JPH05273198A - Analyzing method for semiconductor silicon substrate surface and substrate thin film surface - Google Patents
Analyzing method for semiconductor silicon substrate surface and substrate thin film surfaceInfo
- Publication number
- JPH05273198A JPH05273198A JP4068605A JP6860592A JPH05273198A JP H05273198 A JPH05273198 A JP H05273198A JP 4068605 A JP4068605 A JP 4068605A JP 6860592 A JP6860592 A JP 6860592A JP H05273198 A JPH05273198 A JP H05273198A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- thin film
- hydrofluoric acid
- semiconductor silicon
- silicon substrate
- 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
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Landscapes
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、半導体シリコン基板表
面及び基板上薄膜表面の分析方法に関し、特にフッ素化
合物が低昇華点である元素を分析する分析方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing a surface of a semiconductor silicon substrate and a surface of a thin film on a substrate, and more particularly to an analysis method for analyzing an element whose fluorine compound has a low sublimation point.
【０００２】[0002]
【従来の技術】電子工業分野ではデバイスの微細化に伴
い、使用する材料や製造工程に起因する金属不純物によ
るウエハ汚染（金属汚染）が問題になっている。そし
て、この問題を解決するために金属不純物の超高感度分
析が必要となってきている。2. Description of the Related Art In the field of electronics industry, as devices are miniaturized, wafer contamination (metal contamination) due to metal impurities caused by materials used and manufacturing processes has become a problem. Then, in order to solve this problem, ultra-sensitive analysis of metal impurities is required.
【０００３】近年、ＬＳＩ製造プロセスではゲルマニウ
ム等のフッ素化合物が低昇華点である元素が使われるよ
うになってきた。そして、これらの元素によるウエハ汚
染、ライン汚染のおそれがあるため、これらの元素の精
密な分析が必要となってきた。In recent years, elements having a low sublimation point have been used for fluorine compounds such as germanium in the LSI manufacturing process. Since there is a risk of wafer contamination and line contamination due to these elements, precise analysis of these elements has become necessary.
【０００４】従来、半導体シリコン基板表面及び基板上
薄膜表面の分析方法としては、先ず基板上をフッ酸のみ
の蒸気で分解し、その後フッ酸、フッ酸と硝酸、フッ酸
と過酸化水素、塩酸と過酸化水素のいずれかの液を回収
液として基板上に滴下し、その回収液を化学的分析する
ことにより分析を行っていた（特開平２−２８５３３号
参照）。Conventionally, as a method of analyzing the surface of the semiconductor silicon substrate and the surface of the thin film on the substrate, first, the substrate is decomposed by vapor of only hydrofluoric acid, and then hydrofluoric acid, hydrofluoric acid and nitric acid, hydrofluoric acid and hydrogen peroxide, hydrochloric acid. Analysis was conducted by dropping one of the solutions of hydrogen peroxide and hydrogen peroxide as a recovery solution on the substrate and chemically analyzing the recovery solution (see JP-A-2-28533).
【０００５】[0005]
【発明が解決しようとする課題】上述した従来の分析方
法では、基板上の不純物成分をフッ酸のみの蒸気で分解
させるときに、フッ素化合物が低昇華点である元素は昇
華されてしまうため、回収液に回収することができず分
析できないという問題点があった。In the above-mentioned conventional analysis method, when the impurity component on the substrate is decomposed by the vapor of only hydrofluoric acid, the element having the low sublimation point of the fluorine compound is sublimated. There was a problem that it could not be recovered in the recovery solution and could not be analyzed.
【０００６】本発明の課題は、フッ素化合物が低昇華点
である元素を昇華させることなく回収し、分析すること
が可能な分析方法を提供することにある。An object of the present invention is to provide an analysis method which allows a fluorine compound to be recovered and analyzed without sublimation of an element having a low sublimation point.
【０００７】[0007]
【課題を解決するための手段】本発明の分析方法は、半
導体シリコン基板表面及び基板上薄膜表面に存する、フ
ッ素化合物が低昇華点である元素を分析する方法におい
て、前記半導体シリコン基板表面及び基板上薄膜表面を
糖を含有するフッ酸で処理する如くした分析方法であ
る。The analysis method of the present invention is a method for analyzing an element existing on a surface of a semiconductor silicon substrate and a surface of a thin film on the substrate, which element has a low sublimation point of a fluorine compound. This is an analysis method in which the surface of the upper thin film is treated with hydrofluoric acid containing sugar.
【０００８】更に、本発明の分析方法は、前記半導体シ
リコン基板表面及び基板上薄膜表面に糖を含有するフッ
酸回収液を滴下して基板上を分解し、この分解回収液を
回収して当該回収液中の不純物成分を分析する方法であ
る。Further, in the analysis method of the present invention, a hydrofluoric acid recovery liquid containing sugar is dropped on the surface of the semiconductor silicon substrate and the surface of the thin film on the substrate to decompose the substrate, and the decomposition recovery liquid is recovered to This is a method of analyzing impurity components in the recovered liquid.
【０００９】更に、本発明の分析方法は、前記半導体シ
リコン基板表面及び基板上薄膜表面を糖を含有するフッ
酸蒸気で分解し、その後前記基板上の分解物を分解回収
液を用いて回収する如くした分析方法である。Further, in the analysis method of the present invention, the surface of the semiconductor silicon substrate and the surface of the thin film on the substrate are decomposed with hydrofluoric acid vapor containing sugar, and then the decomposed products on the substrate are recovered using a decomposition recovery liquid. This is the analysis method.
【００１０】更に他の本発明の分析方法は、前記分解回
収液として純水を用いた分析方法である。Still another analysis method of the present invention is an analysis method using pure water as the decomposition recovery liquid.
【００１１】[0011]
【作用】半導体シリコン基板表面及び基板上薄膜表面を
糖を含有するフッ酸で処理することにより、フッ素化合
物が低昇華点である元素の昇華を抑制することができ、
当該元素を含んだ液を回収し、分析することができるよ
うになった。By treating the surface of the semiconductor silicon substrate and the surface of the thin film on the substrate with hydrofluoric acid containing sugar, it is possible to suppress the sublimation of the element whose fluorine compound has a low sublimation point,
The liquid containing the element can now be collected and analyzed.
【００１２】[0012]
【実施例】次に本発明について図面を参照して説明す
る。The present invention will be described below with reference to the drawings.
【００１３】本発明に係わる実施例では、ゲルマニウム
で汚染させたウエハをフッ酸のみの蒸気を使わずに、糖
を含むフッ酸で処理を行なうことにより好結果を得たも
のである。In the embodiment according to the present invention, a favorable result was obtained by treating a wafer contaminated with germanium with hydrofluoric acid containing sugar without using vapor of hydrofluoric acid alone.
【００１４】図１は、本発明に係わる第１の実施例にお
ける処理方法のフローチャートを示す。半導体シリコン
基板表面又は基板上薄膜表面に、分解回収液として糖を
含むフッ酸を滴下してウエハ上全面を分解し、分解終了
後、分解回収液中の不純物成分を高感度分析装置で分析
する。FIG. 1 shows a flow chart of a processing method in a first embodiment according to the present invention. Hydrofluoric acid containing sugar is dropped on the surface of the semiconductor silicon substrate or the thin film on the substrate to decompose the entire surface of the wafer, and after the decomposition is completed, the impurity components in the decomposition and recovery liquid are analyzed with a high-sensitivity analyzer. ..
【００１５】図２は、１×１０13原子／ｃｍ2 のゲルマ
ニウムで汚染させたシリコンウエハを、図１で示す処理
を行い、分析した結果と従来技術とを比較して示してあ
る。分解回収液としては、従来から知られているフッ酸
のみと、本発明の糖を含んだフッ酸の２種類を比較のた
めに用いて、それぞれのゲルマニウムの回収率を測定し
た結果を示すものである。FIG. 2 shows the result of analysis of the silicon wafer contaminated with 1 × 10 13 atoms / cm 2 of germanium, which was subjected to the process shown in FIG. As the decomposition recovery liquid, only the conventionally known hydrofluoric acid and two types of hydrofluoric acid containing the sugar of the present invention were used for comparison, and the results of measuring the respective germanium recovery rates are shown. Is.
【００１６】図２では、１枚の汚染ウエハで５回回収操
作を繰り返したときの各回のゲルマニウムの回収率を示
している。 この結果から、フッ酸のみでも多少回収さ
れてはいるが、本発明の実施例に係わる糖を含むフッ酸
を分解回収液として用いることにより、全量回収、分析
が可能となる。しかも、１回の回収操作でほぼ全量を回
収することができる。このときの定量下限は、５×１０
9 原子／ｃｍ2 であり、データの再現性も良いことか
ら、本発明に係わる分析方法の問題はない。即ち、シリ
コンウエハ上のゲルマニウムを分析対象とする場合、分
解回収液として糖を含むフッ酸を用いることにより、全
量を定量分析できるようになった。FIG. 2 shows the recovery rate of germanium at each time when the recovery operation is repeated 5 times for one contaminated wafer. From this result, although the hydrofluoric acid alone was recovered to some extent, it is possible to recover and analyze the whole amount by using the hydrofluoric acid containing the sugar according to the embodiment of the present invention as the decomposition recovery liquid. Moreover, almost all the amount can be recovered by one recovery operation. The lower limit of quantification at this time is 5 x 10
Since it is 9 atoms / cm 2 and the data reproducibility is good, there is no problem in the analysis method according to the present invention. That is, when germanium on a silicon wafer is used as an analysis target, the total amount can be quantitatively analyzed by using hydrofluoric acid containing sugar as a decomposition recovery liquid.
【００１７】第２の実施例では、基板上をフッ酸蒸気で
分解し、基板上の分解物を回収液により回収して、その
回収液中の不純物成分を高感度分析装置で分析する分析
方法でフッ酸蒸気に糖を含有させて処理を行ったときの
分析例である。In the second embodiment, an analysis method in which the substrate is decomposed with hydrofluoric acid vapor, the decomposed products on the substrate are recovered by a recovery liquid, and the impurity components in the recovery liquid are analyzed by a high-sensitivity analyzer It is an example of analysis when processing is carried out by adding sugar to hydrofluoric acid vapor.
【００１８】図３は、本発明に係わる第２の実施例にお
ける処理方法のフローチャートを示す。半導体シリコン
基板表面及び基板上薄膜表面を、糖を含むフッ酸蒸気で
基板上全面を分解し、その後基板上に純水回収液を滴下
して回収して、回収液中の不純物成分を高感度分析装置
で分析する。FIG. 3 shows a flowchart of the processing method in the second embodiment according to the present invention. The surface of the semiconductor silicon substrate and the surface of the thin film on the substrate are decomposed over the entire surface of the substrate with hydrofluoric acid vapor containing sugar, and then a pure water recovery solution is dropped on the substrate to recover it, and the impurity components in the recovery solution are highly sensitive. Analyze with an analyzer.
【００１９】図４は、１×１０13原子／ｃｍ2 のゲルマ
ニウムで汚染させたシリコンウエハを図３で示す処理を
行い分析した結果と従来技術とを比較して示したもので
ある。比較のために、従来から知られているフッ酸蒸気
のみと本発明の糖を含むフッ酸蒸気の２種類で分解を行
い、純水回収液で回収したそれぞれの回収率の差を見て
いる。また、図４は、１枚の汚染ウエハで５回回収操作
を繰り返したときの各回の回収率を示している。FIG. 4 shows a comparison between the analysis result of the silicon wafer contaminated with 1 × 10 13 atoms / cm 2 germanium and the analysis shown in FIG. 3 and the prior art. For comparison, the difference between the recovery rates obtained by decomposing with only the conventionally known hydrofluoric acid vapor and hydrofluoric acid vapor containing the sugar of the present invention and recovering with pure water recovery liquid is observed. .. Further, FIG. 4 shows the recovery rate at each time when the recovery operation is repeated 5 times for one contaminated wafer.
【００２０】この結果から、フッ酸蒸気のみで分解し純
水回収を行った従来技術ではゲルマニウムの回収率が悪
く、本発明に係わる糖を含むフッ酸で分解し純水回収を
行った場合は、全量回収、分析が可能となった。しか
も、１回の回収操作でほぼ全量を回収することができ、
このときの定量下限は、７×１０9 原子／ｃｍ2 であ
り、データの再現性も良い。From this result, the recovery rate of germanium was poor in the prior art in which pure water was recovered by decomposing only with hydrofluoric acid vapor, and when pure water was recovered by decomposing with hydrofluoric acid containing sugar according to the present invention, , It became possible to collect and analyze all. Moreover, it is possible to recover almost all the amount in one recovery operation,
The lower limit of quantification at this time is 7 × 10 9 atoms / cm 2 , and the reproducibility of data is good.
【００２１】このことにより、シリコンウエハ上のゲル
マニウムを分析するには、糖を含むフッ酸蒸気で分解を
行うことにより、全量を定量分析することができる。従
って、基板上のフッ素化合物が低昇華点である元素の分
解、回収には、分解回収液を糖を含むフッ酸にするか又
は糖を含むフッ酸蒸気で分解することにより、高感度に
これら元素を分析することが可能となった。なお、上記
本発明の実施例においては汚染金属としてゲルマニウム
の例につき説明したが、この他に当該元素のフッ素化合
物が低昇華点特性を有する元素にも適用することができ
る。As a result, in analyzing germanium on a silicon wafer, the total amount can be quantitatively analyzed by decomposing with hydrofluoric acid vapor containing sugar. Therefore, for the decomposition and recovery of the element whose fluorine compound on the substrate has a low sublimation point, the decomposition recovery liquid is converted to hydrofluoric acid containing sugar or decomposed with hydrofluoric acid vapor containing sugar to achieve high sensitivity. It became possible to analyze the elements. In the embodiments of the present invention described above, the example of germanium as the contaminating metal has been described, but in addition to this, the fluorine compound of the element can be applied to an element having a low sublimation point characteristic.
【００２２】[0022]
【発明の効果】以上説明したように、半導体シリコン基
板表面及び基板上薄膜表面のフッ素化合物が低昇華点で
ある元素を分析するには、分解回収液を基板上に滴下し
て分解し、分解回収液を回収して、回収液中の不純物成
分を高感度分析装置で分析する分析方法の分解回収液と
して糖を含むフッ酸にする。または、基板上をフッ酸蒸
気で分解し、基板上の分解物を純水回収液で回収して、
その回収液中の不純物成分を高感度分析装置で分析する
分析方法のフッ酸蒸気に糖を含有させることにより、従
来、昇華してしまって分析することのできなかったこれ
ら元素を定量的で、かつ高感度に分析することが可能と
なった。As described above, in order to analyze an element in which the fluorine compound on the surface of the semiconductor silicon substrate and the surface of the thin film on the substrate has a low sublimation point, the decomposition recovery liquid is dropped on the substrate to decompose and decompose. The recovered liquid is recovered, and hydrofluoric acid containing sugar is used as a decomposed recovered liquid in an analysis method in which an impurity component in the recovered liquid is analyzed by a high-sensitivity analyzer. Alternatively, the substrate is decomposed with hydrofluoric acid vapor, and the decomposed product on the substrate is recovered with pure water recovery liquid,
By containing sugar in the hydrofluoric acid vapor of the analysis method for analyzing the impurity components in the recovered liquid with a high-sensitivity analyzer, these elements that were previously sublimated and could not be analyzed quantitatively, And it became possible to analyze with high sensitivity.
【００２３】よって、本発明の分析方法を行うことによ
り、半導体製造におけるこれら元素の金属汚染の低減が
可能となり、高品質、高生産歩留りの半導体製品を製造
することができる。Therefore, by carrying out the analysis method of the present invention, it is possible to reduce the metal contamination of these elements in semiconductor production, and it is possible to produce semiconductor products of high quality and high production yield.
【図１】 本発明の第１の実施例に係わる分析方法を説
明するためのフローチャート図。FIG. 1 is a flowchart diagram for explaining an analysis method according to a first embodiment of the present invention.
【図２】 本発明の第１の実施例により分析したときの
回収率を従来例と比較して示す特性図である。FIG. 2 is a characteristic diagram showing a recovery rate when analyzed by the first example of the present invention in comparison with a conventional example.
【図３】 本発明の第２の実施例に係わる分析方法を説
明するためのフローチャート図。FIG. 3 is a flow chart diagram for explaining an analysis method according to a second embodiment of the present invention.
【図４】 本発明の第２の実施例により分析したときの
回収率を従来例と比較して示す特性図である。FIG. 4 is a characteristic diagram showing a recovery rate when analyzed by the second example of the present invention in comparison with a conventional example.
Claims (4)
表面に存する、フッ素化合物が低昇華点である元素を分
析する方法において、前記半導体シリコン基板表面及び
基板上薄膜表面を糖を含有するフッ酸で処理することを
特徴とする半導体シリコン基板表面及び基板上薄膜表面
の分析方法。1. A method for analyzing an element having a low sublimation point of a fluorine compound on the surface of a semiconductor silicon substrate and the surface of a thin film on a substrate, wherein the surface of the semiconductor silicon substrate and the surface of the thin film on a substrate are hydrofluoric acid containing sugar. A method for analyzing a surface of a semiconductor silicon substrate and a surface of a thin film on the substrate, which comprises treating.
薄膜表面に糖を含有するフッ酸回収液を滴下して基板上
を分解し、前記分解回収液を回収して当該回収液中の不
純物成分を分析することを特徴とする請求項１記載の半
導体シリコン基板表面及び基板上薄膜表面の分析方法。2. A hydrofluoric acid recovery solution containing sugar is dropped on the surface of the semiconductor silicon substrate and on the surface of the thin film on the substrate to decompose the substrate, and the decomposition recovery solution is recovered to remove impurity components in the recovery solution. The method for analyzing the surface of a semiconductor silicon substrate and the surface of a thin film on a substrate according to claim 1, wherein the method is performed.
薄膜表面を糖を含有するフッ酸蒸気で分解し、その後前
記基板上の分解物を分解回収液を用いて回収することを
特徴とする請求項１記載の半導体シリコン基板表面及び
基板上薄膜表面の分析方法。3. The surface of the semiconductor silicon substrate and the surface of the thin film on the substrate are decomposed by hydrofluoric acid vapor containing sugar, and then the decomposed products on the substrate are recovered by using a decomposition recovery solution. 2. The method for analyzing the surface of a semiconductor silicon substrate and the surface of a thin film on a substrate according to 1.
を特徴とする請求項３記載の半導体シリコン基板表面及
び基板上薄膜表面の分析方法。4. The method for analyzing the surface of a semiconductor silicon substrate and the surface of a thin film on a substrate according to claim 3, wherein pure water is used as the decomposition and recovery liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4068605A JPH05273198A (en) | 1992-03-26 | 1992-03-26 | Analyzing method for semiconductor silicon substrate surface and substrate thin film surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4068605A JPH05273198A (en) | 1992-03-26 | 1992-03-26 | Analyzing method for semiconductor silicon substrate surface and substrate thin film surface |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05273198A true JPH05273198A (en) | 1993-10-22 |
Family
ID=13378579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4068605A Pending JPH05273198A (en) | 1992-03-26 | 1992-03-26 | Analyzing method for semiconductor silicon substrate surface and substrate thin film surface |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05273198A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0198944A (en) * | 1987-10-12 | 1989-04-17 | Kyushu Electron Metal Co Ltd | Surface analysis of silicon semiconductor substrate |
| JPH01189558A (en) * | 1988-01-23 | 1989-07-28 | Kyushu Electron Metal Co Ltd | Analyzing method of surface of si semiconductor substrate |
| JPH01272939A (en) * | 1988-04-25 | 1989-10-31 | Toshiba Corp | Measuring method for impurity |
| JPH0228533A (en) * | 1988-04-25 | 1990-01-30 | Toshiba Corp | Method and instrument for measuring impurity |
| JPH0413430A (en) * | 1990-04-29 | 1992-01-17 | Fuji Eng Kk | Sheet carrying device |
-
1992
- 1992-03-26 JP JP4068605A patent/JPH05273198A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0198944A (en) * | 1987-10-12 | 1989-04-17 | Kyushu Electron Metal Co Ltd | Surface analysis of silicon semiconductor substrate |
| JPH01189558A (en) * | 1988-01-23 | 1989-07-28 | Kyushu Electron Metal Co Ltd | Analyzing method of surface of si semiconductor substrate |
| JPH01272939A (en) * | 1988-04-25 | 1989-10-31 | Toshiba Corp | Measuring method for impurity |
| JPH0228533A (en) * | 1988-04-25 | 1990-01-30 | Toshiba Corp | Method and instrument for measuring impurity |
| JPH0413430A (en) * | 1990-04-29 | 1992-01-17 | Fuji Eng Kk | Sheet carrying device |
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