JP2832298B2 - Insulation analysis method - Google Patents
Insulation analysis methodInfo
- Publication number
- JP2832298B2 JP2832298B2 JP1075848A JP7584889A JP2832298B2 JP 2832298 B2 JP2832298 B2 JP 2832298B2 JP 1075848 A JP1075848 A JP 1075848A JP 7584889 A JP7584889 A JP 7584889A JP 2832298 B2 JP2832298 B2 JP 2832298B2
- Authority
- JP
- Japan
- Prior art keywords
- insulator
- window
- sample
- ion
- amount
- 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.)
- Expired - Fee Related
Links
- 238000004458 analytical method Methods 0.000 title description 16
- 238000009413 insulation Methods 0.000 title 1
- 239000012212 insulator Substances 0.000 claims description 52
- 150000002500 ions Chemical group 0.000 claims description 43
- 238000009826 distribution Methods 0.000 claims description 14
- 238000010884 ion-beam technique Methods 0.000 claims description 14
- 238000001004 secondary ion mass spectrometry Methods 0.000 claims description 6
- 238000004949 mass spectrometry Methods 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims 1
- 239000010408 film Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 17
- 238000010894 electron beam technology Methods 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229910052732 germanium Inorganic materials 0.000 description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
- Electron Tubes For Measurement (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は絶縁物分析法、さらに詳細には二次イオン質
量分析法を用いた絶縁物の分析法に関する。Description: FIELD OF THE INVENTION The present invention relates to an insulator analysis method, and more particularly to an insulator analysis method using secondary ion mass spectrometry.
（従来技術） 二次イオン質量分析法ではイオンビーム照射を用いる
ため、イオンビームのもたらす電荷や二次的に発生する
電子、イオンにより絶縁物表面に帯電が生じる。帯電が
生じると試料表面の電位が変化するために二次イオンの
軌道が変化する。このため、絶縁物の分析を行う場合質
量分析器を二次イオンが通過することが妨げられ、二次
イオンの検出が困難になる。従来、二次イオン質量分析
法による絶縁物分析の帯電を防止する方法としては、
絶縁物の表面の電荷を導電性の物質を介して逃がす方
法、負イオンビームを一次イオンとして用いることに
より、二次電子放出による正電荷の蓄積を補償する方
法、及び、過剰な正電荷を電子ビーム照射により直接
的に補償する方法、の３手法が主に用いられていた。(Prior Art) In the secondary ion mass spectrometry, since ion beam irradiation is used, the surface of an insulator is charged by the charge generated by the ion beam and the electrons and ions generated secondarily. When the charging occurs, the trajectory of the secondary ion changes because the potential of the sample surface changes. This prevents secondary ions from passing through the mass spectrometer when analyzing insulators, making it difficult to detect secondary ions. Conventionally, as a method of preventing electrification in insulator analysis by secondary ion mass spectrometry,
A method for releasing charges on the surface of an insulator through a conductive substance, a method for compensating for the accumulation of positive charges due to secondary electron emission by using a negative ion beam as primary ions, and a method for removing excess positive charges from electrons. The three methods of directly compensating by beam irradiation have been mainly used.
（発明が解決しようとする問題点） 第１の方法は導電性のメッシュを絶縁物の表面に接触
させるか、導電性薄膜を絶縁物表面に蒸着するものであ
った。この場合、一般的に試料表面から二次イオンを検
出する領域のサイズ（一辺または直径）が数十μｍ以上
であったため、分析中に絶縁物が露出している面積を10
0μｍ×100μｍ以上にし、導電膜あるいはメッシュ中に
含まれる元素を検出しないようにしていた。しかし、こ
の方法単独では絶縁物表面に生じた電荷を完全に逃がす
ことができない場合が多く、上に第３の方法として挙げ
た電子ビーム照射と併用する必要があった（y.Honma.M.
Oshima and Y.Ishii:質量分析32（（1984）345）。(Problems to be Solved by the Invention) The first method involves contacting a conductive mesh with the surface of an insulator or depositing a conductive thin film on the surface of the insulator. In this case, since the size (one side or diameter) of the region for detecting secondary ions from the sample surface is generally several tens μm or more, the area where the insulator is exposed during the analysis is 10 μm or less.
The size was set to 0 μm × 100 μm or more so that elements contained in the conductive film or the mesh were not detected. However, in many cases, the charge generated on the surface of the insulator cannot be completely escaped by this method alone, and it has been necessary to use the electron beam irradiation described above as the third method in combination (y.Honma.M.
Oshima and Y. Ishii: Mass spectrometry 32 ((1984) 345).
第２の負イオンビームを用いる方法の有効性は、試料
の二次電子放出能や試料電位に強く依存し、この方法単
独で絶縁物表面の電荷を補償できる場合は第１の方法以
上に限定されていた。このため、上記の第１、あるいは
第３の方法と併用して用いられる場合が多かった。The effectiveness of the second method using a negative ion beam strongly depends on the secondary electron emission ability of the sample and the sample potential. If this method alone can compensate for the charge on the insulator surface, it is limited to the first method or more. It had been. For this reason, it was often used in combination with the above-mentioned first or third method.
第３の電子ビーム照射法は、他の２法と組み合わせも
含め、従来最も広く用いられていた方法である。しか
し、この場合にも次のような問題があった。まず第１
に、低融点の材料や電子線損傷の大きな材料には適用で
きなかった。例えば、有機材料では電子ビーム照射によ
り炭化を起こす場合があった。また、脱ガス量が大きい
薄膜材料では、電子ビーム照射により薄膜の剥離が生じ
る場合があった。第２に、帯電補償に最適な電子ビーム
照射量は一次イオンビーム量や二次電子放出量との微妙
なバランスで決まっており、長時間、例えば１時間の連
続測定が必要な場合、一次イオンビーム量や電子ビーム
量の変動により、あるいは、試料の温度変化に伴う二次
電子放出量の変動により、帯電補償条件が変化して安定
な二次イオン測定ができない場合があった。例えば、厚
い絶縁物試料を一次イオンビームによりスパッタしなが
ら試料中の深さ方向の元素分布を得ようとする場合、所
望の深さまで到達する前に帯電補償条件が崩れ、再び表
面から分析をやり直すということが少なかった。特に、
試料が複数の種類の絶縁物の薄膜を積み重ねた多層絶縁
膜の場合、各絶縁層ごとに帯電補償条件が変化し、多層
絶縁膜全体の深さ方向の元素分布を一度に得ることは極
めて困難であった。The third electron beam irradiation method is the method most widely used conventionally, including the combination with the other two methods. However, this case also has the following problem. First,
However, it cannot be applied to a material having a low melting point or a material having a large electron beam damage. For example, an organic material may cause carbonization by electron beam irradiation. Further, in the case of a thin film material having a large degassing amount, the thin film may be peeled off by electron beam irradiation. Second, the optimal amount of electron beam irradiation for charging compensation is determined by a delicate balance between the amount of primary ion beam and the amount of secondary electron emission. Due to fluctuations in the beam amount or electron beam amount, or fluctuations in the amount of secondary electrons emitted due to a change in the temperature of the sample, charging compensation conditions changed, and stable secondary ion measurement could not be performed. For example, when trying to obtain an element distribution in the depth direction in a sample while sputtering a thick insulator sample with a primary ion beam, the charge compensation conditions are broken before reaching the desired depth, and analysis is performed again from the surface. That was few. Especially,
When the sample is a multilayer insulating film in which multiple types of insulator thin films are stacked, the charge compensation condition changes for each insulating layer, and it is extremely difficult to obtain the element distribution in the depth direction of the entire multilayer insulating film at once. Met.
本発明は上述の問題点に鑑みなされたものであり、従
来の絶縁物分析法における上記の欠点を改善するために
提案されたもので、その目的は、二次イオン質量分析法
による絶縁物分析を容易ならしめる分析法を提供するこ
とにある。The present invention has been made in view of the above-described problems, and has been proposed to improve the above-described drawbacks in the conventional insulator analysis method. An object of the present invention is to provide an analysis method that facilitates the analysis.
（問題点を解決するために手段） 上記の目的を達成するため、本発明は二次イオン質量
分析法を用いた斜め研磨した絶縁物の表面に100μｍ以
内の幅を持つ絶縁物の露出した領域と、前記絶縁物の露
出領域を囲む導電性領域を形成し、前記絶縁物の露出領
域から発生する二次イオンを位置敏感検出器を用いて検
出し、絶縁物表面の元素分布を分析することを特徴とす
るものである。(Means for Solving the Problems) In order to achieve the above-mentioned object, the present invention provides an obliquely polished insulator surface using a secondary ion mass spectrometry on an exposed surface of an insulator having a width of 100 μm or less. Forming a conductive region surrounding the exposed region of the insulator, detecting secondary ions generated from the exposed region of the insulator using a position-sensitive detector, and analyzing element distribution on the surface of the insulator. It is characterized by the following.
しかして本発明は電子ビーム照射などの補助的手段を
必要とせず、低融点の試料や多層構造の絶縁物にも適用
できること、および、試料面内や斜め研磨による深さ方
向の情報を一度に得られることを主要な特徴とする。Therefore, the present invention does not require auxiliary means such as electron beam irradiation, and can be applied to a sample having a low melting point or an insulator having a multilayer structure. The main feature is that it can be obtained.
実施例 次に本発明の実施例について説明する。なお、実施例
は一つの例示であって、本発明の精神を逸脱しない範囲
で、種々の変更あるいは改良を行いうることは言うまで
もない。Embodiment Next, an embodiment of the present invention will be described. It should be noted that the embodiments are merely examples, and it is needless to say that various changes or improvements can be made without departing from the spirit of the present invention.
（絶縁物表面が露出している部分（以下窓部という）の
巾と帯電量の関係を示す実験） 第１図は窓部の巾と帯電量の関係を示す実験に使用し
た試料の説明図であり、第２図は第１図の試料を用いた
絶縁物分析法の第１の実施例を説明する図である。(Experiment showing the relationship between the width of the portion where the surface of the insulator is exposed (hereinafter referred to as a window) and the amount of charge) FIG. 1 is an explanatory view of the sample used in the experiment showing the relationship between the width of the window and the amount of charge FIG. 2 is a view for explaining a first embodiment of the insulator analysis method using the sample of FIG.
第１図において、１は絶縁物、２は導電膜、３は導電
膜２に開けられた穴であって絶縁物１の表面が露出して
いる部分（窓部）である。第２図において、４は導電膜
と同電位に保たれた試料ホルダ、５は一次イオンビー
ム、６は二次イオン、７は二次イオンの光学系および質
量分析系、８は二次イオン像、９は位置敏感検出器、10
は画像メモリーを有するコンピュータである。以下、図
に従って絶縁物の分析法を説明する。In FIG. 1, reference numeral 1 denotes an insulator, 2 denotes a conductive film, and 3 denotes a hole formed in the conductive film 2 and a portion (a window portion) where the surface of the insulator 1 is exposed. In FIG. 2, reference numeral 4 denotes a sample holder maintained at the same potential as the conductive film, 5 denotes a primary ion beam, 6 denotes a secondary ion, 7 denotes a secondary ion optical system and mass spectrometry system, and 8 denotes a secondary ion image. , 9 is a position sensitive detector, 10
Is a computer having an image memory. Hereinafter, a method of analyzing an insulator will be described with reference to the drawings.
分析に先立って、絶縁物１の表面に金属などの導電性
の膜２を被着する。膜の被着法としては、真空蒸着法、
スパッタ法、塗布法などを用いることができる。窓部３
は導電膜２の被着時にマスクを用いるか、あるいは、導
電膜２の被着後にエッチングすることにより形成する。
窓部３の幅はこの中にある絶縁物の表面に生じる帯電量
に大きく影響する。Prior to the analysis, a conductive film 2 such as a metal is deposited on the surface of the insulator 1. Vacuum evaporation,
A sputtering method, a coating method, or the like can be used. Window 3
Is formed by using a mask during the deposition of the conductive film 2 or by etching after the deposition of the conductive film 2.
The width of the window 3 greatly affects the amount of charge generated on the surface of the insulator in the window 3.
第３図に窓部３内の絶縁物表面の帯電量と窓部の幅と
の関係を、絶縁物１としてガラス、導電膜２として銀、
一次イオンビーム５として酸素イオンビームを用いた場
合について示す。帯電量は一次イオン照射下において、
試料ホルダ４の電位に対する窓部３の中央部の絶縁物表
面の電位の変化量を用いて表現した。帯電が生じない場
合には電位変化量は０であり、帯電量が大きいほど電位
変化量が大きくなる。電位変化量は窓部の幅が100μｍ
で約60Vであり、それ以下の場合、窓部の幅にほぼ比例
して増加する。窓部の幅が100μｍより大きくなると、
電位変化量は急激に増加し、二次イオン６の軌道に与え
る影響が無視できなくなる。電位変化が60V以下であれ
ば、軌道の変化は小さく、二次イオン光学系７内部のエ
ネルギーフィルタのウインド幅や、試料ホルダ４に印加
するバイアス電圧により、軌道変化に伴う二次イオン強
度の減少を容易に補償することができる。従って、窓部
３の幅は100μｍ以下、望ましくは、50μｍ以下である
のがよい。窓部３の長さは任意で良い。導電膜２は、一
次イオンビーム５によりスパッタエッチングされるの
で、分析中にスパッタし尽くされない程度の厚さ、例え
ば１μｍとする。FIG. 3 shows the relationship between the amount of charge on the surface of the insulator in the window portion 3 and the width of the window portion.
The case where an oxygen ion beam is used as the primary ion beam 5 will be described. The charge amount under primary ion irradiation,
It was expressed using the amount of change in the potential of the insulator surface at the center of the window 3 with respect to the potential of the sample holder 4. When no charging occurs, the potential change amount is 0, and the larger the charge amount, the larger the potential change amount. Potential change is 100μm in width of window
In this case, the voltage increases approximately in proportion to the width of the window. When the width of the window is larger than 100 μm,
The amount of potential change increases rapidly, and the effect on the trajectory of the secondary ions 6 cannot be ignored. If the potential change is 60 V or less, the change in the trajectory is small, and the secondary ion intensity decreases with the trajectory change due to the window width of the energy filter inside the secondary ion optical system 7 and the bias voltage applied to the sample holder 4. Can be easily compensated. Therefore, the width of the window 3 is preferably 100 μm or less, and more preferably, 50 μm or less. The length of the window 3 may be arbitrary. Since the conductive film 2 is sputter-etched by the primary ion beam 5, the conductive film 2 has a thickness such as not to be completely sputtered during the analysis, for example, 1 μm.
上記の手順で導電化処理を施した試料を二次イオン質
量分析装置の試料室に導入し、一次イオンビーム５を窓
部３を含む領域に照射する。これにより、絶縁物１に含
まれている元素の二次イオン６が表面から発生する。こ
の二次イオン６を二次イオン光学系および質量分析系７
を通して質量分離し、かつ、窓部３内部から発生した二
次イオン６を試料表面の像として結像面に二次イオン像
８として結像させる。この二次イオン像８を位置敏感検
出器９により検出し、像を構成する各点の強度をコンピ
ュータ10を用いて取り込み、メモリーに記録する。分析
後にメモリーに記録されたイオン強度のデータを処理す
ることにより、窓部３内にある絶縁物１の表面の元素分
布、例えば、窓部３内部の平面的な元素分布や、ある線
に沿った元素の濃度分布などを得ることができる。ま
た、表面をスパッタしながら表面元素の時間的な濃度変
化を記録することにより、窓部３内部の３次元的な元素
の濃度分布や、ある点における深さ方向の濃度分布など
を得ることができる。なお、窓部３の周囲から発生した
二次イオン６には導電膜２の中の元素も含まれている
が、メモリーに記録されたイオン像８の各点のイオン強
度のうち、窓部３の周囲の部分のイオン強度を取り除く
ことにより、導電膜２の中の元素の影響を容易に除くこ
とができる。The sample subjected to the conductivity treatment according to the above procedure is introduced into the sample chamber of the secondary ion mass spectrometer, and the region including the window 3 is irradiated with the primary ion beam 5. Thereby, secondary ions 6 of the element contained in the insulator 1 are generated from the surface. The secondary ions 6 are converted into a secondary ion optical system and a mass spectrometry system 7.
And secondary ions 6 generated from the inside of the window 3 are formed as an image of the sample surface as a secondary ion image 8 on the image forming surface. The secondary ion image 8 is detected by the position-sensitive detector 9, and the intensity of each point constituting the image is captured using the computer 10 and recorded in the memory. By processing the data of the ion intensity recorded in the memory after the analysis, the element distribution on the surface of the insulator 1 in the window 3, for example, the planar element distribution inside the window 3 or along a certain line Concentration distribution of the elements can be obtained. Further, by recording the temporal concentration change of the surface element while sputtering the surface, it is possible to obtain a three-dimensional element concentration distribution inside the window portion 3 and a depth concentration distribution at a certain point. it can. Although the secondary ions 6 generated from the periphery of the window 3 include elements in the conductive film 2, the ion intensity at each point of the ion image 8 recorded in the memory includes the secondary ions 6. By removing the ionic strength in the surrounding area, the influence of the elements in the conductive film 2 can be easily removed.
なお、導電膜２の代わりに窓部３に接する線状あるい
はメッシュ状の導電体を使用することもできる。Note that, instead of the conductive film 2, a linear or mesh-shaped conductor in contact with the window portion 3 can be used.
（実施例１） 第４図は本発明の実施例における試料の導電化処理を
説明する図であり、11は斜め研磨した絶縁物、12は研磨
面である。(Example 1) FIG. 4 is a view for explaining a conductive treatment of a sample in an example of the present invention, wherein 11 is an insulator polished obliquely, and 12 is a polished surface.
本実施例では絶縁物11を表面に対し角度Θで鏡面に研
磨し、深さ方向の長さを1/sinΘ倍に拡大する。例え
ば、Θ＝２゜53′であれば拡大率は20倍、Θ＝１゜８′
では50倍となる。また、第４図に示すように、研磨面を
角度φが90度よりも大きくなるようにして研磨すれば、
試料面方向の拡大を行うこともできる。この研磨面12に
窓部３を残して導電膜２を被着することにより、第２図
と同様の方法で窓部３内にある絶縁物１の研磨面12の表
面の元素分布を得ることができる。この場合のイオン像
は深さ方向の拡大像であるので、表面の元素分布は深さ
方向の元素分布に対応するものである。なお、導電膜２
の代わりに窓部３に接する線状あるいはメッシュ状の導
電体を使用することもできある。In this embodiment, the insulator 11 is polished to a mirror surface at an angle Θ with respect to the surface, and the length in the depth direction is increased by 1 / sinΘ. For example, if Θ = 2 ゜ 53 ′, the magnification is 20 times, Θ = 1 ゜ 8 ′
Then it becomes 50 times. Also, as shown in FIG. 4, if the polishing surface is polished so that the angle φ is larger than 90 degrees,
Enlargement in the sample surface direction can also be performed. By depositing the conductive film 2 on the polished surface 12 while leaving the window 3, the element distribution on the polished surface 12 of the insulator 1 in the window 3 can be obtained in the same manner as in FIG. Can be. Since the ion image in this case is an enlarged image in the depth direction, the element distribution on the surface corresponds to the element distribution in the depth direction. The conductive film 2
Alternatively, a linear or meshed conductor in contact with the window 3 may be used.
第５図は本実施例の効果を示す図であって、同図
（ａ）に示すようなシリコン基板20上に窒化シリコン
（膜厚１μｍ）13、ゲルマニウムガラス（膜厚５μｍ）
14、ホウ素ガラス（膜厚20μｍ）15からなる絶縁物１の
多層膜中の元素の深さ方向分布を測定した結果である。
測定に用いた試料は斜め研磨角度は、Θ＝２゜53′、φ
＝90゜とし、深さ方向を20倍に拡大したものである。導
電膜としては銀２を蒸着し、窓部の大きさは25μｍ×20
0μｍとした。この試料にセシウムイオンビームを照射
し、シリコンと窒素が結合した二次イオン、SiN-の像、
ゲルマニウムの二次イオン、Ge-の像、および、シリコ
ンとホウ素が結合した二次イオン、SiB-の像を観察し
た。得られた各元素の二次イオン像を模式的に第５図
（ｂ）に示した。FIG. 5 is a view showing the effect of the present embodiment, in which silicon nitride (1 μm thick) 13 and germanium glass (5 μm thick) are formed on a silicon substrate 20 as shown in FIG.
14 shows the results of measuring the depth distribution of elements in the multilayer film of the insulator 1 made of boron glass (film thickness 20 μm) 15.
The sample used for the measurement has an oblique polishing angle of Θ = 2 ゜ 53 ′, φ
= 90 ° and the depth direction is enlarged 20 times. Silver 2 is deposited as a conductive film, and the size of the window is 25 μm × 20.
It was set to 0 μm. This sample is irradiated with a cesium ion beam, and secondary ions in which silicon and nitrogen are combined, an image of SiN − ,
Germanium secondary ions, Ge - of the image, and, secondary ions silicon and boron bound, SiB - and an image of the observation. FIG. 5B schematically shows the obtained secondary ion images of the respective elements.
これらの二次イオン像をコンピュータのメモリに取り
込み、Ａ−Ｂ線に沿ったイオン強度のデータを取り出し
て、各イオンの強度分布を重ねてプロットした結果が第
５図（ｃ）のグラフである。グラフの横軸は、Ａ−Ｂ線
に沿った二次イオン像の長さを表面からの深さに換算し
た値を示した。異なる種類の絶縁物からなる多層膜であ
るにも係わらず、各層間で帯電量の差が生じることな
く、安定な二次イオン強度が得られ、ゲルマニウムガラ
スとホウ素ガラスとの間の元素の拡散の様子が明瞭に認
められる。しかも、10μｍに渡る深さ方向の情報が５分
以内の二次イオン像測定で得ることができた。These secondary ion images were taken into the memory of the computer, the data of the ion intensity along the line AB was taken out, and the intensity distribution of each ion was superimposed and plotted. The result is shown in FIG. 5 (c). . The horizontal axis of the graph shows the value obtained by converting the length of the secondary ion image along the line AB into the depth from the surface. Despite being a multilayer film composed of different types of insulators, stable secondary ionic strength can be obtained without a difference in charge amount between each layer, and diffusion of elements between germanium glass and boron glass Is clearly recognized. In addition, information in the depth direction over 10 μm could be obtained by secondary ion image measurement within 5 minutes.
（発明の効果） 以上説明したように、絶縁物の表面に、100μｍ以内
の幅を持つ絶縁物の露出した領域と、絶縁物の露出領域
を囲む試料ホルダと同電位に保たれた導電性領域を形成
し、この絶縁物の露出した領域から発生する二次イオン
を位置敏感検出器を用いて分析することにより、二次イ
オン質量分析法による絶縁物の分析が容易になり、か
つ、分析可能な材料の種類を広げることができた。これ
により、ガラス材料やセラミックス材料、有機材料など
絶縁性材料の研究開発に多大な効果をもたらす。(Effects of the Invention) As described above, on the surface of the insulator, the exposed region of the insulator having a width of 100 μm or less and the conductive region maintained at the same potential as the sample holder surrounding the exposed region of the insulator. By using a position-sensitive detector to analyze the secondary ions generated from the exposed region of the insulator, the analysis of the insulator by secondary ion mass spectrometry becomes easier and possible. We were able to expand the kinds of materials. This has a great effect on research and development of insulating materials such as glass materials, ceramic materials, and organic materials.
第１図は窓部の巾と帯電量の関係を示す実験に使用した
試料の説明図、第２図は上記実験及び実施例に使用した
分析方法の説明図、第３図は帯電量と窓部の幅との関係
を説明する図、第４図は本発明の第２の実施例における
導電化処理の説明図、第５図は本発明の第２の実施例の
効果を説明する図であって、シリコン基板上の窒化シリ
コン、ゲルマニウムガラス、ホウ素ガラスの３層からな
る絶縁性多層膜の分析例を示す。 １……絶縁物、２……導電膜、３……窓部、４……試料
ホルダ、５……一次イオンビーム、６……二次イオン、
７……二次イオン光学系・質量分析系、８……イオン
像、９……位置敏感検出器、10……コンピュータ、11…
…斜め研磨した絶縁物、12……研磨面。FIG. 1 is an explanatory view of a sample used in an experiment showing the relationship between the width of a window portion and an amount of charge, FIG. 2 is an explanatory view of an analysis method used in the above experiment and Example, and FIG. FIG. 4 is a diagram for explaining the relationship with the width of the portion, FIG. 4 is a diagram for explaining the conductive treatment in the second embodiment of the present invention, and FIG. 5 is a diagram for explaining the effect of the second embodiment of the present invention. Next, an analysis example of an insulating multilayer film including three layers of silicon nitride, germanium glass, and boron glass on a silicon substrate will be described. DESCRIPTION OF SYMBOLS 1 ... Insulator, 2 ... Conductive film, 3 ... Window part, 4 ... Sample holder, 5 ... Primary ion beam, 6 ... Secondary ion,
7: secondary ion optical system / mass spectrometry system, 8: ion image, 9: position sensitive detector, 10: computer, 11 ...
... diagonally polished insulator, 12 ... polished surface.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭64−50351（ＪＰ，Ａ) 特開 昭55−114935（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) H01J 37/252,37/20,49/26 H01L 21/66 G01N 23/225────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-64-50351 (JP, A) JP-A-55-114935 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) H01J 37 / 252,37 / 20,49 / 26 H01L 21/66 G01N 23/225
Claims (1)
射し、それによって前記絶縁物表面から発生する二次イ
オンを引き出して質量分析することにより前記絶縁物中
に含まれる元素の種類と量を分析する絶縁物の二次イオ
ン質量分析法において、斜め研磨した絶縁物の表面に、
100μｍ以内の幅を持つ絶縁物の露出した領域と、前記
絶縁物の露出領域を囲む導電性領域を形成し、前記絶縁
物の露出領域から発生する二次イオンを位置敏感検出器
を用いて検出し、絶縁物表面の元素分布を分析すること
を特徴とする絶縁物分析法。1. A kind of an element contained in an insulator by irradiating a sample which is an insulator with a primary ion beam, extracting secondary ions generated from the surface of the insulator, and performing mass spectrometry. In the secondary ion mass spectrometry of the insulator to analyze the surface of the obliquely polished insulator,
An exposed region of the insulator having a width of 100 μm or less and a conductive region surrounding the exposed region of the insulator are formed, and secondary ions generated from the exposed region of the insulator are detected using a position-sensitive detector. And analyzing the element distribution on the surface of the insulator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1075848A JP2832298B2 (en) | 1989-03-28 | 1989-03-28 | Insulation analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1075848A JP2832298B2 (en) | 1989-03-28 | 1989-03-28 | Insulation analysis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02253553A JPH02253553A (en) | 1990-10-12 |
| JP2832298B2 true JP2832298B2 (en) | 1998-12-09 |
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ID=13588045
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1075848A Expired - Fee Related JP2832298B2 (en) | 1989-03-28 | 1989-03-28 | Insulation analysis method |
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| Country | Link |
|---|---|
| JP (1) | JP2832298B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002005309A1 (en) * | 2000-07-07 | 2002-01-17 | Leo Elektronenmikroskopie Gmbh | Detector for variable pressure areas and an electron microscope comprising a corresponding detector |
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|---|---|---|---|---|
| JPH0754683B2 (en) * | 1987-08-20 | 1995-06-07 | 株式会社日立製作所 | Antistatic method |
-
1989
- 1989-03-28 JP JP1075848A patent/JP2832298B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02253553A (en) | 1990-10-12 |
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