CN105158073A - Carbon nano tube end and carbon fiber surface grafting strength measuring method - Google Patents
Carbon nano tube end and carbon fiber surface grafting strength measuring method Download PDFInfo
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Abstract
The invention discloses a carbon nano tube end and carbon fiber surface grafting strength measuring method. In a high-magnification scanning electron microscope cavity, a carbon nano tube/carbon fiber multi-scale reinforcement body is fixed to a metal bracket through micro-nano operation, and a weak force measuring system is adopted for carbon nano tube in-site drawing grafting strength testing. By means of the measuring method, the experiment basis is provided for mechanical enhancement of the carbon nano tube/carbon fiber multi-scale reinforcement composite material, and an experiment foundation is laid for the quantitative analysis of macro-mechanical properties of the carbon nano tube/carbon fiber multi-scale reinforcement composite material.
Description
Technical field
The present invention relates to micro nanometer mechanics field of measuring technique, particularly relate to the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity.
Background technology
As everyone knows, the mechanical property of carbon fiber and matrix and carbon fiber and matrix form interface mechanical property directly determine the mechanical property of carbon fibre composite entirety.But, because graphite-structure that carbon fiber surface is smooth result in the defects such as interface cohesion between carbon fiber and matrix is weak, result in carbon fibre composite and easily interfacial detachment occurs under external load function, thus have impact on the performance of carbon fibre reinforced composite macro-mechanical property.
In order to thoroughly solve carbon fiber with basal body interface in conjunction with this difficult problem weak, nearly ten years, some researchers propose a kind of new design on material structure theory, namely by different treatment process, carbon nano-tube is grafted to carbon fiber surface and forms a kind of multi-scale reinforcing body crossing nanoscale from micro-meter scale newly, so far, method carbon nano-tube being grafted to fiber surface mainly comprises: chemical graft process, chemical vapour deposition technique (CVD), electrophoresis and coating.As everyone knows, carbon nano-tube has the performance of a series of excellences such as high-specific surface area, high strength, high-modulus, be regarded as the ultimate form of expression of composite material reinforcement body, while this carbon nano-tube/carbon fiber multi-scale reinforcing body is combined with matrix, carbon nano-tube also can be embedded in matrix goes, when material is subject to extraneous load effect, interaction can be produced between fiber and matrix, existence due to carbon nano-tube can improve the mechanical engagement effect between fiber and matrix greatly, thus can improve boundary strength and toughness.Namely radial dimension is a kind of Multi-scale model that one end of the carbon nano-tube of Nano grade grafts on carbon fiber surface that radial dimension is micron level by chemical graft process or chemical vapour deposition technique by so-called carbon nano-tube/carbon fiber multi-scale reinforcing body.
Carbon nano-tube directly determines the mechanical property of material from the mechanism of extracting matrix, and on the one hand, carbon nano-tube effectively can intercept Interface Crack expansion from extracting matrix, thus improves the mechanical strength of composites; On the other hand, a large amount of energy can be absorbed by the friction in withdrawal process between carbon nano-tube and matrix, thus effectively can improve the toughness of material.
Therefore, exist in prior art and how carbon nano-tube is accurately measured from extracting matrix, especially how carbon nano-tube end and carbon fiber surface grafting intensity are carried out to the needs accurately measured.
Summary of the invention
The embodiment provides the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity, the grafting intensity between carbon nano-tube end and carbon fiber accurately can be measured by the method, for the mechanics enhancing of carbon nano-tube/carbon fiber multi-dimension reinforced composite provides experimental basis, simultaneously for experiment basis has been established in the quantitative analysis of the macro-mechanical property of this kind of material.
According to an aspect of the present invention, provide the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity, it is characterized in that, described method comprises: in the thorax of high power scanning electron microscope chamber, by micro-nano operation, carbon nano-tube/carbon fiber multi-scale reinforcing body is fixed on metal bracket, adopts faint force measuring system to carry out the grafting strength test of carbon nano-tube original position drawing.
Preferably, described method comprises,
Steps A, cutting out and assembling of carbon nano-tube/carbon fiber multi-scale reinforcing body;
Step B, the experiment assembling before carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement;
Step C, the measurement of carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power.
Preferably, cutting out of carbon nano-tube/carbon fiber multi-scale reinforcing body described in steps A comprises with assembling: carbon nano-tube/carbon fiber multi-scale reinforcing body is cut into the sample that specification is 1-5mm length under an optical microscope, and is fixed on metal bracket by described sample.
Preferably, described carbon nano-tube/carbon fiber multi-scale reinforcing body cuts into the sample that specification is 3mm length under an optical microscope.
Preferably, described metal bracket is I shape, and its upper surface is flat surface, is of a size of 3mm*5mm.
Preferably, experiment assembling before described step B carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement is specially, by the atomic force needle point of force sensor and in step ready sample be placed in the chamber thorax of high power field emission scanning electron microscope, ensure the beam of atomic force needle point and carbon fiber axis keeping parallelism by the Real Time Observation of scanning electron microscope in conjunction with micro-nano operation.
Preferably, the measurement of described step C carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power is specially:
Step C1, by the calibration (Standard Beam spring constant is 9.38 μ N/ μm) of Standard Beam, the transformation ratio obtained between the power of atomic force needle point and piezoelectricity is 1 μ N/V;
Step C2, find a single-root carbon nano-tube, guarantee that it is axially vertical with carbon fiber surface, by micro-nano operation, by atomic force needle point slowly near the free end of this carbon nano-tube, until a carbon nano-tube part contacts with each other with atomic force needle point, by the burnt electron irradiation of copolymerization in the surface sweeping Electronic Speculum chamber thorax in carbocyclic ring border, carbon nano-tube and atomic force needle point joint is made to deposit one deck agraphitic carbon, carbon nano-tube and needle point are bonded together securely, the cohesive strength that this Carbon deposition method obtains is 40-100Gpa;
Step C3, along perpendicular to carbon nano tube surface direction slowly even drawing carbon nano-tube, until carbon nano-tube and carbon fiber surface grafting end destroy, records drawing force-displacement curve and the maximal destruction load Fmax of whole process; And pass through formula
Calculate the grafting intensity σ between carbon nano-tube end and carbon fiber.
Preferably, be also included in the thorax of scanning electron microscope chamber before described step C1, selected single-root carbon nano-tube to be measured, axially choose 5 diverse locations along carbon nano-tube and measure carbon nano-tube external diameter, average d.
The measuring method of a kind of carbon nano-tube end of the present invention and carbon fiber surface grafting intensity, tool has the following advantages:
1, metal bracket is real core I shape, and this design overcomes bracket in prior art and adopts the deficiency of hollow, distortion of arching upward in the middle of carbon fiber during hollow bracket drawing carbon fiber, causes measuring the inaccurate problem of grafting intensity.
2, an initiative proposition carbon nano-tube part contacts with each other and interconnection technique with atomic force needle point, by the burnt electron irradiation of copolymerization in the surface sweeping Electronic Speculum chamber thorax in carbocyclic ring border, make carbon nano-tube and atomic force needle point joint deposit one deck agraphitic carbon, thus achieve the connection of nanoscale atomic force needle point and carbon nano-tube.
3, drawing carbon nano-tube adopts three-dimensional orientation mobile operating device, overcomes the error problem of prior art Atom force probe around the draw direction power caused by a point of fixity rotation.
Accompanying drawing explanation
Fig. 1 is metal bracket schematic diagram;
Fig. 2 is that atomic force needle point schematic diagram handled by micro-nano operating means;
Fig. 3 is that carbon nano-tube and atomic force needle point fix schematic diagram;
Fig. 4 is that atomic force needle point breaks carbon nano-tube schematic diagram;
Fig. 5 is operation steps process flow diagram of the present invention.
Embodiment
For making object of the present invention, technical scheme and advantage clearly understand, enumerate preferred embodiment referring to accompanying drawing, the present invention is described in more detail.But it should be noted that, the many details listed in instructions are only used to make reader to have a thorough understanding, even if do not have these specific details also can realize these aspects of the present invention to one or more aspect of the present invention.
The embodiment provides the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity, the grafting intensity between carbon nano-tube end and carbon fiber accurately can be measured by the method, for the mechanics enhancing of carbon nano-tube/carbon fiber multi-dimension reinforced composite provides experimental basis, simultaneously for experiment basis has been established in the quantitative analysis of the macro-mechanical property of this kind of material.
According to an aspect of the present invention, provide the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity, it is characterized in that, described method comprises: in the thorax of high power scanning electron microscope chamber, by micro-nano operation, carbon nano-tube/carbon fiber multi-scale reinforcing body is fixed on metal bracket, adopts faint force measuring system to carry out the grafting strength test of carbon nano-tube original position drawing.
Preferably, described method comprises,
Steps A, cutting out and assembling of carbon nano-tube/carbon fiber multi-scale reinforcing body;
Step B, the experiment assembling before carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement;
Step C, the measurement of carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power.
Preferably, cutting out of carbon nano-tube/carbon fiber multi-scale reinforcing body described in steps A comprises with assembling: carbon nano-tube/carbon fiber multi-scale reinforcing body is cut into the sample that specification is 1-5mm length under an optical microscope, and is fixed on metal bracket by described sample.
Preferably, described carbon nano-tube/carbon fiber multi-scale reinforcing body cuts into the sample that specification is 3mm length under an optical microscope.
Preferably, described metal bracket is I shape, and its upper surface is flat surface, is of a size of 3mm*5mm.
Preferably, experiment assembling before described step B carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement is specially, by the atomic force needle point of force sensor and in step ready sample be placed in the chamber thorax of high power field emission scanning electron microscope, ensure the beam of atomic force needle point and carbon fiber axis keeping parallelism by the Real Time Observation of scanning electron microscope in conjunction with micro-nano operation.
Preferably, the measurement of described step C carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power is specially:
Step C1, by the calibration (Standard Beam spring constant is 9.38 μ N/ μm) of Standard Beam, the transformation ratio obtained between the power of atomic force needle point and piezoelectricity is 1 μ N/V;
Step C2, find a single-root carbon nano-tube, guarantee that it is axially vertical with carbon fiber surface, by micro-nano operation, by atomic force needle point slowly near the free end of this carbon nano-tube, until a carbon nano-tube part contacts with each other with atomic force needle point, by the burnt electron irradiation of copolymerization in the surface sweeping Electronic Speculum chamber thorax in carbocyclic ring border, carbon nano-tube and atomic force needle point joint is made to deposit one deck agraphitic carbon, carbon nano-tube and needle point are bonded together securely, the cohesive strength that this Carbon deposition method obtains is 40-100Gpa;
Step C3, along perpendicular to carbon nano tube surface direction slowly even drawing carbon nano-tube, until carbon nano-tube and carbon fiber surface grafting end destroy, records drawing force-displacement curve and the maximal destruction load Fmax of whole process; And pass through formula
Calculate the grafting intensity σ between carbon nano-tube end and carbon fiber.
Preferably, be also included in the thorax of scanning electron microscope chamber before described step C1, selected single-root carbon nano-tube to be measured, axially choose 5 diverse locations along carbon nano-tube and measure carbon nano-tube external diameter, average d.The technical scheme of the embodiment of the present invention is described in detail below in conjunction with accompanying drawing.In the present invention, the measuring method of carbon nano-tube end and carbon fiber surface grafting intensity adopts structure as shown in Figure 1.Cutting out of carbon nano-tube/carbon fiber multi-scale reinforcing body described in steps A comprises with assembling: carbon nano-tube/carbon fiber multi-scale reinforcing body is cut into the sample that specification is 1-5mm length under an optical microscope, be preferably the sample of 3mm length, it is that the sample of 3mm length can carry out test operation under an optical microscope that carbon nano-tube/carbon fiber multi-scale reinforcing body cuts into specification under an optical microscope, reduce difficulty of test, the carbon fiber rigidity of this yardstick is large simultaneously, be not easy distortion, and described sample is fixed on metal bracket, metal bracket is I shape, its upper surface is flat surface, preferably, metal bracket height 5mm, length is 3mm.Metal bracket is real core I shape, and this design overcomes bracket in prior art and adopts the deficiency of hollow, distortion of arching upward in the middle of carbon fiber during hollow bracket drawing carbon fiber, causes measuring the inaccurate problem of grafting intensity.
Fig. 2 is that atomic force needle point schematic diagram handled by micro-nano operating means.First the experiment assembling before carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement will be carried out before drawing experiment, the atomic force needle point of force sensor and ready sample are placed in the chamber thorax of high power field emission scanning electron microscope, operate in conjunction with micro-nano the beam and the axial keeping parallelism of carbon fiber that ensure atomic force needle point by the Real Time Observation of scanning electron microscope.
Fig. 3 is that carbon nano-tube and atomic force needle point fix schematic diagram, and Fig. 4 is that atomic force needle point breaks carbon nano-tube schematic diagram.In the thorax of scanning electron microscope chamber, selected single-root carbon nano-tube to be measured, axially choose 3-10 diverse location along carbon nano-tube and measure carbon nano-tube external diameter, average d.Preferably 5 diverse locations measure carbon nano-tube external diameter, average.Then, by the calibration (Standard Beam spring constant is 9.38 μ N/ μm) of Standard Beam, the transformation ratio obtained between the power of atomic force needle point and piezoelectricity is 1 μ N/V; Then a single-root carbon nano-tube is found, guarantee that it is axially vertical with carbon fiber surface, by micro-nano operation, by atomic force needle point slowly near the free end of this carbon nano-tube, until a carbon nano-tube part contacts with each other with atomic force needle point, by the burnt electron irradiation of copolymerization in the surface sweeping Electronic Speculum chamber thorax in carbocyclic ring border, carbon nano-tube and atomic force needle point joint is made to deposit one deck agraphitic carbon, carbon nano-tube and needle point are bonded together securely, the cohesive strength that this Carbon deposition method obtains is 40-100Gpa; Drawing force-displacement curve and the maximal destruction load Fmax of whole process, perpendicular to carbon nano tube surface direction slowly even drawing carbon nano-tube, until carbon nano-tube and carbon fiber surface grafting end destroy, are recorded in last edge; And pass through formula
Calculate the grafting intensity σ between carbon nano-tube end and carbon fiber.
The invention provides the measuring method of a kind of carbon nano-tube end and carbon fiber surface grafting intensity, the grafting intensity between carbon nano-tube end and carbon fiber accurately can be measured by the method, for the mechanics enhancing of carbon nano-tube/carbon fiber multi-dimension reinforced composite provides experimental basis, simultaneously for experiment basis has been established in the quantitative analysis of the macro-mechanical property of this kind of material.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the measuring method of a carbon nano-tube end and carbon fiber surface grafting intensity, it is characterized in that, described method comprises: in the thorax of high power scanning electron microscope chamber, by micro-nano operation, carbon nano-tube/carbon fiber multi-scale reinforcing body is fixed on metal bracket, adopts faint force measuring system to carry out the grafting strength test of carbon nano-tube original position drawing.
2. the measuring method of carbon nano-tube end as claimed in claim 1 and carbon fiber surface grafting intensity, it is characterized in that, described method comprises,
Steps A, cutting out and assembling of carbon nano-tube/carbon fiber multi-scale reinforcing body;
Step B, the experiment assembling before carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement;
Step C, the measurement of carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power.
3. the measuring method of carbon nano-tube end as claimed in claim 2 and carbon fiber surface grafting intensity, wherein,
Cutting out of carbon nano-tube/carbon fiber multi-scale reinforcing body described in steps A comprises with assembling: carbon nano-tube/carbon fiber multi-scale reinforcing body is cut into the sample that specification is 1-5mm length under an optical microscope, and is fixed on metal bracket by described sample.
4. the measuring method of carbon nano-tube end as claimed in claim 3 and carbon fiber surface grafting intensity, is characterized in that: described carbon nano-tube/carbon fiber multi-scale reinforcing body cuts into the sample that specification is 3mm length under an optical microscope.
5. the measuring method of carbon nano-tube end as claimed in claim 3 and carbon fiber surface grafting intensity, is characterized in that: described metal bracket is I shape, and its upper surface is flat surface, is of a size of 3mm*5mm.
6. the measuring method of carbon nano-tube end as claimed in claim 2 and carbon fiber surface grafting intensity, it is characterized in that: the experiment assembling before described step B carbon nano-tube/carbon fiber multi-scale reinforcing body in-situ mechanical measurement is specially, by the atomic force needle point of force sensor and in step ready sample be placed in the chamber thorax of high power field emission scanning electron microscope, ensure the beam of atomic force needle point and carbon fiber axis keeping parallelism by the Real Time Observation of scanning electron microscope in conjunction with micro-nano operation.
7. the measuring method of carbon nano-tube end as claimed in claim 2 and carbon fiber surface grafting intensity, is characterized in that:
The measurement of described step C carbon nano-tube/carbon fiber multi-scale reinforcing body carbon nano-tube grafting power is specially:
Step C1, by the calibration (Standard Beam spring constant is 9.38 μ N/ μm) of Standard Beam, the transformation ratio obtained between the power of atomic force needle point and piezoelectricity is 1 μ N/V;
Step C2, find a single-root carbon nano-tube, guarantee that it is axially vertical with carbon fiber surface, by micro-nano operation, by atomic force needle point slowly near the free end of this carbon nano-tube, until a carbon nano-tube part contacts with each other with atomic force needle point, by the burnt electron irradiation of copolymerization in the surface sweeping Electronic Speculum chamber thorax in carbocyclic ring border, carbon nano-tube and atomic force needle point joint is made to deposit one deck agraphitic carbon, carbon nano-tube and needle point are bonded together securely, the cohesive strength that this Carbon deposition method obtains is 40-100Gpa;
Step C3, along perpendicular to carbon nano tube surface direction slowly even drawing carbon nano-tube, until carbon nano-tube and carbon fiber surface grafting end destroy, records drawing force-displacement curve and the maximal destruction load Fmax of whole process; And pass through formula
Calculate the grafting intensity σ between carbon nano-tube end and carbon fiber.
8. the measuring method of carbon nano-tube end as claimed in claim 2 and carbon fiber surface grafting intensity, it is characterized in that: be also included in the thorax of scanning electron microscope chamber before described step C1, selected single-root carbon nano-tube to be measured, axially choose 5 diverse locations along carbon nano-tube and measure carbon nano-tube external diameter, average d.
9. the measuring method of carbon nano-tube end as claimed in claim 7 and carbon fiber surface grafting intensity, it is characterized in that: described step C3 is controlled along perpendicular to the slow evenly drawing carbon nano-tube in carbon nano tube surface direction by three-dimensional mobile operating device, makes drawing carbon nano-tube at vertical direction.
10. the measuring method of carbon nano-tube end as claimed in claim 7 and carbon fiber surface grafting intensity, is characterized in that: it is 9.38 μ N/ μm that the calibration of described Standard Beam is specially Standard Beam spring constant.
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| CN110926974A (en) * | 2019-11-27 | 2020-03-27 | 北京大学 | Method for testing mechanical property of small sample |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105300794A (en) * | 2015-09-23 | 2016-02-03 | 上海大学 | Nano fiber parallel tensile testing system and method |
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| CN106556535A (en) * | 2016-11-09 | 2017-04-05 | 深圳烯湾科技有限公司 | A kind of mechanic property test method based on mechanics sensor |
| CN106645806A (en) * | 2016-11-09 | 2017-05-10 | 深圳烯湾科技有限公司 | Mechanical property testing method based on atomic force microscope probe |
| CN110926974A (en) * | 2019-11-27 | 2020-03-27 | 北京大学 | Method for testing mechanical property of small sample |
| CN111370077A (en) * | 2020-02-24 | 2020-07-03 | 浙江大学 | Method for predicting failure mode of carbon nano tube in composite material |
| CN114279833A (en) * | 2021-12-03 | 2022-04-05 | 南京航空航天大学 | Electron irradiation in-situ stretching and compressing experimental device and method |
| CN114279833B (en) * | 2021-12-03 | 2024-04-12 | 南京航空航天大学 | Electron irradiation in-situ stretching compression experimental device and method |
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