7/00—Selective separation of solid materials carried by, or dispersed in, gas currents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Combined Means For Separation Of Solids (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for efficiently producing metal powder with narrow particle size distribution. The method comprises an air flow classification step of air flow classification of metal powder attached with alcohol at a classification temperature of below 35 ℃. The fractionation pressure may be 0.2MPa or more, and the alcohol may have a vapor pressure of 18.7hPa or more at 20 ℃. The metal powder to which the alcohol is attached may contain 40% or more of the alcohol in the saturated adsorption amount. The number average particle diameter of the metal powder may be 200nm or less.
Description
Technical Field
One embodiment of the present invention relates to a method for efficiently classifying a metal powder, particularly a Ni powder, into a metal powder having a narrow particle size distribution.
Background
As a method for producing the metal powder, for example, a gas phase reaction method is known in which a metal chloride gas of Ni or Cu is obtained and the metal chloride gas is reduced by a reducing gas such as hydrogen gas. In addition, a liquid phase reaction method is known in which a metal powder is formed from a metal salt after forming a metal salt or the like.
The metal powder is used as an internal electrode material of a multilayer ceramic capacitor (MLCC) having a multilayer structure of internal electrodes and dielectrics. It is desired that the metal powder used for the internal electrode of the multilayer ceramic capacitor has a narrow particle size distribution as well as a small particle size. If the metal powder contains coarse particles, the flatness of the internal electrodes is lost, electric field concentration or short-circuiting occurs, and the particles having a relatively large particle diameter cause electrical short-circuiting of the multilayer ceramic capacitor.
As a method for adjusting the particle size of the metal powder, a gas classification method is well known. Patent document 1 below discloses a method for classifying a powder by gas flow. More specifically, disclosed is a method for air-classifying the following powder, which comprises the steps of: mixing the powder with an alcohol auxiliary agent with a boiling point lower than 200 ℃; and classifying the mixture of the powder and the auxiliary agent at a classification temperature of about 110 ℃ under the condition of supplying the heating gas.
Documents of the prior art
Patent document
Patent document 1: international publication WO 2010/047175.
Disclosure of Invention
(problems to be solved by the invention)
Patent document 1 has a problem in that even when powder having a particle diameter of less than 1 μm is classified, the powder can be classified with high efficiency without adhering to a classifier, and the invention effect obtained in patent document 1 is to efficiently classify the powder into fine powder having a desired classification point or less and the remaining coarse powder. However, in the examples of patent document 1, the median diameter of the powder is 400 to 700nm, and a method for classifying a powder having a smaller diameter is desired.
(means for solving the problems)
The present inventors have made extensive studies and as a result, have focused on the use of alcohol and a reduction in the fractionation temperature. If the volatilization of alcohol is promoted in the classification, the recovery rate of the fine powder is increased. Therefore, the present inventors considered that it is effective to use alcohol in the gas flow fractionation.
Further, when the classification temperature is focused, if the classification temperature of the classifier is increased, the air viscosity in the classifier is increased. When the air viscosity increases, the removal of coarse particles by centrifugal force becomes insufficient.
Therefore, the inventors have succeeded in narrowing the particle size distribution of the metal powder as a result of lowering the classification temperature. Further, the production efficiency of the metal powder is also good. Based on the above findings, the present invention has been completed.
One embodiment of the present invention is a method for producing a metal powder. The production method comprises an air flow classification step of air flow classification of the metal powder with the alcohol attached at a classification temperature of 35 ℃ or lower.
In the production method, the classification pressure in the gas flow classification step may be 0.2MPa or more.
The alcohol may have a vapor pressure of 18.7hPa or more at 20 ℃.
The metal powder to which the alcohol is attached may contain 40% or more of the alcohol in the saturated adsorption amount.
The number average particle diameter of the metal powder may be 200nm or less.
The metal powder may be Ni powder.
(effect of the invention)
According to the present embodiment, metal powder having a narrow particle size distribution can be efficiently produced.
Drawings
Fig. 1 is a flowchart of a classification method according to an embodiment of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described. As shown in fig. 1, the classification method of the present embodiment includes the steps of: attaching an alcohol to a metal powder raw material; and carrying out airflow classification on the metal powder attached with the alcohol to obtain the metal powder without coarse powder. As described below, it is considered that the adhered alcohol is volatilized in the step of performing gas flow classification, and it is possible to obtain a metal powder having high purity and a narrow particle size distribution.
The method for producing the metal powder to which the classification method of the present embodiment can be applied is not particularly limited. For example, a metal powder obtained by a gas phase reaction method may be used, and a metal powder obtained by a liquid phase reaction method may be used. From the viewpoint of efficiently obtaining a metal powder having a small particle diameter, it is preferable to use a metal powder obtained by a gas phase reaction method.
The metal powder to which the classification method of the present embodiment can be applied is not particularly limited, and in order to attach alcohol to the metal powder to be classified, preferable metal powders include Ni powder, Ni alloy powder, Cu alloy powder, Ag alloy powder, Pd alloy powder, and the like. More preferably Ni powder, Cu powder, Ag powder. Among these, Ni powder and Cu powder are particularly preferable because of their close specific gravities.
The alcohol used in the fractionation method of the present embodiment is not particularly limited. Specific examples of alcohols that can be preferably used include methanol, ethanol, 1-propanol, and 2-propanol. The Alcohol may be a modified Alcohol, and examples thereof include Solmix A-7 manufactured by Japan Alcohol tracing Co., Ltd. Among them, ethanol is preferably used because methanol has high toxicity and propanol has low volatility. Further, as the alcohol, the above-mentioned modified alcohol is also preferable.
As the alcohol used in the fractionation method of the present embodiment, a specific alcohol may be used, or an alcohol that is a mixture of two or more kinds may be used.
Since the air flow fractionation step is performed at a low temperature, the alcohol is preferably one having a vapor pressure of 18.7hPa or more at 20 ℃. This is because dispersion of the metal powder which is likely to aggregate at low temperature is easily promoted, and the metal powder after classification is prevented from alcohol remaining. The upper limit of the vapor pressure is not limited, and the vapor pressure at 20 ℃ is preferably 65hPa or less in consideration of the operation at a temperature of 20 ℃ or less.
The vapor pressure of the alcohol at 20 ℃ was measured by the static method: 30mL of the sample was placed in a closed vessel under reduced pressure, and the temperature of the sample was controlled to 20 ℃ by a heater and a thermocouple, and the sample was measured by a pressure gauge.
The method for adhering the alcohol to the metal powder is not particularly limited. Examples of the method include a method of impregnating metal powder with alcohol and removing the remaining alcohol, a method of spraying alcohol onto metal powder at normal temperature, and a method of applying alcohol vaporized by heating to metal powder. In addition, in the present embodiment, since the gas flow classification is performed at a low temperature, the oxidation of the metal powder is not easily performed, and the amount of the oxide in the metal powder can be reduced. From the viewpoint of ensuring this effect, the step of adhering the alcohol to the metal powder is preferably performed under conditions capable of suppressing the formation of an oxide, for example, in the presence of an inert gas.
In the present embodiment, the metal powder to which the alcohol is adhered preferably contains the alcohol in an amount of 40% or more of the saturated adsorption amount, from the viewpoint of improving the recovery rate of the metal powder. More preferably, the alcohol amount is 50% or more of the saturated adsorption amount. On the other hand, the upper limit of the alcohol amount is preferably 90% or less of the saturated adsorption amount from the viewpoint of efficient gas flow classification.
The amount of alcohol adhering to the metal powder can be determined by the following method. First, the saturated adsorption amount of alcohol of the metal powder to which alcohol is adhered is determined by the pour point method. That is, the alcohol was added to 2g of the metal powder by a dropper and mixed, and the amount of the alcohol added when the metal powder was made into a slurry was a saturated adsorption amount. Next, the metal powder to which the alcohol has adhered is put in a drying furnace, heated at a temperature equal to or higher than the boiling point of the alcohol to evaporate the alcohol, and the amount of the alcohol in the metal powder to which the alcohol has adhered is determined from the weight difference before and after heating. The alcohol amount is divided by the saturated adsorption amount to obtain the alcohol deposition amount (%) of the metal powder.
(air flow classification step)
In the present embodiment, the metal powder to which the alcohol has adhered can be air-classified by using a known air-classifying device as appropriate. Among them, the classification temperature is set to 35 ℃ or less from the viewpoint of reducing the air viscosity and achieving a reduction in the amount of oxides. On the other hand, the lower limit of the classification temperature is not particularly limited, but is preferably 0 ℃ or higher.
In the gas flow classification, the classification pressure is not particularly limited. From the viewpoint of removing coarse particles of the metal powder, the classification pressure is preferably 0.2MPa or more. Further, the classification pressure may be set to 0.2MPa or more and 0.8MPa or less for the following reason. The classification pressure is more preferably 0.3MPa or more and 0.6MPa or less.
In the present embodiment, the alcohol in the metal powder can be sufficiently removed by air classification. The removal of the alcohol in the gas stream classification is preferable not only from the viewpoint of obtaining fine metal powder but also from the viewpoint of reducing the C content in the metal powder. On the other hand, the upper limit of the classification pressure is not particularly limited, and the inventors have conducted experiments and have found that it is difficult to expect further improvement in the effect even if the classification pressure is set to exceed 0.8 MPa. Therefore, the upper limit value of the classification pressure in the gas stream classification step may be set to 0.8MPa or less.
According to the present embodiment, fine powder having a narrow particle size distribution can be produced. The average particle diameter of the metal powder to be subjected to the alcohol adhesion treatment and the gas flow classification is not particularly limited, and for example, a metal powder having a number average particle diameter of 30nm or more and 200nm or less, or a metal powder having a number average particle diameter of 70nm or more and 200nm or less can be used. Thus, the number average particle diameter of the metal powder to be produced can be 200nm or less. In the present embodiment, the number average particle diameter is a photograph of the metal powder taken by a scanning electron microscope, and the particle diameters of about 1,000 particles are measured from the photograph, and the average value thereof is used. Further, the particle diameter refers to the diameter of the smallest circle that encloses the particle.
(examples)
Hereinafter, examples of the above embodiments will be described. The technical scope of the present embodiment is not limited to the following examples.
The following test was carried out using Ni powder having a number average particle diameter of 180nm and a CV value of 30% determined by the following method. That is, the alcohols shown in table 1 were attached to the Ni powder by a heat gasification method, a normal temperature spray method, or an immersion and drying method. Ethanol or Solmix A-7 (methanol, ethanol, 1-propanol mixture, manufactured by Japan Alcohol tracing Co., Ltd.) was used as the Alcohol.
In the thermal gasification method, an alcohol is heated to about 80 ℃ in an inert gas atmosphere and gasified to obtain a heated gas alcohol, and the heated and gasified alcohol is introduced into Ni powder under stirring to adhere the alcohol. In the normal temperature spraying method, alcohol is sprayed to Ni powder under stirring at normal temperature to adhere the alcohol to the Ni powder. The amount of alcohol deposited in the Ni powder after the alcohol deposition treatment is shown in table 1.
The Ni powder having alcohol adhered thereto was subjected to air-flow classification by a classifier Cnine manufactured by Nippon Pneumatic Mfg Co., Ltd, with a classification pressure of 0.4MPa and a classification temperature in the classifier set to room temperature (35 ℃ or lower) or 75 ℃ by various methods. The Ni metal powder to be produced was collected in a fine powder hopper, and the remainder was collected in a coarse powder hopper. In addition, as the compressed gas introduced into the classifier, compressed air obtained by a compressor is used. The recovery rate, particle size distribution, and oxide amount of the obtained Ni powder are shown in table 1.
(recovery rate)
The recovery rate (%) of the Ni powder recovered in the fine hopper was determined based on the following formula. The recovery rate of 13% or more was evaluated as "good", and was regarded as good. The comparative examples evaluated as "x" each had a recovery rate of 10% or less, and did not satisfy the above-mentioned standards for acceptability, and were insufficient.
{ [ (raw material input amount) - (coarse powder hopper amount) ]/raw material input amount } × 100
(particle size distribution)
Using image analysis software (product name macview4.0, manufactured by Mountech corporation), 1 field (the number of particles is about 500) was observed at a magnification of 30k, and the number average particle diameter and the standard deviation thereof were determined. CV was determined by the formula of "[ standard deviation (unit: μm)/number average particle diameter (unit: μm) ] X100". The CV value of 22% or less was evaluated as "good", and was accepted.
The CV values of example Nos. 1 to 4 were small (particle size distribution was narrow), and the powder could be efficiently recovered. In addition, the number average particle diameter of examples 1 to 4 was in the range of 160nm to 180 nm. Comparative example 5 was carried out under alcohol-free conditions and the classification temperature was high, so that the CV value did not reach the target value and the recovery rate was insufficient. Comparative example No.6 was conducted under alcohol-free conditions, and therefore the recovery rate was insufficient. Comparative example No.7 had a high classification temperature, and therefore the CV value did not reach the target value.
In addition, in Nos. 1 to 5, the number of coarse particles having a particle diameter of 0.4 μm or more was confirmed. Specifically, 10 fields of view were photographed at 10k times using the image analysis software, and the number of coarse particles of 0.4 μm or more was measured. In Nos. 1 to 4, the number of coarse particles was 0 to 1, while in No.5, the number of coarse particles was 3. Considering the result of No.6, it is considered that the number of coarse particles increases when the gas flow classification temperature is high.
(amount of oxide)
The amount of oxides was estimated by X-ray photoelectron spectroscopy (XPS) for the examples. Specifically, the following is described. As the equipment used, k-alpha + manufactured by Thermo Fisher Scientific Co., Ltd was used. As the light source, AlK α rays were used. The measured energy range of Ni2p is 884 to 844(eV), and the measured energy range of C1s is 298 to 279 (eV). After background subtraction is performed on the obtained spectrum by using a Shirley method, waveform separation is performed by using a function in which a lorentz function and a gaussian function are combined. The area of the peak attributed to metallic nickel, that is, the peak derived from the Ni-Ni bond was set to the sum of the peak areas of 852.4(eV) and 858.5 (eV). The peak areas ascribed to Ni-O bonds were set to the sum of the peak areas of 853.4(eV), 854.2(eV), 855.3(eV), 858.2(eV), 860.6(eV), 863.2(eV), and 865.4 (eV). The peak area attributed to the Ni-OH bond was determined as follows. First, the sum of peak areas of 854.5(eV), 855.7(eV), 857.4(eV), 861.1(eV), 862.4(eV), and 865.4(eV) was determined. The peak area attributed to 288.5(eV) bonded to Ni-C was subtracted from the sum to set the peak area attributed to Ni-OH bond. The ratio of the peak area attributed to Ni-Ni bond to the sum of the peak area attributed to Ni-Ni bond, the peak area attributed to Ni-O bond, and the peak area attributed to Ni-OH bond is the ratio of metallic nickel determined by XPS measurement.
In addition, if Ni is used as a standard, it is possible to specify the goldBelongs to the peak position of the peak of nickel. If NiO is used as a standard, the peak position of the peak attributed to the Ni-O bond can be specified. If Ni (OH) is used2Then, the peak position of the peak attributed to the Ni-OH bond can be specified. If NiCO is used3Then the peak position attributed to the Ni-C bond can be specified.
As a result of XPS measurement, it was confirmed that: the nickel powder obtained in the examples had a peak area attributed to metallic Ni of 30 to 35% relative to the total area of metallic Ni, Ni-O and Ni-OH, and had a high Ni content in the surface layer portion of the Ni powder, thereby suppressing the oxidation of the Ni powder.
[ Table 1]
TABLE 1 influence of various conditions on the classification of nickel powder
As shown by experiments in this example, by applying this embodiment, it is possible to efficiently produce a metal powder having a narrow particle size distribution.
Claims (6)
1. A method for producing a metal powder, comprising an air flow classification step of air flow classifying metal powder to which an alcohol has adhered at a classification temperature of 0 ℃ to 35 ℃.
2. The method for producing a metal powder according to claim 1, wherein,
the classification pressure in the gas flow classification step is 0.2MPa or more and 0.8MPa or less.
3. The method for producing a metal powder according to claim 1, wherein,
the vapor pressure of the alcohol at 20 ℃ is 18.7hPa or more and 65hPa or less.
4. The method for producing a metal powder according to claim 1, wherein,
the metal powder to which the alcohol is attached contains the alcohol in an amount of 40% to 90% of a saturated adsorption amount.
5. The method for producing a metal powder according to claim 1, wherein,
the number average particle diameter of the metal powder is 30nm to 200 nm.
6. The method for producing a metal powder according to claim 1, wherein,
the metal powder is Ni powder.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2018063644 | 2018-03-29 | ||
| JP2018-063644 | 2018-03-29 | ||
| PCT/JP2019/009514 WO2019188149A1 (en) | 2018-03-29 | 2019-03-08 | Method for manufacturing metal powder |
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| CN111918724A true CN111918724A (en) | 2020-11-10 |
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| JP (2) | JP7145932B2 (en) |
| KR (1) | KR102484800B1 (en) |
| CN (1) | CN111918724A (en) |
| TW (1) | TWI699240B (en) |
| WO (1) | WO2019188149A1 (en) |
Citations (5)
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| JP2007029859A (en) * | 2005-07-27 | 2007-02-08 | Nisshin Seifun Group Inc | Production method of fine particles and apparatus |
| WO2010106716A1 (en) * | 2009-03-18 | 2010-09-23 | 日清エンジニアリング株式会社 | Method for classifying powder |
| CN102196868A (en) * | 2008-10-24 | 2011-09-21 | 株式会社日清制粉集团本社 | Method for classifying powder |
| US20140027353A1 (en) * | 2011-03-16 | 2014-01-30 | Nisshin Seifun Group Inc. | Powder-classification method |
| CN105107739A (en) * | 2015-07-08 | 2015-12-02 | 湘潭大学 | High efficiency ultrafine powder jet flow grading purification method and special-purpose device thereof |
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| JPH01180285A (en) * | 1988-01-11 | 1989-07-18 | Nkk Corp | Classifying method |
| JPH0211701A (en) * | 1988-06-29 | 1990-01-16 | Showa Denko Kk | Production of fe-si alloy powder |
| KR100558270B1 (en) | 2003-10-28 | 2006-03-10 | 엔티베이스 주식회사 | Nano unit metal powder wet classifying apparatus and method and liquid composition |
| JP4540364B2 (en) * | 2004-03-01 | 2010-09-08 | 東邦チタニウム株式会社 | Nickel powder, and conductive paste and multilayer ceramic capacitor using the same |
| JP5026303B2 (en) * | 2007-03-30 | 2012-09-12 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder manufacturing method |
| JP2010084222A (en) | 2008-10-02 | 2010-04-15 | Daiken Chemical Co Ltd | Classification treatment method for metal fine particle |
| GB201403731D0 (en) * | 2014-03-03 | 2014-04-16 | P V Nano Cell Ltd | Nanometric copper formulations |
| CN107206353A (en) * | 2015-01-19 | 2017-09-26 | 花王株式会社 | Absorbent commodity material, its manufacture method and use its absorbent commodity |
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2019
- 2019-03-08 CN CN201980023373.1A patent/CN111918724A/en active Pending
- 2019-03-08 WO PCT/JP2019/009514 patent/WO2019188149A1/en active Application Filing
- 2019-03-08 KR KR1020207024895A patent/KR102484800B1/en active IP Right Grant
- 2019-03-08 JP JP2020509803A patent/JP7145932B2/en active Active
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007029859A (en) * | 2005-07-27 | 2007-02-08 | Nisshin Seifun Group Inc | Production method of fine particles and apparatus |
| CN102196868A (en) * | 2008-10-24 | 2011-09-21 | 株式会社日清制粉集团本社 | Method for classifying powder |
| WO2010106716A1 (en) * | 2009-03-18 | 2010-09-23 | 日清エンジニアリング株式会社 | Method for classifying powder |
| US20140027353A1 (en) * | 2011-03-16 | 2014-01-30 | Nisshin Seifun Group Inc. | Powder-classification method |
| CN105107739A (en) * | 2015-07-08 | 2015-12-02 | 湘潭大学 | High efficiency ultrafine powder jet flow grading purification method and special-purpose device thereof |
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| WO2019188149A1 (en) | 2019-10-03 |
| KR102484800B1 (en) | 2023-01-05 |
| TWI699240B (en) | 2020-07-21 |
| KR20200113266A (en) | 2020-10-06 |
| JP7145932B2 (en) | 2022-10-03 |
| TW201941831A (en) | 2019-11-01 |
| JPWO2019188149A1 (en) | 2021-02-12 |
| JP2022163005A (en) | 2022-10-25 |
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