JP2002131224A - Apparatus and method for measurement of characteristics of sample oil - Google Patents
Apparatus and method for measurement of characteristics of sample oilInfo
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- JP2002131224A JP2002131224A JP2000318732A JP2000318732A JP2002131224A JP 2002131224 A JP2002131224 A JP 2002131224A JP 2000318732 A JP2000318732 A JP 2000318732A JP 2000318732 A JP2000318732 A JP 2000318732A JP 2002131224 A JP2002131224 A JP 2002131224A
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- prism
- sample oil
- sample
- light
- oil
- 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、潤滑油などの試料
油の特性（特に、粘度などに関連した特性）を測定して
評価解析するための試料油特性測定装置および試料油特
性測定方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample oil characteristic measuring device and a sample oil characteristic measuring method for measuring and evaluating and analyzing characteristics (particularly characteristics relating to viscosity, etc.) of a sample oil such as a lubricating oil. Things.
【０００２】[0002]
【従来の技術】潤滑油などの試料油の重要な特性とし
て、粘度や粘度特性（粘度の温度依存性）があるが、こ
れらの値は毛細管粘度計で測定されている。2. Description of the Related Art Important properties of sample oils such as lubricating oils include viscosity and viscosity characteristics (temperature dependence of viscosity), and these values are measured by a capillary viscometer.
【０００３】[0003]
【発明が解決しようとする課題】ところで、この毛細管
粘度計は、測定時の剪断速度が１００/sec程度であり、
実使用条件である約１０6/sec に比べて著しく低く、実
使用状態の特性値を示すものとは限らない。また、実使
用状態では、粘度特性は、被潤滑物体の固体表面と潤滑
油とが接する界面近傍の剪断場における潤滑油構造（油
分子の配列構造および、基油と添加剤との混合状態）に
強く依存するが、これまで前記界面近傍における潤滑油
の構造を動的に解析する方法がなかった。By the way, this capillary viscometer has a shear rate of about 100 / sec during measurement,
It is significantly lower than the actual use condition of about 10 6 / sec, and does not always indicate the characteristic value in the actual use state. In the actual use state, the viscosity characteristics are determined by the lubricating oil structure in the shearing field near the interface between the solid surface of the object to be lubricated and the lubricating oil (the arrangement structure of the oil molecules and the mixed state of the base oil and the additive). Until now, there has been no method for dynamically analyzing the structure of the lubricating oil near the interface.
【０００４】そこで本発明は、高い剪断速度における試
料油の特性を測定することができる試料油特性測定装置
および試料油特性測定方法を提供することを目的とす
る。Accordingly, an object of the present invention is to provide a sample oil characteristic measuring device and a sample oil characteristic measuring method capable of measuring the characteristics of a sample oil at a high shear rate.
【０００５】[0005]
【課題を解決するための手段】このため、本発明が採用
した課題解決手段は、試料油膜が表面に形成されこの表
面に形成された試料油膜を搬送する搬送手段と、搬送手
段の表面に対して間隔を有するとともに前記試料油膜に
接すべく配置されるプリズムと、このプリズムに光線を
入射する発光装置およびプリズムから反射された光線を
受光する受光装置を具備するエリプソメータとを備えた
ことを特徴とする試料油特性測定装置であり、試料油を
溜めた試料油溜に一部が浸漬されるとともに外周面に試
料油膜を形成すべく回転駆動されるローターと、このロ
ーターの外周面に対して間隔を有するとともにこのロー
ターの外周面の試料油膜に接すべく配置されるプリズム
と、このプリズムに光線を入射する発光装置およびプリ
ズムから反射された光線を受光する受光装置を具備する
エリプソメータとを備えたことを特徴とする試料油特性
測定装置であり、試料油が潤滑油であることを特徴とす
る試料油特性測定装置であり、発光装置からプリズムへ
の入射角が変更可能であることを特徴とする試料油特性
測定装置であり、搬送装置の表面に対して間隔を有して
プリズムを配置し、このプリズムと搬送装置の表面との
間の隙間に試料油膜を前記プリズムおよび前記搬送装置
の表面とに接する状態で形成するとともに、前記搬送装
置の表面を移動させることにより前記試料油膜を搬送
し、エリプソメータの発光装置から前記プリズムに光線
を入射するとともに、プリズムから反射された光線をエ
リプソメータの受光装置で受光して、試料油の特性を測
定していることを特徴とする試料油特性測定方法であ
り、試料油を溜めた試料油溜に一部が浸漬されたロータ
ーの外周面に対して間隔を有してプリズムを配置し、ロ
ーターを回転させて、このローターの外周面と前記プリ
ズムとの間の隙間に試料油膜を前記プリズムおよび前記
ローターの外周面とに接する状態で形成し、エリプソメ
ータの発光装置から前記プリズムに光線を入射するとと
もに、プリズムから反射された光線をエリプソメータの
受光装置で受光して、試料油の特性を測定していること
を特徴とする試料油特性測定方法であり、試料油が潤滑
油であることを特徴とする試料油特性測定方法であり、
潤滑油に添加する添加剤の量または種類を異ならしめて
複数の潤滑油の特性を測定していることを特徴とする試
料油特性測定方法であり、発光装置からプリズムへの入
射角を変更して、試料油の特性を測定していることを特
徴とする試料油特性測定方法である。For this reason, the object of the present invention is to provide a conveying means for forming a sample oil film on a surface and conveying the sample oil film formed on the surface; A prism disposed at an interval and in contact with the sample oil film, and an ellipsometer including a light-emitting device for entering light into the prism and a light-receiving device for receiving light reflected from the prism. A rotor that is partially immersed in a sample oil reservoir containing the sample oil and that is rotationally driven to form a sample oil film on the outer peripheral surface; A prism having an interval and arranged to be in contact with the sample oil film on the outer peripheral surface of the rotor, and a light-emitting device and a prism that receive light rays incident on the prism. An ellipsometer having a light-receiving device for receiving light rays, wherein the sample oil characteristic measuring device is characterized in that the sample oil is a lubricating oil. A sample oil characteristic measuring device characterized in that the angle of incidence on the prism can be changed, wherein a prism is arranged at an interval with respect to the surface of the transfer device, and a gap between the prism and the surface of the transfer device A sample oil film is formed in a gap between the prism and the surface of the transfer device in contact with the surface, and the sample oil film is transferred by moving the surface of the transfer device, and a light beam is emitted from the light emitting device of the ellipsometer to the prism. The sample oil is characterized by measuring the characteristics of the sample oil by receiving the light that has entered and reflected from the prism with the light receiving device of the ellipsometer. It is a measuring method, a prism is arranged at an interval with respect to the outer peripheral surface of the rotor partially immersed in the sample oil reservoir storing the sample oil, the rotor is rotated, the outer peripheral surface of the rotor and the A sample oil film is formed in a gap between the prism and the outer peripheral surface of the prism and the rotor, and a light beam enters the prism from a light emitting device of the ellipsometer, and a light beam reflected from the prism is received by the ellipsometer. A sample oil characteristic measurement method characterized in that light is received by the device and the characteristics of the sample oil are measured, and the sample oil characteristic measurement method is characterized in that the sample oil is a lubricating oil.
This is a sample oil characteristic measuring method characterized by measuring the characteristics of a plurality of lubricating oils with different amounts or types of additives added to the lubricating oil, by changing the angle of incidence from the light emitting device to the prism. And measuring the characteristics of the sample oil.
【０００６】[0006]
【実施の形態】次に、本発明における試料油特性測定装
置および試料油特性測定方法の実施の一形態を図１ない
し図７を用いて説明する。図１は本発明の実施の形態の
試料油特性測定装置の概略図である。図２はローターお
よびプリズムの説明図で、（ａ）が斜視図、（ｂ）が
（ａ）の要部平面図である。図３はプリズムおよび試料
油膜の説明図である。図４は入射角と潜り込み深さとの
関係を示すグラフである。図５は液晶および基油のタイ
ムチャートで、（ａ）が液晶のタイムチャート、（ｂ）
が基油のタイムチャートである。図６は各種剪断速度ｗ
におけるＰＡＯ４０のタイムチャートである。図７は添
加剤が添加された場合における基油のタイムチャートで
ある。Next, an embodiment of a sample oil characteristic measuring apparatus and a sample oil characteristic measuring method according to the present invention will be described with reference to FIGS. FIG. 1 is a schematic diagram of a sample oil characteristic measuring device according to an embodiment of the present invention. 2A and 2B are explanatory views of a rotor and a prism. FIG. 2A is a perspective view, and FIG. 2B is a plan view of a main part of FIG. FIG. 3 is an explanatory diagram of the prism and the sample oil film. FIG. 4 is a graph showing the relationship between the angle of incidence and the penetration depth. FIG. 5 is a time chart of the liquid crystal and the base oil, (a) is a time chart of the liquid crystal, and (b).
Is a time chart of the base oil. FIG. 6 shows various shear rates w
5 is a time chart of PAO40 in FIG. FIG. 7 is a time chart of the base oil when the additive is added.
【０００７】偏平な円柱状のローター１の軸には、回転
駆動手段としてのモータ２が連結されており、ローター
１は、その軸を中心としてモータ２で回転駆動される。
ローター１は一部が図示しない試料油溜に浸漬される。
この試料油溜には、潤滑油や液晶などの試料油が溜めら
れており、ローター１が回転すると、ローター１の外周
面に試料油膜３が形成される。このローター１の外周面
に対して間隔ｈを有してプリズム６が配置されている。
この全反射型のプリズム６は三角柱または台形柱であ
り、光線１１が入射される入射面７、光線１１が反射さ
れる反射面８および反射された光線１１が出射される出
射面９を有している。入射面７と反射面８とのなす角度
α１は、出射面９と反射面８とのなす角度α２と略同じ
である。入射光線１１は入射面７に対して略直角に入射
しており、入射光線１１とプリズム６の中心線１２との
なす角度φ（以下、「入射角φ」と呼ぶ）は、角度α１
および角度α２と略同じである。なお、プリズム６の中
心線１２は反射面８に対して直角である。[0007] A motor 2 as a rotary driving means is connected to the shaft of the flat columnar rotor 1, and the rotor 1 is driven to rotate by the motor 2 about the shaft.
The rotor 1 is partially immersed in a sample oil reservoir (not shown).
The sample oil reservoir stores sample oil such as lubricating oil and liquid crystal. When the rotor 1 rotates, a sample oil film 3 is formed on the outer peripheral surface of the rotor 1. The prism 6 is arranged at an interval h with respect to the outer peripheral surface of the rotor 1.
The total reflection type prism 6 is a triangular prism or trapezoidal prism, and has an incident surface 7 on which the light beam 11 is incident, a reflecting surface 8 on which the light beam 11 is reflected, and an exit surface 9 on which the reflected light beam 11 is emitted. ing. The angle α1 between the incident surface 7 and the reflecting surface 8 is substantially the same as the angle α2 between the emitting surface 9 and the reflecting surface 8. The incident light beam 11 is incident on the incident surface 7 at a substantially right angle.
And the angle α2. The center line 12 of the prism 6 is perpendicular to the reflecting surface 8.
【０００８】エリプソメータ２１は市販されており、発
光装置２２および受光装置２３を具備している。発光装
置２２はＨｅ−Ｎｅ（ヘリウム−ネオン）レーザーで構
成され、発光装置２２からレーザー光線１１がプリズム
６に向かって照射される。この光線１１がプリズム６の
入射面７に入射され、反射面８および試料油膜３で反射
されて、この反射光線１１が出射面９から出射される。
そして、反射光線１１が受光装置２３で受光される。と
ころで、試料表面（試料油表面）でのｐ成分（反射面８
に平行に振動する成分）および、ｓ成分（反射面８に垂
直に振動する成分）の各振幅反射率をγｐ，γｓで、ま
た、ｐ成分およびｓ成分の各位相のとびをδｐ，δｓで
表現している。この時、ｔａｎΨ（＝γｐ／γｓ）は試
料表面のｐ成分とｓ成分との振幅反射比を、また、Δ
（＝δｐ−δｓ）はｐ成分とｓ成分との位相差を表して
おり、このΔおよびΨが偏向解析パラメータと呼ばれて
おり、反射光線１１の偏向の状態を示している。エリプ
ソメータ２１には、図示しないマイコンなどの演算装置
が設けられており、この演算装置が発光装置２２および
受光装置２３からのデータに基づいて、前述の偏向解析
パラメータΔおよびΨを算出して出力する。The ellipsometer 21 is commercially available and includes a light emitting device 22 and a light receiving device 23. The light emitting device 22 is composed of a He-Ne (helium-neon) laser, and the laser beam 11 is emitted from the light emitting device 22 toward the prism 6. The light beam 11 enters the incident surface 7 of the prism 6, is reflected by the reflection surface 8 and the sample oil film 3, and is emitted from the emission surface 9.
Then, the reflected light beam 11 is received by the light receiving device 23. By the way, the p component (reflection surface 8) on the sample surface (sample oil surface)
And s component (a component that vibrates perpendicularly to the reflection surface 8) and s component (a component that vibrates perpendicularly to the reflecting surface 8) are represented by .gamma.p and .gamma.s. expressing. At this time, tan Ψ (= γp / γs) represents the amplitude reflection ratio between the p component and the s component on the sample surface, and Δ
(= Δp−δs) represents the phase difference between the p component and the s component, and Δ and Ψ are called deflection analysis parameters, and indicate the state of deflection of the reflected light beam 11. The ellipsometer 21 is provided with an arithmetic unit such as a microcomputer (not shown). The arithmetic unit calculates and outputs the above-described deflection analysis parameters Δ and Ψ based on data from the light emitting device 22 and the light receiving device 23. .
【０００９】この様に構成されている試料油特性測定装
置で、潤滑油や液晶などの試料油の特性を測定する。測
定した試料油の代表例の名称および物性値を〔表１〕に
示す。測定した液晶は、４−ペンチル−４′−シアノビ
フェニル（略称５ＣＢ）であり、また、測定した基油
は、ポリαオレフィンの２種（ＰＡＯ１０，ＰＡＯ４
０）、およびポリブテンの２種（ＰＢ１０，ＰＢ３０）
である。The characteristics of the sample oil such as lubricating oil and liquid crystal are measured by the sample oil characteristic measuring device having the above-mentioned configuration. Table 1 shows the names and physical properties of representative examples of the measured sample oils. The measured liquid crystal was 4-pentyl-4'-cyanobiphenyl (abbreviated as 5CB), and the measured base oil was two kinds of poly-α-olefins (PAO10, PAO4).
0) and polybutene (PB10, PB30)
It is.
【００１０】[0010]
【表１】 [Table 1]
【００１１】試料油の特性を測定する際には、試料油溜
に測定する潤滑油や液晶などの試料油を溜める。ロータ
ー１の外周面とプリズム６との隙間ｈが、計測する試料
油膜３の厚みｈ（以下、「油膜厚さｈ」と呼ぶ）となる
ので、ローター１とプリズム６との間隔を、たとえば、
約１０〜５００μｍに調整する。そして、モータ２を稼
働してローター１を回転させる。その際のローター１の
外周面の速度ｖは、たとえば、約０．０６〜１２．２ｍ
／ｓである。このローター１の回転により、ローター１
の外周面には、潤滑油膜や液晶膜などの試料油膜３が形
成される。この試料油膜３は、ローター１の外周面およ
びプリズム６の反射面８に接触し、その剪断速度ｗ（＝
ｖ／ｈ）は約１．２×１０2 〜１．２×１０6 ／ｓであ
る。試験温度は適宜選択可能であるが、２３±３℃で行
った。また、エリプソメータ２１の発光装置２２から光
線１１をプリズム６に照射し、その反射光線１１を受光
装置２３で受光する。そして、エリプソメータ２１は、
偏向解析パラメータΔおよびΨのデータを出力する。When measuring the properties of the sample oil, the sample oil such as lubricating oil or liquid crystal to be measured is stored in the sample oil reservoir. Since the gap h between the outer peripheral surface of the rotor 1 and the prism 6 is the thickness h of the sample oil film 3 to be measured (hereinafter, referred to as “oil film thickness h”), the distance between the rotor 1 and the prism 6 is, for example,
Adjust to about 10-500 μm. Then, the motor 2 is operated to rotate the rotor 1. At that time, the speed v of the outer peripheral surface of the rotor 1 is, for example, about 0.06 to 12.2 m.
/ S. By the rotation of the rotor 1, the rotor 1
A sample oil film 3 such as a lubricating oil film or a liquid crystal film is formed on the outer peripheral surface of the sample oil film. The sample oil film 3 comes into contact with the outer peripheral surface of the rotor 1 and the reflecting surface 8 of the prism 6, and the shear rate w (=
v / h) is about 1.2 × 10 2 to 1.2 × 10 6 / s. The test temperature can be appropriately selected, but the test was performed at 23 ± 3 ° C. The light beam 11 is emitted from the light emitting device 22 of the ellipsometer 21 to the prism 6, and the reflected light beam 11 is received by the light receiving device 23. And the ellipsometer 21
The data of the deflection analysis parameters Δ and Ψ are output.
【００１２】光線１１の潜り込み深さｄは数十〜数百ｎ
ｍであるが、図４に図示するように、試料油の屈折率ｎ
や入射角φに依存する。屈折率ｎが小さい程、潜り込み
深さｄは小さくなる。また、入射角φが大きい程、潜り
込み深さｄが小さくなる。なお、入射角φを変更する際
には、それに対応したプリズム６（すなわち、前記角度
α１および角度α２が略入射角φであるプリズム６）に
交換するとともに、発光装置２２や受光装置２３の配置
位置を変更する。この様にして潜り込み深さｄを変更す
ることにより、分析する深さを変更することができる。
また、エリプソメータ２１から偏向解析パラメータΔお
よびΨが得られるが、偏向解析パラメータΔを用いて試
料油の剪断の状態の動的挙動を解析した。The penetration depth d of the light beam 11 is several tens to several hundreds n.
m, the refractive index n of the sample oil as shown in FIG.
And the incident angle φ. The smaller the refractive index n is, the smaller the immersion depth d is. Also, the greater the incident angle φ, the smaller the dive depth d. When the incident angle φ is changed, the prism 6 corresponding to the incident angle φ (that is, the prism 6 in which the angles α1 and α2 are substantially equal to the incident angle φ) is exchanged, and the arrangement of the light emitting device 22 and the light receiving device 23 is changed. Change position. The depth to be analyzed can be changed by changing the immersion depth d in this manner.
In addition, the deflection analysis parameters Δ and 得 are obtained from the ellipsometer 21, and the dynamic behavior of the sample oil in the shearing state is analyzed using the deflection analysis parameter Δ.
【００１３】図５（ａ）に、ローター１の外周面の速度
ｖが０．８〜０．９ｍ／ｓで、油膜厚さｈが１０μｍの
状態における液晶（５ＣＢ）の偏向解析パラメータΔの
経時的変化が示されている。液晶における偏向解析パラ
メータΔは、剪断に対して矩形的な応答を示した。この
偏向解析パラメータΔの低下は、液晶分子が剪断方向に
配列したことを示している。FIG. 5 (a) shows the time course of the deflection analysis parameter Δ of the liquid crystal (5CB) when the speed v of the outer peripheral surface of the rotor 1 is 0.8 to 0.9 m / s and the oil film thickness h is 10 μm. The target change is shown. The deflection analysis parameter Δ in the liquid crystal showed a rectangular response to shear. This decrease in the deflection analysis parameter Δ indicates that the liquid crystal molecules are arranged in the shear direction.
【００１４】また、図５（ｂ）に、潤滑油の基油である
ＰＢ３０およびＰＡＯ４０の偏向解析パラメータΔの経
時的変化が示されている。この場合には、ローター１の
外周面の速度ｖが０．８〜０．９ｍ／ｓで、油膜厚さｈ
が１００μｍの状態で行われた。この図５（ｂ）におけ
る偏向解析パラメータΔの変化は、基油の分子が剪断方
向に配列したためと思われる。しかし、液晶の場合と異
なり、偏向解析パラメータΔに緩和現象が見られる。こ
の緩和現象は、剪断による温度上昇または圧力上昇の影
響、特に温度上昇の影響を受けたためと考えられる。FIG. 5B shows the change over time in the deflection analysis parameter Δ of the PB 30 and the PAO 40 which are the base oils of the lubricating oil. In this case, the speed v of the outer peripheral surface of the rotor 1 is 0.8 to 0.9 m / s, and the oil film thickness h
Was performed in a state of 100 μm. The change in the deflection analysis parameter Δ in FIG. 5B is considered to be due to the base oil molecules being arranged in the shear direction. However, unlike the case of the liquid crystal, a relaxation phenomenon is observed in the deflection analysis parameter Δ. This relaxation phenomenon is considered to be due to the influence of the temperature rise or the pressure rise due to the shearing, particularly the influence of the temperature rise.
【００１５】次に、剪断速度ｗの依存性を検討した。図
６には、油膜厚さｈが１００μｍである基油ＰＡＯ４０
のタイムチャートが示されており、この図６において、
剪断中において定常状態に達したΔｅから剪断前のΔｏ
を減じた定常変化量で比較すると、剪断速度ｗが増大す
るに伴って定常変化量が増加する。このことから偏向解
析パラメータΔによって示される固液界面付近の構造変
化は剪断速度ｗが上昇することによって大きくなると考
えられる。また、グラフは添付していないが、分子構造
が類似し動粘度の異なるＰＡＯ１０とＰＡＯ４０との比
較、および、ＰＢ１０とＰＢ３０との比較では、動粘度
の高いＰＡＯ４０およびＰＢ３０が、動粘度の低いＰＡ
Ｏ１０およびＰＢ１０よりも定常変化量が大きいことが
分かった。この様に、粘度が偏向解析パラメータΔの変
化に関係しており、偏向解析パラメータΔの変化を検討
することにより、剪断場における粘度を考察することが
できる。また、偏向解析パラメータΔのピーク値Δｍａ
ｘ（図６参照）と、剪断中において定常状態に達したΔ
ｅとの差は、試料油の種類により異なっており、試料油
の分子構造に依存すると考えられる。そして、この差が
大きいものは、粘度の温度依存性が高く、温度による粘
度の変化が大きくなる。Next, the dependence of the shear rate w was examined. FIG. 6 shows a base oil PAO40 having an oil film thickness h of 100 μm.
FIG. 6 shows a time chart of FIG.
From Δe which reached steady state during shearing to Δo before shearing
When the shear rate w is increased, the steady change amount increases as the shear rate w increases. From this, it is considered that the structural change near the solid-liquid interface indicated by the deflection analysis parameter Δ increases as the shear rate w increases. In addition, although a graph is not attached, in the comparison between PAO10 and PAO40 having similar molecular structures and different kinematic viscosities, and in the comparison between PB10 and PB30, PAO40 and PB30 having high kinematic viscosities are compared with PAO having low kinematic viscosities.
It was found that the steady change amount was larger than O10 and PB10. As described above, the viscosity is related to the change in the deflection analysis parameter Δ, and the viscosity in the shear field can be considered by examining the change in the deflection analysis parameter Δ. Also, the peak value Δma of the deflection analysis parameter Δ
x (see FIG. 6) and Δ reached steady state during shearing
The difference from e differs depending on the type of the sample oil, and is considered to depend on the molecular structure of the sample oil. Those having a large difference have a high temperature dependency of the viscosity, and the change in the viscosity depending on the temperature is large.
【００１６】さらに、潤滑油の基油（ＰＡＯ４０）に添
加剤（たとえば、オートマトランスミッションで使用さ
れるＰＢＳＩ）を添加した場合を検討した。試料油とし
て、基油だけの場合と、基油に添加剤を１０ｗｔ％加え
た場合と、基油に添加剤を３０ｗｔ％加えた場合との３
個の場合において、上記試料油特性測定装置で試験を行
った。試験結果は、図７に図示するように、添加剤の量
が多い程、偏向解析パラメータΔの立ち上がりが大きく
なる。この現象は、添加剤がプリズム６の表面に吸着
し、潤滑特性を発揮しているためと考えられる。Further, the case where an additive (for example, PBSI used in an automatic transmission) was added to a lubricating base oil (PAO40) was examined. Three types of sample oils were used: the base oil alone, the base oil with 10 wt% additive, and the base oil with 30 wt% additive.
In the case of individual pieces, a test was performed with the sample oil property measuring device. As shown in FIG. 7, the test results show that the larger the amount of the additive, the larger the rise of the deflection analysis parameter Δ. This phenomenon is considered to be because the additive is adsorbed on the surface of the prism 6 and exhibits lubricating properties.
【００１７】この様に、実施の形態の試料油特性測定装
置を用いて、種々の試料油に対して各種条件で試験を行
い、エリプソメータ２１から偏向解析パラメータΔおよ
びΨを得て、試料油の特性を検証することができる。そ
して、ローター１の回転速度を大きくすることにより、
試料油に加わる剪断速度ｗを簡単に大きくすることがで
きる。また、入射角φを変更することにより、潜り込み
深さｄを変更して、固液界面付近の構造変化をより細か
く検証することができる。As described above, various sample oils are tested under various conditions using the sample oil characteristic measuring apparatus according to the embodiment, and deflection analysis parameters Δ and Ψ are obtained from the ellipsometer 21 to obtain sample oil characteristics. Characteristics can be verified. Then, by increasing the rotation speed of the rotor 1,
The shear rate w applied to the sample oil can be easily increased. In addition, by changing the incident angle φ, the immersion depth d can be changed, and the structural change near the solid-liquid interface can be more finely verified.
【００１８】前述の実施の形態では、偏向解析パラメー
タΔを用いて、試料油の特性を検証しているが、偏向解
析パラメータΨを用いて検証することも可能である。ま
た、試料油膜を搬送することができるならば、ローター
１に代えて種々の搬送装置を採用することができ、たと
えば、ベルトコンベア式にすることも可能である。さら
に、エリプソメータ２１は偏向解析パラメータΔおよび
Ψを出力しているが、偏向解析パラメータΔまたはΨの
少なくとも何れか一方を出力することができれば良い。
そして、試料油の温度を検出する試料油温度検出装置を
設けることも可能である。また、試料油を加熱または冷
却して温度調整する試料油温度調整装置を設けることも
可能であり、たとえば、この試料油温度調整装置を試料
油溜に設置することができる。以上、本発明の実施の形
態について説明したが、本発明の趣旨の範囲内で種々の
形態を実施することが可能である。In the above-described embodiment, the characteristics of the sample oil are verified using the deflection analysis parameter Δ, but it is also possible to verify using the deflection analysis parameter Ψ. Further, if the sample oil film can be transported, various transporting devices can be adopted instead of the rotor 1, and for example, a belt conveyor type can be used. Further, the ellipsometer 21 outputs the deflection analysis parameters Δ and Ψ, but it is sufficient that the ellipsometer 21 can output at least one of the deflection analysis parameters Δ and Ψ.
And it is also possible to provide a sample oil temperature detecting device for detecting the temperature of the sample oil. It is also possible to provide a sample oil temperature adjusting device for adjusting the temperature by heating or cooling the sample oil. For example, the sample oil temperature adjusting device can be installed in the sample oil reservoir. Although the embodiments of the present invention have been described above, various embodiments can be implemented within the scope of the present invention.
【００１９】[0019]
【発明の効果】以上述べた如く、本発明によれば、ロー
ターなどの搬送装置とプリズムとの間に試料油膜が形成
され、この試料油膜の特性をエリプソメータで測定する
ので、試料油の搬送速度を増大することにより、試料油
膜に高い剪断速度を与えることができるとともに、試料
油の動的挙動を解析することができる。また、エリプソ
メータの発光装置からプリズムへの光線の入射角を変更
することにより、試料油膜を分析する分析深さを変更す
ることができ、固液界面付近の試料油膜の構造変化をよ
り細かく検証することができる。As described above, according to the present invention, a sample oil film is formed between a transfer device such as a rotor and a prism, and the characteristics of the sample oil film are measured by an ellipsometer. By increasing the value, it is possible to give a high shear rate to the sample oil film and to analyze the dynamic behavior of the sample oil. In addition, by changing the incident angle of the light beam from the light emitting device of the ellipsometer to the prism, the analysis depth for analyzing the sample oil film can be changed, and the structural change of the sample oil film near the solid-liquid interface can be more finely verified. be able to.
【図１】本発明の実施の形態の試料油特性測定装置の概
略図である。FIG. 1 is a schematic diagram of a sample oil characteristic measuring device according to an embodiment of the present invention.
【図２】ローターおよびプリズムの説明図で、（ａ）が
斜視図、（ｂ）が（ａ）の要部平面図である。2A and 2B are explanatory views of a rotor and a prism, wherein FIG. 2A is a perspective view and FIG. 2B is a plan view of a main part of FIG.
【図３】プリズムおよび試料油膜の説明図である。FIG. 3 is an explanatory diagram of a prism and a sample oil film.
【図４】入射角と潜り込み深さとの関係を示すグラフで
ある。FIG. 4 is a graph showing a relationship between an incident angle and a penetration depth.
【図５】液晶および基油のタイムチャートで、（ａ）が
液晶のタイムチャート、（ｂ）が基油のタイムチャート
である。5A and 5B are time charts of the liquid crystal and the base oil, wherein FIG. 5A is a time chart of the liquid crystal and FIG. 5B is a time chart of the base oil.
【図６】各種剪断速度ｗにおけるＰＡＯ４０のタイムチ
ャートである。FIG. 6 is a time chart of PAO40 at various shear rates w.
【図７】添加剤が添加された場合における基油のタイム
チャートである。FIG. 7 is a time chart of a base oil when an additive is added.
φ 入射角 ｈ プリズムとローターとの間の隙間 １ ローター（搬送装置） ３ 試料油膜 ６ プリズム １１ 光線 ２１ エリプソメータ ２２ 発光装置 ２３ 受光装置 φ Incident angle h Gap between prism and rotor 1 Rotor (transport device) 3 Sample oil film 6 Prism 11 Light beam 21 Ellipsometer 22 Light emitting device 23 Light receiving device
─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成１２年１０月２４日（２０００．１０．
２４）[Submission date] October 24, 2000 (2000.10.
24)
【手続補正１】[Procedure amendment 1]
【補正対象書類名】図面[Document name to be amended] Drawing
【補正対象項目名】図１[Correction target item name] Fig. 1
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【図１】 FIG.
【手続補正２】[Procedure amendment 2]
【補正対象書類名】図面[Document name to be amended] Drawing
【補正対象項目名】図２[Correction target item name] Figure 2
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【図２】 FIG. 2
【手続補正３】[Procedure amendment 3]
【補正対象書類名】図面[Document name to be amended] Drawing
【補正対象項目名】図３[Correction target item name] Figure 3
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【図３】 FIG. 3
Claims (9)
成された試料油膜を搬送する搬送手段と、 前記搬送手段の表面に対して間隔を有するとともに前記
試料油膜に接すべく配置されるプリズムと、 このプリズムに光線を入射する発光装置およびプリズム
から反射された光線を受光する受光装置を具備するエリ
プソメータとを備えたことを特徴とする試料油特性測定
装置。1. A sample oil film is formed on a surface, a transport means for transporting a sample oil film formed on the surface, and a distance from the surface of the transport means and arranged to be in contact with the sample oil film. A sample oil property measuring device, comprising: a prism; and an ellipsometer including a light emitting device for entering a light beam into the prism and a light receiving device for receiving a light beam reflected from the prism.
るとともに、外周面に試料油膜を形成すべく回転駆動さ
れるローターと、 このローターの外周面に対して間隔を有するとともに、
このローターの外周面の試料油膜に接すべく配置される
プリズムと、 このプリズムに光線を入射する発光装置およびプリズム
から反射された光線を受光する受光装置を具備するエリ
プソメータとを備えたことを特徴とする試料油特性測定
装置。2. A rotor which is partially immersed in a sample oil reservoir storing sample oil, and is rotatably driven to form a sample oil film on an outer peripheral surface, and has a space with respect to the outer peripheral surface of the rotor. ,
A prism arranged to be in contact with the sample oil film on the outer peripheral surface of the rotor; and an ellipsometer including a light emitting device for entering a light beam into the prism and a light receiving device for receiving a light beam reflected from the prism. Sample oil characteristic measuring device.
る請求項１または２に記載の試料油特性測定装置。3. An apparatus according to claim 1, wherein said sample oil is a lubricating oil.
更可能であることを特徴とする請求項１，２または３に
記載の試料油特性測定装置。4. The sample oil characteristic measuring device according to claim 1, wherein an incident angle from the light emitting device to the prism can be changed.
ズムを配置し、 このプリズムと搬送装置の表面との間の隙間に試料油膜
を前記プリズムおよび前記搬送装置の表面とに接する状
態で形成するとともに、前記搬送装置の表面を移動させ
ることにより前記試料油膜を搬送し、 エリプソメータの発光装置から前記プリズムに光線を入
射するとともに、プリズムから反射された光線をエリプ
ソメータの受光装置で受光して、試料油の特性を測定し
ていることを特徴とする試料油特性測定方法。5. A state in which a prism is arranged at an interval with respect to the surface of the transfer device, and a sample oil film is in contact with the prism and the surface of the transfer device in a gap between the prism and the surface of the transfer device. In addition, the sample oil film is transported by moving the surface of the transport device, and light is incident on the prism from the light emitting device of the ellipsometer, and the light reflected from the prism is received by the light receiving device of the ellipsometer. And measuring the characteristics of the sample oil.
たローターの外周面に対して間隔を有してプリズムを配
置し、 前記ローターを回転させて、このローターの外周面と前
記プリズムとの間の隙間に試料油膜を前記プリズムおよ
び前記ローターの外周面とに接する状態で形成し、 エリプソメータの発光装置から前記プリズムに光線を入
射するとともに、プリズムから反射された光線をエリプ
ソメータの受光装置で受光して、試料油の特性を測定し
ていることを特徴とする試料油特性測定方法。6. A prism is disposed at an interval from an outer peripheral surface of a rotor partially immersed in a sample oil reservoir in which a sample oil is stored, and the rotor is rotated to rotate the outer peripheral surface of the rotor. A sample oil film is formed in a gap between the prism and the outer peripheral surface of the prism and the rotor, and light is incident on the prism from a light emitting device of the ellipsometer, and the light reflected from the prism is reflected by the ellipsometer. A method for measuring characteristics of a sample oil, wherein the characteristics of the sample oil are measured by receiving light with a light receiving device.
る請求項５または６に記載の試料油特性測定方法。7. The method according to claim 5, wherein the sample oil is a lubricating oil.
類を異ならしめて複数の潤滑油の特性を測定しているこ
とを特徴とする請求項７に記載の試料油特性測定方法。8. The method according to claim 7, wherein the characteristics of the plurality of lubricating oils are measured by changing the amount or type of the additive to be added to the lubricating oil.
更して、試料油の特性を測定していることを特徴とする
請求項５，６，７または８に記載の試料油特性測定方
法。9. The method according to claim 5, wherein the characteristic of the sample oil is measured by changing an incident angle from the light emitting device to the prism. .
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| JP2000318732A JP3668120B2 (en) | 2000-10-19 | 2000-10-19 | Sample oil characteristic measuring apparatus and sample oil characteristic measuring method |
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2000
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011033622A (en) * | 2009-07-24 | 2011-02-17 | Chevron Oronite Sa | System and method for inspecting liquid composition |
| WO2015031567A1 (en) * | 2013-08-29 | 2015-03-05 | Corning Incorporated | Prism-coupling systems and methods for characterizing curved parts |
| US10156488B2 (en) | 2013-08-29 | 2018-12-18 | Corning Incorporated | Prism-coupling systems and methods for characterizing curved parts |
| US10495530B2 (en) | 2013-08-29 | 2019-12-03 | Corning Incorporated | Prism-coupling systems and methods for characterizing curved parts |
| US9983064B2 (en) | 2013-10-30 | 2018-05-29 | Corning Incorporated | Apparatus and methods for measuring mode spectra for ion-exchanged glasses having steep index region |
| US11079280B2 (en) | 2013-10-30 | 2021-08-03 | Corning Incorporated | Apparatus and methods for measuring mode spectra for ion-exchanged glasses having steep index region |
| US9696207B2 (en) | 2014-04-23 | 2017-07-04 | Corning Incorporated | Method of enhancing contrast in prism coupling measurements of stress |
| US11384011B2 (en) | 2014-07-17 | 2022-07-12 | Corning Incorporated | Glass sheet and system and method for making glass sheet |
| US9534981B2 (en) | 2014-12-23 | 2017-01-03 | Corning Incorporated | Prism-coupling systems and methods for characterizing ion-exchanged waveguides with large depth-of-layer |
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| LAPS | Cancellation because of no payment of annual fees |