CN105973703A - Apparatus and method for detecting interfacial shear strength of composite material based on laser Raman spectrometer - Google Patents
Apparatus and method for detecting interfacial shear strength of composite material based on laser Raman spectrometer Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 110
- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims description 26
- 239000000835 fiber Substances 0.000 claims abstract description 114
- 238000001514 detection method Methods 0.000 claims abstract description 46
- 239000012783 reinforcing fiber Substances 0.000 claims description 50
- 239000011347 resin Substances 0.000 claims description 34
- 229920005989 resin Polymers 0.000 claims description 34
- 239000011159 matrix material Substances 0.000 claims description 29
- 238000010521 absorption reaction Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 229920013657 polymer matrix composite Polymers 0.000 claims description 6
- 239000011160 polymer matrix composite Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 230000004308 accommodation Effects 0.000 claims description 3
- 150000001721 carbon Chemical group 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000003750 conditioning effect Effects 0.000 claims description 3
- 238000009795 derivation Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 230000006798 recombination Effects 0.000 claims description 3
- 238000005215 recombination Methods 0.000 claims description 3
- 229920005992 thermoplastic resin Polymers 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000002787 reinforcement Effects 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000001419 dependent effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000805 composite resin Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000010271 massa medicata fermentata Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
- G01N3/068—Special adaptations of indicating or recording means with optical indicating or recording means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
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Abstract
The invention provides an apparatus for detecting interfacial shear strength of a composite material based on a laser Raman spectrometer. The apparatus comprises the laser Raman spectrometer, a sample bearing mechanism, and a tension mechanism; the sample bearing mechanism comprises a bearing framework, a sample fixing end I, a sample fixing end II, a stress sensor, a micrometer for metering, and a stress reading display; the bearing framework is rectangular and is vertically installed under a laser beam, the sample fixing end I is fixedly arranged at the inner side of one end of the rectangular framework, and the sample fixing end II is movably arranged at the other end, so that a fixing mechanism for fixing a sample to be tested is formed; one end of the sample fixing end I is fixed at the inner side of the bearing framework, and the other end is fixedly connected to the sample to be tested by the stress sensor; one end of the sample fixing end II is fixedly connected to the sample to be tested, and the other end traverses the rectangle framework and is connected to the tension mechanism by the micrometer for metering; the stress reading display and the stress sensor are connected electrically. The detection is accurate, and provides basic data for calculating residual stress of a microscopic area on the surface of fiber.
Description
Technical field
The present invention relates to fiber-reinforced resin matrix compound material interface shear strength detection technique, be related specifically to one
Composite material interface shear strength based on laser Raman spectrometer detection device and method.
Background technology
Fiber-reinforced resin matrix compound material becomes numerous skill with unique light weight effect (high specific strength and specific modulus)
The master in art field (technical field such as auto industry, wind-power electricity generation, track traffic, Leisure Sport, household electrical appliances, building and Aero-Space)
Flow Technique trend.It occupies critical role in national economy, is the industry of national industrial policies emphasis encouragement development, development sky
Between huge.Especially current automotive light weight technology technology is to save one of the energy, the effective ways improving driving performance, is also domestic and international
One of key technology target that automaker pursues.But, due to reinforcing fiber and matrix resin thermal expansion in composite
The difference of coefficient, result in composite and is producing in solidification process, or the later stage use during with the change of ambient temperature, lead
Cause composite inner and produce internal stress.Tensile property and the fatigue behaviour of composite can be produced by the stress axial along fiber
The biggest impact, tensile property and the fatigue behaviour of composite can be had a huge impact by the stress axial along fiber, and
The interface shear strength of fiber-reinforced resin matrix compound material directly influences intensity and the toughness of composite.Therefore, accurately
Measure the interface shear strength of fiber-reinforced resin matrix compound material, for promoting the comprehensive of fiber-reinforced resin matrix compound material
Mechanical property and the safety in utilization under various complex environments thereof are significant.
At present, prior art fiber strengthens the detection method of polymer matrix composites interface shear strength, mainly has fiber
Extract, fiber press-in, four kinds of method of testings such as fibrous fracture and microballon unsticking, its feature is all to allow ultimate fibre interface bear cut
Power, draws interface shear strength according to interfacial detachment LOAD FOR, and its difference is only that profile and the load mode of test specimen used
Different.But, different owing to have ignored interface key groove, cause various method of testing for same fiber and the detection of resin,
Generally draw different interface shear strengths.It addition, these methods can only measure critical interfaces shear strength, for there is not boundary
The shear stress that face is destroyed then cannot be measured.
Obviously, prior art fiber strengthens the detection method of polymer matrix composites interface shear strength and there is interface and cut
Shearing stress is measured inaccurate and can only measure the problems such as critical interfaces shear strength.
Summary of the invention
The interface that the detection method of polymer matrix composites interface shear strength exists is strengthened for solving prior art fiber
Shear strength is measured inaccurate and can only measure the problems such as critical interfaces shear strength, and the present invention proposes a kind of based on LR laser raman
The composite material interface shear strength detection device and method of spectrogrph.
Present invention composite material interface based on laser Raman spectrometer shear strength detection device, including, LR laser raman
Spectrogrph, sample load carrier and drawing mechanism；Described sample load carrier, including, bearing frame, sample fix termination I, examination
Sample fixes termination II, strain gauge, thousand points of measuring rulers and stress read-out display；Described bearing frame is rectangle and vertically pacifies
Being contained in the underface of laser beam, be installed with sample and fix termination I inside one end of its rectangular frame, other end activity is installed
There is sample to fix termination II, thus constitute the fixed mechanism of fixing sample to be tested；Described sample is fixed one end of termination I and is fixed on
Inside bearing frame, the other end is connected by strain gauge and sample to be tested are fixing；One end of termination II fixed by described sample
Fixing with sample to be tested and be connected, the other end is connected through rectangular frame and by thousand points of measuring rulers with drawing mechanism；Described stress
Read-out display electrically connects with strain gauge.
Further, described sample load carrier is additionally provided with and promotes bearing frame according to the distance set along level or fibre
The stepping mechanism that dimension axis direction moves.
Further, described stepping mechanism belt pulley stepping mechanism, rack-and-pinion stepping mechanism or worm and gear stepper
Structure, its distance set is as 0.01mm-2.00mm.
Further, the wavelength of described laser Raman spectrometer laser beam is 514nm or 633nm；Described LR laser raman light
Spatial resolution≤2 μm of spectrometer.
Further, described drawing mechanism is provided with stretching variable adjusting means, and the range of accommodation of described stretching variable is
0.05%-100%.
Present invention composite material interface based on laser Raman spectrometer shear strength detection method, use the present invention based on
Composite material interface shear strength is detected by the composite material interface shear strength detection device of laser Raman spectrometer, bag
Include following steps；
S101, for non-carbon-reinforced fiber use graphene fiber surface conditioning agent reinforcing fiber is carried out surface process,
Make non-carbon-reinforced fiber surface attachment have carbon atom, carbon-reinforced fiber is not the most made to any process；
S102, single fiber is sticked at the scraps of paper as sample, reinforcing fiber is fixedly connected on sample and fixes termination I and examination
Sample is fixed on termination II, and by the laser beam vertical irradiation of laser Raman spectrometer on reinforcing fiber surface；
S103, set different stretching variablees and start drawing mechanism, can detect that tested fibre single thread is in different deformation
Raman absorption spike number ν in the case of amount ε；Draw the relation curve of ε Yu ν, after linear fit, calibrate slope s；
Reinforcing fiber after S104, employing step S101 process is combined with thermosetting resin or thermoplastic resin prepares fiber
Strengthen polymer matrix composites, and take bar shaped composite sample；
S105, bar shaped composite sample is fixed termination I and sample is fixed on termination II, show at Raman spectrometer optics
Find the fiber in composite sample under micro mirror, and the laser beam focus vertical irradiation of laser Raman spectrometer is being strengthened fibre
On dimension microcell, it is thus achieved that the Raman absorption spike number of corresponding microcell；
S106, the stepping mechanism of unlatching sample load carrier, make composite sample have along level or fibre axis direction
Sequence moves setpoint distance, by the laser beam focus of laser Raman spectrometer on the different microcells of reinforcing fiber, it is thus achieved that the most micro-
The Raman absorption spike number in district；
S107, set different stretching variablees and start drawing mechanism, composite is applied the stretching variable set, weight
Multiple step S106 and S107, obtain composite under conditions of different deformation amount, along drawing of fibre axis diverse location microcell
Graceful absworption peak wave number；
S108, employing following formula calculate the microcell strain stress of Fiber In Composite Material surface diverse locationx,
In formula, vxThe Raman absorption spike number obtained for step S105, S106 and S 107, v0It is zero for fiber surface stress
Time obtain Raman absorption spike number, s be step S103 obtain slope；Thus, composite is obtained in differently strained amount
In the case of, its internal reinforcing fiber strains along the microcell of fibre axis diverse location；
S109, relation according to fibre stress strain, try to achieve composite in the case of different deformation amount, and internal carbon is fine
Tieing up the micro-sized stress along fibre axis diverse location, and state with curve, described curve is position-stress curve；
When the stress that outer bound pair composite applies is zero, the stress of the fiber surface difference microcell obtained is enhancing
Fiber is produced residual stress with matrix resin recombination process；The stress applied when outer bound pair composite is certain setting value
Time, the microcell strain of the fiber surface diverse location obtained is this composite by this microcell fiber and matrix after this stress
The strain of interlaminar resin；
The data of position-stress curve are fitted by S110, employing following formula,
In formula, EfFor the Young's modulus of reinforcing fiber, εmFor the strain of resin, l by composite the length of survey fiber
Degree, β uses below equation to try to achieve:
In formula, r1For the diameter of reinforcing fiber, EmFor the Young's modulus of resin matrix, VmAnd VfIt is respectively in composite
Resin matrix and the volume content of reinforcing fiber, GmAnd GfIt is respectively resin matrix and the modulus of shearing of reinforcing fiber.
G can be tried to achieve by below equation:
In formula, E is Young's modulus, and v is the Poisson's ratio of material；
S111, to the fitting data of step S110 gained according to below equation relative to position x derivation, i.e. can get interface
Shear strength τ；
In formula, r1Diameter for reinforcing fiber.
Further, the wavelength of described laser Raman spectrometer laser beam is 514nm or 633nm；Described LR laser raman light
Spatial resolution≤2 μm of spectrometer.
Further, in step S103, the set point of described stretching variable is 0.05%-100%.
Further, in step 106, described setpoint distance is 0.01mm-2.00mm.
Present invention composite material interface based on laser Raman spectrometer shear strength detection device and method Advantageous
Effect is can be to the wave number at the reinforcing fiber monofilament Raman absorption peak of reinforcing fiber monofilament or composite inner and fiber list
The strain of silk accurately detects, and provides basic data for calculating the residual stress of fiber surface microcosmos area, and thus calculates
Go out interface shear strength.
Accompanying drawing explanation
Accompanying drawing 1 detects device for the present invention and fibre single thread sample carries out the schematic diagram of stretching detection；
Accompanying drawing 2 detects device for the present invention and composite sample carries out the schematic diagram of stretching detection；
Accompanying drawing 3 is the relation curve of detection method embodiment ε and ν；
Accompanying drawing 4 is the detection method embodiment Raman absorption spike number pass along fibre axis diverse location microcell
System；
Accompanying drawing 5 is the detection method embodiment internal reinforcing fiber microcell strain pass along fibre axis diverse location
System；
Accompanying drawing 6 be detection method embodiment composite deformation quantity be the position of 0%, 0.3%, 0.6%, 0.9%
Put-stress curve；
Accompanying drawing 7 be detection method embodiment composite deformation quantity be the position-answer Massa Medicata Fermentata of 1.5% and 1.8%
Line；
Accompanying drawing 8 is 0.3%, 0.6%, 0.9% and 1.2% for detection method embodiment composite dependent variable
Relation along the microcell interface shear strength of fibre axis diverse location；
Accompanying drawing 9 for detection method embodiment composite dependent variable be 1.5% along fibre axis diverse location
The relation of microcell interface shear strength；
Accompanying drawing 10 for detection method embodiment composite dependent variable be 1.8% along fibre axis diverse location
The relation of microcell interface shear strength.
Composite material interface based on laser Raman spectrometer to the present invention with specific embodiment is sheared below in conjunction with the accompanying drawings
Intensity detecting device and method are further described.
Detailed description of the invention
Accompanying drawing 1 detects device for the present invention and reinforcing fiber monofilament carries out the schematic diagram of stretching detection, and accompanying drawing 2 is the present invention
Detection device carries out the schematic diagram of stretching detection to composite sample, and in figure, 11 is bearing frame, and 12 fix termination for sample
I, 13 fix termination II for sample, and 14 is strain gauge, and 15 is thousand points of measuring rulers, and 16 is stress read-out display, and 21 is sharp
Shaven head, 22 is laser beam, and A is fibre single thread sample, and B is composite sample, and the direction of arrow is draw direction.As seen from the figure,
Present invention composite material interface based on laser Raman spectrometer shear strength detection device, including, laser Raman spectrometer is (not
Diagram), sample load carrier and drawing mechanism (not shown)；Described sample load carrier, including, bearing frame 11, sample are solid
Termination II 13,15, thousand points of measuring rulers 14 of strain gauge and stress read-out display 16 are fixed in fixed end I 12, sample；Described hold
Carrying framework 11 is rectangle and the underface being vertically mounted on laser beam 22, is installed with sample inside one end of its rectangular frame
Fixing termination I 12, the other end is movably installed with sample and fixes termination II 13, thus constitutes the fixing of fixing sample to be tested (A or B)
Mechanism；Described sample is fixed one end of termination I 12 and is fixed on inside bearing frame 11, and the other end passes through strain gauge 15 and treats
Test specimens (A or B) is fixing to be connected；Described sample fixes that one end of termination II 13 is fixing with sample to be tested (A or B) to be connected, another
Hold through rectangular frame and be connected with drawing mechanism by thousand points of measuring rulers 14；Described stress read-out display 16 and stress sensing
Device 15 electrically connects.When specifically detecting, for fibre single thread sample, can use and single fiber is sticked at the company of being fixed after the scraps of paper
Connect, make detected fibre single thread fix termination I respectively with sample and sample fixes that termination II is fixing to be connected.Owing to bearing frame hangs down
Directly it is arranged on the underface of laser beam, can ensure that laser beam is vertical with fibre axis by adjustment.Need to set according to detection
The stretching variable of drawing mechanism, opens laser Raman spectrometer, can record fibre single thread under conditions of different deformation amount, institute
Corresponding relation by stress Yu Raman absorption spike number.
For detection fibers monofilament in the case of same deformation quantity, not stress suffered by coaxial position and Raman absorption spike
The corresponding relation of number, the sample load carrier of composite material interface shear strength of the present invention detection device is additionally provided with promotion carrying
The stepping mechanism that framework moves along level or fibre axis direction according to the distance set.Generally can use common stepper
Structure, including belt pulley stepping mechanism, rack-and-pinion stepping mechanism or worm and gear stepping mechanism, its distance set as
0.01mm-2.00mm.Bearing frame can be made to move along level or fibre axis direction according to the distance set by setting,
Thus, it is possible in the case of same deformation quantity being detected, stress suffered by coaxial position is not corresponding with Raman absorption spike number
Relation.
As preferably, composite material interface shear strength of the present invention detects device, described laser Raman spectrometer laser beam
Wavelength be 514nm or 633nm；Spatial resolution≤2 μm of described laser Raman spectrometer.Described drawing mechanism is provided with and draws
Stretching variable adjusting means, the range of accommodation of described stretching variable is 0.05%-100%..
When composite sample being carried out stretching detection, the two ends of composite bar shaped sample are respectively fixedly connected with in examination
Termination I fixed by sample and sample is fixed on termination II, finds the fibre in composite sample under Raman spectrometer optical microscope
Dimension, then, by the laser beam focus vertical irradiation of laser Raman spectrometer on reinforcing fiber microcell.Set as it was previously stated, use
Fixed stretching variable and the distance of setting, i.e. can detect that the situation at same stretching variable of the fiber in composite sample
Under, not stress suffered by coaxial position and the corresponding relation of Raman absorption spike number.
Present invention composite material interface based on laser Raman spectrometer shear strength detects, and uses the present invention based on laser
Composite material interface shear strength is detected, including following step by the composite material interface shear strength detection device of Raman spectrometer
Rapid:
S101, for non-carbon-reinforced fiber use graphene fiber surface conditioning agent reinforcing fiber is carried out surface process,
Make non-carbon-reinforced fiber surface attachment have carbon atom, carbon-reinforced fiber is not the most made to any process；
S102, single fiber is sticked at the scraps of paper as sample, reinforcing fiber is fixedly connected on sample and fixes termination I and examination
Sample is fixed on termination II, and by the laser beam vertical irradiation of laser Raman spectrometer on reinforcing fiber surface (such as accompanying drawing 1 institute
Show)；
S103, set different stretching variablees and start drawing mechanism, can detect that tested fibre single thread is in different deformation
Raman absorption spike number ν in the case of amount ε；Draw the relation curve of ε Yu ν, after linear fit, calibrate slope s；The present embodiment ε
With the relation curve of ν as shown in Figure 3, the deformation quantity ε of tested fibre single thread 0%, 0.4%, 0.8%, 1.2% and respectively
1.8%, calibrating slope s after linear fit is-25.1cm-1/ %；In figure, abscissa is shape fiber variable Fiber Strain,
Vertical coordinate is Raman absorption spike number Raman wavenumber, and Linear fit slope is linear fit slope；
Reinforcing fiber after S104, employing step S101 process is combined with thermosetting resin or thermoplastic resin prepares fiber
Strengthen polymer matrix composites, and take bar shaped composite sample；
S105, bar shaped composite sample is fixed termination I and sample is fixed on termination II (as shown in Figure 2), drawing
Find the fiber in composite sample under graceful spectrogrph optical microscope, and the laser beam focus of laser Raman spectrometer is hung down
Directly it is radiated on reinforcing fiber microcell, it is thus achieved that the Raman absorption spike number of corresponding microcell；In the present embodiment, described Raman spectrometer
Optical microscope uses × 50 times of eyepieces；
S106, the stepping mechanism of unlatching sample load carrier, make composite sample have along level or fibre axis direction
Sequence moves setpoint distance, by the laser beam focus of laser Raman spectrometer on the different microcells of reinforcing fiber, it is thus achieved that the most micro-
The Raman absorption spike number in district；In the present embodiment, described setpoint distance is 0.05mm；
S107, set different stretching variablees and start drawing mechanism, composite is applied the stretching variable set, weight
Multiple step S106 and S107, obtain composite under conditions of different deformation amount, along drawing of fibre axis diverse location microcell
Graceful absworption peak wave number；As shown in Figure 4, in figure, abscissa is along fibre axis difference microcell to the testing result of the present embodiment
Position Position along the fiber, vertical coordinate is Raman absorption spike number Raman wavenumber, Matrix
Strain is composite deformation；
S108, employing following formula calculate the microcell strain stress of Fiber In Composite Material surface diverse locationx,
In formula, vxThe Raman absorption spike number obtained for step S105, S106 and S 107, v0It is zero for fiber surface stress
Time obtain Raman absorption spike number, s be step S103 obtain slope；Thus, composite is obtained in differently strained amount
In the case of, its internal reinforcing fiber strains along the microcell of fibre axis diverse location；The result of calculation of the present embodiment such as accompanying drawing 5 institute
Showing, in figure, abscissa is the position Distance along the fiber of reinforcing fiber length direction difference microcell, vertical coordinate
Microcell strain Local strain, Matrix Strain for reinforcing fiber surface are composite deformation；
S109, relation according to fibre stress strain, try to achieve composite by the case of different deformation amount, internal carbon
Fiber is along the micro-sized stress of fibre axis diverse location, and states with curve, and described curve is position-stress curve；
Position-the stress curve of the present embodiment is as shown in accompanying drawing 6 and accompanying drawing 7；In figure, abscissa is the position along fibre axis difference microcell
Putting Position along the fiber, vertical coordinate is composite subjected to stress Stress, and Stress fit is stress
Matching, Matrix Strain is composite deformation quantity；The composite deformation quantity of accompanying drawing 6 is 0%, 0.3%, 0.6%,
0.9% and 1.2%, the composite deformation quantity of accompanying drawing 7 is 1.5% and 1.8%；
Knowable to the analysis that above calculated Fiber In Composite Material surface diverse location microcell is strained, work as the external world
When the stress applying composite is zero, the stress of the fiber surface difference microcell obtained is reinforcing fiber and matrix resin
Produced residual stress in recombination process；This residual stress includes composite, and during forming and hardening, produced heat should
Power, composite are changed by ambient temperature is affected internal stress and the composite wood that fiber produces because the coefficient of expansion is different from resin
Material expands the internal stress produced by deformation between fiber and resin after absorbing the moisture content in environment；When outer bound pair composite is executed
When the stress added is certain setting value, the microcell strain of the fiber surface diverse location obtained is this composite by this stress
After strain between this microcell fiber and matrix resin；
The data of position-stress curve are fitted by S110, employing following formula,
In formula, EfFor the Young's modulus of reinforcing fiber, εmFor the strain of resin, l by composite the length of survey fiber
Degree, β uses below equation to try to achieve:
In formula, r1For the diameter of reinforcing fiber, EmFor the Young's modulus of resin matrix, VmAnd VfIt is respectively in composite
Resin matrix and the volume content of reinforcing fiber, GmAnd GfIt is respectively resin matrix and the modulus of shearing of reinforcing fiber.
G can be tried to achieve by below equation:
In formula, E is Young's modulus, and v is the Poisson's ratio of material；
S111, to the fitting data of step S110 gained according to below equation relative to position x derivation, i.e. can get interface
Shear strength τ；
In formula, r1Diameter for reinforcing fiber.The present embodiment composite by during differently strained amount along fibre axis not
The relation of the microcell interface shear strength of co-located is as shown in accompanying drawing 8,9 and 10, and in figure, abscissa is micro-along fibre axis difference
The position Distance along the fiber in district, vertical coordinate is composite material interface shear strength ISS；Matrix
Strain is composite dependent variable；The composite deformation quantity of accompanying drawing 8 is 0.3%, 0.6%, 0.9% and 1.2%, accompanying drawing 9
Composite deformation quantity be 1.5%, the composite deformation quantity of accompanying drawing 10 is 1.8%.
After composite is by extraneous stress, its stress is delivered to reinforcing fiber by interface, strong for interfacial adhesion
Spending high composite, the deformation of its reinforcing fiber is the most consistent or close with the deformation of matrix resin.But, usual resin base
The elongation at break of body be much larger than reinforcing fiber, so when composite deformation along with apply stress increase up to certain journey
When spending, its internal reinforcing fiber starts to occur to destroy fracture.And the number of fracture of fiber increases along with the increase of extraneous stress
Many, when the fibre length of fracture is short to a certain degree, and after it can bear the shearing force of resin boundary surface transmission, fiber will not be sent out again
Raw fracture, fiber number now reaches saturated.In this state, by the maximum interface shear strength measured by step S11
Critical interfaces shear strength for this composite.
It is evidenced from the above discussion that, side of the present invention detection device and method use micro-focusing Raman spectrometer, its laser beam light
Spot diameter is less than 2 microns, and measuring resolution is high, it is possible to deeply measure fiber-reinforced resin matrix compound material fiber and resin matrix
Interface microcell, test result is more accurate, solves the problem that conventional test methodologies test result error is bigger.The inventive method is not only
Can measure the residual stress between fiber and matrix resin, the critical shear that can not only measure fiber and matrix resin interface should
Power, can also measure composite when receiving ectocine, the interim microstress at interface simultaneously.The inventive method belongs to lossless
Detection, when not measuring interface critical shearing stress, does not has destructiveness to composite.
Obviously, present invention composite material interface based on laser Raman spectrometer shear strength detection device and method is useful
Having the technical effect that can be to the fibre single thread Raman absorption spike number of reinforcing fiber monofilament or composite inner and fibre single thread
Strain accurately detects, and provides basic data for calculating the residual stress of fiber surface microcosmos area, and thus calculates out-of-bounds
Face shear strength.
Claims (9)
1. composite material interface shear strength based on a laser Raman spectrometer detection device, it is characterised in that this detection
Device includes, laser Raman spectrometer, sample load carrier and drawing mechanism；Described sample load carrier, including, bearing frame
Termination I fixed by frame, sample, termination II fixed by sample, strain gauge, thousand points of measuring rulers and stress read-out display；Described hold
Carrying framework is rectangle and the underface being vertically mounted on laser beam, is installed with sample and fixes inside one end of its rectangular frame
Termination I, the other end is movably installed with sample and fixes termination II, thus constitutes the fixed mechanism of fixing sample to be tested；Described sample
One end of fixing termination I is fixed on inside bearing frame, and the other end is connected by strain gauge and sample to be tested are fixing；Described
Sample fixes that one end of termination II is fixing with sample to be tested to be connected, and the other end is through rectangular frame and passes through thousand points of measuring rulers and draws
Stretch mechanism to connect；Described stress read-out display electrically connects with strain gauge.
The most according to claim 1, composite material interface shear strength based on laser Raman spectrometer detection device, it is special
Levying and be, described sample load carrier is additionally provided with and promotes bearing frame according to the distance set along level or fibre axis direction
The stepping mechanism of movement.
The most according to claim 2, composite material interface shear strength based on laser Raman spectrometer detection device, it is special
Levying and be, described stepping mechanism belt pulley stepping mechanism, rack-and-pinion stepping mechanism or worm and gear stepping mechanism, it sets
Distance is 0.01mm-2.00mm.
The most according to claim 1, composite material interface shear strength based on laser Raman spectrometer detection device, it is special
Levying and be, the wavelength of described laser Raman spectrometer laser beam is 514nm or 633nm；The space of described laser Raman spectrometer
Resolution≤2 μm.
The most according to claim 1, composite material interface shear strength based on laser Raman spectrometer detection device, it is special
Levying and be, described drawing mechanism is provided with stretching variable adjusting means, and the range of accommodation of described stretching variable is 0.05%-
100%.
6. a composite material interface shear strength detection method based on laser Raman spectrometer, it is characterised in that use power
Profit requires that according to any one of 1 to 5, composite material interface shear strength based on laser Raman spectrometer detection device is to compound
Material interface shear strength detects, and comprises the following steps；
S101, for non-carbon-reinforced fiber use graphene fiber surface conditioning agent reinforcing fiber is carried out surface process, make non-
Carbon-reinforced fiber surface attachment has carbon atom, carbon-reinforced fiber is not the most made to any process；
S102, single fiber is sticked at the scraps of paper as sample, reinforcing fiber is fixedly connected on sample and fixes termination I and sample is solid
On fixed end II, and by the laser beam vertical irradiation of laser Raman spectrometer on reinforcing fiber surface；
S103, set different stretching variablees and start drawing mechanism, can detect that tested fibre single thread is in different deformation amount ε feelings
Raman absorption spike number ν under condition；Draw the relation curve of ε Yu ν, after linear fit, calibrate slope s；
Reinforcing fiber after S104, employing step S101 process is combined preparation fiber reinforcement with thermosetting resin or thermoplastic resin
Polymer matrix composites, and take bar shaped composite sample；
S105, bar shaped composite sample is fixed termination I and sample is fixed on termination II, at Raman spectrometer optical microscope
Under find the fiber in composite sample, and by micro-in reinforcing fiber for the laser beam focus vertical irradiation of laser Raman spectrometer
Qu Shang, it is thus achieved that the Raman absorption spike number of corresponding microcell；
S106, the stepping mechanism of unlatching sample load carrier, make composite sample move in order along level or fibre axis direction
Dynamic setpoint distance, by the laser beam focus of laser Raman spectrometer on the different microcells of reinforcing fiber, it is thus achieved that corresponding microcell
Raman absorption spike number；
S107, set different stretching variablees and start drawing mechanism, composite being applied the stretching variable set, repeats step
Rapid S106 and S107, obtains composite under conditions of different deformation amount, and the Raman along fibre axis diverse location microcell is inhaled
Receive spike number；
S108, employing following formula calculate the microcell strain stress of Fiber In Composite Material surface diverse locationx,
In formula, vxThe Raman absorption spike number obtained for step S105, S106 and S107, v0Obtain when being zero for fiber surface stress
The Raman absorption spike number obtained, s is the slope that step S103 obtains；Thus, the composite situation in differently strained amount is obtained
Under, its internal reinforcing fiber strains along the microcell of fibre axis diverse location；
S109, relation according to fibre stress strain, try to achieve composite in the case of different deformation amount, internal carbon fibers edge
The micro-sized stress of fibre axis diverse location, and state with curve, described curve is position-stress curve；
When the stress that outer bound pair composite applies is zero, the stress of the fiber surface difference microcell obtained is reinforcing fiber
The produced residual stress with matrix resin recombination process；When the stress that outer bound pair composite applies is certain setting value,
The microcell strain of the fiber surface diverse location obtained is this composite by this microcell fiber after this stress and matrix tree
Strain between fat；
The data of position-stress curve are fitted by S110, employing following formula,
In formula, EfFor the Young's modulus of reinforcing fiber, εmFor the strain of resin, l by composite the length of survey fiber, β adopts
Try to achieve by below equation:
In formula, r1For the diameter of reinforcing fiber, EmFor the Young's modulus of resin matrix, VmAnd VfIt is respectively resin base in composite
Body and the volume content of reinforcing fiber, GmAnd GfIt is respectively resin matrix and the modulus of shearing of reinforcing fiber.
G can be tried to achieve by below equation:
In formula, E is Young's modulus, and v is the Poisson's ratio of material；
S111, to the fitting data of step S110 gained according to below equation relative to position x derivation, i.e. can get cutting of interface
Shearing stress τ；
In formula, r1Diameter for reinforcing fiber.
The most according to claim 6, composite material interface shear strength detection method based on laser Raman spectrometer, it is special
Levying and be, the wavelength of described laser Raman spectrometer laser beam is 514nm or 633nm；The space of described laser Raman spectrometer
Resolution≤2 μm.
The most according to claim 6, composite material interface shear strength detection method based on laser Raman spectrometer, it is special
Levying and be, in step S103, the set point of described stretching variable is 0.05%-100%.
The most according to claim 6, composite material interface shear strength detection method based on laser Raman spectrometer, it is special
Levying and be, in step 106, described setpoint distance is 0.01mm-2.00mm.
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