JP7087860B2 - A method for preparing a sample for measuring the particle size distribution and / or the particle shape of the powder, and a method for measuring the particle size distribution and / or the particle shape of the powder. - Google Patents
A method for preparing a sample for measuring the particle size distribution and / or the particle shape of the powder, and a method for measuring the particle size distribution and / or the particle shape of the powder. Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims description 158
- 239000000843 powder Substances 0.000 title claims description 93
- 238000000034 method Methods 0.000 title claims description 31
- 238000005259 measurement Methods 0.000 claims description 49
- 238000003703 image analysis method Methods 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、粉体の粒度分布および／または粒子形状の測定に用いる測定用試料の作製方法、並びに、作製された当該測定用試料を用いた、粉体の粒度分布および／または粒子形状の測定方法に係る。 The present invention relates to a method for preparing a measurement sample used for measuring the particle size distribution and / or particle shape of a powder, and the measurement of the particle size distribution and / or particle shape of a powder using the prepared measurement sample. It concerns the method.
粉体の物理的特性の把握を目的として、粒度分布測定装置は広く用いられている。中でも、測定対象粉体の粒子形状を測定、評価することも可能な、画像解析法を用いた乾式粒度分布計が広く用いられている。
当該画像解析法を用いた乾式粒度分布計においては、当該乾式粒度分布計に装備された測定用プレート（本発明において、単に「測定用プレート」と記載する場合がある。）上に存在する測定対象粉体の粒子を専用のＣＣＤカメラで撮影し、撮影画像から粒子の大きさや数、粒子形状を測定するという測定フローにより画像解析を実施する。従って、測定用プレート上に存在する測定対象粉体の粒子には、均一、且つ粒子同士の重なりがない様、十分に分散していることが望まれる。
A particle size distribution measuring device is widely used for the purpose of grasping the physical characteristics of powder. Among them, a dry particle size distribution meter using an image analysis method, which can measure and evaluate the particle shape of the powder to be measured, is widely used.
In the dry particle size distribution meter using the image analysis method, the measurement existing on the measurement plate (may be simply referred to as “measurement plate” in the present invention) equipped on the dry particle size distribution meter. The particles of the target powder are photographed with a dedicated CCD camera, and image analysis is performed by a measurement flow of measuring the size, number, and particle shape of the particles from the photographed image. Therefore, it is desired that the particles of the powder to be measured existing on the measurement plate are uniformly dispersed so that the particles do not overlap with each other.
上述の要請を満足する為、従来の技術において、所定の分散チャンバーを用い、当該チャンバー上に、例えばフィルムを介して測定対象粉体を貯留しておく。一方、当該チャンバー内の底部には測定用プレートを載置する。そして、当該チャンバー内部を減圧することによって、当該チャンバーの内外に、チャンバー内部を低圧側とする気圧差を設定する方法がある。
そして、前記フィルムが減圧により破れることで、当該チャンバー上に貯留された測定対象粉体を、気圧差によりチャンバー内に飛散させる。この結果、当該チャンバー内に飛散した測定対象粉体の粒子は、前記載置された測定用プレート上に、均一、且つ粒子同士の重なりなく分散することを目論むものである。
In order to satisfy the above-mentioned requirements, in the conventional technique, a predetermined dispersion chamber is used, and the powder to be measured is stored on the chamber, for example, via a film. On the other hand, a measurement plate is placed on the bottom of the chamber. Then, there is a method of setting a pressure difference with the inside of the chamber as the low pressure side inside and outside the chamber by reducing the pressure inside the chamber.
Then, when the film is torn by the reduced pressure, the powder to be measured stored in the chamber is scattered in the chamber due to the difference in atmospheric pressure. As a result, the particles of the powder to be measured scattered in the chamber are intended to be uniformly dispersed on the measurement plate placed above without overlapping with each other.
以上説明した、気圧差を用いた粒子の減圧分散の他にも、例えば、特許文献１には、粒子を液体溶媒に分散させ、スラリー状にしたものを測定用プレート上に塗布して、測定対象粉体の粒子を測定用プレート上に、均一、且つ粒子同士の重なりなく分散する方法が記載されている。
In addition to the vacuum dispersion of particles using the pressure difference described above, for example, in
しかしながら、本発明者らの検討によると、例えばアルカリ金属元素の水酸化物のように脆性の高い粒子を含む粉体を測定対象粉体とし、上述した気圧差を用いる粒子の減圧分散方法を適用した場合、粒子の破砕が生じてしまうことを知見した。
一方、当該アルカリ金属元素の水酸化物のように水等の溶媒に対する溶解性の高い粒子の場合は、当該測定対象粉体を液体溶媒に分散させ、スラリー状にしたものを測定用プレート上に塗布する方法も適応が困難であった。
However, according to the study by the present inventors, a powder containing highly brittle particles such as a hydroxide of an alkali metal element is used as the measurement target powder, and the above-mentioned vacuum dispersion method of particles using the pressure difference is applied. It was found that if this is the case, the particles will be crushed.
On the other hand, in the case of particles having high solubility in a solvent such as water such as the hydroxide of the alkali metal element, the powder to be measured is dispersed in a liquid solvent and made into a slurry on the measurement plate. The method of application was also difficult to adapt.
本発明は、上述の状況の下で為されたもので、その解決しようとする課題は、脆性が高く、溶解性も高い粒子を含む粉体であっても、当該粒子の破砕を生じることなく、均一、且つ粒子同士の重なりなく測定用プレート上に分散させる、粉体の粒度分布および／または粒子形状の測定に用いる測定用試料の作製方法、並びに、作製された当該測定用試料を用いた、粉体の粒度分布および／または粒子形状の測定方法を提供することである。 The present invention has been made under the above-mentioned circumstances, and the problem to be solved is that even a powder containing particles having high brittleness and high solubility does not cause crushing of the particles. The method for preparing a measurement sample used for measuring the particle size distribution and / or the particle shape of the powder, which is uniformly dispersed on the measurement plate without overlapping of the particles, and the prepared measurement sample were used. , To provide a method for measuring particle size distribution and / or particle shape of a powder.
本発明者は、上述の課題を解決するため研究を行った。
そして、測定対象粉体に含まれる粒子の最大粒子径（本発明において「ｒｍａｘ」と記載する場合がある。また、本発明において単位は（μｍ）を用いている。）を超える目開き（開孔部）を有する網を選択し、当該選択された網を測定用プレート上に設置する。
そして、前記測定用プレート上に設置された網上へ前記測定対象粉体を載せ、前記測定対象粉体に含まれる粒子を、前記開孔部を介して前記測定用プレート上に分散させることで、粒子の破砕を生じさせることなく、均一、且つ粒子同士の重なりなく分散させることが出来るとの画期的な知見を得て、本発明を完成した。
尚、測定対象粉体に含まれる粒子における最大粒子径は、あらかじめ、適宜な方法により測定対象粉体の粒度分布測定を行って、把握しておけば良い。
The present inventor conducted research to solve the above-mentioned problems.
Then, the opening exceeds the maximum particle size of the particles contained in the powder to be measured (may be described as "r max " in the present invention, and the unit is (μm) in the present invention). A net having a perforation) is selected and the selected net is placed on the measuring plate.
Then, the measurement target powder is placed on the net installed on the measurement plate, and the particles contained in the measurement target powder are dispersed on the measurement plate through the pores. The present invention has been completed with the epoch-making finding that the particles can be dispersed uniformly and without overlapping with each other without causing crushing of the particles.
The maximum particle size of the particles contained in the powder to be measured may be known in advance by measuring the particle size distribution of the powder to be measured by an appropriate method.
即ち、上述の課題を解決する為の第１の発明は、
粉体の粒度分布および／または粒子形状を、画像解析法により測定する際に用いられる測定用試料の作製方法であって、
測定対象粉体の粒子径測定を行い、前記測定対象粉体に含まれる粒子の最大粒子径をｒｍａｘ（μｍ）としたとき、
ｒｍａｘ（μｍ）を超える目開きを有する網を選択して、前記画像解析法を用いた粒度分布測定に用いる装置の測定用プレート上に設置し、
前記測定用プレート上に設置された網上へ前記測定対象粉体を載せ、
前記測定対象粉体を、前記網の開孔部を介して落下させることにより、前記測定用プレート上に前記測定対象粉体を分散させることを特徴とする、粉体の粒度分布および／または粒子形状の測定用試料の作製方法である。
第２の発明は、
前記網の選択の際、１．５ｒｍａｘ（μｍ）以上、３．０ｒｍａｘ（μｍ）以下の目開きを有する網を選択することを特徴とする、第１の発明に記載の粉体の粒度分布および／または粒子形状の測定用試料の作製方法である。
第３の発明は、
前記測定対象粉体の粒子径測定を、レーザー回折・散乱方式の粒度分布測定装置を用いて測定することを特徴とする、第１または第２の発明に記載の粉体の粒度分布および／または粒子形状測の測定用試料の作製方法である。
第４の発明は、
前記網として篩を用いることを特徴とする、第１から第３の発明のいずれかに記載の粉体の粒度分布および／または粒子形状の測定用試料の作製方法である。
第５の発明は、
第１から第４の発明のいずれかに記載の粉体の粒度分布および／または粒子形状の測定用試料の作製方法にて作製された測定用試料を用い、画像解析法により測定対象粉体の粒度分布および／または粒子形状の測定を行うことを特徴とする、粉体の粒度分布および／または粒子形状の測定方法である。
That is, the first invention for solving the above-mentioned problems is
A method for preparing a measurement sample used when measuring the particle size distribution and / or particle shape of a powder by an image analysis method.
When the particle size of the powder to be measured is measured and the maximum particle size of the particles contained in the powder to be measured is r max (μm).
A net having a mesh size exceeding r max (μm) was selected and installed on the measurement plate of the apparatus used for the particle size distribution measurement using the image analysis method.
The powder to be measured is placed on a net installed on the measurement plate, and the powder to be measured is placed on the net.
The particle size distribution and / or particles of the powder, which is characterized in that the powder to be measured is dispersed on the plate for measurement by dropping the powder to be measured through the opening of the net. This is a method for preparing a sample for measuring the shape.
The second invention is
The particle size of the powder according to the first invention, which comprises selecting a net having a mesh size of 1.5r max (μm) or more and 3.0r max (μm) or less when selecting the net. A method for preparing a sample for measuring distribution and / or particle shape.
The third invention is
The particle size distribution and / or the powder size distribution according to the first or second invention, wherein the particle size of the powder to be measured is measured by using a laser diffraction / scattering type particle size distribution measuring device. This is a method for preparing a sample for measurement of particle shape measurement.
The fourth invention is
The method for preparing a sample for measuring a particle size distribution and / or a particle shape of a powder according to any one of the first to third inventions, which comprises using a sieve as the net.
The fifth invention is
Using the measurement sample prepared by the method for preparing a sample for measuring the particle size distribution and / or the particle shape of the powder according to any one of the first to fourth inventions, the powder to be measured is subjected to an image analysis method. It is a method for measuring the particle size distribution and / or the particle shape of a powder, which comprises measuring the particle size distribution and / or the particle shape.
本発明に係る粉体の粒度分布および／または粒子形状の測定用試料の作製方法によれば、測定対象粉体の粒子を、粒子の破砕を生じることなく、均一で、且つ粒子同士の重なりなく測定用プレート上に分散させることが出来た。 According to the method for preparing a sample for measuring the particle size distribution and / or the particle shape of the powder according to the present invention, the particles of the powder to be measured are uniform without causing crushing of the particles and without overlapping of the particles. It could be dispersed on the measuring plate.
本発明を実施するための形態について、図１に示す作業フローを参照しながら説明する。 A mode for carrying out the present invention will be described with reference to the work flow shown in FIG.
１．測定対象粉体に含まれる粒子の最大粒子径の把握
本発明においては、後述する網の選択に備えて、あらかじめ測定対象粉体に含まれる粒子の粒度分布を把握し、当該測定対象粉体に含まれる粒子のｒｍａｘ（μｍ）を把握する。
1. 1. Understanding the maximum particle size of the particles contained in the powder to be measured In the present invention, in preparation for the selection of the net described later, the particle size distribution of the particles contained in the powder to be measured is grasped in advance, and the powder to be measured is used. Grasp the r max (μm) of the contained particles.
測定対象粉体に含まれる粒子のｒｍａｘ（μｍ）を把握する方法は特に限定されず、公知の方法から適宜選択すれば良い。
本発明の適用対象となる測定対象粉体は、脆性が高く、溶解性も高い粒子である場合があるので、当該粒子のｒｍａｘ（μｍ）測定方法としては、公知の乾式の分散手段を用いたレーザー回折・散乱法、篩分け法による乾式粒度分布測定等を、好ましく用いることが出来る。
これら従来の技術に係る測定方法によれば、測定対象粉体に含まれる粒子の脆性が高い場合、当該粒子が破砕され、その粒度分布が変化してしまうことが考えられる。しかし、本発明のこの段階においては、測定対象粉体に含まれる粒子の最大粒子径ｒｍａｘ（μｍ）を把握することが目的なので、測定対象粉体の粒子の一部が破砕されていても、当該目的は達成出来る。
The method for grasping the r max (μm) of the particles contained in the powder to be measured is not particularly limited, and a known method may be appropriately selected.
Since the powder to be measured to which the present invention is applied may be particles having high brittleness and high solubility, a known dry dispersion means is used as a method for measuring r max (μm) of the particles. The laser diffraction / scattering method, the dry particle size distribution measurement by the sieving method, and the like can be preferably used.
According to the measuring methods according to these conventional techniques, if the particles contained in the powder to be measured are highly brittle, it is conceivable that the particles are crushed and the particle size distribution is changed. However, at this stage of the present invention, since the purpose is to grasp the maximum particle diameter r max (μm) of the particles contained in the powder to be measured, even if some of the particles of the powder to be measured are crushed. , The purpose can be achieved.
２．メッシュの選択
測定対象粉体に粒子の破砕を生じることなく、均一、且つ、粒子同士の重なりなく測定用プレート上に、測定対象粉体の粒子を分散させる為、本発明においては所定の目開き（開孔部）を有する網を用いる。
当該網におけるメッシュの選択について図２を参照しながら説明する。
当該図２において、粒子が破砕されなかった場合は、測定対象粉体における最大粒子径を有する粒子１０のｒｍａｘ（μｍ）は、粒子径１１のことである。粒子が破砕された場合は、測定対象粉体における最大粒子径を有する粒子１０のｒｍａｘ（μｍ）は、粒子径１１とは一致せずに小さくなり、実粒子径ｒｒｍａｘが粒子径１１となる。一方、メッシュを構成する線材２１は、開孔部２２を形成するが、本発明においては目開きの大きさを示す単位にμｍを用い、当該開孔部における目開きの大きさを「Ｒ（μｍ）」符号２３で示す。
2. 2. Selection of mesh In order to disperse the particles of the powder to be measured on the measurement plate uniformly and without overlapping of the particles without causing the particles to be crushed in the powder to be measured, a predetermined opening is used in the present invention. A net having (opening portion) is used.
The selection of the mesh in the net will be described with reference to FIG.
In FIG. 2, when the particles are not crushed, the r max (μm) of the
当該メッシュの選択においては、通常の篩の選択とは異なり、ｒｍａｘ（μｍ）を超える目開きＲ（μｍ）を有する網を選択する。そして、当該網の目開きは１．５ｒｍａｘ（μｍ）≦Ｒ（μｍ）≦３．０ｒｍａｘ（μｍ）であることが好ましく、１．５ｒｍａｘ（μｍ）≦Ｒ（μｍ）≦２．０ｒｍａｘ（μｍ）であることがさらに好ましい。
網の目開きが１．５ｒｍａｘ以上であれば、特に粒子の脆性が高い場合、測定されたｒｍａｘに対して、破砕されていない粒子の長径（実粒子径）ｒｒｍａｘが大きくても開孔部を通過することが出来る。網の目開きが３．０ｒｍａｘ以下であれば、粒子は均一に分散することが出来る。また二次凝集塊が開孔部を通過することを抑止出来るからである。
In the selection of the mesh, unlike the selection of a normal sieve, a net having an opening R (μm) exceeding r max (μm) is selected. The mesh opening of the mesh is preferably 1.5r max (μm) ≤ R (μm) ≤ 3.0r max (μm), and 1.5r max (μm) ≤ R (μm) ≤ 2.0r. It is more preferably max (μm).
If the mesh size of the mesh is 1.5 r max or more, especially when the brittleness of the particles is high, even if the major axis (actual particle size) r r max of the uncrushed particles is large with respect to the measured r max , it is open. It can pass through the hole. If the mesh size of the mesh is 3.0 r max or less, the particles can be uniformly dispersed. This is also because it is possible to prevent the secondary agglomerates from passing through the opening.
上述したように、本発明における網の使用目的や選択基準は、通常の篩の使用目的や選択とは異なる。しかし、網それ自体としては、本発明が求める目開きＲ（μｍ）を有する通常の篩を用いることが便宜である。 As described above, the purpose of use and selection criteria of the net in the present invention are different from the purpose of use and selection of ordinary sieves. However, as the net itself, it is convenient to use a normal sieve having the opening R (μm) required by the present invention.
３．選択されたメッシュを有する網による測定対象粉体の分散操作
測定用プレートの上方に選択されたメッシュを有する網を設置し、当該網上に測定対象粉体を載置する。そして、当該網を搖動、または、網上に載置された測定対象粉体を柔らかな刷毛等を用いて軽く掃き撫ぜることにより、測定対象粉体を、網の開孔部を介して落下させ、測定用プレート上に前記測定対象粉体を分散させる。
このとき、網として通常の篩を用いている場合、測定用プレートのプレート径より小さな径を有する篩いを用いることが便宜である。
3. 3. Dispersion operation of the powder to be measured by the net having the selected mesh A net having the selected mesh is installed above the measurement plate, and the powder to be measured is placed on the net. Then, the powder to be measured is dropped through the opening of the net by shaking the net or lightly sweeping the powder to be measured placed on the net with a soft brush or the like. Then, the powder to be measured is dispersed on the measuring plate.
At this time, when a normal sieve is used as the net, it is convenient to use a sieve having a diameter smaller than the plate diameter of the measuring plate.
実施例を参照しながら、本発明をより具体的に説明する。ただし、本発明は当該実施例に限定される訳ではない。 The present invention will be described in more detail with reference to examples. However, the present invention is not limited to the embodiment.
（実施例１）
測定対象粉体として、水酸化リチウムの結晶を含む粉体を準備した。
準備した測定対象粉体に含まれる粒子のｒｍａｘ（μｍ）を、Ｍｉｃｒｏｔｒａｃ社製粒度分布測定装置を用いて測定した。そして測定の結果、測定対象粉体のｒｍａｘ（μｍ）は４００（μｍ）であることが判明した。
(Example 1)
As the powder to be measured, a powder containing lithium hydroxide crystals was prepared.
The r max (μm) of the particles contained in the prepared powder to be measured was measured using a particle size distribution measuring device manufactured by Microtrac. As a result of the measurement, it was found that the r max (μm) of the powder to be measured was 400 (μm).
画像解析法を用いた乾式粒度分布計として、ジャスコインターナショナル社製ＶＤ－４００ｎａｎｏを準備した。当該乾式粒度分布計に装備された測定用プレートのプレート径は、１０ｃｍであった。
そこで、ｒｍａｘ（μｍ）＝４００（μｍ）の２．５倍の目開きを有し、外径が１５ｃｍの篩を網として選択した（ケニス株式会社製ステンレス篩（１６メッシュ））。
A VD-400 nano manufactured by Jusco International Co., Ltd. was prepared as a dry particle size distribution meter using an image analysis method. The plate diameter of the measuring plate mounted on the dry particle size distribution meter was 10 cm.
Therefore, a sieve having a mesh size 2.5 times that of r max (μm) = 400 (μm) and an outer diameter of 15 cm was selected as the mesh (stainless steel sieve (16 mesh) manufactured by KENIS, Ltd.).
選択した篩を測定用プレートの上方に設置し、測定対象粉体の０．１ｇを当該篩上に載置した。そして、当該篩を、測定用プレートの上方に１ｃｍ程度浮かせ、載置した測定対象粉体が全量通過する迄、当該篩を軽く搖動して、測定対象粉体の粒子を測定用プレート上に分散させた。 The selected sieve was placed above the measuring plate, and 0.1 g of the powder to be measured was placed on the sieve. Then, the sieve is floated about 1 cm above the measurement plate, and the sieve is lightly shaken until the entire amount of the placed powder to be measured passes, and the particles of the powder to be measured are dispersed on the measurement plate. I let you.
測定対象粉体の粒子が分散した測定用プレートを、画像解析法を用いた乾式粒度分布計に装填し、測定対象粉体の粒度分布を測定した。
得られた測定対象粉体の粒度分布の測定結果を、図３のグラフに実線で示す。
尚、図３のグラフは縦軸に頻度、横軸に粒子形状を円形と見なしたときの粒子径をとったものである。
The measurement plate in which the particles of the powder to be measured were dispersed was loaded into a dry particle size distribution meter using an image analysis method, and the particle size distribution of the powder to be measured was measured.
The measurement result of the particle size distribution of the obtained powder to be measured is shown by a solid line in the graph of FIG.
In the graph of FIG. 3, the vertical axis shows the frequency and the horizontal axis shows the particle size when the particle shape is regarded as a circle.
図３のグラフより、測定対象粉体の粒子は粒子径９０μｍおよび１０μｍに二山のピークを有する粒度分布を有していることが判明した。 From the graph of FIG. 3, it was found that the particles of the powder to be measured had a particle size distribution having two peaks at the particle diameters of 90 μm and 10 μm.
（比較例１）
実施例１と同様の測定対象粉体を準備した。
画像解析法を用いた乾式粒度分布計として、実施例１と同様のジャスコインターナショナル社製ＶＤ－４００ｎａｎｏを準備した。
測定対象粉体を、減圧分散装置（ジャスコインターナショナル社製分散器）を用いて、当該乾式粒度分布計に装備された測定用プレートに減圧分散させた。
得られた測定対象粉体の粒度分布の測定結果を、図３のグラフに破線で示す
図３のグラフより、測定対象粉体の粒子は粒子径９μｍに一山のピークを有し、８０μｍにわずかなショルダーを有しているとの結果が得られた。
(Comparative Example 1)
The same powder to be measured as in Example 1 was prepared.
As a dry particle size distribution meter using an image analysis method, a VD-400 nano manufactured by Jusco International Co., Ltd., which was the same as in Example 1, was prepared.
The powder to be measured was dispersed under reduced pressure on a measuring plate equipped with the dry particle size distribution meter using a vacuum dispersion device (dispersor manufactured by Jasco International Co., Ltd.).
The measurement result of the particle size distribution of the obtained powder to be measured is shown by a broken line in the graph of FIG. 3. From the graph of FIG. 3, the particles of the powder to be measured have a peak at a particle diameter of 9 μm and reach 80 μm. The result was that it had a slight shoulder.
（まとめ）
図３のデータを検討すると、実施例１では観測出来ていた粒子径９０μｍのピークが、比較例１では殆ど観測出来なかった。このことから、測定対象粉体を、従来の技術に係る減圧分散装置を用いて分散操作を行った場合は粉体粒子が破砕されて、本来の粒度分布が測定出来ていないのではないかと考えられた。
そこで、比較例１に係る分散操作前後における測定対象粉体の５０倍の顕微鏡像を観察した。両者を比較すると、分散操作後の測定対象粉体の粒子は、分散操作前に較べて尖った形状をしており、比較例１に係る減圧分散操作によって破砕が起こったと考えられた。
これに対し、粒度分布が正確に測定出来ている実施例１においては、網による分散操作の前後において、測定対象粉体の粒子形状に殆ど変化は見られなかった。
(summary)
Examining the data in FIG. 3, the peak with a particle size of 90 μm that could be observed in Example 1 was hardly observed in Comparative Example 1. From this, it is considered that when the powder to be measured is dispersed by using the vacuum dispersion device according to the conventional technique, the powder particles are crushed and the original particle size distribution cannot be measured. Was done.
Therefore, a microscope image 50 times larger than that of the powder to be measured before and after the dispersion operation according to Comparative Example 1 was observed. Comparing the two, the particles of the powder to be measured after the dispersion operation had a sharper shape than those before the dispersion operation, and it was considered that crushing occurred by the reduced pressure dispersion operation according to Comparative Example 1.
On the other hand, in Example 1 in which the particle size distribution could be accurately measured, almost no change was observed in the particle shape of the powder to be measured before and after the dispersion operation by the net.
以上より、本発明に係る測定対象粉体の粒度分布および／または粒子形状の測定に用いる測定用試料の作製方法、並びに、作製された当該測定用試料を用いた、粒度分布および／または粒子形状の測定方法によれば、従来の技術に係る方法に較べて、粒度分布や粒子形状が正確に観測出来ているものと考えられた。
Based on the above, the method for preparing a measurement sample used for measuring the particle size distribution and / or particle shape of the powder to be measured according to the present invention, and the particle size distribution and / or particle shape using the prepared measurement sample. According to the measurement method of, it was considered that the particle size distribution and the particle shape could be observed more accurately than the method according to the conventional technique.
Claims (4)
測定対象粉体の粒子径測定を行い、前記測定対象粉体に含まれる粒子の最大粒子径をｒｍａｘ（μｍ）としたとき、
１．５ｒ ｍａｘ （μｍ）以上、３．０ｒ ｍａｘ （μｍ）以下の目開きを有する網を選択して、前記画像解析法を用いた粒度分布測定に用いる装置の測定用プレート上に設置し、
前記測定用プレート上に設置された網上へ前記測定対象粉体を載せ、
前記測定対象粉体を、前記網の開孔部を介して落下させることにより、前記測定用プレート上に前記測定対象粉体を分散させることを特徴とする、粉体の粒度分布および／または粒子形状の測定用試料の作製方法。 A method for preparing a measurement sample used when measuring the particle size distribution and / or particle shape of a powder containing hydroxide particles of an alkali metal element by an image analysis method.
When the particle size of the powder to be measured is measured and the maximum particle size of the particles contained in the powder to be measured is r max (μm).
A net having a mesh size of 1.5r max (μm) or more and 3.0r max (μm) or less was selected and installed on the measurement plate of the device used for the particle size distribution measurement using the image analysis method.
The powder to be measured is placed on a net installed on the measurement plate, and the powder to be measured is placed on the net.
The particle size distribution and / or particles of the powder, which is characterized in that the powder to be measured is dispersed on the plate for measurement by dropping the powder to be measured through the opening of the net. How to prepare a sample for shape measurement.
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