CN114839092B - Interlayer fracture toughness testing method for 1D and 2D continuous fiber reinforced ceramic matrix composite materials - Google Patents

Interlayer fracture toughness testing method for 1D and 2D continuous fiber reinforced ceramic matrix composite materials Download PDF

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CN114839092B
CN114839092B CN202210477073.4A CN202210477073A CN114839092B CN 114839092 B CN114839092 B CN 114839092B CN 202210477073 A CN202210477073 A CN 202210477073A CN 114839092 B CN114839092 B CN 114839092B
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CN114839092A (en
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师维刚
张程煜
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Northwestern Polytechnical University
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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
    • G01N3/32—Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • 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
    • G01N2203/0001—Type of application of the stress
    • G01N2203/0005—Repeated or cyclic
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    • 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
    • G01N2203/006—Crack, flaws, fracture or rupture
    • G01N2203/0062—Crack or flaws
    • G01N2203/0064—Initiation of crack
    • 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
    • G01N2203/006—Crack, flaws, fracture or rupture
    • G01N2203/0062—Crack or flaws
    • G01N2203/0066—Propagation of crack
    • 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
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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
    • G01N2203/067—Parameter measured for estimating the property
    • G01N2203/0682—Spatial dimension, e.g. length, area, angle
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Abstract

The invention relates to a method for testing interlayer fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composite materials, which comprises the steps of clamping a wedge-shaped pressure head and a DCB sample on a universal testing machine, aligning the tip of the wedge-shaped pressure head with a fracture sample prefabricated notch, applying loading force for multiple times, measuring respective loading force-time data when the crack extension length is a 1,a2,a3,a4,a5, and drawing loading curves F y -delta with different crack lengths; programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length aAccording to the formulaAnd calculating the energy release rate, and drawing a crack resistance curve of G Ic -a. The method does not need to manufacture a specific hinged clamp, and realizes the measurement of the high-temperature I-type fracture toughness of the CFCC material on the basis.

Description

Interlayer fracture toughness testing method for 1D and 2D continuous fiber reinforced ceramic matrix composite materials
Technical Field
The invention belongs to the field of continuous fiber reinforced ceramic matrix composite materials, and relates to a method for testing interlayer fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composite materials.
Background
The continuous fiber reinforced ceramic matrix composite (CFCC) has the advantages of high strength ratio, high modulus ratio, corrosion resistance, oxidation resistance and the like, and is an important thermal structure material in the fields of aerospace and the like. The CFCC prepared by adopting the unidirectional tape (1D) or the woven fiber cloth laminated layer (2D) has the advantages of convenient design, simple preparation and excellent in-plane performance, and is widely used in aerospace structural members. Such continuous fiber ceramic matrix composites having a 1D or 2D structure may be subject to loads such as bending, compression, out-of-plane impact or thermal shock, which may cause delamination due to interlayer cracking, and thus delamination resistance must be evaluated. Crack opening (type I) delamination failure is the predominant form by structural delamination failure event statistics. The delamination resistance can be effectively evaluated by characterizing the type I interlayer fracture toughness of the 1D/2D-CFCC using the interlayer fracture Energy Release Rate (ERR).
At present, no standard is formed for the type I interlayer fracture toughness test method of the room temperature 1D/2D-CFCC at home and abroad, and a commonly adopted Double Cantilever Beam (DCB) sample stretching method is developed based on the type I fracture toughness test standard ASTM D5528 of the resin-based composite material. The DCB sample herein has a laminated plate type structure, and a gap of a certain length and width is formed along the layer surface at the center of the layer thickness. As shown in fig. 1. In the testing process, the tester clamp symmetrically stretches the two sides of the notch-containing end of the sample in the direction perpendicular to the layer thickness to cause cracking of the bottom end of the notch of the sample, and the I-type energy release rate of the sample is obtained through calculation of loading force-displacement data recorded by the tester. The test principle is shown in fig. 2. The difficulty of the DCB specimen tensile test method is that: 1. because the layer thickness of the tested CFCC material is generally not more than 4mm, the clamp and the sample can only be adhered by adopting an adhesive method when two sides of a notch of the reverse tensile sample, so that the sample and the clamp need to be adhered in advance during testing; 2. due to the adoption of the reverse stretching method, the symmetry of the stretching force needs to be ensured, and the centering requirement on the test machine and the fixture installation is high. Therefore, the I-type interlayer fracture toughness testing method for 1D/2D-CFCC, which is simple and convenient to operate and accurate in testing, is provided as a technical difficulty.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for testing the interlayer fracture toughness of a 1D and 2D continuous fiber reinforced ceramic matrix composite material, which has the characteristics of simple operation, convenience and accurate measurement.
Technical proposal
A method for testing interlayer fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composite materials is characterized by comprising the following steps:
step 1: designing and processing a DCB test sample, wherein the DCB test sample is rectangular with length and thickness along the layering direction and width of the layering section; one side of the DCB test sample is provided with a prefabricated notch along the layering direction in the layer thickness direction;
Step 2: designing and processing a wedge-shaped pressure head structure, and giving the material type and the Mohs hardness index of the wedge-shaped pressure head;
step 3: measuring the sliding friction coefficient of the wedge-shaped pressure head and the sample material by adopting an existing arbitrary method, and measuring at least 5 groups of data, wherein the discrete coefficient of the data is less than 10%;
step 4: clamping the wedge-shaped pressure head and the DCB test sample on a universal testing machine, and aligning the tip of the wedge-shaped pressure head to a prefabricated notch of the DCB test sample;
Step 5: setting parameters of a testing machine, wherein the displacement control range is 0.1-1.0 mm/min, the measuring range of a force sensor of the testing machine is recommended to 100-200N, and the accuracy requirement is 0.1-0.5% FS;
step 6: starting the testing machine, stopping loading when the crack at the bottom end of the notch grows by 1.0-2.0 mm plus or minus 0.2mm, and withdrawing the wedge-shaped pressure head at 25 mm/min;
step 7: loading the DCB test sample for multiple times, stopping loading when the crack extension length is a 1,a2,a3,a4,a5 each time, storing loading force-time data, and returning the wedge-shaped pressure head at 25 mm/min;
Once the crack is found to be rapidly propagated or a plurality of cracks are generated during each loading, the subsequent loading test should be abandoned, but at least effective measurement data is ensured to be 3 times, otherwise, the test needs to be reworked;
step 8: stopping the testing machine, taking out the test sample, and packaging and storing;
Step 9: according to loading force-time data when cracks with different extension lengths are loaded, loading curves F y -delta with different crack lengths are drawn;
Wherein the method comprises the steps of F is the loading force recorded by the testing machine and N is the crack expansion force; alpha is the angle of the wedge-shaped pressure head, and mu is the dynamic friction coefficient between the wedge-shaped pressure head and the test sample;
Delta=2tan (α/2) vt is the load end opening displacement, mm; v is the loading rate, mm/min; t is loading time, min;
Step 10: programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length a
Wherein F y c is the crack propagation force maximum;
Step 11: according to the formula And calculating the energy release rate, and drawing a crack resistance curve of G Ic -a.
Wherein G Ic is the I-type fracture energy release rate, F y c is the inflection point of the F y -delta curve changing from linear to nonlinear, and B is the width of the sample, and mm; delta is the intercept of the compliance calibration curve with the axis of abscissa, mm.
The width of the rectangle is 5-10 mm plus or minus 0.1mm.
The length of the prefabricated notch is 10-20 mm plus or minus 0.1mm, and the width of the prefabricated notch in the layer thickness direction is 0.2-0.3 mm.
And the displacement control error in the step 5 is not more than 1%.
The crack length is defined as the perpendicular line distance between the crack tip and the top end of the sample notch, and the measurement accuracy is not less than 0.2mm.
Advantageous effects
According to the interlayer fracture toughness testing method for the 1D and 2D continuous fiber reinforced ceramic matrix composite material, a wedge-shaped pressure head and a DCB sample are clamped on a universal testing machine, the tip of the wedge-shaped pressure head is aligned to a fracture sample prefabricated notch, loading force is applied for multiple times, the loading force-time data when the crack extension length is a 1,a2,a3,a4,a5 are measured, and loading curves F y -delta with different crack lengths are drawn; programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length aAccording to the formula/>And calculating the energy release rate, and drawing a crack resistance curve of G Ic -a. The method does not need to manufacture a specific hinged clamp, and realizes the measurement of the high-temperature I-type fracture toughness of the CFCC material on the basis.
The invention has the advantages of simple and convenient operation and accurate measurement. The concrete steps are as follows:
1. Compared with the DCB sample testing method, the method does not need to manufacture a specific hinged clamp;
2. compared with the DCB sample testing method, the method does not need to paste the hinged clamp and the sample before the pre-application;
3. The method only needs to complete the centering between the tip of the wedge-shaped pressure head and the notch of the sample, but the DCB sample method needs to complete the centering of the upper and lower articulated clamps (ensuring the stress symmetry) when the sample is glued, and also needs to complete the centering of the articulated clamps in the loading process;
4. The method does not adopt an adhesive method (no colloid capable of keeping high strength for a long time in a high-temperature environment) in a DCB method to clamp a test piece, so that the measurement of the high-temperature I-type fracture toughness of the CFCC material can be realized on the basis.
Drawings
FIG. 1 shows a test specimen 60mm in length and 10mm in width;
a: front view, b: top view, c: oblique view
FIG. 2 DCB sample test method;
FIG. 3 wedge angle 60 wedge ram;
a: front view, b: top view, c: oblique view
FIG. 4 wedge indenter sample loading method;
FIG. 5 is a graph of the crack between test specimen layers;
FIG. 6 is an enlarged view of a fracture surface of the test specimen;
FIG. 7 is a graph of tensile force versus expansion displacement for test specimens of different crack lengths;
FIG. 8 is a plot of test specimen compliance calibration;
fig. 9 tests the energy release rate of the test specimen.
Detailed Description
The invention will now be further described with reference to examples, figures:
In the description of the present invention, it should be understood that the terms "wedge", "wedge angle", "ply direction", "layer thickness direction", "width", "gap top", "gap bottom", "gap sides", "loading end", and the like are shape descriptions and orientation-directed to the drawings for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.
The technical scheme of the invention is as follows: a wedge-shaped indenter for testing 1D/2D-CFCC type I fracture toughness, characterized by: 1) The geometric feature is a symmetrical wedge body, the wedge angle is 30-60 degrees; 2) The wedge ram material is recommended to have a mohs hardness of 9 or more (including 9), and the sliding friction coefficient is recommended to be 0.1 to 0.3.
A method for testing 1D/2D-CFCC type I fracture toughness is characterized by comprising the following specific steps:
step one: the DCB sample is precisely processed, the structure is shown in figure 1, wherein the length of a prefabricated notch is recommended to be 10-20 mm plus or minus 0.1mm, the width of the sample is recommended to be 5-10 mm plus or minus 0.1mm, and the width of the notch in the layer thickness direction is 0.2-0.3 mm;
step two: designing and processing a wedge-shaped pressure head structure as shown in fig. 3, and marking the type of materials and the Mohs hardness index;
Step three: measuring the sliding friction coefficient of the wedge-shaped pressure head and the sample material by adopting an existing arbitrary method, measuring at least 5 groups of data, marking a data discrete coefficient, wherein the discrete coefficient is less than 10%;
Step four: clamping the wedge-shaped pressure head and the test sample on a universal testing machine according to the diagram shown in fig. 4, and centering the tip of the wedge-shaped pressure head and a pre-notch of the broken sample through an optical microscope;
Step five: setting parameters of a testing machine, adopting displacement control, wherein the recommended range is 0.1-1.0 mm/min, and the control error is not more than 1%; the measuring range of the force sensor of the testing machine is recommended to be 100-200N, and the accuracy requirement is 0.1-0.5% FS;
step six: starting the testing machine, observing crack initiation at the bottom end of the notch through an optical microscope, stopping loading when the crack is expanded by 1.0-2.0 mm plus or minus 0.2mm, and withdrawing the wedge-shaped pressure head at 25 mm/min;
Step seven: loading the sample again, stopping loading when the crack extension length is a 1 through an optical microscope, storing loading force-time data, and withdrawing the wedge-shaped pressure head at 25 mm/min;
note that: the crack length is defined as the perpendicular distance between the crack tip and the top of the specimen notch, and the measurement accuracy is not less than 0.2mm.
Step eight: in accordance with step seven, recording the respective loading force-time data when the crack extension length is a 2,a3,a4,a5;
Note that: in the above steps, once the crack is found to propagate rapidly or a plurality of cracks are generated, the subsequent loading test should be abandoned, but at least the effective measurement data is ensured to be 3 times, otherwise, the test needs to be reworked.
Step nine: stopping the testing machine, taking out the test sample, and packaging and storing;
Step ten: according to loading force-time data when cracks with different extension lengths are loaded, loading curves F y -delta with different crack lengths are drawn;
Wherein the method comprises the steps of F is the loading force recorded by the testing machine and N is the crack expansion force; alpha is the angle of the wedge-shaped pressure head, and mu is the dynamic friction coefficient between the wedge-shaped pressure head and the test sample.
Delta=2tan (α/2) vt is the load end opening displacement, mm; v is the loading rate, mm/min; t is the loading time, min.
Step eleven: programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length a
Wherein F y c is the crack propagation force maximum.
Step twelve: according to the formulaAnd calculating the energy release rate, and drawing a crack resistance curve of G Ic -a.
Wherein G Ic is the I-type fracture energy release rate, F y c is the inflection point of the F y -delta curve changing from linear to nonlinear, and B is the width of the sample, and mm; delta is the intercept of the compliance calibration curve with the axis of abscissa, mm.
Specific examples:
The adopted material is 2D CVI plain weave C/SiC, which is provided by a major laboratory of ultra-high temperature structural composite materials of northwest industrial university, and the thickness of the two-dimensional carbon fiber reinforced carbon-based composite material is generally several millimeters due to the limitation of a chemical vapor deposition (CVI), and a wide flat plate with the thickness of 3mm is selected to process a sample in the example.
Step one: referring to FIG. 1, an original sample sheet having a width of 10.0mm, a length of 60.0mm and a layer thickness of 3.0mm was prepared, and a long notch having a length of 10.0mm was cut at the center of the layer thickness in the direction of the fiber lay-up of the sheet by a diamond saw blade cutter having a thickness of 0.25 mm. The actual width of the notch is 0.3mm.
Step two: referring to fig. 3, a wedge-shaped indenter having an angle of 60 ° was prepared using a zirconia material, and the mohs hardness was 9.0;
step three: the dynamic friction coefficient between the wedge-shaped pressure head and the test sample is 0.21, and the discrete coefficient is 9%;
Step four: as shown in fig. 4, the test specimen is mounted at a lower fixture, a wedge-shaped pressure head is mounted at an upper fixture, a gap is reserved between the tip of the wedge-shaped pressure head and a broken test specimen by an optical microscope, a straight ruler with the scale of 1mm is placed beside the test specimen and parallel to the layering direction, and the straight ruler is used as a crack propagation position mark;
Step five: setting the loading displacement rate of the electronic universal testing machine to be 0.5mm/min, measuring range of a force sensor to be 100.0N, and the precision to be 0.3%FS;
Step six: loading the sample, observing crack initiation at the end of the notch through an optical microscope lens, stopping loading when the expansion length is 1mm, and rapidly retracting the wedge-shaped pressure head at25 mm/min. The crack tip was 11.0mm from the loading end length at this time and was noted as the initial crack length.
Step seven: the sample was reloaded, and the loading was stopped when a crack propagation length of 5.0mm was observed by an optical microscope, and the loading force-time data was saved, and the wedge ram was rapidly retracted at 25 mm/min. The crack length at this time was 16.0mm.
Step eight: in agreement with step seven, the respective loading force-time data were recorded for crack growth lengths of 21.0mm,26.0 mm;
step nine: after the crack growth length was 26.0mm, the crack growth rate was increased, and the test was stopped, and the sample was taken out. Sample type I cracking is shown in figure 5. At the same time, the fracture surface characteristics of the test specimen were recorded as shown in fig. 6.
Step ten: drawing loading curves F y -delta with different crack lengths, as shown in FIG. 7;
Step eleven: programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length a As shown in fig. 8.
Step twelve: according to the formulaThe energy release rate is calculated. FIG. 9 shows a crack resistance curve exhibiting a smooth characteristic, and measured energy release rates of 120.0J/m 2,91.0J/m2,94.1J/m2,111.4J/m2, respectively, with an average value of 104.1J/m 2, and a dispersion coefficient of 13%.

Claims (5)

1. A method for testing interlayer fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composite materials is characterized by comprising the following steps:
step 1: designing and processing a DCB test sample, wherein the DCB test sample is rectangular with length and thickness along the layering direction and width of the layering section; one side of the DCB test sample is provided with a prefabricated notch along the layering direction in the layer thickness direction;
Step 2: designing and processing a wedge-shaped pressure head structure, and giving the material type and the Mohs hardness index of the wedge-shaped pressure head;
step 3: measuring the sliding friction coefficient of the wedge-shaped pressure head and the sample material by adopting an existing arbitrary method, and measuring at least 5 groups of data, wherein the discrete coefficient of the data is less than 10%;
step 4: clamping the wedge-shaped pressure head and the DCB test sample on a universal testing machine, and aligning the tip of the wedge-shaped pressure head to a prefabricated notch of the DCB test sample;
Step 5: setting parameters of a testing machine, wherein the displacement control range is 0.1-1.0 mm/min, the measuring range of a force sensor of the testing machine is recommended to 100-200N, and the accuracy requirement is 0.1-0.5% FS;
step 6: starting the testing machine, stopping loading when the crack at the bottom end of the notch grows by 1.0-2.0 mm plus or minus 0.2mm, and withdrawing the wedge-shaped pressure head at 25 mm/min;
step 7: loading the DCB test sample for multiple times, stopping loading when the crack extension length is a 1,a2,a3,a4,a5 each time, storing loading force-time data, and returning the wedge-shaped pressure head at 25 mm/min;
Once the crack is found to be rapidly propagated or a plurality of cracks are generated during each loading, the subsequent loading test should be abandoned, but at least effective measurement data is ensured to be 3 times, otherwise, the test needs to be reworked;
step 8: stopping the testing machine, taking out the test sample, and packaging and storing;
Step 9: according to loading force-time data when cracks with different extension lengths are loaded, loading curves F y -delta with different crack lengths are drawn;
Wherein the method comprises the steps of F is the loading force recorded by the testing machine and N is the crack expansion force; alpha is the angle of the wedge-shaped pressure head, and mu is the dynamic friction coefficient between the wedge-shaped pressure head and the test sample;
Delta=2tan (α/2) vt is the load end opening displacement, mm; v is the loading rate, mm/min; t is loading time, min;
Step 10: programming and drawing a compliance calibration curve according to the obtained effective loading curve and the corresponding crack initiation length a
Wherein F y c is the crack propagation force maximum;
Step 11: according to the formula Calculating the energy release rate, and drawing a crack resistance curve of G Ic -a;
Wherein G Ic is the I-type fracture energy release rate, F y c is the inflection point of the F y -delta curve changing from linear to nonlinear, and B is the width of the sample, and mm; delta is the intercept of the compliance calibration curve with the axis of abscissa, mm.
2. The method for testing the interlaminar fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composites according to claim 1, wherein: the width of the rectangle is 5-10 mm plus or minus 0.1mm.
3. The method for testing the interlaminar fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composites according to claim 1, wherein: the length of the prefabricated notch is 10-20 mm plus or minus 0.1mm, and the width of the prefabricated notch in the layer thickness direction is 0.2-0.3 mm.
4. The method for testing the interlaminar fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composites according to claim 1, wherein: and the displacement control error in the step 5 is not more than 1%.
5. The method for testing the interlaminar fracture toughness of 1D and 2D continuous fiber reinforced ceramic matrix composites according to claim 1, wherein: the crack length is defined as the perpendicular line distance between the crack tip and the top end of the sample notch, and the measurement accuracy is not less than 0.2mm.
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