JPH01189544A - Extremely small hardness meter - Google Patents
Extremely small hardness meterInfo
- Publication number
- JPH01189544A JPH01189544A JP1415088A JP1415088A JPH01189544A JP H01189544 A JPH01189544 A JP H01189544A JP 1415088 A JP1415088 A JP 1415088A JP 1415088 A JP1415088 A JP 1415088A JP H01189544 A JPH01189544 A JP H01189544A
- Authority
- JP
- Japan
- Prior art keywords
- measured
- substance
- hardness
- presser
- indenter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 15
- 238000007373 indentation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 2
- WHBHBVVOGNECLV-OBQKJFGGSA-N 11-deoxycortisol Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 WHBHBVVOGNECLV-OBQKJFGGSA-N 0.000 abstract 4
- 239000000126 substance Substances 0.000 abstract 2
- 239000010409 thin film Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000005489 elastic deformation Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、例えば半導体プロセス等で製作される薄膜や
、超電導体薄膜、あるいは光学要素等のコーテイング膜
の極微小領域の硬度を評価するための極微小硬度計に関
する。[Detailed Description of the Invention] <Industrial Application Field> The present invention is applicable to evaluating the hardness of extremely small regions of thin films produced in semiconductor processes, superconductor thin films, or coating films for optical elements, etc. Regarding ultra-micro hardness tester.
〈従来の技術〉
半導体プロセス等で製造される薄膜等の硬度を評価する
には、従来、例えば第５図にその構造を示すような微小
硬度計が使用されている。この装置によれば、サンプル
Ｓの表面に負荷機構５１によって圧子５２を所定の力で
押圧し、この押圧によって生じるサンプルＳの変形量を
差動トランス５３によって測定し、変形量と押圧力とか
らサンプルＳの微小領域の硬度を評価する。<Prior Art> In order to evaluate the hardness of thin films manufactured by semiconductor processes, etc., a microhardness tester, the structure of which is shown in FIG. 5, has conventionally been used. According to this device, an indenter 52 is pressed with a predetermined force on the surface of a sample S by a loading mechanism 51, the amount of deformation of the sample S caused by this pressing is measured by a differential transformer 53, and the amount of deformation and the pressing force are calculated. The hardness of the micro region of sample S is evaluated.
〈発明が解決しようとする問題点〉
上述のような微小硬度計によれば、差動トランス５３等
の変位計を用いているので、少くとも１００人程皮取上
の変形量を与えないと測定ができない。<Problems to be solved by the invention> According to the microhardness meter described above, since a displacement meter such as a differential transformer 53 is used, it is necessary to apply the deformation amount for skin removal by at least 100 people. Unable to measure.
半導体プロセス等において作られる薄膜は、その厚さが
数百人程度の薄い膜が多く、このような薄膜の硬度に係
る物理定数を測定するために、１００Å以上の変形を生
じさせることはその膜の弾性限界を越える応力を加える
ことになり、膜に対して大きなダメージを与えてしまい
、その測定値を基に正確な評価をすることは困難である
。Thin films made in semiconductor processes, etc. are often thin films with a thickness of several hundred layers, and in order to measure the physical constants related to the hardness of such thin films, deformation of 100 Å or more is difficult to detect. This applies a stress that exceeds the elastic limit of the membrane, causing significant damage to the membrane, and it is difficult to make accurate evaluations based on the measured values.
本発明の目的は、薄膜等のサンプルにその弾性限界以内
の極微小な応力を加えるだけで、その硬度に係る情報を
得ることができ、もってサンプルにダメージを与えるこ
となく再現性のよい正確な硬度評価をすることのできる
、極微小硬度計を提供することにある。The purpose of the present invention is to obtain information on the hardness of a sample such as a thin film by simply applying a microscopic stress within its elastic limit, thereby providing accurate and reproducible information without damaging the sample. An object of the present invention is to provide a microhardness meter that can evaluate hardness.
〈問題点を解決するための手段〉
上記の目的を達成するため、本発明の極微小硬度計は、
実施例に対応する第１図に示すように、圧子１と、その
圧子１を被測定物Ｓ表面に所定の力で押圧する負荷機構
２と、圧子１による押圧部近傍にレーザ光を照射するた
めのレーザ３と、そのレーザ光の反射散乱光のラマンス
ペクトルを検出する検出手段（例えば集光レンズ４、分
光器５、光電子増倍管６）を備え、検出されたラマンス
ペクトルの圧子１押圧による変化量と圧子１の押圧力か
ら被測定物Ｓの微小領域の硬度に係る情報を得るよう構
成したことによって、特徴づけられる。<Means for solving the problems> In order to achieve the above object, the microhardness tester of the present invention has the following features:
As shown in FIG. 1 corresponding to the embodiment, an indenter 1, a load mechanism 2 that presses the indenter 1 against the surface of the object to be measured S with a predetermined force, and a laser beam irradiated near the pressed part by the indenter 1. It is equipped with a laser 3 and a detection means (for example, a condensing lens 4, a spectrometer 5, a photomultiplier tube 6) for detecting the Raman spectrum of the reflected and scattered light of the laser beam, and a detection means for detecting the Raman spectrum of the detected Raman spectrum by pressing the indenter 1. It is characterized by being configured to obtain information regarding the hardness of a minute region of the object to be measured S from the amount of change due to the amount of change and the pressing force of the indenter 1.
〈作用〉
第２図に示すように、被測定物Ｓの表面に圧子１の先端
が押圧されると、被測定物Ｓはその近傍において変形す
る。この変形の仕方は、例えば押圧力を被測定物Ｓの弾
性限界内で一定にした場合、被測定物Ｓの硬度に応じて
異なる。被測定物Ｓの変形の仕方が異なることは、その
内部応力の分布も異なるということになる。<Operation> As shown in FIG. 2, when the tip of the indenter 1 is pressed against the surface of the object to be measured S, the object to be measured S is deformed in the vicinity thereof. The manner of this deformation differs depending on the hardness of the object to be measured S, for example, when the pressing force is kept constant within the elastic limit of the object to be measured. The fact that the object to be measured S is deformed differently means that its internal stress distribution is also different.
一方、被測定物Ｓの表面にレーザ光を照射して全反射さ
せると、被測定物Ｓの内部へわずかなレーザ光の浸み出
しが生じる。従って、この反射光の中には、被測定物Ｓ
の結晶状態の情報となり得るラマン散乱光が含まれる。On the other hand, when the surface of the object to be measured S is irradiated with laser light and is totally reflected, a small amount of laser light seeps into the inside of the object to be measured S. Therefore, this reflected light includes the object to be measured S.
This includes Raman scattered light that can provide information about the crystal state of
ラマン散乱光のスペクトルは、被測定物Ｓに存在する内
部応力に相関し、従って、圧子１を所定の力で押圧する
前後のラマンスペクトルの変化量を検出すれば、被測定
物Ｓの硬度に係る情報が得られる。The spectrum of Raman scattered light correlates with the internal stress existing in the object S to be measured. Therefore, by detecting the amount of change in the Raman spectrum before and after pressing the indenter 1 with a predetermined force, the hardness of the object S to be measured can be determined. Such information can be obtained.
〈実施例〉 本発明の実施例を、以下、図面に基づいて説明する。<Example> Embodiments of the present invention will be described below based on the drawings.
第１図は本発明実施例の構成図である。FIG. 1 is a block diagram of an embodiment of the present invention.
先端が所定の微小曲率を有する球面形に形成された圧子
１は、例えば電磁力発生装置等をアクチュエータとする
負荷機構２に装着され、評価対称となる酸化膜等の被測
定物Ｓの表面に対して垂直に押圧される。An indenter 1 whose tip is formed into a spherical shape with a predetermined minute curvature is attached to a load mechanism 2 whose actuator is an electromagnetic force generator, for example, and is applied to the surface of an object to be measured S such as an oxide film to be evaluated. It is pressed perpendicularly to the object.
被測定物Ｓの表面の圧子１押圧部近傍には、レーザ３か
らのレーザビームがスポット状に集光される。このレー
ザ３としては、比較的パワーが強く、集光の容易なＡ
ｒ＋レーザ等が適している。A laser beam from the laser 3 is focused into a spot near the pressing portion of the indenter 1 on the surface of the object S to be measured. The laser 3 is A, which has relatively strong power and is easy to focus.
r+ laser etc. are suitable.
レーザ光の被測定物Ｓによる反射散乱光は集光レンズ４
を介して分光器５に導かれ、光電子増倍管６によってそ
の各波長域での強度が検出される。The reflected and scattered light of the laser beam by the object to be measured S is collected by the condenser lens 4.
The light is guided to a spectrometer 5 via a photomultiplier tube 6, and the intensity in each wavelength range is detected by a photomultiplier tube 6.
その検出信号は、増幅器やＡ−Ｄ変換器を主体とするイ
ンターフェース７を介してコンピュータ已に採り込まれ
るよう構成されている。The detection signal is configured to be input into the computer via an interface 7 mainly consisting of an amplifier and an AD converter.
コンピュータ８は、採り込んだスペクトルデータのうち
、後述するラマンスペクトルのみを記憶し、圧子１の押
圧前後のラマンスペクトルの変化量を求める。コンピュ
ータ８はまた、上述した負荷機構２に対し、定められた
押圧力で圧子１が被測定物Ｓに押し付けられるよう、イ
ンターフェース９を介して圧力制御指令を供給するよう
構成されている。Of the acquired spectrum data, the computer 8 stores only the Raman spectrum, which will be described later, and calculates the amount of change in the Raman spectrum before and after the indenter 1 is pressed. The computer 8 is also configured to supply a pressure control command to the load mechanism 2 described above via the interface 9 so that the indenter 1 is pressed against the object S with a predetermined pressing force.
次に作用を述べる。Next, we will discuss the effect.
第２図は圧子１を押し付けたときの被測定物Ｓの弾性変
形の様子を模式的に示す図である。圧子１を被測定物Ｓ
にその弾性限界内の力で押し付けると、その近傍で被測
定物Ｓは弾性変形するが、その変形の仕方は、圧子１の
先端形状および押圧力が一定であれば被測定物Ｓの硬度
によって異なり、従ってその内部における応力の分布も
硬度に応じたものとなる。FIG. 2 is a diagram schematically showing how the object to be measured S undergoes elastic deformation when the indenter 1 is pressed against it. Place the indenter 1 on the object to be measured S
When pressed with a force within its elastic limit, the object to be measured S is elastically deformed in the vicinity, but the manner of deformation depends on the hardness of the object S as long as the shape of the tip of the indenter 1 and the pressing force are constant. Therefore, the stress distribution inside it also depends on the hardness.
レーザ光を被測定物Ｓの表面で全反射するよう照射する
と、レーザ光は被測定物Ｓの内部のわずかな領域にまで
浸み出し、従って、その反射光内にはラマン散乱光が含
まれる。例えば半導体分野において評価対称となる酸化
膜や窒化膜等は、結晶性のよいものが多く、第３図に例
示するように特徴的なラマンスペクトルを示すことが知
られている。このラマンスペクトルは、結晶に応力を作
用させたとき、その応力により歪みが結晶方位に沿った
方向に発生する場合、第３図に示すように、ピーク波長
のシフトとなって現れる。歪が等方的に発生する場合に
は、スペクトルピークの半値幅の広がりになって現れる
。このようなうマンスペクトルの変化量は、第４図に示
すように結晶に作用している応力とよい相関関係を示す
。When the laser beam is irradiated so as to be totally reflected on the surface of the object to be measured S, the laser beam penetrates into a small area inside the object to be measured S, and therefore, the reflected light includes Raman scattered light. . For example, it is known that many of the oxide films, nitride films, etc. that are evaluated in the semiconductor field have good crystallinity and exhibit characteristic Raman spectra as illustrated in FIG. In this Raman spectrum, when stress is applied to the crystal and the stress causes strain in the direction along the crystal orientation, the peak wavelength appears as a shift as shown in FIG. 3. When distortion occurs isotropically, it appears as a broadening of the half-width of the spectral peak. The amount of change in the Uman spectrum shows a good correlation with the stress acting on the crystal, as shown in FIG.
以上のことから、圧子１の押圧中心に対してその近傍に
一定の位置関係で、かつ、一定のスポットでレーザ光を
照射し、その反射光の圧子１の押圧前後におけるラマン
スペクトルの変化量を求めれば、その量は被測定物Ｓの
硬度に相関する量となる。すなわち、圧子１による押圧
部近傍の微小領域、微小深さの被測定物硬度が得られる
。From the above, we irradiate laser light at a fixed spot in a fixed positional relationship and in the vicinity of the pressing center of the indenter 1, and calculate the amount of change in the Raman spectrum of the reflected light before and after pressing the indenter 1. Once determined, the amount will be correlated to the hardness of the object S to be measured. In other words, the hardness of the object to be measured in a minute area and a minute depth near the part pressed by the indenter 1 can be obtained.
なお、以上のような測定を被測定物Ｓの表面各部におい
て行い、マツピングすることにより被測定物Ｓの２次元
硬度分布が得られる。Note that the two-dimensional hardness distribution of the object to be measured S can be obtained by performing the above-mentioned measurements on each part of the surface of the object to be measured and mapping them.
〈発明の効果〉
以上説明したように、本発明によれば、一定条件下で圧
子を被測定物に押圧することにより生ずる変形に伴う被
測定物の内部応力の変化が、被測定物の硬度に相関する
ことに着目し、圧子押圧前後の内部応力の変化をラマン
スペクトルの変化として捕捉することによって、被測定
物の硬度情叩を得るよう構成したから、従来の差動トラ
ンス等を用いて被測定物の変形量を測定する方式に比し
て、極めて微小な変形を与えることによって硬度情報が
得られる。すなわち、被測定物の弾性限界内での応力を
作用させることによって硬度情報が得られることになり
、被測定物にダメージを与えることなく、再現性のよい
測定が可能となる。また、本発明によれば、被測定物の
前処理が特に必要でなく、かつ、大気中での測定も可能
であり、測定の作業性に関しても特に問題はなく、その
実施が容易である。<Effects of the Invention> As explained above, according to the present invention, the change in the internal stress of the object to be measured due to the deformation caused by pressing the indenter against the object to be measured under certain conditions changes the hardness of the object to be measured. By focusing on the correlation between Compared to methods that measure the amount of deformation of the object to be measured, hardness information can be obtained by applying extremely minute deformation. That is, hardness information can be obtained by applying stress within the elastic limit of the object to be measured, making it possible to measure with good reproducibility without damaging the object. Further, according to the present invention, there is no particular need for pretreatment of the object to be measured, and measurement can be performed in the atmosphere, and there are no particular problems with the workability of measurement, and it is easy to carry out.
第１図は本発明実施例の構成図、
第２図はその圧子１を押し付けたときの被測定物Ｓの弾
性変形の様子を模式的に示す図、第３図はレーザ光の反
射光のスペクトルの説明図、
第４図は被測定物Ｓの内部応力とラマンスペクトル変化
量の関係を示すグラフである。
第５図は従来の微小硬度計の構造説明図である。
１・・・圧子
２・・・負荷機構
３・・・レーザ
４・・・集光レンズ
５・・・分光器
６・・・光電子増倍管
特許出願人 株式会社島津製作所代 理 人
弁理士 西１）新
築２図
レーし−貴含ＬFig. 1 is a configuration diagram of an embodiment of the present invention, Fig. 2 is a diagram schematically showing the state of elastic deformation of the object S to be measured when the indenter 1 is pressed, and Fig. 3 is a diagram showing the state of elastic deformation of the object S when the indenter 1 is pressed. 4 is a graph showing the relationship between the internal stress of the object to be measured S and the amount of change in the Raman spectrum. FIG. 5 is a structural explanatory diagram of a conventional microhardness meter. 1...Indenter 2...Loading mechanism 3...Laser 4...Condensing lens 5...Spectrometer 6...Photomultiplier tube Patent applicant Representative of Shimadzu Corporation
Patent Attorney Nishi 1) New construction 2 drawings - Kikan L
Claims (1)
荷機構と、上記圧子による押圧部近傍にレーザ光を照射
するためのレーザと、そのレーザ光の反射散乱光のラマ
ンスペクトルを検出する検出手段を備え、検出されたラ
マンスペクトルの上記圧子押圧による変化量と上記圧子
の押圧力から被測定物の微小領域の硬度に係る情報を得
るよう構成されてなる、極微小硬度計。An indenter, a load mechanism that presses the indenter against the surface of the object to be measured with a predetermined force, a laser that irradiates a laser beam near the area pressed by the indenter, and detects the Raman spectrum of the reflected and scattered light of the laser beam. What is claimed is: 1. A microhardness tester, comprising: a detecting means for detecting the indentation, and is configured to obtain information regarding the hardness of a microscopic region of the object to be measured from the amount of change in the detected Raman spectrum due to the pressure of the indenter and the pressure of the indenter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1415088A JPH01189544A (en) | 1988-01-25 | 1988-01-25 | Extremely small hardness meter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1415088A JPH01189544A (en) | 1988-01-25 | 1988-01-25 | Extremely small hardness meter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01189544A true JPH01189544A (en) | 1989-07-28 |
Family
ID=11853119
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1415088A Pending JPH01189544A (en) | 1988-01-25 | 1988-01-25 | Extremely small hardness meter |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01189544A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996010737A1 (en) * | 1994-09-30 | 1996-04-11 | Renishaw Plc | Methods and apparatus for indentation, scratch or tribological testing |
| WO1997003346A1 (en) * | 1995-07-13 | 1997-01-30 | Renishaw Plc | Strain and/or stress sensitive devices |
| KR100836199B1 (en) * | 2006-10-02 | 2008-06-09 | 한양대학교 산학협력단 | A hardness measuring apparatus |
| WO2013115146A1 (en) * | 2012-02-03 | 2013-08-08 | 日東電工株式会社 | Sample fixing member for nano indenter |
| EP4273533A1 (en) * | 2022-05-06 | 2023-11-08 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Strain measurement apparatus and method for measuring mechanical strain |
-
1988
- 1988-01-25 JP JP1415088A patent/JPH01189544A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996010737A1 (en) * | 1994-09-30 | 1996-04-11 | Renishaw Plc | Methods and apparatus for indentation, scratch or tribological testing |
| WO1997003346A1 (en) * | 1995-07-13 | 1997-01-30 | Renishaw Plc | Strain and/or stress sensitive devices |
| KR100836199B1 (en) * | 2006-10-02 | 2008-06-09 | 한양대학교 산학협력단 | A hardness measuring apparatus |
| WO2013115146A1 (en) * | 2012-02-03 | 2013-08-08 | 日東電工株式会社 | Sample fixing member for nano indenter |
| CN104094097A (en) * | 2012-02-03 | 2014-10-08 | 日东电工株式会社 | Sample fixing member for nano indenter |
| EP4273533A1 (en) * | 2022-05-06 | 2023-11-08 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Strain measurement apparatus and method for measuring mechanical strain |
| WO2023213647A1 (en) * | 2022-05-06 | 2023-11-09 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e. V. | Strain measurement apparatus and method for measuring mechanical strain |
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