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 PDFInfo
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- 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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- Prior art keywords
- fixture
- film material
- small size
- sample
- infrared spectrum
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- 239000010409 thin film Substances 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 22
- 238000010998 test method Methods 0.000 title abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 238000012360 testing method Methods 0.000 claims abstract description 22
- 239000002390 adhesive tape Substances 0.000 claims abstract description 18
- 239000005357 flat glass Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000004154 testing of material Methods 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 16
- 239000011521 glass Substances 0.000 abstract description 8
- 238000007747 plating Methods 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 229910007746 Zr—O Inorganic materials 0.000 description 5
- 238000002310 reflectometry Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Landscapes
- 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
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)
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
- 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.
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CN201711112949.0A CN107741407A (en) | 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 |
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CN201711112949.0A CN107741407A (en) | 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 |
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Cited By (5)
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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Cited By (7)
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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