JP4944859B2 - Particle property measuring device - Google Patents
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- 239000002245 particle Substances 0.000 title claims description 106
- 238000005259 measurement Methods 0.000 claims description 68
- 230000007246 mechanism Effects 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 28
- 230000000704 physical effect Effects 0.000 claims description 27
- 238000000733 zeta-potential measurement Methods 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 5
- 230000005684 electric field Effects 0.000 description 19
- 230000002776 aggregation Effects 0.000 description 10
- 230000003287 optical effect Effects 0.000 description 9
- 238000004220 aggregation Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 6
- 239000011164 primary particle Substances 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000011163 secondary particle Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000010365 information processing Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001370 static light scattering Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
この発明は、アスペクト比や凝集度等の形状物性値、粒径、及び、ゼータ電位等を測定することができる粒子物性測定装置に関するものである。 The present invention relates to a particle property measuring apparatus capable of measuring shape property values such as aspect ratio and degree of aggregation, particle size, zeta potential, and the like.
近時、多様な形状を有するナノ粒子に対する産業界の需要が高まり、ナノ粒子の粒径や他の物性を詳細に計測することへの市場のニーズが高まっている。 Recently, the industry demand for nanoparticles having various shapes has increased, and the market needs for measuring the particle size and other physical properties of nanoparticles in detail.
従来のナノ粒子の物性は、アスペクト比や凝集度等の形状物性値は走査型電子顕微鏡（ＳＥＭ）等の電子顕微鏡又は光学顕微鏡の観察により、粒径は動的光散乱法により、分散度はゼータ電位を測定することにより、それぞれ別個の分析装置を用いて測定されている。 The physical properties of conventional nanoparticles are as follows: physical property values such as aspect ratio and degree of aggregation are observed with an electron microscope such as a scanning electron microscope (SEM) or an optical microscope, the particle size is determined by dynamic light scattering, and the degree of dispersion is Each zeta potential is measured using a separate analyzer.
そして、電子顕微鏡又は光学顕微鏡を用いた場合は、画像処理結果として形状物性値や粒径が算出され、粒径分布測定装置を用いた場合の測定結果は、粒径が数値として、粒径分布がヒストグラムとして提示され、ゼータ電位測定装置を用いた場合は、ゼータ電位が数値又は分布として提示される。ゼータ電位とは、溶液中の微粒子の表面電荷であり、すなわち、溶液中の微粒子の周りに形成する電気二重層中の、液体流動が起こり始める「すべり面」の電位である。微粒子の場合、ゼータ電位の絶対値が増加すれば、粒子間の反発力が強くなり、粒子の安定性は高くなる。逆に、ゼータ電位がゼロに近くなると、粒子は凝集しやすくなる。すなわち、粒子の帯電量（荷電状態）によって、粒子の分散状態の安定性は左右されるため、溶液中の微粒子の凝集・分散制御及び特性評価に際して、ゼータ電位測定の重要度は高まってきている。 When an electron microscope or an optical microscope is used, shape physical property values and particle sizes are calculated as image processing results, and when using a particle size distribution measuring device, the particle size is a numerical value. Is presented as a histogram, and when the zeta potential measuring device is used, the zeta potential is presented as a numerical value or a distribution. The zeta potential is the surface charge of the fine particles in the solution, that is, the potential of the “slip surface” where liquid flow starts to occur in the electric double layer formed around the fine particles in the solution. In the case of fine particles, if the absolute value of the zeta potential increases, the repulsive force between the particles becomes stronger and the stability of the particles becomes higher. Conversely, when the zeta potential is close to zero, the particles tend to aggregate. In other words, since the stability of the dispersion state of the particles depends on the charge amount (charge state) of the particles, the importance of the zeta potential measurement is increasing in the control of the aggregation / dispersion of the fine particles in the solution and the characteristic evaluation. .
しかし、これらの測定結果は、装置の原理に熟知した測定者であれば容易に解釈することができるが、測定に不慣れな者にとっては、得られた数値や分布の持つ意味の解釈が難しいことがあった。
そこで本発明は、粒子の各種物性の測定に不慣れな者であっても、視覚を介して直接的かつ容易に測定結果を理解することが可能な粒子物性測定装置を提供すべく図ったものである。 Therefore, the present invention is intended to provide a particle property measuring apparatus that enables a person who is unfamiliar with measuring various physical properties of particles to understand the measurement result directly and easily through vision. is there.
すなわち本発明に係る粒子物性測定装置は、液体試料中に分散している粒子のアスペクト比や凝集度等を求める形状物性値測定機構と、該粒子の粒径を測定する粒径測定機構と、該粒子のゼータ電位を測定するゼータ電位測定機構と、を少なくとも備えた粒子物性測定装置であって、前記形状物性値測定機構及び前記粒径測定機構における測定結果データに基づき、粒子表面形状と粒子の大きさを画像として表示するための粒子画像データと、前記ゼータ電位測定機構における測定結果データに基づき、粒子のゼータ電位を該粒子の粒子表面からの層の大きさ及び／又は粒子表面からの層の色として表示するためのゼータ電位画像データと、を作成する画像データ作成部を更に備えていることを特徴とする。 That is, the particle property measuring apparatus according to the present invention includes a shape property value measuring mechanism for determining an aspect ratio, a degree of aggregation, and the like of particles dispersed in a liquid sample, a particle size measuring mechanism for measuring the particle size of the particles, A zeta potential measuring mechanism that measures at least a zeta potential of the particle, wherein the particle surface shape and the particle based on the measurement result data in the shape property value measuring mechanism and the particle size measuring mechanism Based on the particle image data for displaying the size of the particle as an image and the measurement result data in the zeta potential measurement mechanism, the zeta potential of the particle is determined from the particle surface of the particle and / or from the particle surface. An image data creation unit for creating zeta potential image data for display as a layer color is further provided.
このようなものであれば、数値等として得られた形状物性値や粒径等の測定結果に基づき、液中における粒子の画像が作成されるので、具現化された測定結果から液中の粒子の状態を立体的かつ感覚的に把握することが可能となり、測定に不慣れな者であっても容易に測定結果を理解することができる。また、前記電場を表す画像は層として表示されて、ゼータ電位の測定結果に応じて、電場を表す層の大きさや色が異なって表示されるので、ゼータ電位の測定結果を一目で容易に把握することができ、理解度が向上する。形状物性値や粒径等の測定結果に基づいて得られた粒子画像データの粒子周囲（外縁）に、ゼータ電位測定結果に基づいて得られた電場データ（ゼータ電位画像データ）を表示するので、測定に不慣れな者にとっても、溶液中での微粒子の状態を理解しやすい。更に、これらの各種物性の測定は液中で行なわれるので、ＳＥＭ等の電子顕微鏡による乾燥状態の観察画像では分からなかった液中での粒子の状態が具体的に把握できる。 If this is the case, an image of the particle in the liquid is created based on the measurement result of the shape physical property value and the particle size obtained as numerical values, etc., so the particle in the liquid is obtained from the embodied measurement result. It is possible to grasp the state of the three-dimensionally and sensuously, and even a person unfamiliar with the measurement can easily understand the measurement result. In addition, the image representing the electric field is displayed as a layer, and depending on the measurement result of the zeta potential, the size and color of the layer representing the electric field are displayed differently, so the measurement result of the zeta potential can be easily grasped at a glance. Can improve understanding. Since the electric field data (zeta potential image data) obtained based on the zeta potential measurement result is displayed around the particle (outer edge) of the particle image data obtained based on the measurement result such as the shape physical property value and the particle size, Even those who are unfamiliar with the measurement can easily understand the state of the fine particles in the solution. Furthermore, since these various physical properties are measured in the liquid, the state of the particles in the liquid that could not be understood from the observation image of the dry state by an electron microscope such as SEM can be specifically grasped.
なお、本発明において色が変化するとは、色相、明度、彩度のいずれかの属性だけが変化してもよく、これらの色の三属性が組み合わさって変化してもよい。 In the present invention, the change of color means that only one of the attributes of hue, brightness, and saturation may be changed, or the three attributes of these colors may be combined and changed.
ゼータ電位の測定結果に応じて、前記電場を表す層の大きさや色が変化するためには、前記ゼータ電位測定機構における測定結果データと、前記粒子表面からの層の大きさ及び／又は前記粒子表面からの層の色とを関連付けているテーブルを格納するテーブル格納部を更に備えていることが好ましい。 In order to change the size and color of the layer representing the electric field according to the measurement result of the zeta potential, the measurement result data in the zeta potential measurement mechanism, the size of the layer from the particle surface and / or the particle It is preferable to further include a table storage unit that stores a table that associates the color of the layer from the surface.
このような本発明によれば、各種物性の測定結果が数値や分布と併せて画像として表示されることにより、粒子の各種物性を初めて測定する者や、あまり測定する機会のない者にとっても、液中における粒子の存在状態が具体的なイメージとして把握できるので、各種物性の測定結果の理解度が向上する。 According to the present invention as described above, the measurement results of various physical properties are displayed as an image together with numerical values and distributions, for those who measure various physical properties of particles for the first time, and those who do not have much opportunity to measure, Since the state of the presence of particles in the liquid can be grasped as a specific image, the degree of understanding of measurement results of various physical properties is improved.
以下、本発明の一実施形態を図面を参照して説明する。 Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
図１は、本実施形態に係る粒子物性測定装置１の構成の概要を示すものである。本実施形態に係る粒子物性測定装置１は、形状物性値測定機構、粒径測定機構、分子量測定機構、及び、ゼータ電位測定機構を備えているものであって、図１に示すように、透明な石英ガラス等からなり、粒子群を水等の分散媒に分散させてなる液体試料を収容するセル２と、前記液体試料にレーザ光Ｌを照射するレーザ３と、前記レーザ光Ｌを照射された液体試料中の粒子群から発される散乱光Ｓを受光し、その光子数に応じたパルス信号又は光強度のゆらぎに応じた電気信号を出力する光電子倍増管からなる受光部４１、４２と、レーザ３から発射されるレーザ光Ｌの一部を分岐するハーフミラー５１、ミラー５２、５３、及び、ミラー５３からの参照光Ｒと散乱光Ｓとを混合するハーフミラー５４からなる参照光学系５と、情報処理装置６と、を備えている。 FIG. 1 shows an outline of the configuration of a particle property measuring apparatus 1 according to this embodiment. The particle property measuring apparatus 1 according to this embodiment includes a shape property value measuring mechanism, a particle size measuring mechanism, a molecular weight measuring mechanism, and a zeta potential measuring mechanism, and is transparent as shown in FIG. Cell 2 that contains a liquid sample made of quartz glass or the like and in which a particle group is dispersed in a dispersion medium such as water, a laser 3 that irradiates the liquid sample with laser light L, and a laser beam L that is irradiated with the laser light L. Light receiving portions 41 and 42 each including a photomultiplier tube that receives scattered light S emitted from a group of particles in a liquid sample and outputs a pulse signal corresponding to the number of photons or an electric signal corresponding to fluctuations in light intensity; A reference optical system comprising a half mirror 51 for branching a part of the laser light L emitted from the laser 3, mirrors 52 and 53, and a half mirror 54 for mixing the reference light R and the scattered light S from the mirror 53. 5 and information processing equipment It is provided with a 6, a.
以下に各測定機構の構成について説明する。
アスペクト比や凝集度等を測定する形状物性値測定機構は、図２に示すように、レーザ３と、偏光子１１、１４と、１／４波長板１２、１３と、受光部４１と、から構成される。偏光子１１はレーザ３から射出されたレーザ光Ｌの偏光方向を固定するために使用されているが、１／４波長板１２、１３は光軸を中心に回転可能であり、１／４波長板１２で直線偏光を楕円偏光に変換し、１／４波長板１３と、偏光子１４で楕円偏光を直線偏光に戻す。
The configuration of each measurement mechanism will be described below.
As shown in FIG. 2, the shape property value measuring mechanism for measuring the aspect ratio, the degree of aggregation, and the like includes a laser 3, polarizers 11 and 14, quarter wave plates 12 and 13, and a light receiving unit 41. Composed. The polarizer 11 is used to fix the polarization direction of the laser light L emitted from the laser 3, but the quarter-wave plates 12 and 13 are rotatable around the optical axis, and the quarter wavelength. The plate 12 converts linearly polarized light into elliptically polarized light, and the quarter wavelength plate 13 and the polarizer 14 return the elliptically polarized light to linearly polarized light.
形状物性値を測定するには、米国特許第６７２１０５１号に記載の方法を用い、まず、セル２中の液体試料のレーザ光Ｌの透過率を測定する。次いで、１／４波長板１２、１３及び偏光子１４を光軸を中心に回転させながらレーザ光Ｌを発射して、複数態様の偏光パターンにおいて、受光部４１の位置（角度）を変化させながら、所定散乱角度での散乱光Ｓの強度を測定する。そして、得られた透過率と散乱光強度比とに所定の演算処理を行うことにより、アスペクト比及び／又は凝集度を算出する。 In order to measure the physical property value of the shape, first, the transmittance of the laser beam L of the liquid sample in the cell 2 is measured using the method described in US Pat. No. 6,721,051. Next, the laser light L is emitted while rotating the quarter-wave plates 12 and 13 and the polarizer 14 around the optical axis, and the position (angle) of the light receiving unit 41 is changed in a plurality of modes of polarization patterns. Then, the intensity of the scattered light S at a predetermined scattering angle is measured. Then, predetermined aspect processing is performed on the obtained transmittance and scattered light intensity ratio to calculate the aspect ratio and / or the degree of aggregation.
粒径測定機構は、図３に示すように、レーザ３と、受光部４１と、コリレータ１５と、から構成される。粒径（粒径分布）を測定するには、動的光散乱法を用い、レーザ光Ｌをセル２中の液体試料に照射して、液体試料中の粒子群から発した散乱光Ｓを受光部４１で受光し、その光子数に応じたパルス信号を受光部４１から受信したコリレータ１５で、そのパルス数の時系列データから自己相関データを生成し、当該自己相関データに基づいて所定の演算処理を行うことにより前記粒子群の粒径分布を算出する。なお、本実施形態では光子数に応じたパルス信号より演算する方法について詳述したが、光強度のゆらぎに応じた電気信号より演算することも可能であるのはいうまでもない。 As shown in FIG. 3, the particle size measuring mechanism includes a laser 3, a light receiving unit 41, and a correlator 15. To measure the particle size (particle size distribution), the dynamic light scattering method is used, the liquid sample in the cell 2 is irradiated with the laser light L, and the scattered light S emitted from the particles in the liquid sample is received. The correlator 15 that receives light from the light receiving unit 41 and receives a pulse signal corresponding to the number of photons from the light receiving unit 41 generates autocorrelation data from the time-series data of the number of pulses, and performs a predetermined calculation based on the autocorrelation data. By performing the processing, the particle size distribution of the particle group is calculated. In the present embodiment, the method of calculating from the pulse signal corresponding to the number of photons has been described in detail, but it is needless to say that the calculation can also be performed from the electric signal corresponding to the fluctuation of the light intensity.
図３に示す実施形態では、受光部４１はレーザ光Ｌと直交する光路の散乱光Ｓを受光しているが、粒径（粒径分布）を測定する際の受光部４１の好適な位置（角度）は、液体試料の濃度によって変わり、形状物性値を測定する際に測定された液体試料のレーザ光透過率に従い、透過率が高い（液体試料の濃度が低い）ときはレーザ光Ｌと直交する光路（散乱角度９０°）の散乱光Ｓを受光し、透過率が低い（液体試料の濃度が高い）ときはレーザ光Ｌと合致する光路（散乱角度１８０°）の散乱光Ｓを受光するように、受光部４１の位置（角度）が調節される。 In the embodiment shown in FIG. 3, the light receiving unit 41 receives the scattered light S in the optical path orthogonal to the laser light L, but a suitable position of the light receiving unit 41 when measuring the particle size (particle size distribution) ( The angle varies depending on the concentration of the liquid sample, and is orthogonal to the laser beam L when the transmittance is high (the concentration of the liquid sample is low) according to the laser beam transmittance of the liquid sample measured when measuring the shape property value. The scattered light S of the optical path (scattering angle 90 °) is received, and when the transmittance is low (the concentration of the liquid sample is high), the scattered light S of the optical path matching the laser light L (scattering angle 180 °) is received. As described above, the position (angle) of the light receiving unit 41 is adjusted.
分子量測定機構は、図４に示すように、レーザ３と、受光部４１と、から構成される。分子量を測定するには、静的光散乱法を用い、濃度を変えた複数種類の液体試料を用い、受光部４１の位置（角度）を変化させながら、セル２中の液体試料にレーザ光Ｌを照射して、当該液体試料中の粒子群から発した散乱光Ｓの光強度の角度分布を計測する。そして、液体試料の濃度と散乱角度変化による散乱光量変化から、Ｚｉｍｍプロットを行い、粒子の分子量を算出する。形状物性値測定機構及び粒径測定機構に加え、分子量測定機構における測定結果データに基づいて粒子表面形状と粒子の大きさを画像として表示するデータを作成することもできる。 As shown in FIG. 4, the molecular weight measurement mechanism includes a laser 3 and a light receiving unit 41. In order to measure the molecular weight, a plurality of types of liquid samples with different concentrations are used using the static light scattering method, and the laser beam L is applied to the liquid sample in the cell 2 while changing the position (angle) of the light receiving unit 41. , And the angular distribution of the light intensity of the scattered light S emitted from the particle group in the liquid sample is measured. Then, from the change in the amount of scattered light due to the concentration of the liquid sample and the change in the scattering angle, a Zimm plot is performed to calculate the molecular weight of the particles. In addition to the shape property value measurement mechanism and the particle size measurement mechanism, data for displaying the particle surface shape and the particle size as an image can be created based on the measurement result data in the molecular weight measurement mechanism.
ゼータ電位測定機構は、図５に示すように、レーザ３と、白金等からなる一対の電極１６と、参照光学系５と、受光部４２と、から構成される。ゼータ電位を測定するには、電気泳動法を用い、セル２に挿入した電極１６に直流又は交流電圧を印加して、液体試料中の粒子に電界をかけながらレーザ光Ｌを照射して、所定角度で散乱される散乱光Ｓを受光し、散乱光Ｓと参照光Ｒとの振動数の差（干渉現象）を測定することにより、液体試料中の粒子の移動速度を算出する。更に、得られた移動速度に所定の演算処理を行うことによりゼータ電位を算出する。 As shown in FIG. 5, the zeta potential measurement mechanism includes a laser 3, a pair of electrodes 16 made of platinum or the like, a reference optical system 5, and a light receiving unit 42. To measure the zeta potential, electrophoresis is applied, a direct current or alternating voltage is applied to the electrode 16 inserted in the cell 2, and laser particles L are irradiated while applying an electric field to particles in the liquid sample. By receiving the scattered light S scattered at an angle and measuring the difference in frequency (interference phenomenon) between the scattered light S and the reference light R, the moving speed of the particles in the liquid sample is calculated. Further, the zeta potential is calculated by performing a predetermined calculation process on the obtained moving speed.
このような各測定機構において受光部４１、４２から出力された信号は、情報処理装置６に送信される。 Signals output from the light receiving units 41 and 42 in each measurement mechanism as described above are transmitted to the information processing device 6.
情報処理装置６は、ＣＰＵの他に、メモリ、キーボード等の入力手段、ディスプレイ等の出力手段等を備えた汎用乃至専用のものであり、メモリに所定のプログラムを格納し、当該プログラムに従ってＣＰＵやその周辺機器を協働動作させることによって、演算処理部６１、画像データ作成部６２、テーブル格納部６３、画像表示部６４等としての機能を発揮するように構成してある。 The information processing apparatus 6 is a general-purpose or dedicated device including an input unit such as a memory and a keyboard, an output unit such as a display, in addition to the CPU, stores a predetermined program in the memory, By operating the peripheral devices in cooperation with each other, the functions as the arithmetic processing unit 61, the image data creation unit 62, the table storage unit 63, the image display unit 64, and the like are exhibited.
演算処理部６１は、各測定機構において受光部４１、４２から発したパルス信号又は光強度信号を直接又はコリレータ１５を介して受信し、所定の演算処理を行ない測定結果を算出する。 The arithmetic processing unit 61 receives pulse signals or light intensity signals emitted from the light receiving units 41 and 42 in each measurement mechanism, directly or via the correlator 15, and performs predetermined arithmetic processing to calculate a measurement result.
画像データ作成部６２は、演算処理部６１から各測定機構における測定結果データを取得し、前記粒子と、前記粒子の周囲に形成された電場とを、各種物性の測定結果に基づき画像として表示する画像データを作成するものである。ここで前記電場を表す層の大きさ又は色はゼータ電位の測定結果に応じて変化する。 The image data creation unit 62 acquires the measurement result data in each measurement mechanism from the arithmetic processing unit 61, and displays the particles and the electric field formed around the particles as an image based on the measurement results of various physical properties. Image data is created. Here, the size or color of the layer representing the electric field changes according to the measurement result of the zeta potential.
画像データ作成部６２より作成される画像は、図６にその一例を示すように、前記粒径測定機構により測定された一次粒子の平均粒径を有する球体Ｓの周囲（外縁）に、前記ゼータ電位測定機構によるゼータ電位の測定結果から一次粒子の平均帯電量を求め、当該帯電量に基づき色等を変えて電場Ｅを層として表示するものである。この画像と同時に、ゼータ電位の測定結果に対応する色見本Ｍも合わせて表示される。また、一次粒子やそれが凝集してなる二次粒子が棒状である場合は、図７に示すように、形状物性値測定結果から得られた平均短径及び平均長径を、当該形状物性値に従い作成された楕円体や円柱等の棒状体Ｂとともに表示する。更に、図８に示すように、一次粒子が凝集して二次粒子Ａを形成している場合は、既に粒径が判明している一次粒子が何個集まって二次粒子Ａを形成しているか、どのようなフラクタル形状に凝集しているか等の凝集状態を３次元的に表示する。このような場合においても、棒状なる一次粒子Ｂや、凝集結果として棒状となった二次粒子Ａの周囲に、前記ゼータ電位測定結果から平均帯電量を求め、当該帯電量に基づき色等を変えて電場Ｅを層として表示する。すなわち、粒子画像データの粒子表面形状と、粒子の大きさのデータと、ゼータ電位の測定結果に基づくゼータ電位画像データとより、粒子表面に層として電場を表示できるようにしている。 An image created by the image data creation unit 62 is, as shown in FIG. 6, an example of the zeta around the sphere S having the average particle size of the primary particles measured by the particle size measuring mechanism. The average charge amount of the primary particles is obtained from the measurement result of the zeta potential by the potential measurement mechanism, and the electric field E is displayed as a layer by changing the color or the like based on the charge amount. Simultaneously with this image, a color sample M corresponding to the measurement result of the zeta potential is also displayed. Further, when the primary particles and the secondary particles formed by agglomeration thereof are rod-shaped, as shown in FIG. 7, the average minor axis and the average major axis obtained from the shape property value measurement results are determined according to the shape property value. It is displayed together with the created ellipsoid or rod B such as a cylinder. Further, as shown in FIG. 8, when the primary particles are aggregated to form the secondary particles A, the secondary particles A are formed by collecting how many primary particles whose particle diameters are already known. The agglomeration state such as whether or not the fractal shape is aggregated is displayed three-dimensionally. Even in such a case, an average charge amount is obtained from the zeta potential measurement result around the rod-shaped primary particles B and the rod-shaped secondary particles A as a result of aggregation, and the color or the like is changed based on the charge amount. The electric field E is displayed as a layer. That is, the electric field can be displayed as a layer on the particle surface based on the particle surface shape of the particle image data, the particle size data, and the zeta potential image data based on the measurement result of the zeta potential.
テーブル格納部６３は、ゼータ電位の測定結果と、前記電場を表す層の大きさ又は色と、が関連付けられているテーブルを格納しているものである。 The table storage unit 63 stores a table in which the measurement result of the zeta potential is associated with the size or color of the layer representing the electric field.
画像表示部６４は、画像データ作成部６２により作成された画像データを取得して、各種物性の測定結果を具現化して画像として表示するものである。 The image display unit 64 acquires the image data created by the image data creation unit 62, embodies measurement results of various physical properties, and displays them as an image.
次に、各測定機構で測定された結果を画像として表示する手順を図９のフローチャートを参照して説明する。 Next, a procedure for displaying the result measured by each measurement mechanism as an image will be described with reference to the flowchart of FIG.
まず、演算処理部６１が受光部４１、４２から発した信号を直接又はコリレータ１５等を介して受信して、所定の演算処理を行ない、各種物性の測定結果を算出する（ステップＳ１）。 First, the arithmetic processing unit 61 receives signals emitted from the light receiving units 41 and 42 directly or via the correlator 15, etc., performs predetermined arithmetic processing, and calculates various physical property measurement results (step S1).
次いで、画像データ作成部６２が、演算処理部６１から各種物性の測定結果データを取得する（ステップＳ２）。 Next, the image data creation unit 62 acquires measurement result data of various physical properties from the arithmetic processing unit 61 (step S2).
続いて、画像データ作成部６２は、テーブル格納部６３から、ゼータ電位の測定結果と前記粒子の周囲に形成された電場を示す画像の大きさ又は色とが対になっているテーブルを取得して、ゼータ電位の測定結果に対応する画像の大きさや色を選び出す（ステップＳ３）。 Subsequently, the image data creation unit 62 acquires from the table storage unit 63 a table in which the measurement result of the zeta potential and the size or color of the image indicating the electric field formed around the particle are paired. Thus, the size and color of the image corresponding to the measurement result of the zeta potential are selected (step S3).
そして、画像データ作成部６２は、前記粒子と、前記粒子の周囲に形成された電場とを、測定された物性に基づき画像として表示する画像データを作成する（ステップＳ４）。ここで前記電場を表す層の大きさ又は色はゼータ電位の測定結果に応じて変化する。 Then, the image data creation unit 62 creates image data that displays the particles and the electric field formed around the particles as an image based on the measured physical properties (step S4). Here, the size or color of the layer representing the electric field changes according to the measurement result of the zeta potential.
画像表示部６４は、画像データ作成部６２で作成された画像データを取得して、
各測定機構により測定された結果を画像として出力する（ステップＳ５）。
The image display unit 64 acquires the image data created by the image data creation unit 62, and
The result measured by each measurement mechanism is output as an image (step S5).
このように構成した本実施形態に係る粒子物性測定装置１によれば、数値等として得られた形状物性値や粒径等の測定結果に基づき、液中における粒子の画像が作成されるので、具現化された測定結果から液中の粒子の状態を立体的かつ感覚的に把握することが可能となり、測定に不慣れな者であっても容易に測定結果を理解することができる。また、前記電場を表す層は、ゼータ電位の測定結果に応じて、大きさや色が異なって表示されるので、ゼータ電位の測定結果を一目で容易に把握することができ、理解度が向上する。アスペクト比や凝集度等の形状物性値や粒径等の測定結果に基づいて得られた粒子画像データの粒子周囲（外縁）に、ゼータ電位測定結果に基づいて得られた電場データ（ゼータ電位画像データ）を表示するので、測定に不慣れな者にとっても、溶液中での微粒子の状態を理解しやすい。更に、これらの各種物性の測定は液中で行なわれるので、ＳＥＭ等の電子顕微鏡による乾燥状態の観察画像では分からなかった液中での粒子の状態が具体的に把握できる。 According to the particle property measuring apparatus 1 according to the present embodiment configured as described above, an image of particles in the liquid is created based on the measurement result of the shape property value and the particle size obtained as numerical values, etc. It is possible to grasp the state of the particles in the liquid three-dimensionally and sensuously from the embodied measurement results, and even a person unfamiliar with the measurement can easily understand the measurement results. In addition, since the layer representing the electric field is displayed in different sizes and colors according to the measurement result of the zeta potential, the measurement result of the zeta potential can be easily grasped at a glance and the understanding level is improved. . Electric field data (zeta potential image) obtained based on the zeta potential measurement result around the particle (outer edge) of the particle image data obtained based on the measurement result of the shape property value such as aspect ratio and aggregation degree and particle size. Data) is displayed, so even those who are unfamiliar with the measurement can easily understand the state of the fine particles in the solution. Furthermore, since these various physical properties are measured in the liquid, the state of the particles in the liquid that could not be understood from the observation image of the dry state by an electron microscope such as SEM can be specifically grasped.
なお、本発明は前記実施形態に限られるものではない。 The present invention is not limited to the above embodiment.
例えば、図６〜８では、前記電場を表す層はゼータ電位の測定結果に応じて色が変化するようにしてあるが、ゼータ電位の測定結果に応じて前記電場を表す層の大きさが変化するように、すなわち、粒子Ｓ、Ａ、Ｂ又はＢの外縁に層として表示してもよく、大きさと色とはいずれか一方又は両方を選択可能であってもよい。 For example, in FIGS. 6 to 8, the layer representing the electric field changes color according to the measurement result of the zeta potential, but the size of the layer representing the electric field changes according to the measurement result of the zeta potential. That is, it may be displayed as a layer on the outer edge of the particle S, A, B or B, and either or both of the size and the color may be selectable.
本発明に係る粒子物性測定装置は、粒子物性測定装置１に備わっている全ての測定機構を有していなくともよく、例えば、分子量測定機構を備えていなくともよい。 The particle physical property measuring apparatus according to the present invention may not have all the measurement mechanisms provided in the particle physical property measuring apparatus 1, and may not include, for example, a molecular weight measuring mechanism.
その他、本発明はその趣旨を逸脱しない範囲で種々の変形が可能であるのは言うまでもない。 In addition, it goes without saying that the present invention can be variously modified without departing from the spirit of the present invention.
１・・・粒子物性測定装置
６２・・・画像データ作成部
Ｓ、Ｂ、Ａ・・・粒子
Ｅ・・・電場
DESCRIPTION OF SYMBOLS 1 ... Particle physical property measuring apparatus 62 ... Image data preparation part S, B, A ... Particle E ... Electric field
Claims (2)
前記形状物性値測定機構及び前記粒径測定機構における測定結果データに基づき、粒子表面形状と粒子の大きさを画像として表示するための粒子画像データと、
前記ゼータ電位測定機構における測定結果データに基づき、粒子のゼータ電位を該粒子の粒子表面からの層の大きさ及び／又は粒子表面からの層の色として表示するためのゼータ電位画像データと、を作成する画像データ作成部を更に備えていることを特徴とする粒子物性測定装置。 A shape property value measurement mechanism for determining the shape property value of particles dispersed in a liquid sample, a particle size measurement mechanism for measuring the particle size of the particles, a zeta potential measurement mechanism for measuring the zeta potential of the particles, A particle physical property measuring apparatus comprising at least
Based on the measurement result data in the shape physical property measurement mechanism and the particle size measurement mechanism, particle image data for displaying the particle surface shape and particle size as an image,
Based on the measurement result data in the zeta potential measurement mechanism, zeta potential image data for displaying the zeta potential of the particle as the size of the layer from the particle surface and / or the color of the layer from the particle surface. An apparatus for measuring particle physical properties, further comprising an image data creation unit for creating.
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| CN2009801370287A CN102159934A (en) | 2008-09-26 | 2009-09-25 | Device for measuring physical property of particle |
| US13/121,170 US8625093B2 (en) | 2008-09-26 | 2009-09-25 | Particle characterization device |
| GB1104774.3A GB2475458B (en) | 2008-09-26 | 2009-09-25 | Particle characterization instrument |
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