JP2001252588A - Powder classifying method - Google Patents
Powder classifying methodInfo
- Publication number
- JP2001252588A JP2001252588A JP2000069537A JP2000069537A JP2001252588A JP 2001252588 A JP2001252588 A JP 2001252588A JP 2000069537 A JP2000069537 A JP 2000069537A JP 2000069537 A JP2000069537 A JP 2000069537A JP 2001252588 A JP2001252588 A JP 2001252588A
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- Japan
- Prior art keywords
- particles
- sieve
- classification
- ultrasonic
- ultrasonic irradiation
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、粉体の分級方法、
分級された粒子、およびその用途に関する。さらに詳し
くは、種々の粒子径を有する粉体を精密に所望の粒度範
囲の粒子に分級する分級方法、それにより分級された粒
子、およびその用途に関する。TECHNICAL FIELD The present invention relates to a method for classifying powder,
Classified particles and their use. More specifically, the present invention relates to a classification method for precisely classifying powders having various particle diameters into particles having a desired particle size range, particles classified thereby, and uses thereof.
【０００２】[0002]
【従来の技術】各種分野で取り扱われる粉体はその種
類、目的、用途によって、必要とされる平均粒子径及び
粒子径の分布が異なる。特に、液晶表示素子用スペーサ
ー、異方導電フィルム用導電性粒子、液体クロマトグラ
フィー用充填剤、フィルム用滑剤あるいは静電荷像現像
用トナーといった用途に用いられる粉体の場合、粒子径
の分布を狭くする必要がある。中でも、液晶表示素子用
スペーサーとして用いられる粉体は、粒子径分布を特に
狭くする必要があり、種々の方法により作製した原料粉
体から目的とする粒子径および粒子径分布となるように
精密に分別して使用する必要がある。2. Description of the Related Art Powders handled in various fields have different required average particle diameters and distributions of particle diameters depending on the kind, purpose and application. In particular, in the case of powders used for spacers for liquid crystal display elements, conductive particles for anisotropic conductive films, fillers for liquid chromatography, lubricants for films or toners for developing electrostatic images, the particle size distribution is narrowed. There is a need to. Above all, the powder used as the spacer for the liquid crystal display element needs to have a particularly narrow particle size distribution, and the raw material powders produced by various methods are precisely adjusted to have the desired particle size and particle size distribution. It needs to be used separately.
【０００３】一般に、粉体の粒子径分布を狭くするため
には、いわゆる分級装置が用いられる。分級装置として
は、サイクロン、沈降塔、あるいはふるい等が乾式また
は湿式で用いられる。しかしながら、旋回流中の遠心力
と重力とのバランスを利用して分級を行うサイクロンで
は、その構造上、分級ゾーンをショートパスする粒子が
存在するため、粒子径分布を狭くすることに限界があ
り、また少量ではあるものの粒子径分布から大きく外れ
た粒子が残存するといった問題を有している。また、媒
体中での沈降速度の差を利用して分級する沈降塔におい
ては、温度、振動などの要因によって沈降速度が変化す
るため、分級精度を上げることが困難であり、また粒子
径の小さいものについては、沈降速度が極めて小さいた
め分級に多大な時間が必要である。沈降塔を改良し、下
方より媒体を供給し上方よりオーバーフローさせる装置
も提案されているが、上記した沈降塔と同様の問題を有
している。Generally, a so-called classifier is used to narrow the particle size distribution of the powder. As a classifier, a cyclone, a sedimentation tower, a sieve, or the like is used in a dry type or a wet type. However, in cyclones that perform classification using the balance between centrifugal force and gravity in swirling flow, there are particles that short-pass the classification zone due to their structure, so there is a limit to narrowing the particle size distribution. In addition, there is a problem that, although in a small amount, particles that largely deviate from the particle size distribution remain. Further, in a sedimentation tower that classifies using a difference in sedimentation velocity in a medium, the sedimentation velocity changes due to factors such as temperature and vibration, so it is difficult to increase the classification accuracy, and the particle diameter is small. For those, the sedimentation speed is extremely low, so that a large amount of time is required for classification. An apparatus in which a settling tower is improved to supply a medium from below and overflow from above has also been proposed, but has the same problem as the above-mentioned settling tower.
【０００４】一方、ふるいは一定の目開きを通過するか
否かで分級を行うものである。目開き１０μｍ以上のも
のについては細線を編んだふるいが用いられ、それ以下
のものについては金属箔などをエッチングにより微細な
孔をあけたものや、電成ふるいと呼ばれる、メッキによ
って矩形の孔を有するスクリーンを作製したものが用い
られ、これらは細線を編んだものと比較して目開きが非
常によくそろっており分級の精度を向上させることがで
きるものである。特に電成ふるいはエッチングにより孔
をあけたものと比較して、厚みより小さな孔加工が可能
であり、サイドエッジがなく断面形状がきれいであり、
優れたふるいである。[0004] On the other hand, a sieve performs classification based on whether or not it passes through a certain opening. For those with an opening of 10 μm or more, a fine wire knitting sieve is used. For those with a mesh size of 10 μm or less, a fine hole made by etching a metal foil or the like, or a rectangular hole by plating, called an electric sieve, is used. The screens are used, and the screens are very well aligned as compared with those obtained by knitting fine wires, and can improve the classification accuracy. In particular, compared to the electric sieve with holes drilled by etching, holes smaller than the thickness can be processed, the cross-sectional shape is beautiful without side edges,
It is an excellent sieve.
【０００５】しかしながら、ふるいを分級装置として使
用した場合、操作中にふるいが目詰まりを起こしたり、
粒子が凝集することによってふるいわけの速度が著しく
低下する現象がしばしば観察される。この現象はふるい
の目開きが小さくなるほど顕著にかつ短時間で発生し、
その都度ふるいの洗浄や粒子の再分散といった操作が必
要である。また、電成ふるいを用いた分級において、超
音波を印加することでさらに分級効率を向上させること
ができるが、その反面電成ふるいは損傷し易くなり、分
級された粒子へ金属系不純物の混入のおそれがある。特
に分級された粒子を液晶表示素子用スペーサー等の電子
材料の用途に用いる場合、金属系不純物の混入は信頼性
低下の原因となるため重大な問題である。However, when the sieve is used as a classifier, the sieve may be clogged during operation,
A phenomenon is often observed in which the agglomeration of the particles significantly reduces the sieving speed. This phenomenon occurs more remarkably and in a shorter time as the sieve opening becomes smaller,
Each time, operations such as washing of a sieve and redispersion of particles are required. In addition, in the classification using an electric sieve, the classification efficiency can be further improved by applying ultrasonic waves.However, the electric sieve is easily damaged, and metal impurities are mixed into the classified particles. There is a possibility of. In particular, when the classified particles are used for an electronic material such as a spacer for a liquid crystal display element, the incorporation of metallic impurities is a serious problem because it causes a decrease in reliability.
【０００６】[0006]
【発明が解決しようとする課題】したがって、本発明の
課題は、超音波を印加しながら電成ふるいを用いて精密
に分級を行う方法において、ふるいの目詰まりや粒子の
凝集を起こさずに、しかも電成ふるいを損傷させること
なく、粉体の分級を行う方法を提供することにある。ま
た、それにより分級された粒子、およびその用途を提供
することにある。SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a method for precisely classifying using an electric sieve while applying ultrasonic waves, without causing clogging of the sieve or aggregation of particles. Another object of the present invention is to provide a method for classifying powder without damaging an electric sieve. Another object of the present invention is to provide particles classified thereby and uses thereof.
【０００７】[0007]
【課題を解決するための手段】上記課題を解決するた
め、本発明は、以下の構成を採用する。すなわち、本発
明の第１から第４の発明の分級方法は、電成ふるいと超
音波照射チップとを備えた分級装置に、原料粉体を液状
媒体に分散させた分散体を、前記超音波照射チップより
超音波を印加しながら通すことによって、前記原料粉体
を所望の粒度範囲の粒子に分級する方法であり、本発明
の第１発明の分級方法は、周波数が１０ｋ〜１００ｋＨ
ｚであり、振幅が１〜５０μｍの超音波を印加すること
を特徴とし、本発明の第２発明の分級方法は、前記超音
波照射チップの先端と前記電成ふるいとの間隔が０．０
５〜１０ｍｍであることを特徴とし、本発明の第３発明
の分級方法は、前記電成ふるいの面積が、前記超音波照
射チップの断面積の０．２５〜１００倍であることを特
徴とし、本発明の第４発明の分級方法は、前記超音波照
射チップの少なくとも先端部分がセラミックからなるこ
とを特徴とする。In order to solve the above-mentioned problems, the present invention employs the following constitution. That is, the classifying method according to the first to fourth aspects of the present invention provides a classifier equipped with an electric sieve and an ultrasonic irradiation tip, wherein the dispersion obtained by dispersing the raw material powder in a liquid medium is subjected to the ultrasonic waves. This is a method of classifying the raw material powder into particles having a desired particle size range by passing ultrasonic waves from an irradiation tip while applying ultrasonic waves. The classification method according to the first invention of the present invention has a frequency of 10 to 100 kHz.
z, and an ultrasonic wave having an amplitude of 1 to 50 μm is applied. According to the classification method of the second invention of the present invention, the distance between the tip of the ultrasonic irradiation tip and the electric sieve is 0.0
5 to 10 mm, the classification method of the third invention of the present invention is characterized in that the area of the electric sieve is 0.25 to 100 times the cross-sectional area of the ultrasonic irradiation tip. The classification method according to a fourth aspect of the present invention is characterized in that at least a tip portion of the ultrasonic irradiation tip is made of ceramic.
【０００８】本発明の分級された粒子は、上記の本発明
の第１から第４の発明のいずれかの粉体の分級方法によ
り分級された粒子である。本発明の液晶表示素子用スペ
ーサーは、上記の本発明の第１から第４の発明のいずれ
かの粉体の分級方法により分級された粒子を本体とす
る。[0008] The classified particles of the present invention are particles classified by the powder classification method according to any one of the first to fourth inventions of the present invention. The spacer for a liquid crystal display element of the present invention has, as a main body, particles classified by the method for classifying a powder according to any one of the first to fourth aspects of the present invention.
【０００９】[0009]
【発明の実施の形態】本発明では、電成ふるいと超音波
照射チップを備えた分級装置を用いて粒子の分級を行
う。電成ふるいとは、メッキによって矩形の孔を有する
スクリーンを作製したものである。電成ふるいの製造方
法としては、高精度にクロスライン状に腐食させたガラ
ス原板上に、真空蒸着、スパッタリング等の物理メッ
キ、あるいは電解メッキ、無電解メッキ等の化学メッキ
により導電性被膜を形成した後、腐食部分の溝以外のメ
ッキ層を除去し、これに電解メッキ等の方法でメッシュ
を形成し、ガラス原板から剥離する方法が挙げられる。
このようにして作製されたメッシュはガラス原板から剥
離後、必要に応じてさらに電解メッキを施してもかまわ
ない。また、他の製造方法として、ガラス平板上に真空
蒸着、スパッタリング等の物理メッキ、あるいは電解メ
ッキ、無電解メッキ等の化学メッキにより導電性被膜を
形成し、その被膜上にレジストを塗布した後、所定の形
状のパターンを形成し、その後エッチングによりパター
ン以外の部分を除去し、ガラス原板から剥離後、電解メ
ッキを施す方法も挙げられる。DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, particles are classified using a classifier provided with an electric sieve and an ultrasonic irradiation tip. The electric sieve is obtained by producing a screen having a rectangular hole by plating. As a method of manufacturing an electric sieve, a conductive film is formed on a glass plate corroded in a cross line shape with high precision by physical plating such as vacuum evaporation, sputtering, or chemical plating such as electrolytic plating or electroless plating. After that, there is a method of removing the plating layer other than the groove in the corroded portion, forming a mesh on the plating layer by a method such as electrolytic plating, and peeling the mesh from the glass plate.
The mesh produced in this manner may be further subjected to electrolytic plating, if necessary, after peeling from the glass base plate. Also, as another manufacturing method, a vacuum plating, physical plating such as sputtering, or electrolytic plating, chemical plating such as electroless plating on a glass flat plate, a conductive film is formed, and after applying a resist on the film, There is also a method of forming a pattern having a predetermined shape, removing portions other than the pattern by etching, exfoliating the glass substrate, and then performing electrolytic plating.
【００１０】電成ふるいの材質としては、金、白金、
銀、銅、鉄、アルミニウム、ニッケル及びこれらをベー
スとする種々の合金が用いられるが、ふるいの耐久性、
耐蝕性やメッキ作業の容易さからニッケルを主成分とす
るものが特に好適に用いられる。電成ふるいは、開孔
径、単位あたりの開孔数の調整が容易であるばかりでな
く、開孔径分布が非常に良好であるため、ふるいとして
用いた場合、非常に精度良く分級することが可能とな
る。電成ふるいは非常に薄いため、しかも本発明では超
音波を印加しながら分級を行うため、簡単に傷ついた
り、破れたりし、分級された粒子へ金属系不純物の混入
のおそれがある。特に分級された粒子を液晶表示素子用
スペーサー等の電子材料の用途に用いる場合、金属系不
純物の混入は信頼性低下の原因となるため重大な問題で
ある。そのため、電成ふるいの片面あるいは両面に格子
状あるいはリング状等のサポートを設けて強度を上げる
ことが好ましい。The materials of the electric sieve include gold, platinum,
Silver, copper, iron, aluminum, nickel and various alloys based on these are used.
A material containing nickel as a main component is particularly preferably used because of its corrosion resistance and ease of plating. The electric sieve is not only easy to adjust the hole diameter and the number of holes per unit, but also has a very good hole diameter distribution, so it can be classified very accurately when used as a sieve. Becomes Since the electric sieve is very thin, and furthermore, in the present invention, the classification is performed while applying ultrasonic waves, there is a risk that the classified sieve is easily damaged or broken, and metal-based impurities are mixed into the classified particles. In particular, when the classified particles are used for an electronic material such as a spacer for a liquid crystal display element, the incorporation of metallic impurities is a serious problem because it causes a decrease in reliability. Therefore, it is preferable to increase the strength by providing a grid-like or ring-like support on one or both sides of the electric sieve.
【００１１】電成ふるいの分級装置への取り付けに関し
ては、超音波の振動などによって、電成ふるいと分級装
置とが擦れて電成ふるいが損傷し分級された粒子へ金属
系不純物が混入するおそれがあるため、エラストマーか
らなる部材を介して取り付けることが好ましい。超音波
照射チップは、分級装置内に挿入されて、媒体に超音波
照射を行うものである。超音波を印加しながら分級を行
うことで、分級の効率を向上させることができる。本発
明の第１発明では、周波数が１０ｋ〜１００ｋＨｚであ
り、振幅が１〜５０μｍの超音波を印加することを特徴
とする。周波数は１５ｋ〜５０ｋＨｚであることが好ま
しく、振幅は５〜３０μｍであることが好ましい。周波
数が１０ｋＨｚより小さい場合、可聴領域に入るため防
音対策等の設備が必要となる。一方、周波数が１００ｋ
Ｈｚを超える場合、媒体中での超音波振動の減衰が大き
くなるため、粒子を分散させるのに必要なエネルギーが
大きくなり、分級効率が低下するため好ましくない。ま
た、振幅が１μｍより小さい場合、粒子を単粒子として
分散させることが困難になるばかりでなく、単粒子に分
散したものも再凝集する恐れがあり、電成ふるい上に粒
子が堆積しやすくなるために分級効率が低下する。一
方、振幅が５０μｍを超える場合、粒子の分散性は向上
するものの、電成ふるい自体に大きなシェアがかかるた
め、電成ふるいを損傷しやすい。特に電成ふるいは箔状
であるため、短時間の運転で破損してしまい、分級の精
度を低下させたり、電成ふるいの交換等に手間がかかる
だけでなく、分級された粉体中への金属系不純物の混入
を引き起こす。Regarding the attachment of the electric sieve to the classifier, the electric sieve and the classifier may be rubbed by ultrasonic vibration or the like, damaging the electric sieve and mixing metallic impurities into the classified particles. For this reason, it is preferable to attach the sheet via a member made of an elastomer. The ultrasonic irradiation tip is inserted into a classification device and performs ultrasonic irradiation on a medium. By performing classification while applying ultrasonic waves, the efficiency of classification can be improved. The first invention of the present invention is characterized in that ultrasonic waves having a frequency of 10 kHz to 100 kHz and an amplitude of 1 to 50 μm are applied. The frequency is preferably 15 kHz to 50 kHz, and the amplitude is preferably 5 to 30 μm. If the frequency is lower than 10 kHz, equipment for soundproofing or the like is required to enter the audible range. On the other hand, if the frequency is 100k
When the frequency exceeds Hz, the attenuation of the ultrasonic vibration in the medium increases, so that the energy required for dispersing the particles increases, and the classification efficiency decreases, which is not preferable. If the amplitude is smaller than 1 μm, not only is it difficult to disperse the particles as single particles, but also the particles dispersed in single particles may re-agglomerate, and the particles are easily deposited on the electric sieve. Therefore, the classification efficiency decreases. On the other hand, when the amplitude exceeds 50 μm, although the dispersibility of the particles is improved, the electric sieve itself has a large share, and thus the electric sieve is easily damaged. In particular, since the electric sieve is in the form of foil, it will be damaged in a short operation, lowering the accuracy of classification, not only replacing the electric sieve with a lot of effort, but also putting it into the classified powder. Metal impurities.
【００１２】本発明の第２発明では、超音波照射チップ
の先端と電成ふるいとの間隔が０．０５〜１０ｍｍであ
ることを特徴とする。好ましくは０．１〜５ｍｍであ
る。前記間隔が０．０５ｍｍよりも狭いと、電成ふるい
に大きな力がかかったり、外的要因で分級装置が振動し
た場合に電成ふるいと超音波照射チップが衝突すること
により、電成ふるいが損傷し、分級した粒子へ金属系不
純物の混入の問題がある。また、前記間隔が１０ｍｍよ
りも広いと、電成ふるい上に粒子が堆積しやすくなるた
め分級効率が低下する。その結果として分級の時間が長
くなったり、あるいは短時間で行うためには強い超音波
を印加する必要が生じるため、電成ふるいが損傷しやす
くなる。In a second aspect of the present invention, the distance between the tip of the ultrasonic irradiation tip and the electric sieve is 0.05 to 10 mm. Preferably it is 0.1-5 mm. When the distance is smaller than 0.05 mm, a large force is applied to the electric sieve, or when the classifying device vibrates due to an external factor, the electric sieve collides with the ultrasonic irradiation tip, so that the electric sieve is There is a problem that metal-based impurities are mixed into the damaged and classified particles. On the other hand, if the distance is larger than 10 mm, the particles are likely to be deposited on the electric sieve, so that the classification efficiency is reduced. As a result, it is necessary to apply a strong ultrasonic wave in order to lengthen the classification time or to perform the classification in a short time, so that the electric sieve is easily damaged.
【００１３】本発明の第３発明では、電成ふるいの面積
が、超音波照射チップの断面積の０．２５〜１００倍で
あることを特徴とする。好ましくは１〜２５倍である。
０．２５倍よりも小さい場合には、電成ふるいに対する
分散体の相対量が少ないために分級効率が悪くなる。一
方、１００倍よりも大きい場合には、電成ふるい上に粒
子が堆積しやすくなるため分級効率が低下する結果、電
成ふるいが損傷しやすくなる。本発明の第４発明では、
超音波照射チップの少なくとも先端部分がセラミックか
らなることを特徴とする。超音波照射チップが金属から
なると磨耗し易く、あるいは磨耗を防ぐために鋼などの
硬い金属を用いると腐食が起こり易く、いずれの場合に
も粉体中への金属系不純物の混入のおそれがある。セラ
ミックを用いれば、磨耗や腐食が起こりにくく、しかも
仮にセラミックが粉体中へ混入してしまったとしても、
信頼性低下の原因とはなりにくい。また、セラミック以
外の非金属の材料では、超音波の印加効率が低く実用的
ではない。超音波照射チップの先端部分が最も超音波振
動が激しいため、本発明では超音波照射チップの少なく
とも先端部分がセラミックからなるものであればよい
が、より効果的に金属系不純物の混入を防ぐためには、
接液部全体がセラミックからなることが好ましく、さら
にはチップ全体がセラミックからなることが好ましい。A third aspect of the present invention is characterized in that the area of the electric sieve is 0.25 to 100 times the sectional area of the ultrasonic irradiation tip. Preferably it is 1 to 25 times.
If it is smaller than 0.25 times, the classification efficiency is deteriorated because the relative amount of the dispersion to the electric sieve is small. On the other hand, when the ratio is larger than 100 times, particles are likely to be deposited on the electric sieve, so that the classification efficiency is lowered. As a result, the electric sieve is easily damaged. In the fourth invention of the present invention,
At least the tip portion of the ultrasonic irradiation tip is made of ceramic. When the ultrasonic irradiation tip is made of a metal, it is easily worn, or when a hard metal such as steel is used to prevent the wear, corrosion tends to occur, and in any case, there is a possibility that metal-based impurities may be mixed into the powder. If ceramics are used, wear and corrosion hardly occur, and even if the ceramics are mixed into the powder,
It is unlikely to cause a decrease in reliability. In addition, non-metallic materials other than ceramics have low ultrasonic wave application efficiency and are not practical. Since the ultrasonic vibration is most intense at the tip portion of the ultrasonic irradiation tip, in the present invention, at least the tip portion of the ultrasonic irradiation tip may be made of ceramic, but in order to more effectively prevent mixing of metal impurities. Is
It is preferable that the whole liquid contact part is made of ceramic, and it is more preferable that the whole chip is made of ceramic.
【００１４】上記セラミックとしては、従来公知のもの
から粉体および媒体の性質に合わせて適宜選択すること
ができ、例えば、アルミナ、マグネシア、ジルコニア、
安定化ジルコニア、部分安定化ジルコニア、ベリリア、
トリア、スピネルおよびムライト等の酸化物系セラミッ
クス；炭化珪素、炭化タングステンおよび炭化チタン等
の炭化物系セラミックス；窒化珪素、窒化アルミニウ
ム、窒化チタンおよびサイアロン等の窒化物系セラミッ
クス等が挙げられる。これらのセラミックスのうち、耐
蝕性および強度の点からジルコニア、安定化ジルコニ
ア、部分安定化ジルコニアを用いることが好ましい。The above-mentioned ceramic can be appropriately selected from conventionally known ceramics according to the properties of the powder and the medium. Examples thereof include alumina, magnesia, zirconia, and the like.
Stabilized zirconia, partially stabilized zirconia, beryllia,
Oxide ceramics such as thoria, spinel and mullite; carbide ceramics such as silicon carbide, tungsten carbide and titanium carbide; and nitride ceramics such as silicon nitride, aluminum nitride, titanium nitride and sialon. Among these ceramics, it is preferable to use zirconia, stabilized zirconia, and partially stabilized zirconia from the viewpoint of corrosion resistance and strength.
【００１５】超音波振動の発振方式は従来公知の方式で
よいが、中でも、負荷変動に対して振動速度を一定に保
つための回路構成を持った、定速度型周波数追尾型の発
振方式をとることで、分散が安定し、かつ電成ふるいに
過度のシェアがかからないため好ましい。本発明では、
上記分級装置に、原料粉体を液状媒体に分散させた分散
体を通すことによって湿式法により分級を行う。媒体と
して不活性ガスや空気などを用いる乾式法と比較して、
湿式法によった場合の方が超音波の照射効率、分散の安
定性が高く、また電成ふるいへの付着が少ない。The oscillation system of the ultrasonic vibration may be a conventionally known system, and among them, a constant speed type frequency tracking type oscillation system having a circuit configuration for keeping the vibration speed constant against a load change is adopted. This is preferable because dispersion is stable and an excessive share is not applied to the electric sieve. In the present invention,
Classification is performed by a wet method by passing a raw material powder dispersed in a liquid medium through the classifier. Compared to the dry method using inert gas or air as the medium,
In the case of the wet method, the ultrasonic irradiation efficiency and the dispersion stability are higher, and the adhesion to the electric sieve is smaller.
【００１６】原料粉体を分散させる液状媒体としては、
用いる電成ふるいの材質、開孔径、線数、および粉体の
性状あるいは粒子径分布などによって適切に選択するこ
とができる。図１に、電成ふるいと超音波照射チップと
を備えた分級装置の一例を示すが、本発明はこれによっ
て何ら限定されるものではない。図１において、電成ふ
るい１は、ハウジング上部４およびハウジング下部４′
によって挟み込まれる形で固定される。電成ふるい１の
強度を上げるためのサポート２が設けられ、エラストマ
ーからなるパッキン３を介してハウジング４、４′に接
続されている。ハウジング上部４内には超音波照射チッ
プ５が挿入され、これによりハウジング内の媒体に超音
波振動が照射される。ハウジング上部４内には媒体の循
環ライン６、６′及び媒体の供給ライン７が設けられて
いる。原料粉体を液状媒体に分散させた分散体はハウジ
ング上部４内に仕込まれ、媒体とともに電成ふるいの開
孔径よりも小さい粒子がハウジング下部４′へと移動す
る。操作の経過に伴い、ハウジング上部４内に存在する
電成ふるいの開孔径よりも小さい粒子が減少していき、
最終的には電成ふるいの開孔径を境にして、粒子径の大
きいもの（ハウジング上部４内に残留した粒子）と粒子
径の小さいもの（ハウジング下部４′に移動した粒子）
とに分級することができる。As the liquid medium in which the raw material powder is dispersed,
It can be appropriately selected depending on the material of the electric sieve to be used, the opening diameter, the number of lines, the properties of the powder, the particle size distribution, and the like. FIG. 1 shows an example of a classifier provided with an electric sieve and an ultrasonic irradiation chip, but the present invention is not limited to this. In FIG. 1, an electric sieve 1 comprises a housing upper part 4 and a housing lower part 4 '.
It is fixed by being sandwiched by. A support 2 for increasing the strength of the electric sieve 1 is provided, and is connected to the housings 4 and 4 'via a packing 3 made of an elastomer. An ultrasonic irradiation chip 5 is inserted into the housing upper part 4, whereby the medium in the housing is irradiated with ultrasonic vibration. Inside the housing upper part 4 are provided medium circulation lines 6, 6 'and a medium supply line 7. The dispersion obtained by dispersing the raw material powder in the liquid medium is charged in the housing upper part 4, and particles smaller than the opening diameter of the electric sieve move to the housing lower part 4 'together with the medium. As the operation progresses, particles smaller than the opening diameter of the electric sieve existing in the housing upper part 4 decrease,
Eventually, particles having a large particle diameter (particles remaining in the upper housing part 4) and small particle diameters (particles moved to the lower housing part 4 ') are separated from the opening diameter of the electric sieve.
And can be classified.
【００１７】上記した本発明の第１から第４の発明の分
級方法により、各種粉体は容易にかつ低コストで精密
に、しかもふるいの目詰まりや粒子の凝集を起こさず
に、また電成ふるいを損傷させずに分級を行うことがで
きる。したがって、得られる粒子の粒子径は極めてそろ
っている。用いる粉体の平均粒子径、粒子径分布および
電成ふるいの開孔径によって、分級により得られる粒子
の平均粒子径および粒子径分布は異なるが、粒子径の標
準偏差と平均粒子径の比Ｃｖを２〜１０％とすることが
できる。また、金属系不純物の混入を抑制することがで
きるため、原料粉体および媒体の性状、分級条件により
変化するが、金属系不純物の濃度を、原料粉体と比較し
て１０ｐｐｍ以下程度の増加にとどめることが可能とな
る。したがって、液晶表示素子用スペーサー等の電子材
料の用途に用いる場合にも信頼性が低下しない。According to the above-described classification methods of the first to fourth aspects of the present invention, various powders can be formed easily and accurately at a low cost without causing clogging of sieves or aggregation of particles. Classification can be performed without damaging the sieve. Therefore, the particle diameters of the obtained particles are extremely uniform. The average particle diameter and particle diameter distribution of the powder used and the average particle diameter and particle diameter distribution of the particles obtained by classification differ depending on the pore size of the electric sieve. It can be 2 to 10%. In addition, since the mixing of metal-based impurities can be suppressed, the concentration of the metal-based impurities is increased by about 10 ppm or less as compared with the raw material powder, although it varies depending on the properties of the raw material powder and the medium and the classification conditions. It is possible to stop. Therefore, the reliability does not decrease even when used for electronic materials such as spacers for liquid crystal display elements.
【００１８】本発明の第１から第４の分級方法により得
られる粒子の平均粒子径は特に限定されず、平均粒子径
が０．５μｍ程度の小さなものから、平均粒子径が１０
０μｍ程度の大きなものまで可能である。中でも、平均
粒子径が１０μｍ以下の小さな粒子を得る場合にも、低
コストで精密に、しかもふるいの目詰まりや粒子の凝集
を起こさずに分級を行うことができるのが本発明の大き
な効果である。上記において、本発明の第１から第４の
分級方法についてそれぞれ説明したが、本発明の第１か
ら第４の分級方法を複数組み合わせて実施することで、
さらなる効果が得られることはもちろんのことである。The average particle diameter of the particles obtained by the first to fourth classification methods of the present invention is not particularly limited, and the average particle diameter can be as small as about 0.5 μm to about 10 μm.
It can be as large as about 0 μm. Among them, even when obtaining small particles having an average particle diameter of 10 μm or less, classification can be performed accurately at low cost and without causing clogging of the sieve and aggregation of the particles. is there. In the above, the first to fourth classification methods of the present invention have been described, respectively. By implementing a plurality of the first to fourth classification methods of the present invention in combination,
Needless to say, further effects can be obtained.
【００１９】本発明の第１から第４の分級方法により分
級することのできる粉体としては、特に限定されない
が、後述する液晶表示素子用スペーサーの他、無電解め
っき粉体およびその基材粉体、クロマトグラフィー用充
填剤、各種標準粒子、免疫学的診断試薬用担体、ブロッ
キング防止剤、滑剤等の各種粉体を挙げることができ
る。また、その材質も特に限定されず、有機架橋重合体
粒子、無機系粒子、有機質無機質複合体粒子等が挙げら
れる。本発明の液晶表示素子用スペーサーは、上記した
本発明の第１から第４の発明の分級方法により分級され
た粒子を本体とする。そのため、粒子径が極めてそろっ
ており、正確な間隔で配置されるべき一対の電極基板間
の隙間距離を精度良く一定に保持することが可能であ
る。また、粒子中への金属系不純物の混入を抑制するこ
とができるので、金属系不純物による液晶は以降の乱れ
あるいは電気特性への影響を防止することができ、従来
公知の方法によって製造されたスペーサーを用いる場合
と比較して、液晶表示素子の画質が格段に向上する。The powder that can be classified by the first to fourth classification methods of the present invention is not particularly limited, but in addition to a spacer for a liquid crystal display element described later, an electroless plating powder and a base powder thereof. Examples include various powders such as a carrier, a filler for chromatography, various standard particles, a carrier for an immunological diagnostic reagent, an antiblocking agent, and a lubricant. Further, the material is not particularly limited, and examples thereof include organic crosslinked polymer particles, inorganic particles, and organic / inorganic composite particles. The spacer for a liquid crystal display element of the present invention has, as its main body, particles classified by the above-described classification method of the first to fourth inventions of the present invention. Therefore, the particle diameters are extremely uniform, and the gap distance between a pair of electrode substrates to be arranged at an accurate interval can be accurately and constantly maintained. In addition, since it is possible to suppress the incorporation of metal-based impurities into the particles, the liquid crystal due to the metal-based impurities can be prevented from subsequently disturbing or affecting the electrical characteristics, and a spacer manufactured by a conventionally known method can be used. The image quality of the liquid crystal display element is remarkably improved as compared with the case of using.
【００２０】本発明の液晶表示素子用スペーサーは、上
記した本発明の第１から第４の発明の分級方法により分
級された粒子を本体とするものであり、該粒子のみから
なるものであってもよいし、本体である粒子の表面に接
着剤層を有する接着性スペーサーであってもよい。ま
た、本体である粒子が染料および／または顔料を含むこ
とにより着色した着色粒子からなる着色スペーサーであ
ってもよい。液晶表示素子において、従来のスペーサー
の代わりに本発明の液晶表示素子用スペーサーを電極基
板間に介在させることで、同スペーサーとほぼ同じ隙間
距離を有する液晶表示素子を作製することができる。使
用されるスペーサーの量は、そのスペーサーの材質や基
板の大きさ等によって左右されるが、通常３０〜３００
個／ｍｍ2であり、従来用いられているスペーサーと同
様の条件をとることができる。The spacer for a liquid crystal display element of the present invention has, as its main body, particles classified by the classification method of the first to fourth inventions of the present invention, and is composed of only the particles. Alternatively, it may be an adhesive spacer having an adhesive layer on the surface of the particle as the main body. Further, a colored spacer composed of colored particles in which the main particles are colored by containing a dye and / or a pigment may be used. In a liquid crystal display element, by interposing the spacer for a liquid crystal display element of the present invention between electrode substrates instead of the conventional spacer, a liquid crystal display element having substantially the same gap distance as the spacer can be manufactured. The amount of the spacer to be used depends on the material of the spacer, the size of the substrate, and the like.
Pcs / mm 2 , and the same conditions as those of a conventionally used spacer can be taken.
【００２１】液晶表示素子は、たとえば、図２にみるよ
うに、第１電極基板と、第２電極基板と、液晶表示素子
用スペーサーと、シール材と液晶とを備えている。第１
電極基板は、第１基板と、第１基板の表面に形成された
第１電極とを有する。第２電極基板は、第２基板と、第
２基板の表面に形成された第２電極とを有し、第１電極
基板と対向している。液晶表示素子用スペーサとしては
上述の本発明のものが使用され、第１電極基板と第２電
極基板との間に介在し、その電極基板間の間隔を保持す
る。シール材は、第１電極基板と第２電極基板とを周辺
部で接着する。液晶は、第１電極基板と第２電極基板と
の間に封入されており、第１電極基板と第２電極基板と
シール材とで囲まれた空間に充填されている。As shown in FIG. 2, for example, the liquid crystal display element includes a first electrode substrate, a second electrode substrate, a spacer for a liquid crystal display element, a sealing material, and liquid crystal. First
The electrode substrate has a first substrate and a first electrode formed on a surface of the first substrate. The second electrode substrate has a second substrate and a second electrode formed on the surface of the second substrate, and faces the first electrode substrate. The above-described spacer of the present invention is used as a spacer for a liquid crystal display element, and is interposed between the first electrode substrate and the second electrode substrate to maintain a space between the electrode substrates. The sealant adheres the first electrode substrate and the second electrode substrate at a peripheral portion. The liquid crystal is sealed between the first electrode substrate and the second electrode substrate, and is filled in a space surrounded by the first electrode substrate, the second electrode substrate, and a sealing material.
【００２２】本発明の液晶表示板において、スペーサー
以外の、電極基板、シール材、液晶などについては従来
と同様のものを同様に使用することができる。電極基板
は、ガラス基板、フィルム基板などの基板と、基板の表
面に形成された電極とを有しており、必要に応じて、電
極基板の表面に電極を覆うように形成された配向膜をさ
らに有する。シール材としては、エポキシ樹脂接着シー
ル材などが使用される。液晶としては、従来より用いら
れているものでよく、たとえば、ビフェニル系、フェニ
ルシクロヘキサン系、シッフ塩基系、アゾ系、アゾキシ
系、安息香酸エステル系、ターフェニル系、シクロヘキ
シルカルボン酸エステル系、ビフェニルシクロヘキサン
系、ピリミジン系、ジオキサン系、シクロヘキシルシク
ロヘキサンエステル系、シクロヘキシルエタン系、シク
ロヘキセン系、フッ素系などの液晶が使用できる。In the liquid crystal display panel of the present invention, as for the electrode substrate, the sealing material, the liquid crystal, etc., other than the spacers, the same ones as those in the related art can be used. The electrode substrate has a substrate such as a glass substrate and a film substrate, and an electrode formed on the surface of the substrate.If necessary, an alignment film formed on the surface of the electrode substrate so as to cover the electrode is formed. Have more. As the sealing material, an epoxy resin adhesive sealing material or the like is used. As the liquid crystal, those conventionally used may be used, for example, biphenyl, phenylcyclohexane, Schiff base, azo, azoxy, benzoate, terphenyl, cyclohexylcarboxylate, biphenylcyclohexane , Pyrimidine, dioxane, cyclohexylcyclohexane ester, cyclohexylethane, cyclohexene, and fluorine liquid crystals can be used.
【００２３】液晶表示素子を作製する方法としては、た
とえば、本発明のスペーサーを面内スペーサーとして２
枚の電極基板のうちの一方の電極基板に湿式法または乾
式法により均一に散布したものに、本発明のスペーサー
をシール部スペーサーとしてエポキシ樹脂等の接着シー
ル材に分散させた後、もう一方の電極基板の接着シール
部分にスクリーン印刷などの手段により塗布したものを
載せ、適度の圧力を加え、１００〜１８０℃の温度で１
〜６０分間の加熱、または、照射量４０〜３００ｍＪ／
ｃｍ2の紫外線照射により、接着シール材を硬化させた
後、液晶を注入し、注入部を封止して、液晶表示素子を
得る方法を挙げることができるが、液晶表示板の作製方
法によって本発明が限定されるものではない。例えば、
面内スペーサーは、上記方法以外に、面内スペーサーを
分散含有するポリマー溶液を用いて配向膜を形成して、
配向膜の形成と同時に面内スペーサーをも形成する方法
によって形成してもよい。As a method of manufacturing a liquid crystal display element, for example, the spacer of the present invention is used as an in-plane spacer.
After the spacer of the present invention is dispersed in an adhesive sealing material such as an epoxy resin as a sealing portion spacer on one of the two electrode substrates uniformly dispersed by a wet method or a dry method on one of the electrode substrates, The adhesive applied to the electrode substrate is placed on the adhesive seal by means of screen printing or the like, and an appropriate pressure is applied.
Heating for up to 60 minutes, or irradiation dose of 40 to 300 mJ /
After the adhesive sealing material is cured by irradiating ultraviolet rays of 2 cm 2, a method of injecting liquid crystal and sealing the injected portion to obtain a liquid crystal display element can be mentioned. The invention is not limited. For example,
In-plane spacer, in addition to the above method, forming an alignment film using a polymer solution containing dispersed in-plane spacer,
It may be formed by a method of forming an in-plane spacer at the same time as forming the alignment film.
【００２４】本発明の液晶表示素子は、従来の液晶表示
素子と同じ用途、たとえば、テレビ、モニター、パーソ
ナルコンピューター、ワードプロセッサー、カーナビゲ
ーションシステム、ＤＶＤ、デジタルビデオカメラ、Ｐ
ＨＳ（携帯情報端末）などの画像表示素子として使用さ
れる。The liquid crystal display device of the present invention has the same applications as conventional liquid crystal display devices, for example, televisions, monitors, personal computers, word processors, car navigation systems, DVDs, digital video cameras,
It is used as an image display element of an HS (portable information terminal) or the like.
【００２５】[0025]
【実施例】以下に本発明を実施例によりさらに詳細に説
明するが、下記実施例は本発明を限定する性質のもので
はなく、前・後記の趣旨の範囲で設計変更することはい
ずれも本発明の技術的範囲に含まれるものである。実施
例中で「部」、「％」とは特にことわりがない限り、そ
れぞれ「重量部」、「重量％」を表すものとする。 （実施例１）懸濁重合により製造した平均粒子径４．７
μｍ、粒子径の標準偏差０．５２μｍのジビニルベンゼ
ン系球状粒子からなる粉体を図１に示した装置を用いて
分級を行った。分級に際して用いた超音波照射チップは
ジルコニア製であり、周波数２０ｋＨｚ、振幅１０μｍ
の振動を印可して分級操作を行った。超音波照射チップ
と電成ふるいの間隔は３ｍｍ、電成ふるいの有効面積と
チップの断面積の比は４７．９であった。The present invention will be described in more detail with reference to the following examples. However, the following examples do not limit the scope of the present invention. It is within the technical scope of the invention. In the examples, “parts” and “%” represent “parts by weight” and “% by weight”, respectively, unless otherwise specified. (Example 1) Average particle size of 4.7 produced by suspension polymerization
The powder comprising divinylbenzene-based spherical particles having a particle diameter of 0.5 μm and a standard deviation of the particle diameter of 0.52 μm was classified using the apparatus shown in FIG. The ultrasonic irradiation tip used for classification is made of zirconia, and has a frequency of 20 kHz and an amplitude of 10 μm.
The classification operation was performed by applying the vibration of. The distance between the ultrasonic irradiation tip and the electric sieve was 3 mm, and the ratio of the effective area of the electric sieve to the cross-sectional area of the chip was 47.9.
【００２６】電成ふるいとしてニッケル系で開孔径３．
９μｍ、線数１５００本／インチのもの（ふるいＡ）を
用い、上記条件で１時間分級を行った後、ハウジング上
部に残存した液を回収し（下分級）、これをニッケル系
で開孔径４．７μｍ、線数１５００本／インチの電成ふ
るい（ふるいＢ）を用いて再び１０分間分級し、ハウジ
ング下部に流出した分散体を回収した（上分級）。回収
した分散体のろ過、乾燥を行い、分級粒子１を得た。分
級粒子１の平均粒子径は４．２８μｍで、粒子径の標準
偏差は０．１８μｍであった。また、分級前後における
分級粒子１中の鉄原子の差を蛍光Ｘ線により分析したと
ころ４ｐｐｍ以下であった。As an electric sieve, a nickel-based sieve having an opening diameter of 3.
After classifying for 1 hour under the above conditions using a 9 μm, 1500 lines / inch (Sieve A), the liquid remaining at the top of the housing was collected (lower classification), and this was nickel-based and the pore size was 4 mm. Classification was again performed for 10 minutes using an electric sieve (sieve B) having a line size of 1.7 μm and a number of lines of 1500 / inch, and the dispersion flowing out to the lower portion of the housing was collected (upper classification). The collected dispersion was filtered and dried to obtain classified particles 1. The average particle diameter of the classified particles 1 was 4.28 μm, and the standard deviation of the particle diameter was 0.18 μm. Further, when the difference between the iron atoms in the classified particles 1 before and after the classification was analyzed by X-ray fluorescence, it was 4 ppm or less.
【００２７】（実施例２）実施例１と同様の装置を用い
て、平均粒子径６．５μｍ、粒子径の標準偏差０．７３
μｍの球状シリカ粒子を、ニッケル系で開孔径６．０μ
ｍ、線数１０００本／インチのふるい（ふるいＣ）およ
びニッケル系で開孔径７．０μｍ、線数１０００本／イ
ンチのふるい（ふるいＤ）を用いて、分級を行った。超
音波照射チップと電成ふるいの間隔は５ｍｍ、電成ふる
いの有効面積とチップの断面積の比は１．７であった。
この分級の結果、平均粒子径６．５２μｍ、粒子径の標
準偏差０．２１μｍの分級粒子２が得られた。また、分
級前後における分級粒子２中の鉄原子の差を蛍光Ｘ線に
より分析したところ４ｐｐｍ以下であった。Example 2 Using the same apparatus as in Example 1, the average particle diameter was 6.5 μm, and the standard deviation of the particle diameter was 0.73.
μm spherical silica particles, nickel-based
Classification was performed using a sieve having a diameter of 1,000 m / inch (sieve C) and a sieve having a pore size of 7.0 μm and a number of lines of 1000 / inch (sieve D) of nickel. The distance between the ultrasonic irradiation tip and the electric sieve was 5 mm, and the ratio of the effective area of the electric sieve to the cross-sectional area of the chip was 1.7.
As a result of this classification, classified particles 2 having an average particle diameter of 6.52 μm and a standard deviation of the particle diameter of 0.21 μm were obtained. Further, the difference between the iron atoms in the classified particles 2 before and after the classification was analyzed by fluorescent X-ray and found to be 4 ppm or less.
【００２８】（実施例３）実施例１と同様の装置を用い
て、平均粒子径５．３μｍ、粒子径の標準偏差０．３４
μｍのアクリル−シロキサン複合球状粒子を、実施例１
で使用したふるいＡおよび実施例２で使用したふるいＣ
を用いて、照射する超音波の振幅１５μｍで分級を行っ
た。超音波照射チップと電成ふるいの間隔は１ｍｍ、電
成ふるいの有効面積とチップの断面積の比は６．２５で
あった。この分級の結果、平均粒子径５．３４μｍ、粒
子径の標準偏差０．１８μｍの分級粒子３が得られた。
また、分級前後における分級粒子３中の鉄原子の差を蛍
光Ｘ線により分析したところ４ｐｐｍ以下であった。Example 3 Using the same apparatus as in Example 1, the average particle diameter was 5.3 μm and the standard deviation of the particle diameter was 0.34.
Example 1 Acrylic-siloxane composite spherical particles having a particle diameter of
Sieve A used in Example 2 and sieve C used in Example 2
Was used to classify the applied ultrasonic waves at an amplitude of 15 μm. The distance between the ultrasonic irradiation tip and the electric sieve was 1 mm, and the ratio of the effective area of the electric sieve to the cross-sectional area of the chip was 6.25. As a result of this classification, classified particles 3 having an average particle diameter of 5.34 μm and a standard deviation of the particle diameter of 0.18 μm were obtained.
Further, the difference between the iron atoms in the classified particles 3 before and after the classification was analyzed by fluorescent X-ray and found to be 4 ppm or less.
【００２９】（実施例４）コア粒子として実施例３で得
られた分級粒子３の表面をスチレン−アクリル樹脂（平
均粒子径０．４μｍ、Ｔｇ６８℃）で乾式コーティング
を行い、熱可塑性樹脂コーティング粒子とした。この粒
子の平均粒子径は６．２μｍ、粒子径の標準偏差０．７
８μｍであった。このコーティング粒子を、実施例１と
同様の装置を用いて、実施例１で使用したふるいＡおよ
び実施例２で使用したふるいＣを用いて、分級を行っ
た。超音波照射チップと電成ふるいの間隔は１ｍｍ、電
成ふるいの有効面積とチップの断面積の比は６．２５で
あった。Example 4 The surface of the classified particles 3 obtained in Example 3 as core particles was dry-coated with a styrene-acrylic resin (average particle diameter 0.4 μm, Tg 68 ° C.) to form thermoplastic resin-coated particles. And The average particle diameter of the particles is 6.2 μm, and the standard deviation of the particle diameter is 0.7.
It was 8 μm. The coated particles were classified using the same apparatus as in Example 1, using sieve A used in Example 1 and sieve C used in Example 2. The distance between the ultrasonic irradiation tip and the electric sieve was 1 mm, and the ratio of the effective area of the electric sieve to the cross-sectional area of the chip was 6.25.
【００３０】この分級の結果、平均粒子径５．５４μ
ｍ、粒子径の標準偏差０．２７μｍの分級粒子４が得ら
れた。また、分級前後における分級粒子３中の鉄原子の
差を蛍光Ｘ線により分析したところ４ｐｐｍ以下であっ
た。 （比較例１）実施例１において照射する超音波の周波数
を１２０ｋＨｚに変更した以外は同様の操作を行ったと
ころ、ふるいＢ上に多量の粒子が沈降しわずかしか分級
粒子（比較分級粒子１）が得られなかった。なお、比較
分級粒子１の平均粒子径は４．２２μｍ、粒子径の標準
偏差０．２７μｍであった。As a result of this classification, the average particle size was 5.54 μm.
m, classified particles 4 having a standard deviation of particle diameter of 0.27 μm were obtained. Further, the difference between the iron atoms in the classified particles 3 before and after the classification was analyzed by fluorescent X-ray and found to be 4 ppm or less. (Comparative Example 1) When the same operation was performed as in Example 1 except that the frequency of the ultrasonic wave to be irradiated was changed to 120 kHz, a large amount of particles settled on the sieve B, and the particles were slightly classified (Comparative classified particles 1). Was not obtained. The average particle diameter of the comparative classified particles 1 was 4.22 μm, and the standard deviation of the particle diameter was 0.27 μm.
【００３１】（比較例２）実施例１において照射する超
音波の振幅を６０μｍに変更した以外は同様の操作を行
ったところ、分級中３０分経過したところでハウジング
下部への液の流出量が増加した。この時点で分級を中断
し電成ふるいを観察したところ、ふるいが破れており分
級を継続することができなかった。 （比較例３）実施例２において超音波照射チップと電成
ふるいの間隔を１３ｍｍに変更した以外は同様の操作を
行ったところ、ふるいＣ上に多量の粒子が沈降しハウジ
ング下部への分級液の流出が著しく低下したため下分級
を終了した。その後ふるいＤを用いて上分級を行った
後、ろ過、乾燥を行い、比較分級粒子３を得た。(Comparative Example 2) The same operation as in Example 1 was carried out except that the amplitude of the ultrasonic wave to be irradiated was changed to 60 µm, and the amount of liquid flowing out to the lower portion of the housing increased after 30 minutes during the classification. did. At this time, the classification was interrupted and the electric sieve was observed. As a result, the sieve was broken and the classification could not be continued. (Comparative Example 3) The same operation was performed as in Example 2 except that the distance between the ultrasonic irradiation tip and the electric sieve was changed to 13 mm. A large amount of particles settled on the sieve C, and the classification liquid was moved to the lower part of the housing. The lower classification was terminated because the outflow of methane decreased significantly. Then, after performing upper classification using a sieve D, filtration and drying were performed to obtain comparative classified particles 3.
【００３２】比較分級粒子３の平均粒子径は６．５０μ
ｍ、粒子径の標準偏差は０．２５μｍであった。 （比較例４）実施例２において電成ふるいの有効面積と
チップの断面積の比を２２５に変更した以外は同様の操
作を行ったところ、ハウジング下部に液が流出せず、分
級することができなかった。 （比較例５）実施例２において照射する超音波の周波数
を８ｋＨｚに変更した以外は同様の操作を行ったとこ
ろ、多大な騒音が発生し分級を継続することができなか
った。The average particle diameter of the comparative classified particles 3 is 6.50 μm.
m, the standard deviation of the particle diameter was 0.25 μm. (Comparative Example 4) The same operation as in Example 2 was performed except that the ratio of the effective area of the electric sieve to the cross-sectional area of the chip was changed to 225. could not. (Comparative Example 5) A similar operation was performed except that the frequency of the ultrasonic wave to be applied was changed to 8 kHz in Example 2, and a large amount of noise was generated, and the classification could not be continued.
【００３３】（比較例６）実施例２において照射する超
音波の振幅を０．８μｍに変更した以外は同様の操作を
行ったところ、ふるいＣおよびＤ上に多量の粒子が沈降
しわずかしか分級粒子（比較分級粒子６）が得られなか
った。なお比較分級粒子６の平均粒子径は６．５１μ
ｍ、粒子径の標準偏差は０．２６μｍであった。 （比較例７）実施例３において超音波照射チップのみを
ステンレス製のものに交換した以外は同様の操作を行い
比較分級粒子７を得た。比較分級粒子７の平均粒子径は
５．３３ｍｍ、粒子径の標準偏差は０．１８μｍであ
り、分級前後における比較分級粒子７中の鉄原子の差を
蛍光Ｘ線により分析したところ７ｐｐｍであった。(Comparative Example 6) A similar operation was performed as in Example 2 except that the amplitude of the ultrasonic wave to be irradiated was changed to 0.8 µm. A large amount of particles settled on the sieves C and D, and the particles were classified only slightly. No particles (comparatively classified particles 6) were obtained. The average particle diameter of the comparative classified particles 6 was 6.51 μm.
m, the standard deviation of the particle diameter was 0.26 μm. Comparative Example 7 Comparative classified particles 7 were obtained in the same manner as in Example 3, except that only the ultrasonic irradiation tip was replaced with a stainless steel tip. The average particle diameter of the comparative classified particles 7 was 5.33 mm, the standard deviation of the particle diameter was 0.18 μm, and the difference between the iron atoms in the comparative classified particles 7 before and after classification was analyzed by fluorescent X-ray, and was 7 ppm. .
【００３４】（比較例８）実施例３において超音波照射
チップと電成ふるいの間隔を０．０４ｍｍに変更した以
外は同様の操作を行ったところ、分級中３分経過したと
ころでハウジング下部への液の流出量が著しく増加し
た。この時点で分級を中断し電成ふるいを観察したとこ
ろ、ふるいが破れており分級を継続することができなか
った。 （比較例９）実施例４において電成ふるいの有効面積と
チップの断面積の比が０．２０であるニッケル系で開孔
径４．０μｍ、線数１０００本／インチのもの（ふるい
Ｅ）、および、ニッケル系で開孔径６．２μｍ、線数１
０００本／インチのもの（ふるいＦ）をそれぞれふるい
Ａ、ふるいＢに代えて同様の操作を行ったところ、上分
級・下分級ともにハウジング下部への液の流出が少な
く、わずかしか分級粒子（比較分級粒子９）の平均粒子
径は５．６１μｍ、粒子径の標準偏差は０．２７μｍで
あった。Comparative Example 8 The same operation as in Example 3 was performed except that the distance between the ultrasonic irradiation tip and the electric sieve was changed to 0.04 mm. The outflow of liquid increased significantly. At this time, the classification was interrupted and the electric sieve was observed. As a result, the sieve was broken and the classification could not be continued. (Comparative Example 9) A nickel-based sieve having an opening area of 4.0 μm and a number of lines of 1000 lines / inch (sieve E) in Example 4, in which the ratio of the effective area of the electric sieve to the cross-sectional area of the chip is 0.20, And a nickel-based pore size of 6.2 μm and a line number of 1
When the same operation was performed with the sieve A and sieve B, respectively, for 2,000 lines / inch (sieve F), the outflow of liquid to the lower part of the housing was small in both the upper and lower classifications, and the classified particles were only slightly The average particle diameter of the classified particles 9) was 5.61 μm, and the standard deviation of the particle diameter was 0.27 μm.
【００３５】（実施例５）図２に示すような液晶表示素
子を以下の方法により作製した。まず、３００ｍｍ×３
４５ｍｍ×１．１ｍｍの下側ガラス基板２１上に、透明
電極１５およびポリイミド配向膜１４を形成した後、ラ
ビングを行って、下側電極基板２１０を得た。その下側
電極基板２１０に、メタノール３０重量部、イソプロパ
ノール２０重量部、水５０重量部の混合溶媒中に実施例
１で得られた分級粒子１を液晶表示素子用スペーサー１
８として１重量％となるように均一に分散させたものを
５秒間散布した。Example 5 A liquid crystal display device as shown in FIG. 2 was manufactured by the following method. First, 300mm × 3
After forming the transparent electrode 15 and the polyimide alignment film 14 on the lower glass substrate 21 of 45 mm × 1.1 mm, rubbing was performed to obtain the lower electrode substrate 210. On the lower electrode substrate 210, the classified particles 1 obtained in Example 1 were mixed in a mixed solvent of 30 parts by weight of methanol, 20 parts by weight of isopropanol, and 50 parts by weight of water.
A dispersion uniformly dispersed so as to be 1% by weight as 8 was sprayed for 5 seconds.
【００３６】一方、３００ｍｍ×３４５ｍｍ×１．１ｍ
ｍの上側ガラス基板２２上に、透明電極１５およびポリ
イミド配向膜１４を形成した後、ラビングを行って、上
側電極基板２２０を得た。そして、エポキシ樹脂接着シ
ール剤中に実施例１で得られた分級粒子１をシール部ス
ペーサー１３として３０重量％となるように分散させた
ものを上側電極基板２２０の接着シール部分にスクリー
ン印刷した。最後に、上側電極基板２２０、下側電極基
板２１０を電極１５および配向膜１４がそれぞれ対向す
るように、液晶表示素子用スペーサー１８を介して貼り
合わせ、４ｋｇ／ｃｍ2の圧力を加え、１５０℃の温度
で３０分間加熱し、接着シール剤１２を硬化させた。そ
の後、２枚の電極基板２１０、２２０の隙間を真空と
し、さらに大気圧に戻すことによりビフェニル系および
フェニルシクロヘキサン系の液晶物質を混合した液晶１
７を注入し、注入部を封止した。そして、上下ガラス基
板２２、２１の外側にポリビニルアルコール系偏光膜１
６を貼り付けて液晶表示素子１とした。On the other hand, 300 mm × 345 mm × 1.1 m
After forming the transparent electrode 15 and the polyimide alignment film 14 on the m upper glass substrate 22, rubbing was performed to obtain the upper electrode substrate 220. Then, the classified particles 1 obtained in Example 1 dispersed in an epoxy resin adhesive sealant so as to be 30% by weight as a seal spacer 13 were screen-printed on the adhesive seal portion of the upper electrode substrate 220. Finally, the upper electrode substrate 220 and the lower electrode substrate 210 are bonded via the liquid crystal display element spacer 18 so that the electrode 15 and the alignment film 14 face each other, and a pressure of 4 kg / cm 2 is applied, and The adhesive sealant 12 was cured by heating at a temperature of 30 minutes. Thereafter, the gap between the two electrode substrates 210 and 220 is evacuated, and the pressure is returned to the atmospheric pressure.
7, and the injection portion was sealed. Then, the polyvinyl alcohol-based polarizing film 1 is provided outside the upper and lower glass substrates 22 and 21.
6 was attached to the liquid crystal display element 1.
【００３７】液晶表示素子１について画像むらおよび静
止画像を４８時間連続表示した後の残像の有無を目視に
より評価した。結果を表１に示す。 （実施例６〜８、比較例６〜１０）実施例２〜４、比較
例１、３、６、７および９で得られた分級粒子を用い
て、実施例５と同様にして液晶表示素子２〜４、比較液
晶表示素子１〜５をそれぞれ作製し、実施例５と同じ方
法で評価を行った。結果を表１に示す。The liquid crystal display element 1 was visually evaluated for image unevenness and the presence or absence of an afterimage after continuously displaying a still image for 48 hours. Table 1 shows the results. (Examples 6 to 8, Comparative Examples 6 to 10) Using the classified particles obtained in Examples 2 to 4 and Comparative Examples 1, 3, 6, 7 and 9, in the same manner as in Example 5, a liquid crystal display element 2 to 4 and comparative liquid crystal display elements 1 to 5 were produced, respectively, and evaluated in the same manner as in Example 5. Table 1 shows the results.
【００３８】[0038]
【表１】 [Table 1]
【００３９】[0039]
【発明の効果】本発明の第１発明の分級方法では、周波
数が１０ｋ〜１００ｋＨｚであり、振幅が１〜５０μｍ
の超音波を印加するため、分級効率が高く、電成ふるい
の損傷も少ない。本発明の第２発明の分級方法では、超
音波照射チップの先端と電成ふるいとの間隔が０．０５
〜１０ｍｍとであるため、分級効率が高く、電成ふるい
の損傷も少ない。本発明の第３発明の分級方法では、電
成ふるいの面積が、超音波照射チップの断面積の０．２
５〜１００倍であるため、分級効率が高く、電成ふるい
の損傷も少ない。According to the classification method of the first invention of the present invention, the frequency is 10 kHz to 100 kHz and the amplitude is 1 μm to 50 μm.
, The classification efficiency is high and the electric sieve is less damaged. In the classification method according to the second invention of the present invention, the distance between the tip of the ultrasonic irradiation tip and the electric sieve is 0.05.
Since it is 10 to 10 mm, the classification efficiency is high and the electric sieve is hardly damaged. In the classification method according to the third aspect of the present invention, the area of the electric sieve is 0.2% of the sectional area of the ultrasonic irradiation tip.
Since the ratio is 5 to 100 times, the classification efficiency is high and the electric sieve is hardly damaged.
【００４０】本発明の第４発明の分級方法では、超音波
照射チップの少なくとも先端部分がセラミックからなる
ため、磨耗や腐食が起こりにくく、しかも仮にセラミッ
クが粉体中へ混入してしまったとしても、信頼性低下の
原因とはなりにくい。本発明の分級された粒子は、上記
の本発明の第１から第４の発明のいずれかの粉体の分級
方法により分級された粒子であるため、粒子径が極めて
そろったものである。また、金属系不純物の混入を抑制
することができるため、液晶表示素子用スペーサー等の
電子材料の用途に用いる場合にも信頼性が低下しない。
本発明の液晶表示素子用スペーサーは、上記の本発明の
第１から第４の発明のいずれかの粉体の分級方法により
分級された粒子を本体とするため、粒子径が極めてそろ
っており、正確な間隔で配置されるべき一対の電極基板
間の隙間距離を精度良く一定に保持することが可能であ
る。また、粒子中への金属系不純物の混入を抑制するこ
とができるので、金属系不純物による液晶は以降の乱れ
あるいは電気特性への影響を防止することができ、従来
公知の方法によって製造されたスペーサーを用いる場合
と比較して、液晶表示素子の画質が格段に向上する。In the classification method according to the fourth invention of the present invention, at least the tip of the ultrasonic irradiation tip is made of ceramic, so that it is difficult for abrasion and corrosion to occur, and even if ceramic is mixed into the powder. , And is unlikely to cause a reduction in reliability. Since the classified particles of the present invention are particles classified by the powder classification method of any one of the first to fourth inventions of the present invention, the particle diameters are extremely uniform. In addition, since metal impurities can be prevented from being mixed, the reliability does not decrease even when used for electronic materials such as a spacer for a liquid crystal display element.
Since the spacer for a liquid crystal display element of the present invention has, as a main body, particles classified by the method for classifying a powder according to any one of the first to fourth inventions of the present invention, the particle diameter is extremely uniform, The gap distance between the pair of electrode substrates to be arranged at accurate intervals can be accurately and constantly maintained. In addition, since it is possible to suppress the incorporation of metal-based impurities into the particles, the liquid crystal due to the metal-based impurities can be prevented from subsequently disturbing or affecting the electrical characteristics, and a spacer manufactured by a conventionally known method can be used. The image quality of the liquid crystal display element is remarkably improved as compared with the case of using.
【図１】 本発明の分級方法に用いられる分級装置の一
例を表す概略断面図である。FIG. 1 is a schematic sectional view illustrating an example of a classification device used in a classification method of the present invention.
【図２】 本発明の液晶表示素子用スペーサーが用いら
れる液晶表示素子の一例を表す概略断面図である。FIG. 2 is a schematic cross-sectional view illustrating an example of a liquid crystal display device using the spacer for a liquid crystal display device of the present invention.
１ 電成ふるい ２ サポート ３ パッキン ４ ハウジング上部 ４′ ハウジング下部 ５ 超音波照射チップ ６、６′ 媒体循環ライン ７ 媒体供給ライン １２ 接着シール材 １３ シール部スペーサー １４ 配向膜 １５ 電極 １６ 偏光膜 １７ 液晶 １８ 面内スペーサー ２１ 下側ガラス基板 ２２ 上側ガラス基板 ２１０ 下側電極基板 ２２０ 上側電極基板 DESCRIPTION OF SYMBOLS 1 Electric sieve 2 Support 3 Packing 4 Housing upper part 4 'Housing lower part 5 Ultrasonic irradiation chip 6, 6' Medium circulation line 7 Medium supply line 12 Adhesive sealing material 13 Seal part spacer 14 Alignment film 15 Electrode 16 Polarization film 17 Liquid crystal 18 In-plane spacer 21 Lower glass substrate 22 Upper glass substrate 210 Lower electrode substrate 220 Upper electrode substrate
───────────────────────────────────────────────────── フロントページの続き (72)発明者 若槻 伸治 大阪府吹田市西御旅町５番８号 株式会社 日本触媒内 (72)発明者 佐々木 令晋 大阪府吹田市西御旅町５番８号 株式会社 日本触媒内 (72)発明者 粟嶋 優 大阪府吹田市西御旅町５番８号 株式会社 日本触媒内 (72)発明者 北垣戸 寛之 大阪府吹田市西御旅町５番８号 株式会社 日本触媒内 Ｆターム(参考） 2H089 LA07 LA15 LA19 MA01X MA04Y MA07Y NA10 NA24 NA41 NA60 QA12 QA14 TA04 4D071 AA02 AB45 AB62 BB06 DA20 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Shinji Wakatsuki 5-8 Nishiburi-cho, Suita-shi, Osaka Nippon Shokubai Co., Ltd. (72) Inventor Reisin Sasaki 5-8 Nishi-Maburi-cho, Suita-shi, Osaka Company Nippon Shokubai Co., Ltd. (72) Inventor Yu Awashima 5-8, Nishiobari-cho, Suita-shi, Osaka Nippon Shokubai Co., Ltd. (72) Inventor Hiroyuki Kitagaki 5-8 Nishiobari-cho, Suita-shi, Osaka Japan F term in catalyst (reference) 2H089 LA07 LA15 LA19 MA01X MA04Y MA07Y NA10 NA24 NA41 NA60 QA12 QA14 TA04 4D071 AA02 AB45 AB62 BB06 DA20
Claims (6)
た分級装置に、原料粉体を液状媒体に分散させた分散体
を、前記超音波照射チップより超音波を印加しながら通
すことによって、前記原料粉体を所望の粒度範囲の粒子
に分級する方法であって、周波数が１０ｋ〜１００ｋＨ
ｚであり、振幅が１〜５０μｍの超音波を印加すること
を特徴とする粉体の分級方法。1. A dispersant obtained by dispersing a raw material powder in a liquid medium is passed through a classifier provided with an electric sieve and an ultrasonic irradiation chip while applying ultrasonic waves from the ultrasonic irradiation chip. A method for classifying the raw material powder into particles having a desired particle size range, wherein the frequency is 10 kH to 100 kH.
A method for classifying powder, wherein z is applied and ultrasonic waves having an amplitude of 1 to 50 μm are applied.
た分級装置に、原料粉体を液状媒体に分散させた分散体
を、前記超音波照射チップより超音波を印加しながら通
すことによって、前記原料粉体を所望の粒度範囲の粒子
に分級する方法であって、前記超音波照射チップの先端
と前記電成ふるいとの間隔が０．０５〜１０ｍｍである
ことを特徴とする粉体の分級方法。2. A classifier having an electric sieve and an ultrasonic irradiation chip, and passing a dispersion obtained by dispersing the raw material powder in a liquid medium while applying ultrasonic waves from the ultrasonic irradiation chip. A method for classifying the raw material powder into particles having a desired particle size range, wherein a distance between a tip of the ultrasonic irradiation tip and the electric sieve is 0.05 to 10 mm. Classification method.
た分級装置に、原料粉体を液状媒体に分散させた分散体
を、前記超音波照射チップより超音波を印加しながら通
すことによって、前記原料粉体を所望の粒度範囲の粒子
に分級する方法であって、前記電成ふるいの面積が、前
記超音波照射チップの断面積の０．２５〜１００倍であ
ることを特徴とする粉体の分級方法。3. A classifier provided with an electric sieve and an ultrasonic irradiation tip, by passing a dispersion obtained by dispersing the raw material powder in a liquid medium while applying ultrasonic waves from the ultrasonic irradiation tip. A method of classifying the raw material powder into particles having a desired particle size range, wherein an area of the electric sieve is 0.25 to 100 times a cross-sectional area of the ultrasonic irradiation tip. Classification method of powder.
た分級装置に、原料粉体を液状媒体に分散させた分散体
を、前記超音波照射チップより超音波を印加しながら通
すことによって、前記原料粉体を所望の粒度範囲の粒子
に分級する方法であって、前記超音波照射チップの少な
くとも先端部分がセラミックからなることを特徴とする
粉体の分級方法。4. A classifier provided with an electric sieve and an ultrasonic irradiation chip, and a dispersion obtained by dispersing the raw material powder in a liquid medium is passed while applying ultrasonic waves from the ultrasonic irradiation chip. A method of classifying the raw material powder into particles having a desired particle size range, wherein at least a tip portion of the ultrasonic irradiation tip is made of ceramic.
の分級方法により分級された粒子。5. Particles classified by the method for classifying powder according to any one of claims 1 to 4.
の分級方法により分級された粒子を本体とする、液晶表
示素子用スペーサー。6. A spacer for a liquid crystal display element, comprising as a main body particles classified by the powder classification method according to claim 1. Description:
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| JP2000069537A JP4012357B2 (en) | 2000-03-13 | 2000-03-13 | Powder classification method |
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| JP4012357B2 JP4012357B2 (en) | 2007-11-21 |
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|---|---|---|---|---|
| US7572315B2 (en) * | 2003-08-28 | 2009-08-11 | Tekna Plasma Systems Inc. | Process for the synthesis, separation and purification of powder materials |
| US7674300B2 (en) | 2006-12-28 | 2010-03-09 | Kimberly-Clark Worldwide, Inc. | Process for dyeing a textile web |
| US7673516B2 (en) | 2006-12-28 | 2010-03-09 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment system |
| US7703698B2 (en) | 2006-09-08 | 2010-04-27 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment chamber and continuous flow mixing system |
| US7712353B2 (en) | 2006-12-28 | 2010-05-11 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment system |
| US7740666B2 (en) | 2006-12-28 | 2010-06-22 | Kimberly-Clark Worldwide, Inc. | Process for dyeing a textile web |
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| US8057573B2 (en) | 2007-12-28 | 2011-11-15 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for increasing the shelf life of formulations |
| US8143318B2 (en) | 2007-12-28 | 2012-03-27 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for preparing emulsions |
| US8163388B2 (en) | 2008-12-15 | 2012-04-24 | Kimberly-Clark Worldwide, Inc. | Compositions comprising metal-modified silica nanoparticles |
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| US9239036B2 (en) | 2006-09-08 | 2016-01-19 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment and delivery system and process |
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| US9421504B2 (en) | 2007-12-28 | 2016-08-23 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for preparing emulsions |
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|---|---|---|---|---|
| US7572315B2 (en) * | 2003-08-28 | 2009-08-11 | Tekna Plasma Systems Inc. | Process for the synthesis, separation and purification of powder materials |
| US8034286B2 (en) | 2006-09-08 | 2011-10-11 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment system for separating compounds from aqueous effluent |
| US7703698B2 (en) | 2006-09-08 | 2010-04-27 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment chamber and continuous flow mixing system |
| US9283188B2 (en) | 2006-09-08 | 2016-03-15 | Kimberly-Clark Worldwide, Inc. | Delivery systems for delivering functional compounds to substrates and processes of using the same |
| US9239036B2 (en) | 2006-09-08 | 2016-01-19 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment and delivery system and process |
| US8616759B2 (en) | 2006-09-08 | 2013-12-31 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment system |
| US7673516B2 (en) | 2006-12-28 | 2010-03-09 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment system |
| US7712353B2 (en) | 2006-12-28 | 2010-05-11 | Kimberly-Clark Worldwide, Inc. | Ultrasonic liquid treatment system |
| US7740666B2 (en) | 2006-12-28 | 2010-06-22 | Kimberly-Clark Worldwide, Inc. | Process for dyeing a textile web |
| US7674300B2 (en) | 2006-12-28 | 2010-03-09 | Kimberly-Clark Worldwide, Inc. | Process for dyeing a textile web |
| US8182552B2 (en) | 2006-12-28 | 2012-05-22 | Kimberly-Clark Worldwide, Inc. | Process for dyeing a textile web |
| US7785674B2 (en) | 2007-07-12 | 2010-08-31 | Kimberly-Clark Worldwide, Inc. | Delivery systems for delivering functional compounds to substrates and processes of using the same |
| US7947184B2 (en) | 2007-07-12 | 2011-05-24 | Kimberly-Clark Worldwide, Inc. | Treatment chamber for separating compounds from aqueous effluent |
| US7998322B2 (en) | 2007-07-12 | 2011-08-16 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber having electrode properties |
| US8454889B2 (en) | 2007-12-21 | 2013-06-04 | Kimberly-Clark Worldwide, Inc. | Gas treatment system |
| US8858892B2 (en) | 2007-12-21 | 2014-10-14 | Kimberly-Clark Worldwide, Inc. | Liquid treatment system |
| US8632613B2 (en) | 2007-12-27 | 2014-01-21 | Kimberly-Clark Worldwide, Inc. | Process for applying one or more treatment agents to a textile web |
| US8215822B2 (en) | 2007-12-28 | 2012-07-10 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for preparing antimicrobial formulations |
| US8143318B2 (en) | 2007-12-28 | 2012-03-27 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for preparing emulsions |
| US8057573B2 (en) | 2007-12-28 | 2011-11-15 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for increasing the shelf life of formulations |
| US9421504B2 (en) | 2007-12-28 | 2016-08-23 | Kimberly-Clark Worldwide, Inc. | Ultrasonic treatment chamber for preparing emulsions |
| US8163388B2 (en) | 2008-12-15 | 2012-04-24 | Kimberly-Clark Worldwide, Inc. | Compositions comprising metal-modified silica nanoparticles |
| US8685178B2 (en) | 2008-12-15 | 2014-04-01 | Kimberly-Clark Worldwide, Inc. | Methods of preparing metal-modified silica nanoparticles |
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