CN107860696A - The supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity - Google Patents
The supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity Download PDFInfo
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- CN107860696A CN107860696A CN201710990363.8A CN201710990363A CN107860696A CN 107860696 A CN107860696 A CN 107860696A CN 201710990363 A CN201710990363 A CN 201710990363A CN 107860696 A CN107860696 A CN 107860696A
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- porosity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
Abstract
The invention discloses a kind of supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity, it is characterized in that detection method and step are：（1）Detected using Ultrasonic C-Scan method, record ultrasonic attenuation；（2）The methods of being detected using the test of micro- metallographic, field emission microscope test and high-precision CT, porosity detection is carried out to the carbon fiber enhancement resin base composite material laminate of Ultrasonic C-Scan detection respectively, the relation of Ultrasonic C-Scan attenuation coefficient and porosity is obtained, calculates porosity；（3）The accuracy of detection is 0.01%.
Description
Technical field
The present invention relates to the supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity.The invention belongs to
Field of non destructive testing.
Background technology
Carbon fiber-reinforced resin composite materials laminate is the advanced composite material for being widely used in aerospace field, hole
The presence of gap has a great impact to its performance, and control porosity is one of key technology in production process.For aviation carbon
Fibre reinforced epoxy resin composite laminate, the requirement to porosity are：A levels be less than 0.2%, B levels be 0.2%~
0.5%th, C levels are 0.5%~1.0%.
The present invention says the supersonic detection method being related to, and can accurately detect carbon fiber enhancement resin base composite material lamination
The porosity of plate.
The content of the invention
, can be accurate the present invention relates to a kind of supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity
Determine the porosity of carbon fiber reinforced epoxy resin-based composite laminate.
The present invention is by being achieved in, the ultrasound detection side of carbon fiber enhancement resin base composite material laminate porosity
Method, its characterization step are：
1. the Ultrasonic C-Scan detection of carbon fibre laminate composites；Using the 5MHz flat probes of immersion, water is coupling
Agent, capture card collection ultrasonic signal, by comparing sound pressure variations, derives the attenuation coefficient of different zones.
(1) frequency probe is 5MHz, wafer size 6mm, focal length 30mm.The frequency probe first selected by, sets pulse
The relevant parameters such as transmitter frequency, couplant are water.
(2) carbon fiber enhancement resin base composite material laminate is kept flat in water, and probe is moved to above laminate, passes through sight
Examine waveform, mobile probe regulation left and right, front and rear drift angle, when focusing probe when bottom ripple wave amplitude reaches maximum；When once bottom ripple
Wave amplitude reaches 80%, and is appropriate gain when noise is relatively low.The gain of setting is 5dB.
(3) scanning step pitch and the mobile Scanning speed of probe (gathering a data every 0.5mm) are determined, determines scanning road
Footpath, and the position for preserving data is set, then it is scanned.
2. micro- metallographic and field emission microscope the observation test of carbon fiber enhancement resin base composite material laminate；
The carbon fiber enhancement resin base composite material laminate that ultrasound detection is crossed, it is micro- with micro- metallographic method and field emission electron respectively
Mirror method is observed, and counts porosity, the relation established between ultrasonic attenuation and porosity.
(1) the micro- metallographic method observation of carbon fiber enhancement resin base composite material laminate；The carbon fiber that ultrasound detection is crossed
Reinforced resin based composites laminate, is observed, concrete operation step is as follows with micro- metallographic method：
(A) inlay：It is 20mm that carbon fiber enhancement resin base composite material laminate is cut into size with precision gas cutting machine
× 10mm × 2mm sample.4~5 pieces of samples of well cutting are inlayed with metallographic curing agent and metallographic rubber powder.Metallographic curing agent and gold
The proportioning of phase rubber powder is 1:2 (volume ratios), are slowly poured into mould after stirring, and after ambient temperature curing 10min, are treated solid
Taken out after changing completely, mark is numbered.
(B) grinding and polishing：By No.400 sand paper on the polishing pad of polished machine, section is ground under the low speed, pays attention to keeping hanging down
Directly；Change No.800 sand paper to continue to polish, polishing direction before is rotated by 90 °, then use No.1200, No.2000 sand successively
Paper continues to polish, until section is smooth.
Nylon cloth and partially soft grinding agent (such as MgO, ZnO) are selected, rubbing down is smooth shinny to surface, no marking,
It is put into afterwards equipped with absolute ethyl alcohol, 5min is cleaned in instrument is cleaned by ultrasonic, removes the antiscuffing paste and spot of surface adhesion, finally
Quickly dried up through hair-dryer.
(C) observation by light microscope：First select 50 times to observe overall picture, the suitable multiplication factor shooting of reselection is aobvious
Micro- picture, as shown in Figures 2 and 3.The arithmetic mean of instantaneous value of hole is exactly area porosity, grinds off 5~10 sections successively, will be each
Porosity on section, which is added, averages, that is, obtains volumetric porosity.Fig. 2 and 3 is unidirectional T700/ composite polyimide materials
The microscopic appearance figure of laminate.
(2) the field emission scanning electron microscope observation of carbon fiber enhancement resin base composite material laminate；Use Flied emission
The carbon fiber enhancement resin base composite material laminate sample that SEM observation ultrasound detection is crossed, concrete operation step
It is as follows：
(A) carbon fiber enhancement resin base composite material laminate sample is prepared by micro- metallographic method, surface spraying is certain
The gold of thickness is to obtain clearly image.The design parameter of metal spraying is：Vacuum 1.3 × 10-6Pa, 5~10s of spray time, gold
0.5~0.8 μm of thickness degree.
(B) field emission microscope is observed.The micro-image of field emission microscope observation is as illustrated in figures 4-5.Hole
The arithmetic mean of instantaneous value of gap is exactly area porosity, grinds off 5~10 sections successively, and the porosity on each section is added and made even
Average, that is, obtain volumetric porosity.Fig. 4-5 is the T300/ epoxy resin composite materials lamination of field emission microscope observation
The microscopic appearance of plate hole gap, multiplication factor are 10 000 times.
3. the high-precision CT detections of fiber-reinforced resin matrix compound material laminate and defect imaging；Detected with high-precision CT
The carbon fiber enhancement resin base composite material laminate crossed to ultrasound detection detects, detection specimen size be 4mm × 2mm ×
2mm。
Detected, had using the GE Phoenix nanotom micro-CT systems of General Electric's Phoenix
Body operating procedure is as follows：The carbon fiber enhancement resin base composite material test agent processed be fixed on ray tube and detector it
Between, resolution ratio and contrast that tuning parameter is optimized to, then calibration detectors, then carry out two-dimensional projection data collection.Entirely
During need to ensure that ray penetrates, 360 ° of rotary sample during scanning, sample often rotates an angle acquisition one and opens two dimensional image, revolves
Gyration<1 °, original image is handled by inverse, filtered, imported after linear analysis processing VG studio softwares carry out it is three-dimensional
Reconstruct, realize that three-dimensional data visualizes.
(1) two-dimensional projection image；X, Y, Z axis direction after the segmentation of carbon fiber enhancement resin base composite material laminate is rebuild
Faultage image, see Fig. 6.Y-axis fault trend is 90 ° of directions of fiber, and X, Z axis fault trend are 0 ° of direction of fiber, high brightness in figure
Hickie be mingled with for high density.Carbon fiber and resin and layer structure can be clearly told from figure, is seen with micro- metallographic method
The Cross Section Morphology observed is consistent.(donut in Y direction faultage image is caused ring image during reconstruction, no
Influence observation.) X and Y direction reconstruction faultage image hole it is mutually corresponding, the porosity of interlayer will be apparently higher than fibre bundle
Between porosity；The hole random distribution of faultage image is rebuild along Z axis.Fig. 7 is the faultage image of Z-direction from left to right.Figure
6th, Fig. 7 composite is T700/ composite polyimide material laminates.
(2) tripleplane's image；One group of continuous faultage image for scanning gained is imported into three-dimensional visualization software VG
Studio carries out three-dimensional reconstruction, rebuilds effect and sees Fig. 8.High-precision CT detections have high-precision three-dimensional three-dimensional imaging, by figure
As processing obtains two dimension, 3D shape size and the distribution of volumetric porosity and each defect.Fig. 8 is that T700/ polyimides is answered
Condensation material laminate.
4. the relation of ultrasound detection attenuation coefficient and porosity；It is fine according to the carbon that micro- metallographic and high-precision CT analyses calculate
Reinforced resin based composites laminate porosity is tieed up, data comparison is carried out with the attenuation coefficient of Ultrasonic C-Scan detection, is united
Counting result is：When the minimum porosity P of detection is 0.00%, attenuation coefficient α is k (unit dB/mm), and this is by fiber and tree
Decay caused by fat.As porosity raises, attenuation coefficient also gradually increases.When porosity P is less than some threshold value, porosity
It is linear with attenuation coefficient；When porosity P is more than the threshold value, hole and attenuation coefficient are in quadratic function relation.In formula
P be porosity, α is attenuation coefficient, and a, b, c are constant.
By the attenuation coefficient of Ultrasonic C-Scan, above-mentioned equation is solved, can obtain carbon fiber-reinforced resin composite materials lamination
The porosity of plate, accuracy 0.01%.
It is sub- for die pressing, the carbon-fibre reinforced epoxy resin composite material of autoclave method shaping, fibre reinforced polyamides
Polyimide resin composite, constant k, a, b, c are respectively：2.14dB/mm, 0.06,0.27, -0.47, the threshold value of porosity are
0.70%.
Brief description of the drawings
Fig. 1 is the Ultrasonic C-Scan detection principle diagram of the present invention.
Fig. 2 is the microcosmic shape of the unidirectional T700/ composite polyimide materials laminate of the micro- metallographic method detection of the present invention
Looks figure one.
Fig. 3 is the microcosmic shape of the unidirectional T700/ composite polyimide materials laminate of the micro- metallographic method detection of the present invention
Looks figure two.
Fig. 4 is the T300/ epoxy resin composite material laminate holes of the field emission microscope observation of the present invention
Microscopic appearance figure one.
Fig. 5 is the T300/ epoxy resin composite material laminate holes of the field emission microscope observation of the present invention
Microscopic appearance figure two.
The T700/ composite polyimide materials that Fig. 6 is the present invention are laminated plate high precision CT two-dimensional projection images reconstruction tomography
Image.
The Z-direction that Fig. 7 is the present invention rebuilds faultage image.
The T700/ composite polyimide materials that Fig. 8 is the present invention are laminated plate high precision CT tripleplanes image reconstruction figure.
Fig. 9 is the Ultrasonic C-Scan decay of the T700/ composite polyimide material laminates of the autoclave method shaping of the present invention
Figure.
Figure 10 is the Ultrasonic C-Scan decay pattern of the compression molding method T700/ composite polyimide material laminates of the present invention.
Figure 11 is the ultrasonic attenuation figure of 20 layers of unidirectional laying T700/ epoxy resin composite material laminates of the present invention.
Figure 12 is the ultrasonic attenuation figure of the compression molding T300/ epoxy resin composite material laminates of the present invention.
Embodiment
1st, the supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity, it is characterized in that detection method and
Step is：
(1) using Ultrasonic C-Scan method detection composite, ultrasonic attenuation is recorded；Specially：Using ultrasonic water immersion bounce technique
Measure the decay of carbon fiber enhancement resin base composite material；Assume initially that the surfacing of carbon fiber enhancement resin base composite material
Smooth, the steel plate that flat smooth is then placed in bottom passes twice through sample to tell Bottom echo and sound wave, can improve
Measurement sensitivity；Using the 5MHz flat probes of immersion, water is couplant, and capture card gathers ultrasonic signal, by comparing acoustic pressure
Change, derive the attenuation coefficient of different zones；
(2) decayed according to Ultrasonic C-Scan, the relation with porosity, calculate porosity；Specially：
When the minimum porosity P of detection is 0.00%, attenuation coefficient α=k, k unit dB/mm, this be by carbon fiber and
Decay caused by resin；As porosity raises, attenuation coefficient also gradually increases；
When porosity P is less than some threshold value, porosity and attenuation coefficient are linear；
When porosity P is more than the threshold value, hole and attenuation coefficient are in quadratic function relation；
P in formula is porosity, and α is attenuation coefficient, and a, b, c are constant；
Embodiment one
The distribution of the Ultrasonic C-Scan decay of autoclave molding method T700/ composite polyimide material laminates, such as Fig. 9 institutes
Show.Laminate is the thick orthogonal laying laminates of 2mm, and laminate mean attenuation coefficient is 2.71dB/mm, the hole being calculated
Rate is respectively 0.57%.
Embodiment two
The distribution of the Ultrasonic C-Scan decay of compression molding method T700/ composite polyimide material laminates, such as Figure 10 institutes
Show.Laminate is the multidirectional laying laminate of 2 millimeters thicks, and laminate mean attenuation coefficient is 4.31dB/mm.The hole being calculated
Gap rate is 1.76%.
Embodiment three
The unidirectional laying T700/ epoxy resin composite materials laminate of 20 layers of compression molding (thickness is 2.58~2.62mm)
The distribution of Ultrasonic C-Scan decay, as shown in figure 11,6 zone leveling attenuation coefficients are 4.08dB/mm.The hole being calculated
Rate is respectively 1.64%.
Example IV
The attenuation distribution of the Ultrasonic C-Scan of compression molding T300/ epoxy resin composite material laminates, as shown in figure 12.
The attenuation coefficient of the laminate is 5.88dB/mm, and the porosity being calculated is 3.19%.
Claims (1)
1. the supersonic detection method of carbon fiber enhancement resin base composite material laminate porosity, it is characterized in that detection method and step
For：
（1）Composite is detected using Ultrasonic C-Scan method, records ultrasonic attenuation；Specially：Using ultrasonic water immersion reflection method for measuring
The decay of carbon fiber enhancement resin base composite material；Assume initially that the surfacing light of carbon fiber enhancement resin base composite material
Sliding, the steel plate that flat smooth is then placed in bottom passes twice through sample to tell Bottom echo and sound wave, can improve survey
Measure sensitivity；Using 5 MHz flat probes of immersion, water is couplant, capture card collection ultrasonic signal, is become by comparing acoustic pressure
Change, derive the attenuation coefficient of different zones；
（2）Decayed according to Ultrasonic C-Scan, the relation with porosity, calculate porosity；Specially：
When the minimum porosity of detectionPFor 0.00% when, attenuation coefficient α=k, k unit dB/mm, this is by carbon fiber and resin production
Raw decay；As porosity raises, attenuation coefficient also gradually increases；
Work as porosityPDuring less than some threshold value, porosity and attenuation coefficient are linear；
Work as porosityPDuring more than the threshold value, hole and attenuation coefficient are in quadratic function relation；
In formulaPFor porosity, α is attenuation coefficient, and a, b, c are constant；
。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112033874A (en) * | 2019-06-04 | 2020-12-04 | 中国航发商用航空发动机有限责任公司 | Method for obtaining porosity and interface strength of composite material cementing interface |
| CN112085693A (en) * | 2020-06-24 | 2020-12-15 | 中国科学院武汉岩土力学研究所 | Method and system for evaluating porosity ratio and reconstructing form of internal structure of soil-rock mixture |
Citations (1)
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897550A (en) * | 2015-06-17 | 2015-09-09 | 大连理工大学 | Method for confirming relation between porosity of CFRP (carbon fiber reinforced plastics) and ultrasonic attenuation coefficient |
Non-Patent Citations (1)
| Title |
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| 罗明: "碳纤维增强树脂基复合材料孔隙率超声无损检测", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112033874A (en) * | 2019-06-04 | 2020-12-04 | 中国航发商用航空发动机有限责任公司 | Method for obtaining porosity and interface strength of composite material cementing interface |
| CN112085693A (en) * | 2020-06-24 | 2020-12-15 | 中国科学院武汉岩土力学研究所 | Method and system for evaluating porosity ratio and reconstructing form of internal structure of soil-rock mixture |
| CN112085693B (en) * | 2020-06-24 | 2022-09-20 | 中国科学院武汉岩土力学研究所 | Method and system for evaluating porosity ratio and reconstructing form of internal structure of soil-rock mixture |
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