CN104390996A - Test analysis method for elementary composition and structure on carbon fiber surface - Google Patents
Test analysis method for elementary composition and structure on carbon fiber surface Download PDFInfo
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- CN104390996A CN104390996A CN201410641498.XA CN201410641498A CN104390996A CN 104390996 A CN104390996 A CN 104390996A CN 201410641498 A CN201410641498 A CN 201410641498A CN 104390996 A CN104390996 A CN 104390996A
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Abstract
The invention belongs to the technical field of analysis test and relates to a test analysis method for elementary composition and structure on a carbon fiber surface. The method comprises the following steps: using an X-ray photoelectron spectrometer, preparing a test sample, testing the sample, performing data processing, thereby obtaining the elementary composition and structure on the carbon fiber surface. The method is characterized in that in the step of preparing the test sample, monofilaments are taken as test samples which are suspended on a sample stage; and in the step of testing the sample, X rays are irradiated to each single sample, and the signals are acquired for several times. According to the method, the defect that a multiple-peak form or severe peak shift occurs in the conventional beam sample test result is overcome, the test precision is improved, the elementary composition and structure on the carbon fiber surface can be accurately detected, and the method is particularly suitable for testing polyacrylonitrile-based carbon fibers or asphalt-based carbon fibers.
Description
Technical field
The invention belongs to the technical field of analytical test, in particular to the accurate method of testing detecting element the Nomenclature Composition and Structure of Complexes x-ray photoelectron power spectrum (XPS) of carbon fiber surface, this analytical approach is applicable to polyacrylonitrile (PAN) base carbon fibre and asphalt base carbon fiber.
Background technology
Polyacrylonitrile (PAN) base carbon fibre occupies very important status in the carbon fibers, in national defence such as space flight and aviation, weapons, boats and ships, there is irreplaceable effect, be also widely used in the civil areas such as high-end sports goods, industry and transport.But the interfacial adhesion of not surface treated carbon fiber and resin matrix is poor, causes the interlaminar shear strength of compound substance low, limit the widespread use of carbon fibre composite.Research finds, the interface binding power between carbon fiber and resin depends primarily on the surface nature of carbon fiber, the configuration of surface of such as fiber, the character of surface functional group and number etc.Wherein the kind of surface functional group and number have very important effect for the interfacial adhesion state of carbon fibre composite.Therefore, the accurately element the Nomenclature Composition and Structure of Complexes of test carbon fiber surface, significant to the kind and number analyzing surface functional group.
X-ray photoelectron power spectrum (XPS) test on current PAN base carbon fibre surface is all measure with a synnema, through testing the process of sample preparation, sample test and data processing.Described test sample preparation adheres on sample stage by the whole bundle of multifibres sample test sample; Sample test be radiation exposure on a branch of sample, signals collecting is once.During test, X ray gets to the tow not in same plane, and multimodal and serious peak move to cause test result to occur.As Fig. 1, be domestic PAN base carbon fibre sample 1 one synnema XPS test result, because result is inaccurate, so do not provide swarming result.In some experimental result, though only occur a C-C peak, but peak width is also wider, do not get rid of multiple sample interact peak position superposition possibility.Be difficult to realize the accurate detection to carbon fiber surface element the Nomenclature Composition and Structure of Complexes, therefore also cannot realize the accurate analysis to PAN base carbon fibre surface functional group.
Summary of the invention
The technical problem to be solved in the present invention overcomes the inaccurate difficult problem of result that may occur when PAN base carbon fibre one synnema XPS tests; During this method test, individual carbon fibers is fixed on customized sample frame, accurately measures the XPS on individual carbon fibers surface, provide the method for testing of the precise results of carbon fiber surface element the Nomenclature Composition and Structure of Complexes.
A method for testing and analyzing for carbon fiber surface element the Nomenclature Composition and Structure of Complexes, uses x-ray photoelectron spectroscopy, through test sample preparation, sample test and data processing, obtains carbon fiber surface element the Nomenclature Composition and Structure of Complexes; It is characterized in that, described test sample preparation, is take monofilament as test sample, unsettled placement on sample stage; Described sample test, be roentgenogram on single sample, signals collecting 6 ~ 15 times.
The process of sample test and data processing is the same with existing conventional testing procedures and data handling procedure.
Carbon fiber of the present invention is PAN-based carbon fiber or asphalt base carbon fiber.
The test result that beneficial effect of the present invention in avoiding conventional pencil sample occurs improving the shortcoming that multimodal or serious peak move measuring accuracy, realize the accurate detection to carbon fiber surface element the Nomenclature Composition and Structure of Complexes.The XPS device (x-ray photoelectron power spectrum equipment) that application claims accurately measures individual carbon fibers surface-element the Nomenclature Composition and Structure of Complexes has higher sensitivity and resolution.
Accompanying drawing explanation
Fig. 1 is the C that prior art detects domestic carbon fibre one synnema
1SxPS spectrum figure.
Fig. 2 is specimen holder structural representation of the present invention.
Fig. 3 is the XPS spectrum figure of the domestic carbon fibre sample 1 monofilament surface full scan of embodiment 1.
Fig. 4 is the C of domestic carbon fibre sample 1 monofilament of embodiment 1
1Sthe XPS spectrum figure of swarming.
Embodiment
Embodiment 1
The ESCALAB 250 model x-ray photoelectron spectroscopy that the present embodiment uses U.S.'s thermoelectricity to produce is tested, and this energy spectrometer is equipped with Watt microfocus x-ray monochromator, hyperchannel plate electron-multiplier.Fig. 2 provides a kind of specimen holder for method of testing of the present invention.The middle part of specimen holder is fluted, and the two ends of test sample are fixed on the bossing at specimen holder two ends, makes monofilament measure the middle tested part of sample unsettled.The two ends of described test sample are fixed on the bossing at specimen holder two ends, with common glue (as gummed paper, adhesive tape, transparent adhesive tape, double faced adhesive tape etc.), test sample monofilament can be bonded at specimen holder.3 monofilament test samples have been drawn in Fig. 2.
Select five kinds of domestic PAN base carbon fibres to be example, test sample is numbered sample 1, sample 2, sample 3, sample 4, sample 5 respectively.Each single test sample is fixed on the specimen holder as Fig. 2.
Sample test is that ray impinges upon on single sample, the signals collecting of every root monofilament 10 times.
Full spectrum and the C of domestic carbon fibre is obtained after test
1Sspectrogram, and to C
1Sspectrogram carries out swarming, as Fig. 3, Fig. 4.To C
1Sthe analysis result of spectrogram, in table 1.
The C of table 1 domestic carbon fibre monofilament
1Sspectrum elucidation result.
As can be seen from table 1, Fig. 3, Fig. 4 compared to Figure 1, the Nomenclature Composition and Structure of Complexes analysis of the carbon fiber surface surface element measured by the present invention is more accurate.
Embodiment 2
Embodiment 1 is tested sample and replaces with asphalt base carbon fiber, test process is also completely applicable.
Claims (2)
1. a method for testing and analyzing for carbon fiber surface element the Nomenclature Composition and Structure of Complexes, uses x-ray photoelectron spectroscopy, through test sample preparation, sample test and data processing, obtains carbon fiber surface element the Nomenclature Composition and Structure of Complexes; It is characterized in that, described test sample preparation, is be measure sample, unsettled placement on sample stage with monofilament; Described sample test, be roentgenogram on single sample, signals collecting 6 ~ 15 times.
2. the method for testing and analyzing of carbon fiber surface element the Nomenclature Composition and Structure of Complexes according to claim 1, is characterized in that, described carbon fiber is PAN-based carbon fiber or asphalt base carbon fiber.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410641498.XA CN104390996A (en) | 2014-11-12 | 2014-11-12 | Test analysis method for elementary composition and structure on carbon fiber surface |
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| CN201410641498.XA CN104390996A (en) | 2014-11-12 | 2014-11-12 | Test analysis method for elementary composition and structure on carbon fiber surface |
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| CN104390996A true CN104390996A (en) | 2015-03-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198593A (en) * | 2016-07-06 | 2016-12-07 | 天津工业大学 | A kind of method of accurate sign γ irradiation carbon fiber microstructure |
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| US5209975A (en) * | 1989-10-30 | 1993-05-11 | Tonen Kabushiki Kaisha | High elongation, high strength pitch-type carbon fiber |
| CN102459728A (en) * | 2009-06-10 | 2012-05-16 | 三菱丽阳株式会社 | Carbon fiber bundle that develops excellent mechanical performance |
| CN102661963A (en) * | 2012-06-01 | 2012-09-12 | 吉林大学 | Special X-ray diffraction and scattering analysis device for fiber material |
| CN104011288A (en) * | 2011-12-27 | 2014-08-27 | 东丽株式会社 | Carbon fiber coated with sizing agent, process for producing carbon fiber coated with sizing agent, prepreg, and carbon fiber reinforced composite material |
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2014
- 2014-11-12 CN CN201410641498.XA patent/CN104390996A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5209975A (en) * | 1989-10-30 | 1993-05-11 | Tonen Kabushiki Kaisha | High elongation, high strength pitch-type carbon fiber |
| CN102459728A (en) * | 2009-06-10 | 2012-05-16 | 三菱丽阳株式会社 | Carbon fiber bundle that develops excellent mechanical performance |
| CN104011288A (en) * | 2011-12-27 | 2014-08-27 | 东丽株式会社 | Carbon fiber coated with sizing agent, process for producing carbon fiber coated with sizing agent, prepreg, and carbon fiber reinforced composite material |
| CN102661963A (en) * | 2012-06-01 | 2012-09-12 | 吉林大学 | Special X-ray diffraction and scattering analysis device for fiber material |
Non-Patent Citations (3)
| Title |
|---|
| L.PORTE ET AL.: "Evidence for silicon oxycarbide phase in the Nicalon silicon carbide fibre", 《JOURNAL OF MATERIALS SCIENCE》 * |
| 华中 等: "高模量PAN基炭纤维结构的表征与性能分析", 《新型炭材料》 * |
| 罗云烽 等: "上浆剂对国产T700级碳纤维复合材料界面性能的影响", 《材料科学与工艺》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198593A (en) * | 2016-07-06 | 2016-12-07 | 天津工业大学 | A kind of method of accurate sign γ irradiation carbon fiber microstructure |
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Application publication date: 20150304 |