CN107741407A - A kind of fixture and method of testing based on small size thin-film material examination of infrared spectrum - Google Patents

A kind of fixture and method of testing based on small size thin-film material examination of infrared spectrum Download PDF

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Publication number
CN107741407A
CN107741407A CN201711112949.0A CN201711112949A CN107741407A CN 107741407 A CN107741407 A CN 107741407A CN 201711112949 A CN201711112949 A CN 201711112949A CN 107741407 A CN107741407 A CN 107741407A
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CN
China
Prior art keywords
fixture
film material
small size
sample
infrared spectrum
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Pending
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CN201711112949.0A
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Chinese (zh)
Inventor
宁洪龙
蔡炜
姚日晖
陶瑞强
陈建秋
朱镇南
郑泽科
章红科
彭俊彪
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South China University of Technology SCUT
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South China University of Technology SCUT
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Priority to CN201711112949.0A priority Critical patent/CN107741407A/en
Publication of CN107741407A publication Critical patent/CN107741407A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention belongs to thin-film material analysis field, discloses a kind of fixture and method of testing based on small size thin-film material examination of infrared spectrum.The fixture is made up of the double faced adhesive tape in the metal substrate and metal substrate on sheet glass, sheet glass.The method for carrying out examination of infrared spectrum to small size thin-film material using above-mentioned fixture is as follows:Small size thin-film material testing sample is pasted on the double faced adhesive tape of the fixture, is then inverted in the fixture for being pasted with testing sample on the specimen holder of Shimadzu Fourier infrared spectrograph, testing sample is placed in specimen holder perforate middle position, you can to start to test.The present invention is with a kind of simple sample clamp, solve the problems, such as small size film sample sample for running into being tested using Shimadzu Fourier infrared spectrum drop, signal it is weak, and strengthen the test intensity of sample by plating layer of metal film on a glass substrate, there is very strong practicality.

Description

A kind of fixture and method of testing based on small size thin-film material examination of infrared spectrum
Technical field
The invention belongs to thin-film material analysis field, and in particular to one kind is based on small size thin-film material examination of infrared spectrum Fixture and method of testing.
Background technology
In modern thin-film material constituent analysis, infrared spectrum is in quantitative detection film functional group composition, thus it is speculated that forming thin film During have a wide range of applications.The characteristics of infra-red sepectrometry is:Quickly, sample size is few (several micrograms-several milligrams), and characteristic is strong (various materials have its specific infrared spectrogram), the sample of various states (gas, liquid, solid) can be analyzed and do not destroy sample. The principle of existing Fourier infrared spectrograph is:The light that light source is sent is divided into two beams by beam splitter (similar semi-transparent semi-reflecting lens), and one Shu Jing is transmitted to up to index glass, and another Shu Jing is reflexed to up to horizontal glass.Two-beam returns beam splitter through horizontal glass and index glass reflection respectively, Index glass is for linear motion with a constant speed, thus the two-beam after beam splitter beam splitting forms optical path difference, produces interference.Interference Light, by sample cell, reaches detector by the interference light containing sample message after sample, then passed through after beam splitter congregation Fourier transform pairs signal is handled, and finally gives transmitance or absorbance with wave number or the infrared absorpting light spectra of wavelength.
Film in reflection absorption spectrum method energy high sensitivity measuring metallic substrates, when polarizing light irradiation is in metallic substrates On, when being reflected in metal surface, its phase can change.In the case of orthogonal polarized light, mutually it is changed into about 180 °, with Incidence angle is unrelated, therefore the vector of reflected light cancels each other, and standing wave amplitude is almost nil, can't detect the absorption of sample.In water In the case of flat polarised light, the continuous change of phase changes to 90 ° from 0 °, and standing wave amplitude equally changes with incidence angle.Work as selection Standing wave amplitude increase during big incidence angle, the effect enhancing of light beam and sample, so as to produce high detection sensitivity.Metallic reflection Rate is higher, therefore this method can detect the film on metal with sensitivity.
In practical operation, (the light path principle figure of its sample test such as Fig. 1 institutes by taking Shimadzu IR series RAS8000 (A) as an example Show, M in figure1~M6For speculum), as can be seen from Figure 1, because light source is under, sample surface should be placed down.Actually equipment There is sample cell with holes to be used to place sample, sample cell there are tri- kinds of specifications of Ф 8/15/25mm, in hollow circular hole.Preferable sample is Film in metal substrate, and substrate dimension have to be larger than Ф 8mm, therefore too small sample will fall off, and can not test.This is to a variety of The sample test prepared on different type substrate brings certain difficulty.
The content of the invention
In place of shortcoming and defect existing for above prior art, primary and foremost purpose of the invention is that providing one kind is based on The fixture of small size thin-film material examination of infrared spectrum.
Another object of the present invention is to provide a kind of method based on small size thin-film material examination of infrared spectrum.
The object of the invention is achieved through the following technical solutions:
A kind of fixture based on small size thin-film material examination of infrared spectrum, by the metal substrate on sheet glass, sheet glass Formed with the double faced adhesive tape in metal substrate.
Further, the size of the sheet glass is 30mm*30mm~50mm*50mm.
Further, the thickness of the metal substrate is 50~150nm.Aluminium, silver, copper etc. can be selected in the material of metal substrate The high metal of reflectivity.
Further, the double faced adhesive tape is located at metal substrate center.
Further, the size of the double faced adhesive tape is less than 2mm*2mm.
A kind of method based on small size thin-film material examination of infrared spectrum, comprises the following steps:
Small size thin-film material testing sample is pasted on the double faced adhesive tape of above-mentioned fixture, then will be pasted with testing sample Fixture be inverted on the specimen holder of Shimadzu Fourier infrared spectrograph, testing sample is placed in specimen holder perforate middle position, It can start to test.
Further, the size of the small size thin-film material is 2mm*2mm~20mm*20mm.
The present invention principle be:By sample being bonded at below the fixture with metal substrate so that small sample is not Directly it can be fallen down from specimen holder tapping, and infrared light directly acts on sample surfaces, fixture has metal substrate in addition, so as to have Larger reflectivity, it is ensured that sample signal intensity is sufficiently high.
The invention has the advantages that and beneficial effect:
The present invention solves small size film sample and is using Shimadzu fourier infrared light with a kind of simple sample clamp The problem of sample run into spectrum test drops, signal is weak, test size scope is extended to not less than area of section 2mm*2mm Sample, and strengthen the test intensity of sample by plating layer of metal film on a glass substrate, there is very strong practicality.
Brief description of the drawings
Fig. 1 is the light path principle figure of Shimadzu IR series RAS8000 (A) sample test.
Fig. 2 is that a kind of fixture based on small size thin-film material examination of infrared spectrum in inventive embodiments 1 pastes sample Structural representation;Numbering is described as follows in figure:1- sheet glass, 2- metal substrates, 3- double faced adhesive tapes, 4- samples.
Fig. 3 is to be tested using the fixture in embodiment 1 in Shimadzu IR series RAS8000 (A) Fourier infrared spectrograph The result figure of zirconia film sample.
Fig. 4 is to be tested using the fixture in comparative example 1 in Shimadzu IR series RAS8000 (A) Fourier infrared spectrograph The result figure of zirconia film sample.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment 1
A kind of fixture based on small size thin-film material examination of infrared spectrum of the present embodiment, it is pasted the structure of sample and shown It is intended to as shown in Figure 2.It is made up of the double faced adhesive tape 3 in the metal substrate 2 and metal substrate on sheet glass 1, sheet glass, double faced adhesive tape 3 It is upper to be used to paste sample 4.Wherein sheet glass size is 30mm*30mm, and metal substrate is that thickness is 100nm without graphical aluminium film, Double faced adhesive tape coverage rate is 1mm*1mm.The preparation method and the use fixture of the present embodiment fixture are carried out to small size thin-film material The method of examination of infrared spectrum is as follows:
(1) 30mm*30mm sheet glass is cut;
(2) sheet glass obtained by step (1) is taken, one layer of 100nm is deposited without graphical aluminium film as metal substrate, by aluminium film face It is positioned over down on instrument sample seat and is used as background scans;
(3) it is 1mm*1mm in metal substrate intermediate region sticking two-faced adhesive tape, double faced adhesive tape coverage rate, obtains described based on small The fixture of size thin-film material examination of infrared spectrum;
(4) take step (3) to paste the fixture of double faced adhesive tape, 100nm aluminium plated on the glass of 10mm*10mm cross-sectional sizes, Then spin coating zirconia film prepares sample on aluminium, will be bonded at outside specimen face side on the double faced adhesive tape of fixture;
(5) fixture that step (4) is stained with to testing sample is inverted in Shimadzu IR series RAS8000 (A) fourier infrared light Specification is on Ф 25mm specimen holder in spectrometer, testing sample is placed in specimen holder perforate middle position, you can to start to test.Survey Test result is as shown in figure 3, can be observed-Zr-O in Fig. 3 ,-O-O ,-C-O ,-OH peaks, and peak intensity is big.
Comparative example 1
Compared with Example 1, the non-deposition of aluminum film of fixture is as metal substrate.Gained fixture uses similarly to Example 1 Sample and method are tested.As a result as shown in figure 4, Fig. 4 to can be observed sample-Zr-O characteristic peaks weak, illustrate substrate reflectivity It is not high.
It can be placed not less than section using fixture of the present invention it can be seen from the result of embodiment 1 and comparative example 1 Area 2mm*2mm sample, and the metal film enhancing reflectivity on fixture, can make it that reception signal is stronger, peak position is more obvious. It can be observed-Zr-O ,-O-O ,-C-O in Fig. 3 ,-OH peaks, peak intensity is big.Can be observed in Fig. 4 test result sample characteristic peak- Zr-O is weaker, and O-O peaks are also very weak, is covered substantially by-Zr-O, caused by the non-metal-coated membrane of its substrate causes reflectivity not high.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (7)

  1. A kind of 1. fixture based on small size thin-film material examination of infrared spectrum, it is characterised in that:By on sheet glass, sheet glass Double faced adhesive tape in metal substrate and metal substrate is formed.
  2. A kind of 2. fixture based on small size thin-film material examination of infrared spectrum according to claim 1, it is characterised in that: The size of the sheet glass is 30mm*30mm~50mm*50mm.
  3. A kind of 3. fixture based on small size thin-film material examination of infrared spectrum according to claim 1, it is characterised in that: The thickness of the metal substrate is 50~150nm;The material of metal substrate is aluminium, silver or copper.
  4. A kind of 4. fixture based on small size thin-film material examination of infrared spectrum according to claim 1, it is characterised in that: The double faced adhesive tape is located at metal substrate center.
  5. A kind of 5. fixture based on small size thin-film material examination of infrared spectrum according to claim 1, it is characterised in that: The size of the double faced adhesive tape is less than 2mm*2mm.
  6. A kind of 6. method based on small size thin-film material examination of infrared spectrum, it is characterised in that comprise the following steps:
    Small size thin-film material testing sample is pasted on the double faced adhesive tape of any one of Claims 1 to 5 fixture, then will The fixture for being pasted with testing sample is inverted on the specimen holder of Shimadzu Fourier infrared spectrograph, testing sample is placed in specimen holder Perforate middle position, you can start to test.
  7. A kind of 7. method based on small size thin-film material examination of infrared spectrum according to claim 6, it is characterised in that: The size of the small size thin-film material is 2mm*2mm~10mm*10mm.
CN201711112949.0A 2017-11-13 2017-11-13 A kind of fixture and method of testing based on small size thin-film material examination of infrared spectrum Pending CN107741407A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579432A (en) * 2019-09-24 2019-12-17 南京工业大学 Dual-purpose sealing assembly and operation method
CN112505081A (en) * 2020-11-18 2021-03-16 中国科学院生态环境研究中心 Sample preparation method for hollow fiber membrane ToF-SIMS test
CN113109375A (en) * 2021-03-16 2021-07-13 合肥波林新材料股份有限公司 Thin-film material scanning electron microscope cross section sample preparation clamp and sample preparation method thereof
CN113176219A (en) * 2021-04-30 2021-07-27 福建师范大学 Variable magnetic field-based film optical performance measuring system
WO2022020930A1 (en) * 2020-07-30 2022-02-03 Universidade Federal de Uberlândia Sample platform for use in infrared spectroscopy, system, kit, method and use thereof

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CN207516241U (en) * 2017-11-13 2018-06-19 华南理工大学 A kind of fixture based on small size thin-film material examination of infrared spectrum

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JP2012086661A (en) * 2010-10-19 2012-05-10 Kira Shiko:Kk Heat shielding interior trim material
CN104406773A (en) * 2014-12-02 2015-03-11 中国航天科工集团第三研究院第八三五八研究所 Method for measuring optical constant of Gel-xCx thin film infrared spectroscopy area
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CN207516241U (en) * 2017-11-13 2018-06-19 华南理工大学 A kind of fixture based on small size thin-film material examination of infrared spectrum

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579432A (en) * 2019-09-24 2019-12-17 南京工业大学 Dual-purpose sealing assembly and operation method
WO2022020930A1 (en) * 2020-07-30 2022-02-03 Universidade Federal de Uberlândia Sample platform for use in infrared spectroscopy, system, kit, method and use thereof
CN112505081A (en) * 2020-11-18 2021-03-16 中国科学院生态环境研究中心 Sample preparation method for hollow fiber membrane ToF-SIMS test
CN113109375A (en) * 2021-03-16 2021-07-13 合肥波林新材料股份有限公司 Thin-film material scanning electron microscope cross section sample preparation clamp and sample preparation method thereof
CN113109375B (en) * 2021-03-16 2022-09-16 合肥波林新材料股份有限公司 Thin-film material scanning electron microscope cross section sample preparation clamp and sample preparation method thereof
CN113176219A (en) * 2021-04-30 2021-07-27 福建师范大学 Variable magnetic field-based film optical performance measuring system
CN113176219B (en) * 2021-04-30 2023-07-18 福建师范大学 Film optical performance measurement system based on variable magnetic field

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