JP2017083281A - Method for forming stage for micro-spectroscopic analysis - Google Patents
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- 238000004611 spectroscopical analysis Methods 0.000 title abstract description 3
- 238000000034 method Methods 0.000 title description 12
- 239000000463 material Substances 0.000 claims abstract description 24
- 230000003287 optical effect Effects 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000004458 analytical method Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 150000002170 ethers Chemical class 0.000 claims description 5
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- -1 silane compound Chemical class 0.000 claims description 4
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 claims description 3
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims description 3
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 238000001634 microspectroscopy Methods 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 238000010183 spectrum analysis Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 239000005871 repellent Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 2
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000002042 time-of-flight secondary ion mass spectrometry Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
Description
本発明は、マイクロ分光分析用試料台の作製方法に関する。 The present invention relates to a method for manufacturing a sample stage for microspectral analysis.
例えば、顕微ＦＴＩＲ（フーリエ変換赤外分光光度計）などを用いたマイクロ分光分析法は、微小かつ微量の有機物の定性分析にとって有効な手法である。例えば、顕微ＦＴＩＲで定性分析を行う際、測定する試料の厚さが最適な状態でなければ、正常なＦＴＩＲスペクトルを得ることができないので、正常なＦＴＩＲスペクトルを得るための試料調製は重要となる。例えば、希薄な溶液試料の顕微ＦＴＩＲを行う場合、従来は、特許文献１、２に開示されているように、サンプル台の赤外線反射部材に付されたフッ素樹脂の薄膜上に、溶媒に試料を含ませた溶液の凝縮核となるピンホールを形成し、そのピンホールについて顕微ＦＴＩＲで測定して、微量の希薄溶液の溶質に関する成分情報を得ていた。
For example, a micro-spectroscopic analysis method using a microscopic FTIR (Fourier transform infrared spectrophotometer) or the like is an effective technique for qualitative analysis of minute and minute organic substances. For example, when performing qualitative analysis by microscopic FTIR, a normal FTIR spectrum cannot be obtained unless the thickness of the sample to be measured is in an optimal state, and therefore, sample preparation for obtaining a normal FTIR spectrum is important. . For example, when performing microscopic FTIR of a dilute solution sample, conventionally, as disclosed in
しかしながら、当該手法では凝集核の厚さが厚く、得られるＦＴＩＲスペクトルは全体的に飽和状態となってしまい、成分を定性するため実施されるスペクトル解析に大きな支障を来たす場合に特許文献３に開示されている方法で凝集核の厚みを調節する場合、凝集核が治具に付着して分析できなくなってしまう点や特許文献４に開示されているような部材に付されたフッ素樹脂が塗布されている基板ではフッ素樹脂の薄膜が破壊しやすい点が欠点である。
However, in this method, the thickness of the aggregated nuclei is large, and the obtained FTIR spectrum is saturated as a whole, which is disclosed in
上記課題を解決するため、本発明は以下の構成からなる。つまり
（１）撥水性または撥油性を有する下記構造式（I）で表わされるパーフルオロアルキルポリエーテル基含有シラン化合物を溶媒に溶解してなる液に光学材料を浸漬させ、浸漬後に光学材料を加熱し、次いで光学材料を洗浄して、光学材料の表面が撥水性または撥油性に改質されていることを特徴とする光学材料を用いたマイクロ分光分析用試料台の作製方法、
In order to solve the above problems, the present invention has the following configuration. That is, (1) an optical material is immersed in a solution obtained by dissolving a perfluoroalkyl polyether group-containing silane compound represented by the following structural formula (I) having water repellency or oil repellency in a solvent, and the optical material is heated after the immersion. Then, the optical material is washed, and the surface of the optical material is modified to be water-repellent or oil-repellent. A method for producing a sample stage for micro-spectral analysis using an optical material,
ここで、ａは１〜３０の整数、ｂは１〜１０の整数、ｃは１〜２０の整数、ｄは１〜１０の整数、ｅは１〜２０の整数、ｈは０〜１０の整数、ｇは０〜２０の整数、ｎは１〜３２０の整数であり、ｍおよびｐの和は３である。
（２）前記光学材料が、シリコン、ゲルマニウム、サファイア、フッ化カルシウム、フッ化バリウム、セレン化亜鉛、およびダイヤモンドから選ばれる１種以上を含む（１）または（２）に記載のマイクロ分光分析用試料台の作製方法、
（３）前記光学材料の改質されている側の表面に、幅０．０１〜１mmかつ深さ０．００１〜０．１ｍｍの溝、または、直径０．０１〜１ｍｍかつ深さ０．００１〜０．１ｍｍの凹みがある（１）または（２）に記載のマイクロ分光分析用試料台の作製方法、
（４）前記溶媒が、アルコール類、ケトン類、エーテル類、アルデヒド類、アミン類、脂肪酸類、エステル類およびニトリル類から選ばれる１種以上を含むものであり、かつ、該溶媒はフッ素変性されたものである（１）〜（３）のいずれかに記載のマイクロ分光分析用試料台の作製方法、である。
Here, a is an integer of 1-30, b is an integer of 1-10, c is an integer of 1-20, d is an integer of 1-10, e is an integer of 1-20, h is an integer of 0-10. , G is an integer of 0-20, n is an integer of 1-320, and the sum of m and p is 3.
(2) The optical material includes one or more selected from silicon, germanium, sapphire, calcium fluoride, barium fluoride, zinc selenide, and diamond, for microspectral analysis according to (1) or (2) A method for preparing a sample stage,
(3) A groove having a width of 0.01 to 1 mm and a depth of 0.001 to 0.1 mm, or a diameter of 0.01 to 1 mm and a depth of 0.001 on the surface of the optical material that has been modified. A method for producing a sample stage for microspectral analysis according to (1) or (2), which has a dent of ~ 0.1 mm,
(4) The solvent contains at least one selected from alcohols, ketones, ethers, aldehydes, amines, fatty acids, esters and nitriles, and the solvent is fluorine-modified. A method for producing a sample stage for microspectroscopy analysis according to any one of (1) to (3).
本発明により、たとえば、所望の撥水性、撥油性を有するパーフルオロアルキルエーテル基よりなる薄膜を光学材料の表面に容易に形成することができたプレートで、マイクロ分光分析における濃縮操作を簡便かつより正確に行うことができる。 According to the present invention, for example, a plate capable of easily forming a thin film made of a perfluoroalkyl ether group having desired water repellency and oil repellency on the surface of an optical material. Can be done accurately.
以下、本発明を説明する。 The present invention will be described below.
まず、本発明における撥水性または撥油性を有する化合物としては、下記構造式（Ｉ）で表わされるパーフルオロアルキルポリエーテル基含有シラン化合物が好ましく例示される。 First, as the compound having water repellency or oil repellency in the present invention, a perfluoroalkyl polyether group-containing silane compound represented by the following structural formula (I) is preferably exemplified.
ここで、ａは１〜３０の整数、ｂは１〜１０の整数、ｃは１〜２０の整数、ｄは１〜１０の整数、ｅは１〜２０の整数、ｈは０〜１０の整数、ｇは０〜２０の整数、ｎは１〜３２０の整数である。ｍとｐの和は３である。 Here, a is an integer of 1-30, b is an integer of 1-10, c is an integer of 1-20, d is an integer of 1-10, e is an integer of 1-20, h is an integer of 0-10. , G is an integer of 0-20, and n is an integer of 1-320. The sum of m and p is 3.
本発明における溶媒としては、アルコール類、ケトン類、エーテル類、アルデヒド類、アミン類、脂肪酸類、エステル類およびニトリル類があげられ、かつ、フッ素変性されたものが好ましい。さらに、フッ素変性エーテル類、フッ素変性アルコール類が好ましく、エーテル類、アルコール類は炭素数２〜２０のものが最も好ましい。 Examples of the solvent in the present invention include alcohols, ketones, ethers, aldehydes, amines, fatty acids, esters and nitriles, and those which are fluorine-modified are preferred. Further, fluorine-modified ethers and fluorine-modified alcohols are preferable, and ethers and alcohols having 2 to 20 carbon atoms are most preferable.
撥水性または撥油性を有する化合物を溶媒に溶解してなる液の溶液濃度は０．００１〜１０質量％、さらに０．０１〜１質量％が好ましい。 The solution concentration of a solution obtained by dissolving a compound having water repellency or oil repellency in a solvent is preferably 0.001 to 10% by mass, more preferably 0.01 to 1% by mass.
本発明における表面改質の方法として、ディップ処理またはスピンコートが例示され、なかでもディップ処理で表面改質するのが好ましい。本発明における光学材料としては、赤外線の吸収が少なく、かつ、溝、凹みを容易に加工できる材料が好ましく、シリコン、ゲルマニウム、サファイア、フッ化カルシウム、フッ化バリウム、セレン化亜鉛、およびダイヤモンドが例示される。なかでもシリコンが好ましい。処理対象である光学材料の表面を予め研磨して鏡面仕上げをしておき、試料の厚みを抑制するために、溝または凹みを予め設ける加工をしておくと、簡便、かつ正確に濃縮操作を行うことができる。表面を予め研磨して鏡面に仕上げ、さらに溶液試料を濃縮する側の表面に、表面に、幅０．０１〜１mmかつ深さ０．００１〜０．１ｍｍの溝、または、直径０．０１〜１ｍｍかつ深さ０．００１〜０．１ｍｍの凹みを設けることが好ましい。 Examples of the surface modification method in the present invention include dip treatment or spin coating, and it is preferable to modify the surface by dip treatment. As the optical material in the present invention, a material that absorbs less infrared rays and can easily process grooves and dents is preferable, and examples include silicon, germanium, sapphire, calcium fluoride, barium fluoride, zinc selenide, and diamond. Is done. Of these, silicon is preferable. If the surface of the optical material to be processed is polished in advance to give a mirror finish, and processing to provide grooves or dents in advance to reduce the thickness of the sample, the concentration operation can be performed easily and accurately. It can be carried out. The surface is polished in advance to give a mirror surface. Further, on the surface on which the solution sample is concentrated, a groove having a width of 0.01 to 1 mm and a depth of 0.001 to 0.1 mm, or a diameter of 0.01 to It is preferable to provide a recess having a depth of 1 mm and a depth of 0.001 to 0.1 mm.
前記光学材料を前記処理液中に浸漬した後、該光学材料を、加熱して乾燥する。 After the optical material is immersed in the processing solution, the optical material is heated and dried.
本発明において光学材料を加熱するとは、８０℃から１５０℃で３０分間から３時間に保つことをいう。さらには９０℃から１１０℃で３０分間から１時間に保つことが好ましい。 In the present invention, heating the optical material means maintaining at 80 to 150 ° C. for 30 minutes to 3 hours. Furthermore, it is preferable to maintain at 90 to 110 ° C. for 30 minutes to 1 hour.
以下、本発明を実施例で説明する。 Hereinafter, the present invention will be described with reference to examples.
まず、撥水性または撥油性を有する化合物として、パーフルオロアルキルポリエーテル基含有シラン化合物 First, as a compound having water repellency or oil repellency, a silane compound containing a perfluoroalkyl polyether group
のエチルノナフルオロブチルエーテル０．１質量％、つまり、ＤＳ−５２１０ＴＨ（株式会社ハーベスト製）を使用した。ここで、上記化学式における平均重合度（上記構造式（I）におけるn=32）は、19F NMRから計算した値である。 Of ethyl nonafluorobutyl ether 0.1% by mass, that is, DS-5210TH (manufactured by Harvest Co., Ltd.) was used. Here, the average degree of polymerization in the above chemical formula (n = 32 in the above structural formula (I)) is a value calculated from 19 F NMR.
表面を予め研磨して鏡面を仕上げ、さらに溶液試料を濃縮する側の表面に幅が０．１ｍｍ、深さ０．００５ｍｍの溝のあるシリコンを上記溶液に浸漬させ、浸漬後、シリコンを１００℃で１時間加熱乾燥した。乾燥後、残留したＤＳ−５２１０ＨをＤＳ−ＴＨ（株式会社ハーベスト製）で洗浄除去した。 The surface is polished in advance to finish a mirror surface. Further, silicon having a groove having a width of 0.1 mm and a depth of 0.005 mm is immersed in the above solution on the surface on which the solution sample is concentrated. And dried for 1 hour. After drying, the remaining DS-5210H was removed by washing with DS-TH (manufactured by Harvest Co., Ltd.).
以上の処理により、溝のないシリコンの表面は撥水性、撥油性を有する性質に改質され、実際に5 mm□の領域で、分析深さ１〜数ｎｍの飛行時間型二次イオン質量分析法（ＴＯＦ−ＳＩＭＳ）によるイオンイメージ像で、ＳｉＯ３Ｈイオン、Ｃ３Ｆ５Ｏ２イオン、Ｃ３Ｆ７Ｏイオンなど撥水作用を有する分子構造が均一に存在していることを確認した。 Through the above processing, the surface of the silicon without grooves is modified to have water and oil repellency, and the time-of-flight secondary ion mass spectrometry with an analysis depth of 1 to several nm is actually performed in the 5 mm square region. It was confirmed by the ion image by the method (TOF-SIMS) that a molecular structure having a water-repellent action such as SiO 3 H ion, C 3 F 5 O 2 ion, C 3 F 7 O ion was uniformly present. .
図２における曲線は、大豆油１０００ｎｇを撥水処理したシリコン上で濃縮させてなる試料を用いて透過法による赤外分光分析を行ったときのＦＴＩＲスペクトルであり、図３における曲線は、大豆油１０００ｎｇを赤外線反射部材に付されたフッ素樹脂の薄膜上で濃縮させてなる試料を用いて、反射法による赤外分光分析を行なったときのＦＴＩＲスペクトルを示すものである。 The curve in FIG. 2 is an FTIR spectrum when infrared spectroscopic analysis is performed by a transmission method using a sample obtained by concentrating 1000 ng of soybean oil on water-repellent treated silicon. The curve in FIG. The FTIR spectrum is shown when infrared spectroscopic analysis is performed by a reflection method using a sample obtained by concentrating 1000 ng on a fluororesin thin film attached to an infrared reflecting member.
図２から、７００〜４０００ｃｍ−１の全ての領域において、図３に比べ良好なスペクトルが得られた。 From FIG. 2, a favorable spectrum was obtained compared with FIG. 3 in all regions of 700 to 4000 cm −1 .
比較例
図４における曲線は、大豆油１００μｇをダイヤモンド板に付着させて赤外分光分析を行なったときのＦＴＩＲスペクトルであり、これは試料量が多く採れる場合に行なう方法である。
Comparative Example The curve in FIG. 4 is an FTIR spectrum when infrared spectroscopic analysis is performed with 100 μg of soybean oil attached to a diamond plate, which is a method performed when a large amount of sample can be taken.
図２は、試料量が多く採れる場合に行なう方法で測定されたＦＴＩＲスペクトルとほとんど同じ良好な結果であった。 FIG. 2 shows almost the same good results as the FTIR spectrum measured by the method performed when a large amount of sample can be taken.
１：表面改質部
２：光学材料
３：試料
４：溝
５：検出器
６：赤外線
1: Surface modification part 2: Optical material 3: Sample 4: Groove 5: Detector 6: Infrared ray
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| JP2015211480A JP6519444B2 (en) | 2015-10-28 | 2015-10-28 | Method of preparing sample stand for microspectroscopic analysis |
| KR1020177022013A KR101824948B1 (en) | 2015-04-02 | 2016-03-07 | Preparation method of sample for micro spectrometry |
| CN201680009345.0A CN107430059B (en) | 2015-04-02 | 2016-03-07 | The production method of microspectroscopy sample table |
| EP16772105.9A EP3279639B1 (en) | 2015-04-02 | 2016-03-07 | Method of fabricating sample stage for microspectrometric analysis |
| US15/562,985 US20180111156A1 (en) | 2015-04-02 | 2016-03-07 | Method of fabricating sample stage for microspectrometric analysis |
| PCT/JP2016/056993 WO2016158221A1 (en) | 2015-04-02 | 2016-03-07 | Method of fabricating sample stage for microspectrometric analysis |
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| JPH063267A (en) * | 1992-06-20 | 1994-01-11 | Horiba Ltd | Method and device for detecting organic compound |
| JP2008203020A (en) * | 2007-02-19 | 2008-09-04 | Toppan Printing Co Ltd | Microspectroscopic method |
| JP2010175338A (en) * | 2009-01-28 | 2010-08-12 | Kanagawa Acad Of Sci & Technol | Specimen target used in mass spectroscopy, method for manufacturing the same, and mass spectroscope using such specimen target |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH063267A (en) * | 1992-06-20 | 1994-01-11 | Horiba Ltd | Method and device for detecting organic compound |
| JP2008203020A (en) * | 2007-02-19 | 2008-09-04 | Toppan Printing Co Ltd | Microspectroscopic method |
| JP2010175338A (en) * | 2009-01-28 | 2010-08-12 | Kanagawa Acad Of Sci & Technol | Specimen target used in mass spectroscopy, method for manufacturing the same, and mass spectroscope using such specimen target |
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