JPH10206302A - Particulate dispersing method, particulate dispersing device and particle size distribution measuring device - Google Patents
Particulate dispersing method, particulate dispersing device and particle size distribution measuring deviceInfo
- Publication number
- JPH10206302A JPH10206302A JP9008411A JP841197A JPH10206302A JP H10206302 A JPH10206302 A JP H10206302A JP 9008411 A JP9008411 A JP 9008411A JP 841197 A JP841197 A JP 841197A JP H10206302 A JPH10206302 A JP H10206302A
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- liquid
- droplets
- dispersing
- dispersed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
Landscapes
- Sampling And Sample Adjustment (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は微粒子を気相中に分
散させるための微粒子分散方法と微粒子分散装置及びそ
れを用いた粒径分布測定装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for dispersing fine particles in a gas phase, a fine particle dispersing apparatus, and a particle size distribution measuring apparatus using the same.
【０００２】[0002]
【従来の技術】微粒子はその粒径分布等を測定するため
に、各粒子が凝集していない１次粒子の状態で液体中又
は空気中に分散させて測定が可能となる。しかし微粒子
の相互間にはファンデルワールス力、静電気力、液架橋
力等の力が働いて容易に凝集し、１次粒子にまで分散さ
せることが困難である。従って粒径分布を測定する際に
は、まず微粒子を十分に分散させる必要がある。又微粒
子を測定対象とする種々の機器を校正する場合や、クリ
ーンルーム等に用いられるフィルタの効率試験をする場
合にも、高濃度で十分気相中に分散した微粒子が必要と
なる。従来の微粒子分離方法としては、湿式分散法と乾
式分散法とが考えられている。湿式分散法は水中等液中
に微粒子を混入させ、界面活性剤等を用いて各粒子を分
離するものであり、乾式分離法は凝集体を機械的に粉砕
したり、高速気流中に入れることによって気相中に分散
させる方法である。2. Description of the Related Art Fine particles can be measured by dispersing them in a liquid or air in the form of primary particles in which each particle is not aggregated in order to measure the particle size distribution and the like. However, between the fine particles, forces such as van der Waals force, electrostatic force, liquid bridging force, etc. act, and the particles are easily aggregated, and it is difficult to disperse them into primary particles. Therefore, when measuring the particle size distribution, it is first necessary to sufficiently disperse the fine particles. Also, when calibrating various instruments that measure fine particles or when performing an efficiency test of a filter used in a clean room or the like, fine particles having a high concentration and sufficiently dispersed in a gas phase are required. Conventional methods for separating fine particles include a wet dispersion method and a dry dispersion method. The wet dispersion method involves mixing fine particles in a liquid such as water and separating each particle using a surfactant.The dry separation method involves mechanically pulverizing aggregates or putting them in a high-speed air stream. In the gas phase.
【０００３】[0003]
【発明が解決しようとする課題】しかしながらこのよう
な従来の分散装置においても、粒径の平均が１μｍ以下
の微粒子の場合には、凝集体を効率良く分散させること
は難しいという欠点があった。However, even such a conventional dispersing apparatus has a drawback that it is difficult to efficiently disperse aggregates when the average particle diameter is 1 μm or less.
【０００４】本発明は１μｍ以下の微粒子も比較的容易
に分散させることのできる分散方法と分散装置、及びこ
れを用いて粒子の粒径及び分布を測定するための粒径分
布測定装置を提供することを目的とする。The present invention provides a dispersing method and a dispersing apparatus capable of relatively easily dispersing fine particles having a particle size of 1 μm or less, and a particle size distribution measuring apparatus for measuring the particle diameter and distribution using the same. The purpose is to:
【０００５】[0005]
【課題を解決するための手段】本願の請求項１の発明
は、測定対象となる凝集した微粒子を液体中に分散さ
せ、前記分散させた液体を第１の細管を介して噴霧手段
に導き、前記噴霧手段に高圧空気を流入させることによ
って霧化し、前記霧化された液滴を前記液体の蒸発温度
より高い温度に加熱された加熱管に導くことにより霧化
された液滴を急激に沸騰蒸発させ、凝縮された微粒子を
空気中に分散させることを特徴とするものである。According to a first aspect of the present invention, an agglomerated fine particle to be measured is dispersed in a liquid, and the dispersed liquid is guided to spraying means through a first thin tube. Atomization is performed by flowing high-pressure air into the spraying unit, and the atomized droplets are rapidly boiled by guiding the atomized droplets to a heating tube heated to a temperature higher than the evaporation temperature of the liquid. It is characterized by evaporating and dispersing the condensed fine particles in the air.
【０００６】本願の請求項２の発明は、測定対象となる
凝集した微粒子を含む液体を第１の細管を介して供給す
る試料供給手段と、前記第１の細管の端部が開放された
第２の細管を有し、該第２の細管内に高圧空気を流入さ
せることによって噴霧する噴霧手段と、噴霧された液滴
が導かれ、前記液体の蒸発温度より高い温度に加熱され
た加熱管と、を有し、霧化された液滴を急激に沸騰蒸発
させることにより凝集した微粒子を気中に分散させるこ
とを特徴とするものである。According to a second aspect of the present invention, there is provided a sample supply means for supplying a liquid containing agglomerated fine particles to be measured through a first capillary, and a sample supply means for opening the end of the first capillary. Atomizing means for spraying by flowing high-pressure air into the second thin tube, and a heating tube for guiding the sprayed droplets and heating the liquid to a temperature higher than the evaporation temperature of the liquid And agglomerated fine particles are dispersed in the air by rapidly boiling and evaporating the atomized droplets.
【０００７】本願の請求項３の発明では、前記試料供給
手段の微粒子を分散させる液体はフッ素系不活性液体で
あることを特徴とするものである。According to a third aspect of the present invention, the liquid in which the fine particles of the sample supply means are dispersed is a fluorine-based inert liquid.
【０００８】本願の請求項４の発明は、請求項２又は３
のいずれか１項記載の微粒子分散装置と、前記微粒子分
散装置により気中に分散された微粒子を両極に帯電さ
せ、電圧を印加した二重円筒に導くと共に、円筒の空隙
より一部の微粒子を取り出す微分型電気移動度分析装置
と、前記微分型電気移動度分析装置により捕集された微
粒子の個数を計数する凝縮核カウンタと、を有すること
を特徴とするものである。The invention of claim 4 of the present application is the invention of claim 2 or 3
The fine particle dispersing device according to any one of the above, the fine particles dispersed in the air by the fine particle dispersing device is charged to both poles, and guided to a double cylinder to which a voltage is applied, and a part of the fine particles from the gap of the cylinder is removed. A differential electric mobility analyzer to be taken out, and a condensation nucleus counter for counting the number of fine particles collected by the differential electric mobility analyzer are provided.
【０００９】このような特徴を有する本願の請求項１，
２の発明によれば、凝集した微粒子を液体中に分散させ
て第１の細管を介して噴霧手段に導いている。噴霧手段
では高圧空気を流入させて霧状としており、霧状となっ
た微小な液滴を加熱管により急激に沸騰蒸発させる。こ
うすれば沸騰蒸発時に液滴中で凝集していた微粒子が核
分裂状態となって気中に１次微粒子として分散させるこ
とができる。又請求項４の発明では、これを用いて微粒
子の粒径分布を正確に測定することができるという効果
が得られる。[0009] Claim 1 of the present application having such features.
According to the second aspect, the aggregated fine particles are dispersed in the liquid and guided to the spraying means via the first thin tube. In the spraying means, high-pressure air is flowed in to form a mist, and minute droplets in the form of mist are rapidly boiled and evaporated by a heating tube. In this way, the fine particles that have been agglomerated in the droplet at the time of boiling evaporation become a fission state and can be dispersed in the air as primary fine particles. Further, according to the invention of claim 4, there is an effect that the particle size distribution of the fine particles can be accurately measured by using this.
【００１０】[0010]
【発明の実施の形態】次に本発明の一実施の形態による
微粒子の分散装置について説明する。図１はこの実施の
形態による微粒子分散装置の主要部の構成を示す図であ
る。本図において容器１には試料となる微量の微粒子を
凝集した状態で含む液体を入れる。この容器１を超音波
バス２中に保持し、超音波振動を加えることによって試
料をある程度まで分散させておくものとする。そしてこ
の容器１には第１の細管であるキャピラリ３を挿入して
噴霧手段の第２の細管４に連結するように構成する。第
２の細管４には外部より加圧した清浄な空気をダクト５
を介して流入させる。そして細管４の端部には熱絶縁体
から成るキャビティ６を設けておく。第２の細管４，ダ
クト５及びキャビティ６は噴霧手段７を構成している。
噴霧手段７は第２の細管４からキャビティ６に達すると
きに圧力の急激な低下によって霧状の微小な液滴を発生
させるものであって、その端部にはねじ止めにより継ぎ
手を介して絶縁された分散用の金属管８が連結される。
この金属管８は例えばステンレス製とし、一定の長さＬ
を有するものとする。この金属管８は外部より容器１の
液体の沸点より十分高い温度となるように一定の温度で
加熱しておく加熱用の管である。このためこの金属管８
にはヒータ９及び温度制御装置１０が接続されている。Next, an apparatus for dispersing fine particles according to an embodiment of the present invention will be described. FIG. 1 is a diagram showing a configuration of a main part of a fine particle dispersion apparatus according to this embodiment. In this figure, a container 1 is filled with a liquid containing a minute amount of fine particles serving as a sample in an aggregated state. The container 1 is held in an ultrasonic bath 2 and the sample is dispersed to some extent by applying ultrasonic vibration. The container 1 has a configuration in which a capillary 3 as a first thin tube is inserted and connected to the second thin tube 4 of the spraying means. Clean air pressurized from the outside is introduced into the duct 5 through the second thin tube 4.
Inflow through. A cavity 6 made of a thermal insulator is provided at the end of the thin tube 4. The second thin tube 4, the duct 5 and the cavity 6 constitute a spraying unit 7.
The spraying means 7 generates fine mist droplets due to a sharp drop in pressure when reaching the cavity 6 from the second thin tube 4, and its end is insulated through a joint by screwing. The dispersed metal tube 8 is connected.
The metal tube 8 is made of, for example, stainless steel and has a fixed length L.
Shall be provided. The metal tube 8 is a heating tube that is heated from the outside at a constant temperature so as to be sufficiently higher than the boiling point of the liquid in the container 1. Therefore, this metal tube 8
Is connected to the heater 9 and the temperature control device 10.
【００１１】次にこの微粒子分散装置の動作について説
明する。容器１内に液体中に凝集している微粒子から成
る試料を微量混入させ、超音波バス２によってある程度
分散させる。そしてダクト５より圧縮した空気を導く
と、容器１内の試料を含む溶媒がキャピラリ３を介して
第２の細管４に吸引され、噴霧手段７のキャビティ６で
霧状となる。そして霧状となった微小な液滴は金属管８
に導かれる。キャビティ６は熱絶縁体で構成されている
ため、霧状の空気は金属管８に達してから急激に液滴の
温度が上昇する。従って液滴が沸騰蒸発することとな
り、微小液滴の核となっていた凝集している微粒子は核
分裂状態となって、液滴内に含まれていた微粒子を夫々
の微粒子毎に１次粒子として分離させ、気相中に分散さ
せることができる。そのため分散した微粒子の粒径分布
や個数濃度の測定を行うことができる。尚超音波バス２
により容器１に超音波振動を与えることにより、キャピ
ラリ３での詰まりが回避できるという副次的な効果があ
る。Next, the operation of the fine particle dispersion apparatus will be described. A small amount of a sample composed of fine particles agglomerated in a liquid is mixed into the container 1 and dispersed to some extent by the ultrasonic bath 2. When the compressed air is introduced from the duct 5, the solvent containing the sample in the container 1 is sucked into the second thin tube 4 via the capillary 3, and becomes a mist in the cavity 6 of the spray unit 7. Then, the fine droplets in the form of a mist are applied to the metal tube 8
It is led to. Since the cavity 6 is made of a thermal insulator, the temperature of the droplets of the atomized air rapidly rises after reaching the metal tube 8. Therefore, the droplets will evaporate, and the aggregated fine particles that have been the nucleus of the fine droplets will be in a fission state, and the fine particles contained in the droplet will be converted into primary particles for each fine particle. It can be separated and dispersed in the gas phase. Therefore, the particle size distribution and the number concentration of the dispersed fine particles can be measured. Ultrasonic bath 2
By applying ultrasonic vibration to the container 1, there is a secondary effect that clogging in the capillary 3 can be avoided.
【００１２】次にこの実施の形態による微粒子分散装置
を用いた粒径分布測定装置の全体構成について図２を用
いて説明する。微粒子分散装置の金属管８より分散した
微粒子を含む空気（エアロゾル）をダクト１１を介して
空冷部１２に導く。空冷部１２は多数のフィン１３が接
続されており、このエアロゾルを冷却するものである。
尚、空冷部１２は水冷，電子冷却等の冷却機能によって
常温に温度制御できるものでもよい。又冷却によって生
じる液滴はドレイン１４より排出される。Next, the overall configuration of a particle size distribution measuring apparatus using the fine particle dispersion apparatus according to this embodiment will be described with reference to FIG. Air (aerosol) containing fine particles dispersed from the metal tube 8 of the fine particle dispersion device is guided to the air cooling unit 12 through the duct 11. The air cooling unit 12 is connected with a large number of fins 13 and cools the aerosol.
The air cooling unit 12 may be one that can control the temperature to normal temperature by a cooling function such as water cooling or electronic cooling. Droplets generated by cooling are discharged from the drain 14.
【００１３】次に冷却された空気流は微分型電気移動度
分析装置（以下、ＤＭＡ（ディファレンシャル モビィ
リティ アナライザ）という）に導かれる。ＤＭＡはJo
urnal of Aerosol Science, 1975, Vol.6, pp.443-451,
gAerosol classification by electric mobility : ap
peratus, theory, and applications"に示されているよ
うに、一定の電気移動度を持った粒子を分級する高精度
の分級装置である。図３（ａ）はその構成を示す概略図
であり、図示のように上部円筒２１にＡｍ−２４１等の
放射線源２２を設けて通過する微粒子を両極の平衡帯電
状態とする。そしてこのエアロゾルを二重円筒から成る
微粒子捕集部２３の外筒内の内壁側に導く。内筒の外周
部にはクリーンエアを導き、内筒に一定の電圧Ｖを印加
する。そして内筒の下部に内筒とわずかの間隙を介して
ダクト２４の開口部を配置し、内筒によって捕集されな
かった微粒子をダクト２４に導く。そしてダクト２４に
流入した微粒子の個数を凝縮核カウンタ（ＣＮＣ）２５
によって計数する。凝縮核カウンタ２５は微粒子を含ん
だ空気を水蒸気又はアルコール蒸気で飽和させ、夫々の
微粒子を核として水蒸気又はアルコール蒸気を凝縮さ
せ、成長粗大化して光学的に観察できるようにしてその
数を計数するものである。この場合には図３（ｂ）に示
すように、印加した電圧Ｖに対して粒子の個数が直接得
られることとなる。尚発生粒子個数濃度が凝縮核カウン
タ２５の測定上限濃度を越える場合には、凝縮核カウン
タ２５の前段に希釈装置２６を挿入して希釈した後、凝
縮核カウンタ２５に加える。Next, the cooled airflow is led to a differential mobility analyzer (hereinafter referred to as a DMA (Differential Mobility Analyzer)). DMA is Jo
urnal of Aerosol Science, 1975, Vol. 6, pp. 443-451,
gAerosol classification by electric mobility: ap
As shown in "peratus, theory, and applications", this is a high-precision classifier that classifies particles with a constant electric mobility. FIG. 3 (a) is a schematic diagram showing the configuration of the classifier. As shown in the figure, a radiation source 22 such as Am-241 is provided on an upper cylinder 21 so that fine particles passing therethrough are equilibrium-charged between the two poles. Clean air is guided to the outer periphery of the inner cylinder, a constant voltage V is applied to the inner cylinder, and an opening of the duct 24 is arranged below the inner cylinder with a slight gap from the inner cylinder. Then, the fine particles not collected by the inner cylinder are guided to the duct 24. The number of the fine particles flowing into the duct 24 is counted by a condensation nucleus counter (CNC) 25.
Count by The condensation nucleus counter 25 saturates the air containing the fine particles with water vapor or alcohol vapor, condenses the water vapor or alcohol vapor with each fine particle as a nucleus, grows coarsely, and counts the number so that it can be optically observed. Things. In this case, as shown in FIG. 3B, the number of particles can be directly obtained with respect to the applied voltage V. When the generated particle number concentration exceeds the upper limit of the measurement of the condensation nucleus counter 25, the dilution is performed by inserting a diluting device 26 before the condensation nucleus counter 25 and then added to the condensation nucleus counter 25.
【００１４】ここでＤＭＡに印加する電圧Ｖを変化させ
て捕集される微粒子の粒子数を計測する。こうすれば電
圧の連続的な変化により計数値が変化する。前述したよ
うに微粒子は十分分散しているため、微粒子の粒径分布
を正確に測定することができる。尚、微粒子分散装置に
よって分散された微粒子の粒径分布測定装置としては、
光散乱法をはじめ他の測定方法の適用も可能である。Here, the voltage V applied to the DMA is changed, and the number of collected fine particles is measured. In this case, the count value changes due to the continuous change of the voltage. Since the fine particles are sufficiently dispersed as described above, the particle size distribution of the fine particles can be accurately measured. In addition, as a particle size distribution measuring device of the fine particles dispersed by the fine particle dispersing device,
Other measurement methods such as the light scattering method can be applied.
【００１５】[0015]
【実施例】次に本発明の実施例について説明する。この
実施例においては、キャピラリ３の内径を０．９５mmφ
とし、第２の細管４の内径を１．５mmφとし、金属管の
内径を１１．５mmφとした。又金属管の長さＬは３０cm
とする。又容器１の凝集している粒子を入れる溶媒とし
てフッ素系不活性液体（例えば商品名フロリナート等）
を用いた。フロリナートは沸点５６℃であり、蒸発潜熱
２１cal ／ｇ、比熱０．２５cal ／ｇ・℃であり、水と
比べて沸点及び潜熱が低いので容易に沸騰させることが
できる。又超純水のように不純物を溶かすことがなく蒸
発残渣が少ないので溶媒として好適である。又ダクト５
に加える空気の圧力は２気圧とした。又金属管８の温度
は溶媒であるフロリナートの沸点５６℃より十分高い一
定の温度、例えば３００℃となるようにあらかじめ制御
しておく。尚溶媒はフロリートに限定されているもので
はないが、沸点が低く容易に沸騰せることができる液体
であることが好ましい。又加熱する温度は霧状の液滴を
ごく短時間で沸騰蒸発させることができるように沸点よ
り十分高い温度を選択する。Next, an embodiment of the present invention will be described. In this embodiment, the inner diameter of the capillary 3 is 0.95 mmφ.
The inner diameter of the second thin tube 4 was 1.5 mmφ, and the inner diameter of the metal tube was 11.5 mmφ. The length L of the metal tube is 30cm
And As a solvent for containing the aggregated particles in the container 1, a fluorine-based inert liquid (for example, Fluorinert (trade name) or the like)
Was used. Fluorinert has a boiling point of 56 ° C., a latent heat of vaporization of 21 cal / g and a specific heat of 0.25 cal / g · ° C., and can be easily boiled since it has a lower boiling point and latent heat than water. Further, unlike ultrapure water, it is suitable as a solvent because it does not dissolve impurities and has little evaporation residue. Duct 5
The pressure of the air to be added was 2 atm. The temperature of the metal tube 8 is controlled in advance so as to be a constant temperature sufficiently higher than the boiling point 56 ° C. of the solvent, Fluorinert, for example, 300 ° C. The solvent is not limited to flourit, but is preferably a liquid having a low boiling point and being easily boiled. The heating temperature is selected to be sufficiently higher than the boiling point so that the mist droplets can be boiled and evaporated in a very short time.
【００１６】さてこの実施例では微粒子として（１）単
分散球形ポリスチレンラテックス（以下、ＰＳＬとい
う）粒子、（２）α−Ｆｅ2 Ｏ3 粒子、（３）α−Ｆｅ
ＯＯＨ粒子、（４）カーボンブラック粒子を用いた。
（１）の粒子は表１に示すように対数をとったときの分
散σg が１．０、即ち単分散であり、その粒径は顕微鏡
計測によって０．３５μｍと確認されている。又（２）
〜（４）のα−Ｆｅ2 Ｏ3、α−ＦｅＯＯＨ粒子、カー
ボンブラック粒子については夫々個数基準の幾何平均系
ｄpstg＝０．２２μｍ、０．０８μｍ、０．２６μｍで
ある。In this embodiment, fine particles (1) monodispersed spherical polystyrene latex (hereinafter referred to as PSL) particles, (2) α-Fe 2 O 3 particles, and (3) α-Fe
OOH particles and (4) carbon black particles were used.
As shown in Table 1, the particle (1) has a logarithmic dispersion σ g of 1.0, that is, a monodispersion, and its particle size is confirmed by microscopic measurement to be 0.35 μm. Also (2)
Regarding α-Fe 2 O 3 , α-FeOOH particles and carbon black particles of (4), the number-based geometric average system d pstg = 0.22 μm, 0.08 μm, and 0.26 μm, respectively.
【表１】 [Table 1]
【００１７】これらの微粒子を分散させ、ＤＭＡ２０に
て分級した。ＤＭＡ２０は微粒子捕集部２３の外筒の半
径を１９．５mm、内筒の９．２５mmとし、有効長を４
５．５cmとする。そして流入させるエアロゾルの流量を
０．９５ｌ／分、クリーンエアの流量を１０ｌ／分とし
た。尚ＰＳＬ粒子に対しては２０ｌ／分とした。こうし
て分周した後、微粒子の個数を凝縮核カウンタ２５にて
計数した結果を図４〜図７に示す。尚ＤＭＡにて測定さ
れる粒子径は流体抵抗力相当径ｄpdである。こうして得
られた微粒子の粒径ｄpdと分散σg の結果を表２に示
す。These fine particles were dispersed and classified by DMA20. The DMA 20 has an outer cylinder radius of 19.5 mm, an inner cylinder of 9.25 mm, and an effective length of 4
5.5 cm. The flow rate of the aerosol to be flowed in was 0.95 l / min, and the flow rate of the clean air was 10 l / min. The amount was set to 20 l / min for PSL particles. After dividing the frequency in this manner, the results of counting the number of fine particles by the condensation nucleus counter 25 are shown in FIGS. The particle diameter measured by DMA is a fluid resistance force equivalent diameter d pd . Table 2 shows the results of the particle diameter d pd and the dispersion σ g of the fine particles thus obtained.
【表２】 [Table 2]
【００１８】このように粒径が１μｍ以下の種々の微粒
子について、ほぼ理論値に近い粒径分布が得られた。こ
のため噴霧手段７により液滴として噴霧させ、これを急
速に加熱蒸発させることによって核となっている粒子
を、ほぼ１次粒子に近い形で分散させることができるこ
とが確認できた。このため種々の粒子を簡単に且つ連続
的に分散させることが可能となる。As described above, with respect to various fine particles having a particle size of 1 μm or less, a particle size distribution almost close to the theoretical value was obtained. Therefore, it was confirmed that the droplets were sprayed by the spraying means 7 and rapidly heated to evaporate, whereby the core particles could be dispersed in a form substantially similar to the primary particles. For this reason, various particles can be easily and continuously dispersed.
【００１９】[0019]
【発明の効果】以上詳細に説明したように本願の請求項
１〜３の発明によれば、凝縮し易い微粒子、特に１μｍ
以下の粒径を有する粒子を効果的に連続して分散させる
ことができる。従ってこの分散装置を用いて粉体を測定
対象とする種々の測定機器の構成が可能となる。又クリ
ーンルームに用いられるフィルタの効率試験をするため
には、フィルタの上流側と下流側で粒子濃度を測定する
必要があるが、上流側で高濃度で十分分散した１次粒子
を供給するためにこの微粒子分散装置が有効となる。そ
の他、微粒子を対象とする種々の測定装置にも本発明は
有効となる。又請求項４の発明では、この微粒子分散装
置を用いることによって１μｍ以下の微粒子についても
効果的にその粒径分布を測定することができるという効
果が得られる。As described above in detail, according to the first to third aspects of the present invention, fine particles which are easily condensed, especially 1 μm
Particles having the following particle diameters can be effectively and continuously dispersed. Therefore, it is possible to configure various measuring instruments for measuring powder using this dispersing device. Also, in order to conduct an efficiency test of a filter used in a clean room, it is necessary to measure the particle concentration on the upstream and downstream sides of the filter, but in order to supply high concentration and sufficiently dispersed primary particles on the upstream side. This fine particle dispersion device is effective. In addition, the present invention is also effective for various measuring devices targeting fine particles. According to the fourth aspect of the present invention, by using this fine particle dispersing device, an effect is obtained that the particle size distribution of fine particles of 1 μm or less can be effectively measured.
【図１】本発明の一実施の形態による微粒子分散装置の
構成を示す断面図である。FIG. 1 is a cross-sectional view illustrating a configuration of a fine particle dispersion device according to an embodiment of the present invention.
【図２】この実施の形態による微粒子分散装置を用いた
粒径分布測定装置の全体構成を示す図である。FIG. 2 is a diagram showing an overall configuration of a particle size distribution measuring device using the fine particle dispersion device according to this embodiment.
【図３】ＤＭＡ分級装置の構成を示す概略図である。FIG. 3 is a schematic diagram illustrating a configuration of a DMA classification device.
【図４】ＰＳＬ粒子の分散の実験結果を示すグラフであ
る。FIG. 4 is a graph showing experimental results of dispersion of PSL particles.
【図５】Ｆｅ2 Ｏ3 粒子の分散の実験結果を示すグラフ
である。FIG. 5 is a graph showing experimental results of dispersion of Fe 2 O 3 particles.
【図６】α−ＦｅＯＯＨの粒子の分散の実験結果を示す
グラフである。FIG. 6 is a graph showing experimental results of dispersion of α-FeOOH particles.
【図７】カーボンブラック粒子の分散の実験結果を示す
グラフである。FIG. 7 is a graph showing an experimental result of dispersion of carbon black particles.
１ 容器 ２ 超音波バス ３ キャピラリ ４ 細管 ５，１１，２４ ダクト ７ 噴霧手段 ８ 金属管 ９ ヒータ １０ 温度制御装置 １２ 空冷部 １３ フィン １４ ドレイン ２０ ＤＭＡ ２１ 上部円筒 ２２ 放射線源 ２３ 微粒子捕集部 ２５ 凝縮核カウンタ ２６ 希釈部 DESCRIPTION OF SYMBOLS 1 Container 2 Ultrasonic bath 3 Capillary 4 Capillary tube 5, 11, 24 Duct 7 Spray means 8 Metal tube 9 Heater 10 Temperature control device 12 Air cooling unit 13 Fin 14 Drain 20 DMA 21 Upper cylinder 22 Radiation source 23 Particle collecting unit 25 Condensation Nuclear counter 26 dilution section
Claims (4)
に分散させ、 前記分散させた液体を第１の細管を介して噴霧手段に導
き、 前記噴霧手段に高圧空気を流入させることによって霧化
し、 前記霧化された液滴を前記液体の蒸発温度より高い温度
に加熱された加熱管に導くことにより霧化された液滴を
急激に沸騰蒸発させ、凝縮された微粒子を空気中に分散
させることを特徴とする微粒子分散方法。1. A method for dispersing aggregated fine particles to be measured in a liquid, guiding the dispersed liquid to spraying means through a first thin tube, and atomizing by flowing high-pressure air into the spraying means. Guiding the atomized droplets to a heating tube heated to a temperature higher than the evaporation temperature of the liquid to rapidly evaporate the atomized droplets and disperse the condensed fine particles in the air. A method for dispersing fine particles, characterized in that:
体を第１の細管を介して供給する試料供給手段と、 前記第１の細管の端部が開放された第２の細管を有し、
該第２の細管内に高圧空気を流入させることによって噴
霧する噴霧手段と、 噴霧された液滴が導かれ、前記液体の蒸発温度より高い
温度に加熱された加熱管と、を有し、霧化された液滴を
急激に沸騰蒸発させることにより凝集した微粒子を気中
に分散させることを特徴とする微粒子分散装置。2. A sample supply means for supplying a liquid containing aggregated fine particles to be measured via a first thin tube, and a second thin tube having an open end at the first thin tube,
Spraying means for spraying by causing high-pressure air to flow into the second thin tube; and a heating tube to which the sprayed liquid droplets are guided and heated to a temperature higher than the evaporation temperature of the liquid. A fine particle dispersing apparatus characterized in that agglomerated fine particles are dispersed in the air by rapidly boiling and evaporating formed droplets.
液体はフッ素系不活性液体であることを特徴とする請求
項２記載の微粒子分散装置。3. The fine particle dispersion apparatus according to claim 2, wherein the liquid for dispersing the fine particles in the sample supply means is a fluorine-based inert liquid.
粒子分散装置と、 前記微粒子分散装置により気中に分散された微粒子を両
極に帯電させ、電圧を印加した二重円筒に導くと共に、
円筒の空隙より一部の微粒子を取り出す微分型電気移動
度分析装置と、 前記微分型電気移動度分析装置により捕集された微粒子
の個数を計数する凝縮核カウンタと、を有することを特
徴とする粒径分布測定装置。4. The fine particle dispersing device according to claim 2, wherein the fine particles dispersed in the air by the fine particle dispersing device are charged to both poles and guided to a double cylinder to which a voltage is applied. ,
A differential electric mobility analyzer for extracting a part of the fine particles from the gap of the cylinder; and a condensation nucleus counter for counting the number of fine particles collected by the differential electric mobility analyzer. Particle size distribution measuring device.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00841197A JP3735430B2 (en) | 1997-01-21 | 1997-01-21 | Fine particle dispersion method, fine particle dispersion device, and particle size distribution measuring device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00841197A JP3735430B2 (en) | 1997-01-21 | 1997-01-21 | Fine particle dispersion method, fine particle dispersion device, and particle size distribution measuring device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10206302A true JPH10206302A (en) | 1998-08-07 |
| JP3735430B2 JP3735430B2 (en) | 2006-01-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004023109A1 (en) * | 2002-09-04 | 2004-03-18 | National Institute Of Advanced Industrial Science And Technology | Method and apparatus for measuring particle diameter distribution of powder |
| WO2005100954A1 (en) * | 2004-04-12 | 2005-10-27 | Rion Co., Ltd. | Method for calibrating particle counter |
| JP2012037318A (en) * | 2010-08-05 | 2012-02-23 | Japan Organo Co Ltd | Apparatus and method for measuring particle in liquid |
| WO2017129548A1 (en) * | 2016-01-28 | 2017-08-03 | Laboratoire National De Metrologie Et D'essais | Calibration appliance of a particle analyser |
| CN111766184A (en) * | 2020-06-30 | 2020-10-13 | 吉林大学 | Method for measuring particle size distribution of titanium hydride powder compact |
| CN115362024A (en) * | 2020-04-02 | 2022-11-18 | 吉田工业株式会社 | Wet-type micronizing device and method |
-
1997
- 1997-01-21 JP JP00841197A patent/JP3735430B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004023109A1 (en) * | 2002-09-04 | 2004-03-18 | National Institute Of Advanced Industrial Science And Technology | Method and apparatus for measuring particle diameter distribution of powder |
| WO2005100954A1 (en) * | 2004-04-12 | 2005-10-27 | Rion Co., Ltd. | Method for calibrating particle counter |
| JP2012037318A (en) * | 2010-08-05 | 2012-02-23 | Japan Organo Co Ltd | Apparatus and method for measuring particle in liquid |
| WO2017129548A1 (en) * | 2016-01-28 | 2017-08-03 | Laboratoire National De Metrologie Et D'essais | Calibration appliance of a particle analyser |
| FR3047312A1 (en) * | 2016-01-28 | 2017-08-04 | Laboratoire Nat De Metrologie Et Dessais | APPARATUS FOR CALIBRATING A PARTICULATE ANALYZER |
| CN115362024A (en) * | 2020-04-02 | 2022-11-18 | 吉田工业株式会社 | Wet-type micronizing device and method |
| CN111766184A (en) * | 2020-06-30 | 2020-10-13 | 吉林大学 | Method for measuring particle size distribution of titanium hydride powder compact |
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| Publication number | Publication date |
|---|---|
| JP3735430B2 (en) | 2006-01-18 |
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