JP5101477B2 - Method for analyzing impurities in ceramic members - Google Patents
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- JP5101477B2 JP5101477B2 JP2008313267A JP2008313267A JP5101477B2 JP 5101477 B2 JP5101477 B2 JP 5101477B2 JP 2008313267 A JP2008313267 A JP 2008313267A JP 2008313267 A JP2008313267 A JP 2008313267A JP 5101477 B2 JP5101477 B2 JP 5101477B2
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- 239000012535 impurity Substances 0.000 title claims description 42
- 238000000034 method Methods 0.000 title claims description 34
- 239000000919 ceramic Substances 0.000 title claims description 33
- 239000003929 acidic solution Substances 0.000 claims description 35
- 239000002184 metal Substances 0.000 claims description 25
- 238000004458 analytical method Methods 0.000 claims description 16
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 6
- 238000003892 spreading Methods 0.000 claims description 5
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 238000005530 etching Methods 0.000 description 8
- 230000000873 masking effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000011978 dissolution method Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000004452 microanalysis Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Description
本発明は、セラミックス部材の表面の金属不純物を分析するセラミックス部材の不純物分析方法に関する。 The present invention relates to an impurity analysis method for a ceramic member, which analyzes metal impurities on the surface of the ceramic member.
近年、半導体デバイスの高集積化、高性能化に伴い、半導体製造装置用として用いられるセラミックス部材には、金属不純物をできる限り低減化させた高純度品であることが要求されている。特に、半導体製造装置用セラミックス部材の表面に存在する金属不純物の低減化に対する要求が厳しくなっている。
このため、高純度で高品質のセラミックス部材を製造する上で、セラミックス部材の表面の金属不純物を分析し、品質管理を行うことは重要である。
In recent years, along with the high integration and high performance of semiconductor devices, ceramic members used for semiconductor manufacturing apparatuses are required to be high-purity products in which metal impurities are reduced as much as possible. In particular, demands for reducing metal impurities present on the surface of ceramic members for semiconductor manufacturing equipment have become strict.
For this reason, in manufacturing a high purity and high quality ceramic member, it is important to analyze the metal impurities on the surface of the ceramic member and perform quality control.
前記セラミックス部材の不純物分析は、従来、直接滴下法、浸漬溶解法、マスキング法等により、前記部材の表面または全体の不純物を抽出し、回収した抽出液について、誘導結合プラズマ質量分析（ＩＣＰ−ＭＳ）、誘導結合プラズマ発光分光分析（ＩＣＰ−ＯＥＳ）、原子吸光分析（ＡＡＳ）等により不純物を定量することにより行われていた。 Conventionally, impurity analysis of the ceramic member has been performed by inductively coupled plasma mass spectrometry (ICP-MS) with respect to the extracted liquid obtained by extracting impurities on the surface or the whole of the member by a direct dropping method, immersion dissolution method, masking method, or the like. ), Inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), and the like.
前記各種分析に供するための抽出液を得る方法の一つである直接滴下法は、部材の表面に、フッ化水素酸、塩酸、過酸化水素水等の混合液による酸性溶液を直接滴下し、前記部材表面をエッチングして金属不純物を抽出し、この抽出液を回収する方法である（例えば、特許文献１参照）。
また、浸漬溶解法は、製品のサイズが５０ｍｍ程度以下と小さい場合に適用される方法であり、フッ素樹脂製容器中の上記と同様の酸性溶液に浸漬させて、必要に応じて加圧し、金属不純物を抽出する方法である（例えば、特許文献２，３参照）。
また、マスキング法は、フッ素樹脂製シート等によりマスキングして、部材表面の一定面積の露出面について、上記と同様の酸性溶液や酸蒸気に接触させて不純物の抽出液を得る方法である。
The direct dropping method, which is one of the methods for obtaining an extract for use in the various analyses, directly drops an acidic solution of a mixed liquid such as hydrofluoric acid, hydrochloric acid, and hydrogen peroxide water on the surface of the member, In this method, the surface of the member is etched to extract metal impurities, and this extract is recovered (for example, see Patent Document 1).
The immersion dissolution method is a method applied when the size of the product is as small as about 50 mm or less, and is immersed in an acidic solution similar to the above in a fluororesin container, and pressurized as necessary. This is a method for extracting impurities (see, for example, Patent Documents 2 and 3).
Further, the masking method is a method of obtaining an impurity extract by masking with a fluororesin sheet or the like and bringing the exposed surface of the surface of the member into contact with the same acidic solution or acid vapor as described above.
しかしながら、直接滴下法は、一般的に、シリコン基板表面の不純物分析に用いられる方法であり、これをセラミックス部材に適用する場合には、該部材の形状によっては、該部材の表面以外の部分がエッチングされたり、また、抽出液を回収できなかったりする等の問題があり、高精度の不純物分析に適しているとは言えなかった。 However, the direct dripping method is a method generally used for impurity analysis on the surface of a silicon substrate, and when this is applied to a ceramic member, depending on the shape of the member, a portion other than the surface of the member may be used. There are problems such as etching and the inability to recover the extract, and it has not been suitable for high-precision impurity analysis.
また、浸漬溶解法は、分析対象の部材全体を酸性溶液中に浸漬させて行わなければならず、前記部材のサイズが大きい場合には、酸性溶液および前記部材を収容する容器自体を大きくする必要があり、金属不純物を抽出するための装置自体が大型化し、煩雑となる。
また、マスキング法は、分析対象の部材が、マスキング材によって汚染されるという懸念があった。
また、上述したいずれの方法によっても、部材の表面の一部のみを効率的にエッチングして分析することは、技術的に困難であった。
In addition, the immersion dissolution method must be performed by immersing the entire member to be analyzed in an acidic solution. When the size of the member is large, the acidic solution and the container itself containing the member must be enlarged. Therefore, the apparatus itself for extracting metal impurities becomes large and complicated.
Further, the masking method has a concern that the member to be analyzed is contaminated by the masking material.
Moreover, it was technically difficult to efficiently etch and analyze only a part of the surface of the member by any of the methods described above.
本発明は、上記技術的課題を解決するためになされたものであり、セラミックス部材の表面の一部のみを効率的にエッチングすることが可能であり、また、該部材の形状により、該部材の表面以外の部分がエッチングされたり、抽出液を回収できなかったりする等の不具合が生じることなく、金属不純物の抽出液を簡便かつ効率的に回収して、該部材の表面の金属不純物を高精度で分析することができるセラミックス部材の不純物分析方法を提供することを目的とするものである。 The present invention has been made to solve the above technical problem, and it is possible to efficiently etch only a part of the surface of a ceramic member. The metal impurities extract can be easily and efficiently recovered without causing problems such as etching other than the surface or failure to recover the extract. An object of the present invention is to provide an impurity analysis method for a ceramic member that can be analyzed by the above method.
本発明に係るセラミックス部材の不純物分析方法は、セラミックス部材の表面の一部に、酸性溶液の液滴を形成した後、前記酸性溶液の膜を形成してエッチングし、金属不純物を抽出する工程と、前記金属不純物の抽出液を回収する工程と、前記抽出液に含まれる金属不純物を分析する工程とを備えていることを特徴とする。
このような方法によれば、該液滴が形成された部分の表面が若干エッチングされ、酸性溶液の膜を、広がりすぎたり、流れ落ちたりすることなく、形成することができ、セラミックス部材の表面の一部のみ確実に、効率的にエッチングすることができる。
The method for analyzing impurities of a ceramic member according to the present invention includes a step of forming a droplet of an acidic solution on a part of the surface of the ceramic member, forming a film of the acidic solution, and etching to extract metal impurities. And a step of recovering an extract of the metal impurities, and a step of analyzing the metal impurities contained in the extract.
According to such a method, the surface of the portion where the droplets are formed is slightly etched, and an acidic solution film can be formed without spreading or flowing down, and the surface of the ceramic member can be formed. Only a part can be reliably and efficiently etched.
上記分析方法においては、前記酸性溶液の膜の形成は、円周状に前記酸性溶液の液滴を形成し、前記円周状の内側方向に前記液滴を広げるように行うことが好ましい。
このような方法によれば、前記酸性溶液の膜が円周状の外側方向に広がることなく、確実に、部材の表面を局所的かつ効率的にエッチングすることができる。
In the analysis method, the acidic solution film is preferably formed so as to form droplets of the acidic solution in a circumferential shape and spread the droplets in the circumferential inner direction.
According to such a method, the surface of the member can be locally and efficiently etched reliably without spreading the film of the acidic solution in the outer circumferential direction.
また、上記分析方法においては、金属不純物の抽出液を簡便かつ効率的に回収するため、前記抽出液の回収は、前記部材の表面を傾けて、マイクロピペットを用いて行うことが好ましい。 Further, in the above analysis method, in order to easily and efficiently recover the metal impurity extract, it is preferable to collect the extract using a micropipette with the surface of the member inclined.
前記金属不純物の分析は、高感度微量分析を行う観点から、誘導結合プラズマ質量分析法（ＩＣＰ−ＭＳ）またはフレームレス原子吸光分析法（ＦＬ−ＡＡ）により行うことが好ましい。 The metal impurities are preferably analyzed by inductively coupled plasma mass spectrometry (ICP-MS) or flameless atomic absorption spectrometry (FL-AA) from the viewpoint of performing highly sensitive microanalysis.
本発明によれば、部材の表面の一部のみを効率的にエッチングすることが可能であり、また、該部材の形状により、酸性溶液によって該部材の表面以外の部分がエッチングされたり、抽出液を回収できなかったりする等の不具合が解消され、金属不純物の抽出液を簡便かつ効率的に回収することができ、セラミックス部材の表面の金属不純物を高精度で分析することができる。
したがって、本発明に係る方法は、セラミックス部材の品質管理に好適に利用することができ、ひいては、該部材の品質向上に寄与することができる。
According to the present invention, it is possible to efficiently etch only a part of the surface of the member, and depending on the shape of the member, a portion other than the surface of the member is etched by an acidic solution, or an extract solution Thus, the metal impurity extract can be easily and efficiently recovered, and the metal impurities on the surface of the ceramic member can be analyzed with high accuracy.
Therefore, the method according to the present invention can be suitably used for quality control of the ceramic member, and can contribute to quality improvement of the member.
以下、本発明を、より詳細に説明する。
図１は、本発明に係るセラミックス部材の不純物分析方法を説明するための工程フロー図である。
本発明に係るセラミックス部材の不純物分析方法は、セラミックス部材の表面の一部に酸性溶液の液滴を形成した後、前記酸性溶液の膜を形成してエッチングし、金属不純物を抽出する工程（Ｓ１０１）と、前記金属不純物の抽出液を回収する工程（Ｓ１０２）と、前記抽出液に含まれる金属不純物を分析する工程（Ｓ１０３）とを備えている。
Hereinafter, the present invention will be described in more detail.
FIG. 1 is a process flow diagram for explaining an impurity analysis method for a ceramic member according to the present invention.
In the method for analyzing impurities of a ceramic member according to the present invention, after forming a droplet of an acidic solution on a part of the surface of the ceramic member, forming a film of the acidic solution and etching to extract metal impurities (S101) ), Recovering the metal impurity extract (S102), and analyzing the metal impurities contained in the extract (S103).
前記酸性溶液の膜の形成は、図２に示すような方法により行う。図２は、セラミックス部材の表面に酸性溶液の膜を局所的に形成する方法を説明するための断面図である。
前記酸性溶液の膜は、図２に示すように、セラミックス部材１０の表面１０ａ上に、マイクロピペット２０により酸性溶液３０を滴下し（図２（ａ））、酸性溶液３０の液滴３０ａを形成した後（図２（ｂ））、この液滴３０ａを膜状化させて形成する（図２（ｃ））。
このような方法によれば、セラミックス部材の表面に、局所的かつ効率的に、エッチングするための酸性溶液の膜を容易に形成することができる。
前記液滴の膜状化（図２（ｃ））は、ピペットチップを用いて、該ピペットチップのチップ部で行うことが好ましい。
これにより、前記部材の表面に容易かつ均等に前記酸性溶液の膜を形成することができる。
The acidic solution film is formed by the method shown in FIG. FIG. 2 is a cross-sectional view for explaining a method of locally forming an acidic solution film on the surface of the ceramic member.
As shown in FIG. 2, the acidic solution film is formed by dropping the
According to such a method, it is possible to easily form a film of an acidic solution for etching locally and efficiently on the surface of the ceramic member.
The film formation of the droplets (FIG. 2C) is preferably performed using a pipette tip at the tip portion of the pipette tip.
Thereby, the film of the acidic solution can be easily and evenly formed on the surface of the member.
より具体的には、前記酸性溶液の膜の形成は、前記部材の表面に円周状に酸性溶液の液滴を形成した後、ピペットチップを用いて、前記液滴を前記ピペットチップのチップ部でなぞりながら、前記円周状の内側方向に前記液滴を広げるように行うことが好ましい。 More specifically, the acidic solution film is formed by forming a droplet of the acidic solution circumferentially on the surface of the member, and then using the pipette tip to remove the droplet into the tip portion of the pipette tip. It is preferable that the liquid droplets are spread in the circumferential inner direction while tracing.
図３は、酸性溶液の膜を局所的に形成する工程の他の態様を説明するための上面図である。
図３においては、最初に、セラミックス部材１０の表面１０ａに、円周状に酸性溶液の液滴３０ｂを形成する（図３（ａ））。この円周状の液滴３０ｂの形成は、例えば、ピペットチップを用い、ピペットチップを倒して、前記表面１０ａ上をなぞりながら行う。
次に、ピペットチップを用いて、前記液滴３０ｂを該ピペットチップのチップ部でなぞりながら、前記円周状の内側方向に液滴３０ｂを広げるようにして膜を形成する（図３（ｂ））。
このような方法によれば、前記円周状の液滴を形成した際、該液滴を形成した部分の部材の表面は若干エッチングされるため、前記液滴がその外側方向に広がることなく、確実に、部材の表面を、局所的かつ効率的にエッチングすることが可能となる。
FIG. 3 is a top view for explaining another aspect of the step of locally forming the acidic solution film.
In FIG. 3, first, a droplet 30b of an acidic solution is formed circumferentially on the surface 10a of the ceramic member 10 (FIG. 3 (a)). The circumferential droplet 30b is formed by, for example, using a pipette tip, tilting the pipette tip, and tracing on the surface 10a.
Next, using a pipette tip, a film is formed by spreading the droplet 30b in the circumferential inner direction while tracing the droplet 30b on the tip portion of the pipette tip (FIG. 3B). ).
According to such a method, when the circumferential droplet is formed, the surface of the member in the portion where the droplet is formed is slightly etched, so that the droplet does not spread outwardly, It is possible to reliably and locally etch the surface of the member.
上記のようにして酸性溶液の膜を形成した後、所定時間放置して、前記酸性溶液により部材１０の表面１０ａの前記膜を形成した部分をエッチングし、金属不純物を抽出する。
After the acidic solution film is formed as described above, the film is left for a predetermined time, and the portion of the surface 10a of the
前記金属不純物の抽出液の回収は、図４に示すような方法で行うことができる。図４は、前記酸性溶液の膜により抽出した抽出液を回収する工程を説明するための断面図である。
図４に示すように、液滴３０ａ（３０ｂ）の膜が形成されたセラミックス部材１０の表面１０ａを傾け、膜状化した液滴３０ａ（３０ｂ）を、液滴状態に戻した状態（図４（ｂ））で、マイクロピペット（図示せず）を用いて、抽出液を回収する。
このような方法によれば、前記抽出液の回収の際、マイクロピペットのみを用いれば足り、操作性の点からも簡便であり、効率的に行うことができる。
The extraction of the metal impurity extract can be performed by a method as shown in FIG. FIG. 4 is a cross-sectional view for explaining a process of recovering the extract extracted by the acidic solution membrane.
As shown in FIG. 4, the surface 10a of the
According to such a method, it is sufficient to use only a micropipette when collecting the extract, which is simple from the viewpoint of operability and can be performed efficiently.
本発明においては、エッッチングのために使用する酸性溶液は、特に限定されず、塩酸、硫酸等を用いることができる。 In the present invention, the acidic solution used for etching is not particularly limited, and hydrochloric acid, sulfuric acid and the like can be used.
また、前記抽出液に含まれる金属不純物の分析は、高感度微量分析を迅速に行う観点から、ＩＣＰ−ＭＳやＦＬ−ＡＡを用いて行うことが好ましい。
このような装置分析によれば、１０10ａｔｏｍｓ／ｃｍ2オーダーでの高精度分析も可能である。
The analysis of metal impurities contained in the extract is preferably performed using ICP-MS or FL-AA from the viewpoint of promptly performing a highly sensitive microanalysis.
According to such an apparatus analysis, a high-precision analysis on the order of 10 10 atoms / cm 2 is also possible.
また、上記分析方法を用いることにより、同一領域を複数回繰り返しエッチングし、１回毎の抽出液に含まれる金属不純物量を求め、また、当該１回につきエッチングされたセラミックス部材の厚さと照合して、該部材表面からの深さ方向における不純物量分布も求めることもできる。 Further, by using the above analysis method, the same region is repeatedly etched several times, the amount of metal impurities contained in each extraction liquid is obtained, and the thickness of the ceramic member etched each time is checked. Thus, the impurity amount distribution in the depth direction from the surface of the member can also be obtained.
以下、本発明を実施例に基づきさらに具体的に説明するが、本発明は下記実施例により制限されるものではない。
［実施例１］
アルミナセラミックス製の平板の表面上に、濃度３．０％の塩酸２ｍｌをマイクロピペットにより滴下して、該表面上に液滴を形成した後、ピペットチップのチップ部で、該液滴を膜状化させた。
この状態で３分間保持し、前記平板の表面をエッチングした。その際、水平方向（該表面と平行な方向）に軽い振動を与え、前記平板の表面上のエッチング液（塩酸）の膜の移動の有無を観察したところ、形成された膜の位置は動かなかった。
その後、前記平板の表面を傾けて、マイクロピペットを用いて、エッチングした抽出液を回収したところ、約１．７ｍｌを回収することができた。
EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Example 1]
2 ml of 3.0% hydrochloric acid is dropped on the surface of a plate made of alumina ceramics with a micropipette to form a droplet on the surface, and then the droplet is formed into a film at the tip of the pipette tip. Made it.
This state was maintained for 3 minutes, and the surface of the flat plate was etched. At that time, when a slight vibration was given in the horizontal direction (direction parallel to the surface) and the presence or absence of the movement of the etching solution (hydrochloric acid) film on the surface of the flat plate was observed, the position of the formed film did not move. It was.
Then, when the surface of the flat plate was tilted and the extracted extract was recovered using a micropipette, about 1.7 ml could be recovered.
［実施例２］
アルミナセラミックス製の平板の表面上に、濃度３．０％の塩酸２ｍｌを１ｍｌずつ２回に分けて、マイクロピペットにより、該表面上を軽くなぞりながら、該表面上に直径約２インチの円周状の液滴を形成した後、ピペットチップを用いて、前記液滴をピペットチップのチップ部でなぞりながら、前記円周状の内側方向に該液滴を広げて、前記液滴を膜状化させた。
この状態で３分間保持し、前記平板の表面をエッチングした。その際、水平方向（該表面と平行な方向）に軽い振動を与え、前記平板の表面上のエッチング液（塩酸）の膜の移動の有無を観察したところ、形成された膜の位置は動かなかった。
その後、前記平板の表面を傾けて、マイクロピペットを用いて、エッチングした抽出液を回収したところ、約１．６ｍｌを回収することができた。
[Example 2]
On a surface of an alumina ceramic flat plate, 2 ml of hydrochloric acid with a concentration of 3.0% is divided into two 1 ml portions, and a micropipette is used to gently trace the circumference of the surface with a diameter of about 2 inches on the surface. After forming a droplet, the pipette tip is used to trace the droplet at the tip portion of the pipette tip, spreading the droplet in the circumferential inner direction, and forming the droplet into a film. I let you.
This state was maintained for 3 minutes, and the surface of the flat plate was etched. At that time, when a slight vibration was given in the horizontal direction (direction parallel to the surface) and the presence or absence of the movement of the etching solution (hydrochloric acid) film on the surface of the flat plate was observed, the position of the formed film did not move. It was.
Then, when the surface of the flat plate was tilted and the extracted extract was recovered using a micropipette, about 1.6 ml could be recovered.
［比較例１］
液滴を膜状化させず、それ以外は、実施例１と同様にして、前記平板の表面をエッチングした。その際、水平方向（該表面と平行な方向）に軽い振動を与え、液滴の移動の有無を観察したところ、液滴は最初に形成した位置から水平方向に移動したことが確認された。
[Comparative Example 1]
The surface of the flat plate was etched in the same manner as in Example 1 except that the droplet was not formed into a film. At that time, light vibration was applied in the horizontal direction (direction parallel to the surface) and the presence or absence of movement of the droplet was observed, and it was confirmed that the droplet moved in the horizontal direction from the position where it was first formed.
１０ セラミックス部材
２０ マイクロピペット
３０ 酸性溶液
10
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