CN104777051A - Test method for carbon fiber micro-zone relative hardness - Google Patents
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Abstract
The invention discloses a test method for carbon fiber micro-zone relative hardness. The method is characterized by including: soaking at least two different carbon fiber samples in acetone, then performing drying, and cutting the samples into small segment carbon fiber samples; conducting mechanical test on the treated carbon fiber samples respectively by an atomic force microscope and a high hardness single crystal diamond probe, processing the test data by data processing software to obtain a pressure-displacement curve relation diagram, wherein the vertical coordinate represents the pressure applied by a needle tip to carbon fiber during carbon fiber micromechanics analysis and the unit is nano-newton, the horizontal coordinate represents the total deformation quantity of carbon fiber and needle tip cantilever within certain linear range, and the unit is nanometer. The slope of the force curve can qualitatively represent the hardness of carbon fiber, the greater the hardness is, the higher the force curve slope absolute value. The invention provides a simple and convenient evaluation criterion for qualitative evaluation of the carbon fiber micro-zone relative hardness, and has important significance in studying how to obtain high quality and high performance carbon fiber.
Description
Technical field
The invention belongs to the method carrying out analysis of material by means of the character measuring material, relate to a kind of method of testing of carbon fiber microcell relative hardness.The invention provides a kind of sign evaluation method of mechanical property test of carbon fiber, be applicable to the microcell relative hardness describing carbon fiber qualitatively.
Background technology
Carbon fiber be carbon content higher than 90% inorganic polymer fiber, be the micro crystal graphite material obtained after carbonization and graphitization processing by organic fiber.It has, and intensity is large, modulus is high, density is low, thermal expansivity is little, high temperature resistant, antifatigue, anticorrosive, a series of excellent performance such as rub resistance and self-lubricating.As the one of high-performance fiber, the inherent characteristic of the existing material with carbon element of carbon fiber, have both again the soft processibility of textile fibres, it is the most important reinforcing material of advanced composite material, obtain widespread use, from civilian industries such as space flight, aviation, automobile, electronics, machinery, chemical industry, light textiles to sports equipment and leisure goods etc. in every field that is military and civilian industry.Therefore, carbon fiber is considered to the Typical Representative of infant industry material in high-tech area.Carbon fiber industry, in developed country's mainstay industry and even in overall economic performance raising, plays very important effect.To the adjustment of Industry Structure and the update of traditional material also significant, have very important impact to defence and military and national economy.
China starts the carbon fiber research and development history of existing nearly 60 years so far from the sixties in 20th century, but make slow progress, simultaneously because developed country is to the blockade on new techniques of China's decades, so far large-scale industrial production could not be realized, the long-term dependence on import of demand of industry and civil area, has had a strong impact on the development of China's hi-tech.Compared with the country of carbon fiber production advanced level in the world, on quality and quantity, gap is bigger and bigger, so, development and production high-performance, high-quality carbon fiber, to meet the demand of military project and the product for civilian use, reversing the situation of a large amount of import, is the urgent task of current China Industry of Carbon Fiber development.
The macro property of carbon fiber determined by its micromechanism, understands fully the microstructure characteristic of carbon fiber, prepares high-performance carbon fibre have directive significance for research.Carbon fiber characterization method is a lot, and current Chinese scholars is mainly analyzed the state of aggregation of carbon fiber, morphosis, surface physics state and surface chemistry conditions etc.Concrete characterizing method and selecting of pertinent instruments see the following form 1:
Table 1: the characterizing method of carbon fiber and pertinent instruments
X-ray diffraction (XRD) is the common method to carbon fiber micromechanism, and we can be measured the interplanar distance of carbon fiber, the information such as crystallite dimension and crystallinity by X-ray diffraction.Raman spectrum (Raman) analyzes a kind of method of the research for molecular structure, crystallographic structure, compound qualitative and quantitative analysis.Transmission electron microscope (TEM) is the instrument and equipment can observing carbon fiber crystalline state intuitively.The information such as the overall pattern of carbon fiber and surfaceness can be passed through the analyses of atomic force microscope (AFM), scanning electron microscope (SEM) and scanning tunnel microscope (STM) and obtain.Surface chemistry conditions characterizes and main relies on x-ray photoelectron power spectrum (XPS), and x-ray photoelectron power spectrum is based on photoionization effect, and it is relevant that the photoelectronic energy of its outgoing only combines energy with the energy of incident photon and atomic orbital.
The performance of carbon fiber is determined by its heterogeneous microstructure.Therefore, the sign of micromechanism is very important to raising carbon fiber performance.The structure of carbon fiber belongs to two-dimentional random graphits structure, and along with the change of process conditions, two-dimentional random graphits structure also can change thereupon.They will affect the final performance of carbon fiber in various degree.Therefore to the sign of these structures, how to obtain high-quality carbon fiber have great meaning by researching and analysing us.Along with the development of modern science and technology, the instrument of research fibre structure is also day by day advanced, and research method reaches its maturity.The correlativity of further investigation carbon fiber micromechanism and its mechanical property, improves carbon fiber production Technology, the main flow direction that the mechanical property improving carbon fiber will be Carbon Fiber Technology development.
The heterogeneous microstructure of carbon fiber comprises several aspects such as surface structure, graphite microcrystalline structure, pore texture, orientation texture.The shape of crystallite, size, orientation and arrangement mode are relevant with the preparation technology of fiber, there is the defect on various both macro and micro, and these defects produce conclusive impact to the intensity, modulus etc. of carbon fiber.Thus, to the sign of carbon fiber micromechanism and the analysis of Micro Zone Mechanical Properties, understand fully the architectural feature of more current high-performance commodity carbon fibers, we are researched and analysed and how to obtain high-quality, high performance carbon fiber has great meaning.
Summary of the invention
Object of the present invention is intended to overcome deficiency of the prior art, provides a kind of method of testing of carbon fiber microcell relative hardness, thus provides one can qualitative characterization and evaluate carbon fiber microcell (1 × 1 micron
2in scope) method of relative hardness, it is by the restriction of carbon fiber diameter, density, production batch and different company's product structure, and whether do not distinguish is high strength or high-modulus and high-strength high-modules carbon fibre simultaneously.The present invention is that the size of qualitative evaluation carbon fiber microcell relative hardness provides a kind of more simple and easy to do evaluation method.
Content of the present invention is: a kind of method of testing of carbon fiber microcell relative hardness, is characterized in that: comprise the following steps:
A, carbon fiber samples are except slurry: at least two different carbon fiber samples are put into acetone respectively and soaks 96h, then dry at 80 DEG C of temperature, obtain dry carbon fiber samples;
B, the carbon fiber samples of drying is cut into segment respectively, obtains segment carbon fiber samples, for subsequent use;
C, before testing sample with atomic force microscope (be called for short AFM), single-crystal diamond probe is utilized to do force curve calibration to monocrystalline silicon piece substrate;
D, sample test and test data process: segment carbon fiber samples is placed in monocrystalline silicon piece substrate, with atomic force microscope to segment carbon fiber samples at 1 × 1 micron
2adamas probe is utilized to carry out mechanical test within the scope of microcell; The test data treated (such as: after the data processing software process such as origin software) of sample obtains the pressure force-displacement curve graph of a relation of carbon fiber, ordinate representative in carbon fiber Micromechanics Analysis process needle point to carbon fiber institute applied pressure, unit is for receiving ox, horizontal ordinate represents carbon fiber and the deformation quantity total in range of liner of tip, and unit is nanometer;
Different segment carbon fiber samples after tested and process obtain the pressure force-displacement curve graph of a relation of carbon fiber respectively;
E, data analysis, formulation process is as follows:
In mensuration process, total deformation quantity is:
Z＝Z
tip+δ (1)
In formula: the deformation quantity that Z-is total; Z
tipthe deformation quantity of-(single-crystal diamond probe) tip; The deformation quantity of δ-carbon fiber;
Formula is expressed as further:
In formula: the acting force in F-mensuration process; K
tipthe nominal force constant of-tip;
Read when being subject to uniform pressure F from pressure force-displacement curve graph of a relation, the total deformation quantity Z corresponding to different carbon fiber;
(the pressure force-displacement curve graph of a relation obtained, uses Origin software analysis, can directly read when being subject to identical directed force F from figure, the total deformation quantity Z corresponding to different carbon fiber);
Identical F and different Z is substituted into formula (2), the force constant K of tip in mensuration process
tipbe constant, obtain the formula that two δ are different, two formulas are subtracted each other, draw the size of δ, be i.e. the size of the deformation quantity of carbon fiber;
According to Hertz model:
In formula: R-atomic force microscope probe tip end radius, K-is effective Young modulus, and relevant with the Young modulus of needle point and carbon fiber and Poisson ratio, its pass is:
In formula: E
f, υ
fbe respectively Young modulus and the Poisson ratio of carbon fiber, E
tip, υ
tipfor pattern modulus and the Poisson ratio of needle point, relevant with the material of needle point; Because the present invention adopts the adamas probe of high rigidity, its E
tipvery large, υ
tipvery little, and be that constant is constant in testing, in high-strength carbon fiber test, make the modulus change of K value to high-strength carbon fiber more responsive, to ensure in test process the judgement of modulus of carbon fibres and resolution; Therefore, can judge from analysis: effectively Young modulus is larger, then the Young modulus of carbon fiber and hardness larger;
The size of carbon fiber deformation quantity δ is relevant to K, if: (deformation quantity of the second carbon fiber) δ
2< δ
1(deformation quantity of the first carbon fiber), then K
2>K
1, then (can think): the hardness of the second carbon fiber is greater than the hardness of the first carbon fiber.
In content of the present invention: in the process of sample test described in steps d, the test of different segment carbon fiber samples all uses same probe to test.
In content of the present invention: described equipment is atomic force microscope, because carbon fiber has high strength and modulus characteristic, the single-crystal diamond probe of high rigidity need be adopted to analyze carbon fiber, single crystal substrates is utilized to calibrate force curve before testing, again Micromechanics Analysis is done to carbon fiber, with same probe in test process, to ensure in test process, needle type radius and cantilever spring modulus constant;
In content of the present invention: described within the scope of microcell (namely 1 × 1 micron
2) analyze carbon fiber stiffness characteristics, it is by the restriction of carbon fiber diameter, density, production batch and different company's product structure, and whether do not distinguish is high strength or high-modulus and high-strength high-modules carbon fibre simultaneously;
In content of the present invention: described atomic force microscope can adopt NSK (Seiko) company SPA300HV type atomic force microscope.
The present invention is that the size of qualitative evaluation carbon fiber microcell relative hardness provides a kind of more simple and easy to do evaluation criterion, and namely general hardness is larger, then force curve slope absolute value is higher.
Compared with prior art, the present invention has features and beneficial effect:
(1) the present invention adopts atomic force microscope, high strength single-crystal diamond probe is utilized to characterize carbon fiber microcell relative hardness, inquire into the difference of carbon fiber in Micro Zone Mechanical Properties, analyze the impact of these differences on macro property, not only reference can be provided for selecting when preparing compound substance carbon fiber, more the theoretical foundation of science can be provided for the development of domestic high-performance carbon fibre;
(2) adopt the present invention, can characterize the micromechanism of carbon fiber further, thus reach the object improving carbon fiber performance;
(3) adopt the present invention, the size of energy qualitative evaluation carbon fiber microcell relative hardness, for next step Quantitative Study lays the first stone;
(4) adopt the present invention, simple and easy to do to the evaluation criterion of the size of carbon fiber microcell relative hardness, namely can be judged the hardness of carbon fiber by the slope absolute value of force curve, general slope absolute value is higher, then hardness is larger;
(5) adopt the present invention, simple to the testing process of carbon fiber, data processing is not numerous and diverse, and the image obtained is directly perceived, can compare the hardness level of carbon fiber easily;
(6) adopt the present invention, as can be seen from the derivation of equation, the conclusion obtained is scientific strong;
(7) the present invention operates and uses easily, practical.
Accompanying drawing explanation
Fig. 1 is the pressure force-displacement curve graph of a relation of domestic T700 (3) in embodiment 1 after the process of Origin software and toray T700 (2) carbon fiber, and in figure, ordinate is added load unit for receiving ox, abscissa unit is nanometer; In figure: 2 is that toray T700,3 is for domestic T700;
Fig. 2 is the pressure force-displacement curve graph of a relation of 4 kinds of carbon fibers after the process of Origin software in embodiment 2, and in figure, ordinate is added load unit for receiving ox, abscissa unit is nanometer; In figure: 1 be domestic T800,2 be toray T700,3 be domestic T700,4 for domestic T300;
Fig. 3 is the pressure force-displacement curve graph of a relation of the carbon fiber of toray T700 (2) and domestic T700 (3), T800 (1) comparing result under top load after the process of Origin software in embodiment 2, and in figure, ordinate is added load unit for receiving ox, abscissa unit is nanometer; In figure: 1 be domestic T800,2 be toray T700,3 for domestic T700.
Embodiment
The invention will be further described for embodiment plan given below; but can not be interpreted as it is limiting the scope of the invention; some nonessential improvement and adjustment that person skilled in art makes the present invention according to the content of the invention described above, still belong to protection scope of the present invention.
Embodiment 1:
A method of testing for carbon fiber microcell relative hardness, step is as follows:
One, the preparation of sample is tested
1. experiment material
Domesticly be equivalent to toray T700 grade carbon fiber (being called for short domestic T700), toray T700 carbon fiber, acetone; The mechanical performance index of two kinds of carbon fibers is as shown in table 2 below.
Table 2: the mechanical performance index of two kinds of carbon fibers
2. sample is except slurry
Two kinds of carbon fibers are put into acetone and soaks 96h, dry for standby at 80 DEG C.
3. sample shear
Single fiber is cut into segment, is placed in monocrystalline silicon piece substrate.
Two, sample test
This experiment NSK (Seiko) company SPA300HV type atomic force microscope is tested.Before sample test, force curve calibration is done to monocrystalline silicon piece substrate, then Micromechanics Analysis is done to carbon fiber, with same probe in test process.
Test process is as follows:
Three, data processing
1. drawing image
By measured data importing Origin, obtain the pressure force-displacement curve graph of a relation of two kinds of carbon fibers, ordinate is representative needle point in carbon fiber Micromechanics Analysis process is the deformation quantity total in range of liner of carbon fiber and tip to carbon fiber institute applied pressure, horizontal ordinate.
2. graphical analysis
See the force-displacement curve graph of a relation that Fig. 1, Fig. 1 are domestic T700 after the process of Origin software and toray T700 carbon fiber, in figure, ordinate is added load unit for receiving ox, abscissa unit is nanometer.
In mensuration process, total deformation quantity is:
Z＝Z
tip+δ (1)
In formula: the deformation quantity that Z-is total; Z
tipthe deformation quantity of-tip; The deformation quantity of δ-carbon fiber.
Formula is expressed as further:
In formula: F-is the acting force in mensuration process; K
tipthe force constant of-tip;
Therefore, have in the process of force curve measuring domestic T700 and toray T700 carbon fiber:
Using Origin software analysis, reading when being subject to identical directed force F, total deformation quantity Z, getting arbitrarily ordinate is F=221nN, reads deformation quantity Z total in mensuration process
1=43.14nm, Z
2=37.64nm.
The force constant K of tip in mensuration process
tipbe constant, then have: δ
2-δ
1=-5.5nm, illustrates that the deformation quantity of toray T700 in mensuration process is less than domestic T700, i.e. δ
2< δ
1, according to Hertz model:
have: K
2> K
1.
In sum, the hardness of toray T700 is greater than domestic T700, and the difference of this Micro Zone Mechanical Properties also just result in two kinds of carbon fibers some differences in stretch modulus.
Embodiment 2:
A method of testing for carbon fiber microcell relative hardness, step is as follows:
One, the preparation of sample is tested
1. experiment material
Toray T700, and be domesticly equivalent to eastern beautiful T300, T700, and T800 grade carbon fiber (being called for short domestic T300, domestic T700, domestic T800 respectively), acetone.
2. sample is except slurry
4 kinds of carbon fibers are put into acetone and soaks 96h, dry for standby at 80 DEG C.
3. sample shear
Single fiber is cut into segment, is placed in substrate of glass.
Two, sample test
This experiment NSK (Seiko) company SPA300HV type atomic force microscope is tested.Before sample test, force curve calibration is done to monocrystal silicon substrate, then Micromechanics Analysis is done to carbon fiber, with same probe in test process.
Three, data processing
1. drawing image
By measured data through the process of Origin software, the pressure force-displacement curve graph of a relation of the 4 kinds of carbon fibers obtained.Ordinate represents needle point applies carbon fiber in carbon fiber Micromechanics Analysis process load, and horizontal ordinate is the deformation quantity total in range of liner of carbon fiber and tip.
2. graphical analysis
See the pressure force-displacement curve graph of a relation that Fig. 2, Fig. 2 are 4 kinds of carbon fibers after the process of Origin software.Ordinate be added load unit for receiving ox, abscissa unit is nanometer.
Utilize adamas probe to test toray T700, domestic T300, domestic T700 and domestic T800 pressure respectively, obtain force curve figure, ordinate be added load unit for receiving ox, abscissa unit is nanometer.Can find out that from force curve the slope absolute value of domestic T300 is minimum, hardness is relatively minimum, and domestic T800 at low pressures, comparatively toray T700 carbon fiber slope absolute value is high, and the descending order of tested for hardness is: the domestic T300 of the domestic T700> of domestic T800> toray T700>.Equally at elevated pressures, as right figure, hardness have large to little be the domestic T700 of domestic T800> toray T700>.
Embodiment 3:
A method of testing for carbon fiber microcell relative hardness, comprises the following steps:
A, carbon fiber samples are except slurry: two different carbon fiber samples are put into acetone respectively and soaks 96h, then dry at 80 DEG C of temperature, obtain dry carbon fiber samples;
B, the carbon fiber samples of drying is cut into segment respectively, obtains segment carbon fiber samples, for subsequent use;
C, with atomic force microscope test sample before, utilize single-crystal diamond probe to monocrystalline silicon piece substrate do force curve calibration;
D, sample test and test data process: segment carbon fiber samples is placed in monocrystalline silicon piece substrate, with atomic force microscope to segment carbon fiber samples at 1 × 1 micron
2adamas probe is utilized to carry out mechanical test within the scope of microcell; The test data treated (such as: after the data processing software process such as origin software) of sample obtains the pressure force-displacement curve graph of a relation of carbon fiber, ordinate representative in carbon fiber Micromechanics Analysis process needle point to carbon fiber institute applied pressure, unit is for receiving ox, horizontal ordinate represents carbon fiber and the deformation quantity total in range of liner of tip, and unit is nanometer;
Different segment carbon fiber samples after tested and process obtain the pressure force-displacement curve graph of a relation of carbon fiber respectively;
E, data analysis, formulation process is as follows:
In mensuration process, total deformation quantity is:
Z＝Z
tip+δ (1)
In formula: the deformation quantity that Z-is total; Z
tipthe deformation quantity of-(single-crystal diamond probe) tip; The deformation quantity of δ-carbon fiber;
Formula is expressed as further:
In formula: the acting force in F-mensuration process; K
tipthe nominal force constant of-tip;
Read when being subject to uniform pressure F from pressure force-displacement curve graph of a relation, the total deformation quantity Z corresponding to different carbon fiber;
(the pressure force-displacement curve graph of a relation obtained, uses Origin software analysis, can directly read when being subject to identical directed force F from figure, the total deformation quantity Z corresponding to different carbon fiber);
Identical F and different Z is substituted into formula (2), the force constant K of tip in mensuration process
tipbe constant, obtain the formula that two δ are different, two formulas are subtracted each other, draw the size of δ, be i.e. the size of the deformation quantity of carbon fiber;
According to Hertz model:
In formula: R-atomic force microscope probe tip end radius, K-is effective Young modulus, and relevant with the Young modulus of needle point and carbon fiber and Poisson ratio, its pass is:
In formula: E
f, υ
fbe respectively Young modulus and the Poisson ratio of carbon fiber, E
tip, υ
tipfor pattern modulus and the Poisson ratio of needle point, relevant with the material of needle point; Because the present invention adopts the adamas probe of high rigidity, its E
tipvery large, υ
tipvery little, and be that constant is constant in testing, in high-strength carbon fiber test, make the modulus change of K value to high-strength carbon fiber more responsive, to ensure in test process the judgement of modulus of carbon fibres and resolution; Therefore, can judge from analysis: effectively Young modulus is larger, then the Young modulus of carbon fiber and hardness larger;
The size of carbon fiber deformation quantity δ is relevant to K, if: δ
2(i.e. the deformation quantity of the second carbon fiber) < δ
1(i.e. the deformation quantity of the first carbon fiber), then K
2>K
1, then can think: the hardness of the second carbon fiber is greater than the hardness of the first carbon fiber.
In above-described embodiment 3: in the process of sample test described in steps d, the test of different segment carbon fiber samples all uses same probe to test.
In above-described embodiment: described within the scope of microcell (1 × 1 micron
2) analyze carbon fiber stiffness characteristics, the carbon fiber of test is by the restriction of carbon fiber diameter, density, production batch and different company's product structure, and whether do not distinguish is high strength or high-modulus and high-strength high-modules carbon fibre simultaneously.
In above-described embodiment: equipment used is atomic force microscope, because carbon fiber has high strength and modulus characteristic, the single-crystal diamond probe of high rigidity need be adopted to analyze carbon fiber, single crystal substrates is utilized to calibrate force curve before testing, again Micromechanics Analysis is done to carbon fiber, with same probe in test process, to ensure in test process, needle type radius and cantilever spring modulus constant.
The concrete same prior art of technology contents described in content of the present invention and above-described embodiment.
Above-described embodiment, only for technical characterstic of the present invention is described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
The invention is not restricted to above-described embodiment, all can implement described in content of the present invention and there is described good result.
Claims (2)
1. a method of testing for carbon fiber microcell relative hardness, is characterized in that: comprise the following steps:
A, carbon fiber samples are except slurry: at least two different carbon fiber samples are put into acetone respectively and soaks 96h, then dry at 80 DEG C of temperature, obtain dry carbon fiber samples;
B, the carbon fiber samples of drying is cut into segment respectively, obtains segment carbon fiber samples, for subsequent use;
C, with atomic force microscope test sample before, utilize single-crystal diamond probe to monocrystalline silicon piece substrate do force curve calibration;
D, sample test and test data process: segment carbon fiber samples is placed in monocrystalline silicon piece substrate, with atomic force microscope to segment carbon fiber samples at 1 × 1 micron
2adamas probe is utilized to carry out mechanical test within the scope of microcell; The treated pressure force-displacement curve graph of a relation obtaining carbon fiber of the test data of sample, ordinate representative in carbon fiber Micromechanics Analysis process needle point to carbon fiber institute applied pressure, unit is for receiving ox, horizontal ordinate represents carbon fiber and the deformation quantity total in range of liner of tip, and unit is nanometer;
Different segment carbon fiber samples after tested and process obtain the pressure force-displacement curve graph of a relation of carbon fiber respectively;
E, data analysis, formulation process is as follows:
In mensuration process, total deformation quantity is:
Z＝Z
tip+δ (1)
In formula: the deformation quantity that Z-is total; Z
tipthe deformation quantity of-tip; The deformation quantity of δ-carbon fiber;
Formula is expressed as further:
In formula: the acting force in F-mensuration process; K
tipthe nominal force constant of-tip;
Read when being subject to uniform pressure F from pressure force-displacement curve graph of a relation, the total deformation quantity Z corresponding to different carbon fiber;
Identical F and different Z is substituted into formula (2), the force constant K of tip in mensuration process
tipbe constant, obtain the formula that two δ are different, two formulas are subtracted each other, draw the size of δ, be i.e. the size of the deformation quantity of carbon fiber;
According to Hertz model:
In formula: R-atomic force microscope probe tip end radius, K-is effective Young modulus, and relevant with the Young modulus of needle point and carbon fiber and Poisson ratio, its pass is:
In formula: E
f, υ
fbe respectively Young modulus and the Poisson ratio of carbon fiber, E
tip, υ
tipfor pattern modulus and the Poisson ratio of needle point;
The size of carbon fiber deformation quantity δ is relevant to K, if: δ
2< δ
1, then K
2>K
1, then: the hardness of the second carbon fiber is greater than the hardness of the first carbon fiber.
2., by the method for testing of carbon fiber microcell relative hardness according to claim 1, it is characterized in that: in the process of sample test described in steps d, the test of different segment carbon fiber samples all uses same probe to test.
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| CN113125272B (en) * | 2021-04-25 | 2022-06-28 | 中国石油大学(华东) | Method for quantitatively evaluating mechanical properties of elastic gel dispersion |
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