TW201941831A - Method for manufacturing metal powder - Google Patents
Method for manufacturing metal powder Download PDFInfo
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- TW201941831A TW201941831A TW108108913A TW108108913A TW201941831A TW 201941831 A TW201941831 A TW 201941831A TW 108108913 A TW108108913 A TW 108108913A TW 108108913 A TW108108913 A TW 108108913A TW 201941831 A TW201941831 A TW 201941831A
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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
- 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
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Combined Means For Separation Of Solids (AREA)
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Abstract
Description
本發明之實施型態之一，係關於將金屬粉體──尤其係Ni粉體──有效率分級成粒度分布為窄之金屬粉體的方法。One of the implementation forms of the present invention relates to a method for efficiently classifying metal powders, especially Ni powders, into metal powders with narrow particle size distribution.
作為金屬粉體之製造方法，已知例如獲得Ni或Cu之金屬氯化物氣體，將該金屬氯化物氣體透過氫等還原氣體來還原的氣相反應法。並且，已知於使金屬鹽等形成後自金屬鹽生成金屬粉體的液相反應法。As a method for producing a 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 passing a reducing gas such as hydrogen. In addition, a liquid phase reaction method is known in which a metal powder is formed from a metal salt after the metal salt is formed.
金屬粉體常作為由內部電極與介電質之堆疊結構而成之堆疊陶瓷電容器（MLCC）之內部電極材料等使用。使用於堆疊陶瓷電容器之內部電極等的金屬粉體，並非單純企求小粒徑化，還企求粒度分布為窄者。若於金屬粉體中包含粗大粒子等，則內部電極之平坦性會喪失而發生電場集中或短路等，粒徑相對大的粒子會成為堆疊陶瓷電容器之電性短路的原因。Metal powder is often used as an internal electrode material of a stacked ceramic capacitor (MLCC) formed by a stacked structure of an internal electrode and a dielectric. Metal powders used for internal electrodes of stacked ceramic capacitors are not simply for small particle size, but also for narrow particle size distribution. If coarse particles and the like are contained in the metal powder, the flatness of the internal electrode will be lost and an electric field concentration or short circuit will occur. Particles with a relatively large particle diameter will cause the electrical short circuit of the stacked ceramic capacitor.
已知有氣流分級法作為金屬粉體之粒度調整法。下述專利文獻1已揭露粉體之氣流分級方法。更具體而言，已揭露粉體之氣流分級法，其包含：將粉體與沸點未達200℃之醇助劑混合的工序，以及在加熱氣體供給下以分級溫度110℃之程度將粉體與助劑之混合物分級的工序。An airflow classification method is known as a particle size adjustment method of metal powder. The following patent document 1 discloses a method for classifying a powder by air flow. More specifically, the airflow classification method of powder has been disclosed, which includes a step of mixing the powder with an alcohol auxiliary agent having a boiling point of less than 200 ° C, and powdering the powder at a classification temperature of 110 ° C under the supply of heated gas Classification of admixture with auxiliaries.
『專利文獻』
《專利文獻1》：國際專利公開第WO2010/047175號『Patent Literature』
"Patent Document 1": International Patent Publication No. WO2010 / 047175
在專利文獻1，將課題設為：做到即使在進行粒徑未達1 μm之粉體之分級的情況下，仍可有效率進行分級而不使粉體附著於分級機內，將可有效率分級成期望之分級點以下的微粉與殘餘的粗粉一事視為專利文獻1相關之發明的效果。然而，在專利文獻1之實施例，粉體之中位徑為400～700 nm，更小徑之粉體的分級方法仍為人所企求。In Patent Document 1, the subject is set to achieve efficient classification even when powders with a particle size of less than 1 μm are classified without adhering the powder to the classifier. The effect of classifying the efficiency into fine powder and residual coarse powder below a desired classification point is regarded as the effect of the invention according to Patent Document 1. However, in the example of Patent Document 1, the method for classifying powders with a median diameter of 400-700 nm and smaller diameters is still desired.
本發明人等反覆潛心研究，進而著眼於醇之利用與分級溫度之低溫化。若於分級中促使醇揮發，則微粉之回收率會提升。據此，本發明人等認為在氣流分級時醇的利用實屬有效。The inventors have repeatedly studied intensively, and then focused on the utilization of alcohol and the lowering of the classification temperature. If the volatilization of alcohol is promoted in the classification, the recovery rate of fine powder will increase. Based on this, the present inventors thought that the utilization of alcohol is effective when the air flow is classified.
再者，若著眼於分級溫度，一旦提高分級機之分級溫度，分級機內之空氣黏度就會上升。若空氣黏度上升，則利用離心力之粗大粒子去除會變得不充分。Furthermore, if we focus on the classification temperature, once the classification temperature of the classifier is increased, the viscosity of the air in the classifier will increase. If the viscosity of the air increases, the removal of coarse particles by centrifugal force becomes insufficient.
於是，發明人等降低分級溫度，結果成功窄化金屬粉體之粒度分布。再者，金屬粉體之製造效率亦良好。依據上述知識完成本發明。Then, the inventors lowered the classification temperature, and as a result, successfully narrowed the particle size distribution of the metal powder. Furthermore, the manufacturing efficiency of metal powder is also good. The present invention has been completed based on the above knowledge.
本揭露之實施型態之一係金屬粉體之製造方法。此製造方法包含將附著有醇之金屬粉體在分級溫度35℃以下氣流分級的氣流分級工序。One of the implementation forms disclosed in this disclosure is a method for manufacturing metal powder. This manufacturing method includes an air-flow classification step of classifying a metal powder to which alcohol is adhered at a classification temperature of 35 ° C or lower.
在此製造方法中，於氣流分級工序中之分級壓力亦可為0.2 MPa以上。In this manufacturing method, the classification pressure in the air flow classification step may be 0.2 MPa or more.
醇亦可為在20℃之蒸氣壓為18.7 hPa以上的醇。The alcohol may be an alcohol having a vapor pressure of 18.7 hPa or higher at 20 ° C.
醇附著金屬粉體亦可包含飽和吸附量之40%以上的醇。The alcohol-attached metal powder may also contain an alcohol having a saturated adsorption amount of 40% or more.
金屬粉體之個數平均粒徑亦可為200 nm以下。The number average particle diameter of the metal powder may be 200 nm or less.
金屬粉體亦可為Ni粉體。The metal powder may be a Ni powder.
根據本實施型態，能有效率製造粒度分布為窄之金屬粉體。According to this embodiment, a metal powder having a narrow particle size distribution can be efficiently produced.
以下說明本發明之實施型態。如圖1所示，本實施型態之分級方法包含：使醇附著於金屬粉體原料的工序，以及將附著有醇之金屬粉體氣流分級以獲得去除粗粉後之金屬粉體的工序。如以下所述，附著之醇可認為會在做氣流分級之工序中揮發，而可獲得高純度且粒度分布為窄之金屬粉體。The following describes embodiments of the present invention. As shown in FIG. 1, the classification method according to this embodiment includes a step of attaching alcohol to the raw material of the metal powder, and a step of classifying the metal powder to which the alcohol is adhered by airflow to obtain the metal powder after removing coarse powder. As described below, the attached alcohol can be considered to be volatilized in the process of air flow classification, and metal powder with high purity and narrow particle size distribution can be obtained.
應用本實施型態之分級方法之金屬粉體的製法並不特別受限。舉例而言，可應用藉由氣相反應法獲得之金屬粉體，亦可應用藉由液相反應法獲得之金屬粉體。就有效率獲得粒徑為小之金屬粉體的觀點而言，以使用藉由氣相反應法獲得之金屬粉體為佳。The manufacturing method of the metal powder to which the classification method of the embodiment is applied is not particularly limited. For example, metal powder obtained by a gas phase reaction method can be used, and metal powder obtained by a liquid phase reaction method can also be applied. 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.
應用本實施型態之分級方法的金屬粉體並不特別受限，但為了對於係為分級對象之金屬粉體附著醇，可列舉：Ni粉體、Ni合金粉體、Cu粉體、Cu合金粉體、Ag粉體、Ag合金粉體、Pd粉體及Pd合金粉體等作為良佳之金屬粉體。以Ni粉體、Cu粉體、Ag粉體為較佳。此等之中，由於Ni粉體與Cu粉體之比重接近，故為尤佳。The metal powder to which the classification method of this embodiment is applied is not particularly limited, but in order to adhere alcohol to the metal powder that is a classification object, examples include: Ni powder, Ni alloy powder, Cu powder, Cu alloy Powders, Ag powders, Ag alloy powders, Pd powders and Pd alloy powders are good metal powders. Ni powder, Cu powder, and Ag powder are preferred. Among these, Ni powder and Cu powder are particularly preferable because the specific gravity is close.
使用於本實施型態之分級方法的醇並不特別受限。可列舉例如：甲醇、乙醇、1-丙醇、2-丙醇作為可良佳使用之醇的具體例。醇亦可為改質醇，可舉出例如JAPAN ALCOHOL TRADING CO., LTD.製之SOLMIX A-7。惟甲醇之毒性高，丙醇之揮發性低，故以使用乙醇為符合期望。並且，亦以上述改質醇作為醇為佳。The alcohol used in the classification method of this embodiment is not particularly limited. Specific examples thereof include methanol, ethanol, 1-propanol, and 2-propanol as alcohols which can be used favorably. The alcohol may also be a modified alcohol, and examples thereof include SOLMIX A-7 manufactured by JAPAN ALCOHOL TRADING CO., LTD. However, the toxicity of methanol is high and the volatility of propanol is low, so the use of ethanol is in line with expectations. It is also preferable to use the above-mentioned modified alcohol as an alcohol.
作為使用於本實施型態之分級方法的醇，可使用特定1種醇，亦可使用係為2種以上之混合物的醇。As the alcohol used in the classification method according to the embodiment, one specific alcohol may be used, or an alcohol based on a mixture of two or more may be used.
為了在低溫進行氣流分級工序，醇以在20℃之蒸氣壓為18.7 hPa以上的醇為佳。其理由係因：變得易於促進在低溫易凝集的金屬粉體之分散且避免醇殘留於分級後之金屬粉體。蒸氣壓之上限雖無限制，但若考量在20℃以下之溫度下的處理，則以在20℃之蒸氣壓為65 hPa以下為佳。In order to perform the air flow classification process at a low temperature, the alcohol is preferably an alcohol having a vapor pressure of 18.7 hPa or higher at 20 ° C. The reason is that it becomes easy to promote the dispersion of the metal powder which is easy to agglomerate at a low temperature and to prevent alcohol from remaining in the classified metal powder. Although the upper limit of the vapor pressure is not limited, if the treatment at a temperature of 20 ° C or lower is considered, the vapor pressure at 20 ° C is preferably 65 hPa or lower.
此外，醇在20℃之蒸氣壓，可藉由「將試樣30 mL放入減壓下之密閉容器，以加熱器與熱電偶將試樣溫度控制於20℃，同時使用壓力計來量測」的靜止法來量測。In addition, the vapor pressure of alcohol at 20 ° C can be measured by "putting 30 mL of the sample into a closed container under reduced pressure, controlling the sample temperature to 20 ° C with a heater and a thermocouple, and using a pressure gauge To measure.
使醇附著於金屬粉體的方法並不特別受限。舉例而言，有使金屬粉體浸滲於醇後去除剩餘醇的方法、在常溫將醇噴於金屬粉體的方法、將經加熱氣化之醇應用於金屬粉末的方法等。此外，在本實施型態，由於在低溫進行氣流分級，故金屬粉體之氧化不易進行，可減低金屬粉體中之氧化物量。就確實確保此效果的觀點而言，往金屬粉體附著醇之工序，以在惰性氣體存在下進行等在可抑制氧化物生成之條件下進行為佳。The method for attaching alcohol to the metal powder is not particularly limited. For example, there are a method in which metal powder is impregnated with alcohol to remove excess alcohol, a method in which alcohol is sprayed on metal powder at normal temperature, a method in which heated and vaporized alcohol is applied to metal powder, and the like. In addition, in this embodiment, since the air flow classification is performed at a low temperature, the oxidation of the metal powder is not easy to proceed, and the amount of oxides in the metal powder can be reduced. From the viewpoint of surely ensuring this effect, the step of attaching alcohol to the metal powder is preferably performed in the presence of an inert gas or the like under conditions that can suppress the generation of oxides.
在本實施型態，就提升金屬粉體回收率的觀點而言，有醇附著之金屬粉體以包含飽和吸附量之40%以上的醇為佳。醇量以飽和吸附量之50%以上為較佳。另一方面，醇量之上限值就進行有效率之氣流分級的觀點而言，以飽和吸附量之90%以下為佳。In this embodiment, from the viewpoint of improving the recovery rate of the metal powder, it is preferable that the metal powder with alcohol adheres to an alcohol having a saturated adsorption amount of 40% or more. The amount of alcohol is preferably 50% or more of the saturated adsorption amount. On the other hand, the upper limit of the amount of alcohol is preferably 90% or less of the saturated adsorption amount from the viewpoint of efficient airflow classification.
附著於金屬粉體之醇的量，可藉由以下方法來求得。首先，藉由流點法求得有醇附著之金屬粉體之醇的飽和吸附量。亦即以注射器將醇添加於金屬粉體2 g，同時混合之，於呈漿狀時之醇的添加量係飽和吸附量。其次，有醇附著之金屬粉體中的醇量，係將附著有醇之金屬粉體放入乾燥爐，以醇之沸點以上的溫度加熱以使醇蒸發，由加熱前後的重量差來求得。可將此醇量除以上述飽和吸附量而求得金屬粉體之醇附著量（%）。The amount of the alcohol adhered to the metal powder can be determined by the following method. First, the saturated adsorption amount of the alcohol on the metal powder to which the alcohol is attached is obtained by the flow point method. That is, the alcohol is added to 2 g of the metal powder with a syringe, and mixed at the same time. When the slurry is in a slurry state, the amount of alcohol added is a saturated adsorption amount. Second, the amount of alcohol in the metal powder with the alcohol adhered is to place the metal powder with the alcohol into a drying furnace and heat it at a temperature above the boiling point of the alcohol to evaporate the alcohol. . The alcohol adhesion amount (%) of the metal powder can be obtained by dividing this alcohol amount by the above-mentioned saturated adsorption amount.
（氣流分級工序）(Airflow classification process)
在本實施型態，可適當使用眾所周知的氣流分級裝置將有醇附著之金屬粉體氣流分級。惟就降低空氣黏度且實現氧化物量之減低的觀點而言，分級溫度定為35℃以下。另一方面，分級溫度之下限並不特別受限，但以0℃以上為佳。In this embodiment, a well-known airflow classification device can be used to appropriately classify the metal powder with alcohol adhered to it. However, from the viewpoint of reducing the viscosity of air and reducing the amount of oxides, the classification temperature is set to 35 ° C or lower. On the other hand, the lower limit of the classification temperature is not particularly limited, but is preferably 0 ° C or higher.
在氣流分級中，分級壓力並不特別受限。就消除金屬粉體之粗大粒子的觀點而言，分級壓力以0.2 MPa以上為佳。再者，亦鑑於後述理由，分級壓力可定為0.2 MPa以上且0.8 MPa以下。分級壓力以0.3 MPa以上且0.6 MPa以下為較佳。In air flow classification, the classification pressure is not particularly limited. From the viewpoint of eliminating coarse particles of metal powder, the classification pressure is preferably 0.2 MPa or more. Furthermore, for reasons described below, the classification pressure may be set to be 0.2 MPa or more and 0.8 MPa or less. The classification pressure is preferably 0.3 MPa or more and 0.6 MPa or less.
在本實施型態，可藉由氣流分級來充分去除金屬粉體中的醇。氣流分級中的醇去除，不僅就獲得微細金屬粉體的觀點而言為佳，就減低金屬粉體中之C含量的觀點而言亦為佳。另一方面，分級壓力之上限值並不特別受限，但經發明人等實驗，結果默示：即使將分級壓力定為超過0.8 MPa，亦難以期待有進一步的效果提升。據此，氣流分級工序之分級壓力的上限值可定為0.8 MPa以下。In this embodiment, the alcohol in the metal powder can be sufficiently removed by airflow classification. The removal of alcohol in the air flow classification is not only preferable from the viewpoint of obtaining fine metal powder, but also preferable 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, but the results of experiments by the inventors suggest that even if the classification pressure is set to exceed 0.8 MPa, it is difficult to expect further improvement in effect. Accordingly, the upper limit value of the classification pressure in the air flow classification process can be set to 0.8 MPa or less.
藉由本實施型態，可製造粒度分布為窄的微粉體。供至醇附著處理及氣流分級的金屬粉體之平均粒徑並不特別受限，但舉例而言，以個數平均粒徑計，能使用30 nm以上且200 nm以下的金屬粉體，還能使用70 nm以上且200 nm以下的金屬粉體。藉此，可將所製造之金屬粉體的個數平均粒徑做成200 nm以下。在本實施型態中，個數平均粒徑藉由掃描式電子顯微鏡拍攝金屬粉體之照片，自其照片量測約1,000個粒子的粒徑，採用其平均值。此外，粒徑定為將粒子包入之最小圓的直徑。With this embodiment, a fine powder having a narrow particle size distribution can be manufactured. The average particle size of the metal powder supplied to the alcohol adhesion treatment and air flow classification is not particularly limited, but for example, based on the number average particle size, metal powders of 30 nm to 200 nm can be used. Metal powders above 70 nm and below 200 nm can be used. Thereby, the number average particle diameter of the manufactured metal powder can be made 200 nm or less. In this embodiment, the number average particle diameter is a photograph of a metal powder taken by a scanning electron microscope, and the particle diameter of about 1,000 particles is measured from the photograph, and the average value is used. In addition, the particle diameter is determined as the diameter of the smallest circle in which the particles are enclosed.
『實施例』『Examples』
以下說明上述實施型態之實施例。本實施型態之技術範圍並不受限於以下實施例。Examples of the above implementation modes are described below. The technical scope of this embodiment is not limited to the following examples.
使用「個數平均粒徑180 nm、藉由後述方法求得之CV值為30%」的Ni粉體進行以下試驗。亦即，使表1所示之醇藉由加熱氣化法、常溫噴霧法或浸滲及乾燥法附著於上述Ni粉體。醇使用乙醇或SOLMIX A-7（JAPAN ALCOHOL TRADING CO., LTD.製之甲醇、乙醇、1-丙醇混合物）。The following tests were performed using Ni powder having a "number average particle diameter of 180 nm and a CV value determined by the method described later of 30%". That is, the alcohol shown in Table 1 was adhered to the Ni powder by a heating vaporization method, a normal temperature spray method, or an infiltration and drying method. As the alcohol, ethanol or SOLMIX A-7 (a mixture of methanol, ethanol, and 1-propanol manufactured by JAPAN ALCOHOL TRADING CO., LTD.) Was used.
在加熱氣化法中，使醇在惰性氣體環境下約於80℃加熱氣化而獲得加熱氣化醇，將此加熱氣化醇導入攪拌下的Ni粉體，使醇附著。在常溫噴霧法中，在常溫下將醇噴於攪拌下的Ni粉體，使醇附著於Ni粉體。醇附著處理後之Ni粉體中的醇附著量揭示於表1。In the heating gasification method, the alcohol is heated and gasified at about 80 ° C. in an inert gas environment to obtain a heated gasified alcohol, and the heated gasified alcohol is introduced into a stirred Ni powder to adhere the alcohol. In the normal temperature spray method, alcohol is sprayed on the Ni powder under stirring at normal temperature, so that the alcohol adheres to the Ni powder. The alcohol adhesion amount in the Ni powder after the alcohol adhesion treatment is shown in Table 1.
將分級壓力設定成0.4 MPa，將分級機內之分級溫度設定成室溫（35℃以下）或75℃，藉由NIPPON PNEUMATIC MFG. CO., LTD.製之分級機Cnine，將以各種相異的方法使醇附著的Ni粉體氣流分級。係為製造對象之Ni金屬粉體回收至細粉漏斗，其以外者收集至粗粉漏斗。此外，使用利用壓縮機而獲得之壓縮空氣，作為導入至分級機的壓縮氣體。所獲得之Ni粉體的回收率、粒度分布及氧化物量揭式於表1。The classification pressure is set to 0.4 MPa, and the classification temperature in the classifier is set to room temperature (below 35 ° C) or 75 ° C. The classification machine Cnine by NIPPON PNEUMATIC MFG. CO., LTD. The method is used to classify the airflow of alcohol-attached Ni powder. The Ni metal powder that is the object of manufacture is recovered to the fine powder funnel, and the others are collected to the coarse powder funnel. The compressed air obtained by the compressor was used as the compressed gas introduced into the classifier. The recovery rate, particle size distribution, and oxide amount of the obtained Ni powder are shown in Table 1.
（回收率）(Recovery rate)
依據下式求得回收至細粉漏斗之Ni粉體的回收率（%）。回收率13%以上評價為「〇」，視為合格。「╳」評價之比較例皆為回收率10%以下，搆不著上述合格之基準，為不足的結果。
｛［（原料置入量）－（粗粉漏斗粉體量）］／原料置入量｝×100The recovery rate (%) of the Ni powder recovered to the fine powder funnel was obtained according to the following formula. A recovery rate of 13% or more was evaluated as "0" and it was regarded as a pass. The comparative examples of the "╳" evaluations were all with a recovery rate of 10% or less, which did not constitute the above-mentioned pass criteria, and were insufficient results.
｛[(Injection amount of raw materials)-(Amount of coarse powder funnel powder)] / Injection amount of raw materials｝ × 100
（粒度分布）(Particle size distribution)
使用影像分析軟體（MOUNTECH股份有限公司製，商品名MacView 4.0）在30 k倍觀察1個視野（粒子個數約500個），求得個數平均粒徑與其標準差。由「［標準差（單位：μm）／個數平均粒徑（單位：μm）］×100」之式求得CV。CV值22%以下評價為「〇」，視為合格。An image analysis software (manufactured by MOUNTECH Co., Ltd., MacView 4.0) was used to observe 1 field of view (approximately 500 particles) at 30 k times, and the number average particle diameter and its standard deviation were obtained. The CV was obtained from the formula "[standard deviation (unit: μm) / number average particle size (unit: μm)] × 100". A CV value of 22% or less was evaluated as "0" and considered to be a pass.
實施例之No. 1～4之CV值為小（粒度分布為窄），可有效率妥善回收粉體。此外，該實施例1～4之個數平均粒徑在160 nm～180 nm之範圍內。比較例之No. 5由於在無醇的條件下進行，且分級溫度為高，故CV值未達到目標，且回收率亦不足。比較例之No. 6由於在無醇的條件下進行，故回收率不足。比較例之No. 7由於分級溫度為高，故CV值未達到目標。The CV values of Nos. 1 to 4 in the examples are small (the particle size distribution is narrow), and the powder can be efficiently and properly recovered. The number average particle diameters of Examples 1 to 4 are in the range of 160 nm to 180 nm. Comparative Example No. 5 was performed under alcohol-free conditions and the classification temperature was high, so the CV value did not reach the target, and the recovery rate was also insufficient. Comparative Example No. 6 had insufficient recovery because it was performed under the condition of no alcohol. In Comparative Example No. 7, the classification temperature was high, so the CV value did not reach the target.
此外，針對No. 1～5，確認粒徑0.4 μm以上之粗大粒子數。具體而言，使用上述影像分析軟體在10 k倍拍攝10個視野，量測0.4 μm以上的粗大粒子數。在No. 1～4之粗大粒子數為0～1個，相對在No. 5之粗大粒子數為3個。若亦考量No. 6的結果，則可認為在氣流分級溫度為高之情形中粗大粒子數會增加。In addition, for Nos. 1 to 5, the number of coarse particles having a particle diameter of 0.4 μm or more was confirmed. Specifically, the above image analysis software was used to capture 10 fields of view at 10 k times, and the number of coarse particles above 0.4 μm was measured. The number of coarse particles in No. 1 to 4 is 0 to 1, and the number of coarse particles in No. 5 is three. If the result of No. 6 is also considered, it can be considered that the number of coarse particles increases when the airflow classification temperature is high.
（氧化物量）(Amount of oxide)
針對實施例，藉由X射線光電子光譜（XPS）估算氧化物量。具體上係如以下內容。使用Thermo Fisher Scientific股份有限公司製之K-Alpha+ 作為使用機器。使用AlKα線作為光源。Ni2p之量測能量範圍定為884～844（eV），C1s之量測能量範圍定為298～279（eV）。對於所獲得之光譜，藉由雪萊（Shirley）法去除背景後，以組合了勞侖茲函數與高斯函數的函數進行波形分離。歸於金屬鎳之尖峰──亦即源自於Ni－Ni鍵結之尖峰的面積──定為852.4（eV）及858.5（eV）之尖峰面積的總和。歸於Ni－O鍵結之尖峰面積定為853.4（eV）、854.2（eV）、855.3（eV）、858.2（eV）、860.6（eV）、863.2（eV）及865.4（eV）之尖峰面積的總和。歸於Ni－OH鍵結之尖峰面積係藉由以下方式來求得。首先，求得854.5（eV）、855.7（eV）、857.4（eV）、861.1（eV）、862.4（eV）及865.4（eV）之尖峰面積的總和。自此總和減去歸於Ni－C鍵結之288.5（eV）之尖峰面積，定為源自於Ni－OH鍵結之尖峰面積。歸於Ni－Ni鍵結之尖峰面積、歸於Ni－O鍵結之尖峰面積及歸於Ni－OH鍵結之尖峰面積的合計中，歸於Ni－Ni鍵結之尖峰面積所佔的比例，係藉由XPS量測求得之金屬鎳的比例。For the embodiment, the amount of oxide is estimated by X-ray photoelectron spectroscopy (XPS). The details are as follows. K-Alpha + manufactured by Thermo Fisher Scientific Co., Ltd. was used as a machine. As the light source, AlKα rays were used. The measurement energy range of Ni2p is set to 884 to 844 (eV), and the measurement energy range of C1s is set to 298 to 279 (eV). For the obtained spectrum, the background was removed by the Shirley method, and the waveform was separated by a function combining a Lorentz function and a Gaussian function. The spikes attributed to metallic nickel--that is, the area of the spikes derived from the Ni-Ni bond--were determined as the sum of the peak areas of 852.4 (eV) and 858.5 (eV). The area of the peaks attributed to the Ni-O bond is determined as the sum of the areas of the peaks of 853.4 (eV), 854.2 (eV), 855.3 (eV), 858.2 (eV), 860.6 (eV), 863.2 (eV), and 865.4 (eV). . The area of the peak attributed to the Ni-OH bond was obtained in the following manner. First, find the sum of the peak areas of 854.5 (eV), 855.7 (eV), 857.4 (eV), 861.1 (eV), 862.4 (eV), and 865.4 (eV). The peak area of 288.5 (eV) attributed to the Ni-C bond was subtracted from this sum, and it was determined to be the peak area derived from the Ni-OH bond. The total area of the peak area attributed to the Ni-Ni bond, the area of the peak attributed to the Ni-O bond, and the area of the peak attributed to the Ni-OH bond, the proportion of the area of the peak attributed to the Ni-Ni bond is determined by The ratio of metallic nickel obtained by XPS measurement.
此外，歸於金屬鎳之尖峰的尖峰位置，若使用Ni作為標準品，即能將之特定。歸於Ni－O鍵結之尖峰的尖峰位置，若使用NiO作為標準品即能將之特定。歸於Ni－OH鍵結之尖峰的尖峰位置，若使用Ni（OH）2 即能將之特定。歸於Ni－C鍵結的尖峰位置，若使用NiCO3 即能將之特定。In addition, the peak position attributed to the peak of metallic nickel can be specified by using Ni as a standard. The peak position attributed to the spike of the Ni-O bond can be specified if NiO is used as a standard. The peak position attributed to the peak of the Ni-OH bond can be specified if Ni (OH) 2 is used. The peak position of the Ni-C bond can be specified if NiCO 3 is used.
XPS量測之結果，在實施例中獲得之鎳粉體中，確認到相對於金屬Ni、Ni－O及Ni－OH的合計面積，歸於金屬Ni之尖峰面積皆顯示有30～35%，在Ni粉體表層部之Ni比例為高，Ni粉體之氧化受到抑制。As a result of the XPS measurement, in the nickel powder obtained in the examples, it was confirmed that the peak area attributed to the metal Ni relative to the total area of the metal Ni, Ni-O, and Ni-OH showed 30 to 35%. The Ni ratio in the surface layer portion of the Ni powder is high, and the oxidation of the Ni powder is suppressed.
『表1』
如在本實施例中實驗所示，藉由應用本實施型態，能夠有效率製造粒度分布為窄之金屬粉體。As shown by experiments in this embodiment, by applying this embodiment mode, metal powders with a narrow particle size distribution can be efficiently produced.
無。no.
〈圖1〉本發明之一實施型態相關之分級方法的流程圖。<Fig. 1> A flowchart of a method for grading related to a form of implementation of the present invention.
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