CN103512876A - Method for analyzing bonding interface of bonder based on micro-Raman micro-zone analysis technology - Google Patents
Method for analyzing bonding interface of bonder based on micro-Raman micro-zone analysis technology Download PDFInfo
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- CN103512876A CN103512876A CN201310433566.9A CN201310433566A CN103512876A CN 103512876 A CN103512876 A CN 103512876A CN 201310433566 A CN201310433566 A CN 201310433566A CN 103512876 A CN103512876 A CN 103512876A
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Abstract
The invention provides a method for analyzing the bonding interface of a bonder based on a micro-Raman micro-zone analysis technology. The method comprises the following steps: freezing a bonder sample for slicing in a direction vertical to the bonding interface to obtain a slice-shaped bonder sample with a complete bonding interface layer; selecting one point from each of the two sides of the bonding interface layer of the slice-shaped bonder sample, and performing single-point Raman spectrum scanning on the selected points to obtain single-point Raman spectrograms; comparing peaking positions and peak intensity in the single-point Raman spectrograms of the two selected points, and using one peak position with changed peak intensity as a scanning peak position of micro-Raman micro-zone analysis; using the scanning peak position obtained in the step 3 as a scanning range, and performing micro-Raman micro-zone analysis and scanning on a selected micro zone of the cross bonding interface of the slice-shaped bonder sample to obtain a micro-Raman micro-zone analysis spectrogram for reflecting the state of bonding interface of the bonder. The method can be used for conveniently, accurately, quickly and intuitively observing the state of bonding interface of the bonder and is especially suitable for analyzing and observing the state of bonding interface of HTPB.
Description
Technical field
The present invention relates to the application of micro-Raman microscopy technology, relate in particular to a kind of method based on micro-Raman microscopy (mapping) technical Analysis cementing agent bonding interface.
Background technology
End hydroxy butadiene (HTPB) generally refers to that on average there is homopolymer or the multipolymer of the butadiene of two above hydroxyls at each large molecule two ends, by chain elongation and cross-linking and curing reaction, can be made into the elastic body of three-dimensional net structure.Because HTPB has that glass temperature is low, price is low, viscosity is little, electrical property and the advantage such as shop characteristic is good, be widely used as high-performance adhesive, in the bonding field of extraordinary solid propellant, have important application value especially.
HTPB propellant is the main propellant kind of using in significant period of time at present and in the future, is widely used on various strategies, tactics solid missile.China's most solid type of missile is all used HTPB propellant now.As propellant, HTPB bonding interface must stand a series of tests such as thermal cycle, processing processing, wideband vibrations, igniting supercharging, the insecure serious consequence that tends to cause propellant inefficacy of bonding interface.Whether the combination of the bonding interface of HTPB propellant is firm, durable is the key factor that affects its quality and life-span.In addition, propellant, as disposable strategic materials, often needs through long storage time, in storage process, inevitably physics and chemical change can occur, and these all can cause HTPB adhesive effect to change and even occur interfacial separation.Just because of the state of HTPB bonding interface is key like this, for the Real Time Observation of bonding interface with judge that status is important in actual applications, in national economy and national defense construction, have extremely important meaning simultaneously.
Raman spectrum is mainly as the means of identifying structure and interaction of molecules aspect organic chemistry, and it and infrared spectrum complement one another, and can differentiate special architectural feature or characteristic group.Polymer arts, Raman spectrum can provide many important informations of polymeric material configuration aspects, as molecular structure and composition, tacticity, crystallization and whereabouts, interaction of molecules, and the structure of surface and interface etc.The size of Raman shift, intensity and Raman peaks shape are to identify the important evidence of chemical bond, functional group, and these characteristic peaks can change along with bonding interface state difference.
Micro-Raman mapping technology be a new generation fast, high precision, face scan laser Raman technology, it is combined Laser Scanning Confocal Microscope technology with laser Raman spectroscopy technological perfectionism, as third generation Raman technology, possess the feature of high speed, very high resolution imaging.For traditional Raman spectrum application technology, micro-Raman mapping technology can be carried out the microcell face scanning of face transboundary to the bonding sample of HTPB rapidly, thereby obtains the mapping image of the high score rate of whole microcell, obtains its Raman spectrum distributed intelligence.At present, the conventional means of research HTPB bonding interface has optical microscopy, single-point Raman technology and infrared spectrum etc., micro-Raman mapping technology is applied to the research of the bonding system of HTPB, with respect to conventional means, can obtains abundanter, more intuitive bonding interface analysis result.
Summary of the invention
The object of this invention is to provide a kind of method based on micro-Raman microscopy technical Analysis cementing agent bonding interface, the method can intuitively be observed the variation of cementing agent bonding interface state.
For achieving the above object, the present invention adopts following technical scheme:
Method based on micro-Raman microscopy technical Analysis cementing agent bonding interface, comprises step:
Step 1, carries out freezing microtome section in the direction vertical with bonding interface to cementing agent sample, obtains the cementing agent sheet sample that comprises complete adhesive interface layer;
Step 2, in the bonding interface both sides of cementing agent sheet sample, each choosing a bit, is carried out single-point Raman spectroscopy scans to institute's reconnaissance, obtains single-point Raman spectrogram;
Step 3, contrasts peak position that peak position in the single-point Raman spectrogram of two reconnaissances and Feng Qiang，Jiang peak change by force as the scanning peak position of micro-Raman microscopy;
Step 4, the scanning peak position that the step 3 of take obtains is sweep limit, to cementing agent sheet sample across the selected microcell of bonding interface, carry out micro-Raman microscopy scanning, obtain the micro-Raman microscopy collection of illustrative plates of reflection cementing agent bonding interface state.
Above-mentioned cementing agent is end hydroxy butadiene (HTPB).
In above-mentioned steps 1, the cementing agent sheet thickness of sample obtaining is 1 ~ 10 millimeter.
In above-mentioned steps 1, the cementing agent sheet sample surfaces obtaining is smooth, and surface undulation keeps micron dimension.
In above-mentioned steps 2, institute's reconnaissance is carried out to single-point Raman spectroscopy scans and is specially:
Adopting power is that 5 ~ 10 mW, wavelength are that 100 ~ 4000cm is carried out in the laser instrument institute reconnaissance of 488 ~ 785 nm
-1single-point Raman spectroscopy scans in scope.
Compared to the prior art, the present invention has the following advantages and beneficial effect:
1, can facilitate, observe accurately, rapidly, intuitively the bonding interface state of cementing agent, be particularly useful for analysis and observation HTPB bonding interface state;
2, sampling less, the test duration is short; Without sample is carried out to complex process.
3, adopt micro-Raman microscopy technical Analysis cementing agent bonding interface state, can realize the Real Time Observation of cementing agent bonding interface state; Also can be observed heterogeneity in diffusion and the distribution at cementing agent bonding interface place, there is intuitive and accuracy that conventional means does not possess.
Accompanying drawing explanation
Fig. 1 is the inventive method process flow diagram;
Fig. 2 is the original Raman spectrogram that adopts micro-Raman mapping technology to obtain in embodiment;
Fig. 3 is the HTPB bonding interface photo directly perceived obtaining according to Fig. 2.
Embodiment
Fig. 1 is process flow diagram of the present invention, below in conjunction with Fig. 1, illustrates the specific embodiment of the present invention.
One, sample preparation
In the direction vertical with bonding interface, cementing agent sample is carried out to freezing microtome section, obtain the cementing agent sheet sample that comprises complete adhesive interface layer.Cementing agent sheet sample requirement even thickness, surface undulation is controlled at micron number magnitude.In this concrete enforcement, cementing agent sheet thickness of sample is 1 ~ 10 millimeter.
Two, adopt micro-Raman spectroscopy to obtain the micro-Raman microscopy collection of illustrative plates of reflection cementing agent bonding interface state.
In a side of cementing agent sheet sample bonding interface, select a bit, cementing agent sheet sample to be placed in to micro-Raman spectroscopy test section, by progressively focusing on, select the eyepiece of 100 times to be adjusted to know and see sample surfaces clearly.Open laser instrument, Modulating Power is output as 5 ~ 10mW, and the reconnaissance of cementing agent sheet sample institute is carried out to 100 ~ 4000cm
-1single-point Raman spectroscopy scans in scope, obtains the single-point Raman spectrogram of this reconnaissance.Opposite side at cementing agent sheet sample bonding interface is selected another point, adopts said method to obtain the single-point Raman spectrogram of this another point.
The peak position changing by force by the peak position in the single-point Raman spectrogram of comparative binders sheet sample bonding interface both sides institute reconnaissance and Feng Qiang，Jiang peak is as the scanning peak position scope of micro-Raman microscopy.Adopt microscope across bonding interface, to choose microcell at cementing agent sheet sample, within the scope of definite scanning peak position, the microcell that microscope is chosen carries out micro-Raman microscopy scanning, obtain original micro-Raman microscopy collection of illustrative plates, referring to Fig. 2, adopt NGSLabSpec software to convert the collection of illustrative plates of Fig. 2 to photo shown in Fig. 3.
The scanning peak position quantity of the micro-Raman microscopy of determining according to the Raman spectrogram of cementing agent bonding interface two side areas, may be 1, also may be for a plurality of.If a plurality of scanning peak position quantity, carries out micro-Raman microscopy scanning to the microcell of choosing respectively for each scanning peak position.
Raman spectrum is a kind of Surface Characterization technology, and the incident degree of depth is in micron dimension.The size of Raman shift, intensity and Raman peaks shape are to identify the important evidence of chemical bond, functional group.The characteristic peak of choosing (the scanning peak position of the micro-Raman microscopy that characteristic peak of choosing is determined according to the Raman spectrogram of cementing agent bonding interface two side areas) is demarcated as to particular color, obtain colored micro-Raman microscopy collection of illustrative plates, can reflect that this characteristic peak is in the distribution situation of bonding interface.By analyzing the peak position at bonding interface place, distribute, can have intuitive and accurate observe and decide to the bonding situation of bonding interface.
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment
Step 1, cuts off a fritter as sample from HTPB propellant sample, along the direction of vertical bonding interface, carries out freezing microtome section, obtains the HTPB sheet sample that comprises complete adhesive interface layer.
Step 2, opens 488 nm laser instruments, and Modulating Power is output as 5W, and it is 100 ~ 4000cm that sweep limit is carried out respectively in the both sides of HTPB sheet sample bonding interface
-1single-point Raman spectrum test, obtain single-point Raman spectrogram corresponding to bonding interface two side areas.
Step 3, the single-point Raman spectrogram of contrast bonding interface both sides, determines that Raman shift corresponding to micro-Raman microscopy scanning peak position is 1667.5cm
-1.
Step 4, to HTPB sample across bonding interface, choose a microcell, with 1667.5cm
-1for scanning peak position, this microcell is carried out to micro-Raman microscopy scanning, obtain original spectrum data, see Fig. 2.Photo corresponding to Raman spectral information in Fig. 2 convert to, and by 1667.5cm
-1peak position is demarcated as redness (seeing region 1 in Fig. 3 (b)), obtains 1667.5cm in HTPB sheet sample bonding interface microcell
-1the distributed intelligence of Raman shift, is shown in Fig. 3, and wherein, figure (a) is depicted as the microcell of choosing across bonding interface of HTPB sample; Figure (b) is the micro-Raman microscopy photo of reflection constituency bonding interface state; Scheme (c) for the partial enlarged drawing in region 1 in figure (b), figure (a) ~ (c) middle X represents length dimension.
In Fig. 3, the red area 1 in figure (b) shows that there is 1667.5cm at this place
-1peak position exists, and color represents that peak intensity is higher more deeply, and figure (c) is the enlarged drawing of red area 1.From figure (b) with (c), can know intuitively, exactly 1667.5cm
-1peak position is in situations such as the distribution at HTPB bonding interface place, diffusions.
The present embodiment the has utilized micro-Raman microscopy method system observation and analysis state of HTPB bonding interface, surface adopts micro-Raman microscopy method can intuitively observe the variation of HTPB bonding interface place adhering state, the advantages such as compared to the prior art, this method has intuitively, visualization is high, more accurate.
Claims (5)
1. the method based on micro-Raman microscopy technical Analysis cementing agent bonding interface, is characterized in that, comprises step:
Step 1, carries out freezing microtome section in the direction vertical with bonding interface to cementing agent sample, obtains the cementing agent sheet sample that comprises complete adhesive interface layer;
Step 2, in the bonding interface both sides of cementing agent sheet sample, each choosing a bit, is carried out single-point Raman spectroscopy scans to institute's reconnaissance, obtains single-point Raman spectrogram;
Step 3, contrasts peak position that peak position in the single-point Raman spectrogram of two reconnaissances and Feng Qiang，Jiang peak change by force as the scanning peak position of micro-Raman microscopy;
Step 4, the scanning peak position that the step 3 of take obtains is sweep limit, to cementing agent sheet sample across the selected microcell of bonding interface, carry out micro-Raman microscopy scanning, obtain the micro-Raman microscopy collection of illustrative plates of reflection cementing agent bonding interface state.
2. the method based on micro-Raman microscopy technical Analysis cementing agent bonding interface as claimed in claim 1, is characterized in that:
Described cementing agent sheet thickness of sample is 1 ~ 10 millimeter.
3. the method based on micro-Raman microscopy technical Analysis cementing agent bonding interface as claimed in claim 1, is characterized in that:
Described cementing agent sheet sample surfaces rises and falls and keeps micron number magnitude.
4. the method based on micro-Raman microscopy technical Analysis cementing agent bonding interface as claimed in claim 1, is characterized in that:
Institute's reconnaissance carried out to single-point Raman spectroscopy scans be specially described in step 2:
Adopting power is that 5 ~ 10 mW, wavelength are that 100 ~ 4000cm is carried out in the laser instrument institute reconnaissance of 488 ~ 785 nm
-1single-point Raman spectroscopy scans in scope.
5. the method based on micro-Raman microscopy technical Analysis cementing agent bonding interface as claimed in claim 1, is characterized in that:
Described cementing agent is end hydroxy butadiene.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044450A (en) * | 2019-12-13 | 2020-04-21 | 西安航空职业技术学院 | Laminated composite material interface bonding strength test system |
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| US20020154301A1 (en) * | 2001-02-23 | 2002-10-24 | Shen Ze Xiang | Apertureless near-field scanning raman microscopy using reflection scattering geometry |
| US20070229817A1 (en) * | 2003-05-27 | 2007-10-04 | Hong Wang | Light scattering device having multi-layer micro structure |
| CN102323249A (en) * | 2011-08-29 | 2012-01-18 | 东莞新能源科技有限公司 | Qualitative analysis method for adhesive property of adhesive |
| CN103186803A (en) * | 2013-03-19 | 2013-07-03 | 南京大学 | Raman-spectrum-based nanometer bar code smart label and identification method thereof |
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Patent Citations (4)
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| US20020154301A1 (en) * | 2001-02-23 | 2002-10-24 | Shen Ze Xiang | Apertureless near-field scanning raman microscopy using reflection scattering geometry |
| US20070229817A1 (en) * | 2003-05-27 | 2007-10-04 | Hong Wang | Light scattering device having multi-layer micro structure |
| CN102323249A (en) * | 2011-08-29 | 2012-01-18 | 东莞新能源科技有限公司 | Qualitative analysis method for adhesive property of adhesive |
| CN103186803A (en) * | 2013-03-19 | 2013-07-03 | 南京大学 | Raman-spectrum-based nanometer bar code smart label and identification method thereof |
Non-Patent Citations (2)
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| GAO YUN 等: "Application of Raman spectroscopy in carbon nanotube-based", 《CHINESE SCIENCE BULLETIN》, vol. 55, 31 December 2010 (2010-12-31), pages 3978 - 3988 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044450A (en) * | 2019-12-13 | 2020-04-21 | 西安航空职业技术学院 | Laminated composite material interface bonding strength test system |
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