CN116718116A - Quick and accurate test method for high-performance fiber cross-section structure - Google Patents

Quick and accurate test method for high-performance fiber cross-section structure Download PDF

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Publication number
CN116718116A
CN116718116A CN202311007218.5A CN202311007218A CN116718116A CN 116718116 A CN116718116 A CN 116718116A CN 202311007218 A CN202311007218 A CN 202311007218A CN 116718116 A CN116718116 A CN 116718116A
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China
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fiber
wrapping
wrapper
cross
shell
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CN116718116B (en
Inventor
马海兵
唐凯
刘丽英
雒瑞银
王雪茼
王忠伟
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Ningxia Taihe Aramid Fiber Co ltd
Yantai Taihe New Material Polymer New Material Research Institute Co ltd
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Ningxia Taihe Aramid Fiber Co ltd
Yantai Taihe New Material Polymer New Material Research Institute Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/28—Measuring arrangements characterised by the use of optical techniques for measuring areas
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G01N1/06—Devices for withdrawing samples in the solid state, e.g. by cutting providing a thin slice, e.g. microtome
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36—Embedding or analogous mounting of samples
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2873—Cutting or cleaving
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • Pathology (AREA)
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  • Sampling And Sample Adjustment (AREA)

Abstract

The invention belongs to the field of fiber identification, and particularly discloses a rapid and accurate testing method of a high-performance fiber cross-section structure, which aims to solve the problem that the fiber cross-section structure cannot be accurately measured in the prior art; slicing the wrapper to obtain a wrapper slice; carrying out metal spraying treatment on the wrapper slice to obtain a wrapper slice after metal spraying; and (3) placing the cut piece of the wrapper subjected to metal spraying under an optical microscope or a scanning electron microscope for testing to obtain the size of the fiber cross-section structure. According to the method, the low-melting-point high-hardness alloy material is used as an alloy wrapping agent to wrap and cut the monofilament fiber to be measured, and an optical microscope or a scanning electron microscope is adopted to observe the cross-section structure of the fiber.

Description

Quick and accurate test method for high-performance fiber cross-section structure
Technical Field
The invention belongs to the field of fiber identification, and particularly relates to a rapid and accurate test method for a high-performance fiber section structure.
Background
High-performance fibers such as aramid fibers, ultra-high molecular weight polyethylene, carbon fibers and the like are important chemical fibers, have the characteristics of high strength, high modulus, high melting point and the like, and are widely applied to the fields of industry, national defense, medical treatment, environmental protection, advanced science and the like.
The structure determines the performance, and the different cross-sectional structures of the high-performance fiber have very important influence on the strength, elongation and other performances of the fiber, so that the accurate measurement of the cross-sectional structure of the high-performance fiber has very important significance for the research and development and application of the high-performance fiber.
Generally, the method of determining the cross-sectional structure of a fiber is by using a fiberscope method, for example, in FZ/T01057.3-2007, section 3 of the textile fiber identification test method: microscopy indicates that the morphology of the longitudinal and cross-section of the unknown fiber can be observed using a microscope.
Before observing the fiber cross section with a microscope, the fiber is usually directly cut or wrapped with an unsaturated resin wrapping agent and then cut, and the morphology and the size of the fiber cross section are observed and measured with a microscope. For example, the method used in the patent applications CN102435153A, CN102818533B and CN114964002a to test the cross section of the fiber is to fix the fiber in a special tool, cut the strand along the surface of the base of the sampler with a blade, and then detect the cut end face of the fiber with a microscope; in the standard GB/T29762-2013 'determination of carbon fiber diameter and cross-sectional area' and the patent application with publication number CN114280280A, uncured resin is adopted for wrapping and curing, the wrapped fiber is cut, and the cross-sectional morphology is detected by a microscope; GB/T38902-2020 "determination of the cross-sectional structural dimensions of hollow fiber Membrane filaments-image analysis method" indicates that after the fibers are fixed and placed in a container and wrapped with paraffin, the fibers are cut with a blade and the cross-sectional morphology is observed with a microscope.
However, when high-performance fibers are measured, the resin fixing effect is limited when the high-performance fibers are cut due to the problems of low modulus of the resin, high strength of the fibers and the like, so that the cross section of the fibers is easily deformed when the fibers are cut, the morphology observed by a microscope is changed, and the cross section structure of the fibers cannot be accurately measured.
It is therefore important to find a fast and accurate test method for high performance fiber cross-sectional structures.
Disclosure of Invention
The invention aims to provide a rapid and accurate test method for a high-performance fiber section structure, which aims to overcome the defects of the prior art.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a rapid and accurate test method for a high-performance fiber cross-section structure comprises the following steps:
adopting a fiber wrapping device, straightening monofilament fibers to be measured, immersing the monofilament fibers into a prefabricated molten alloy wrapping agent, and cooling until the alloy wrapping agent is solidified to form a wrapper;
slicing the wrapper to obtain a wrapper slice;
carrying out metal spraying treatment on the wrapper slice to obtain a wrapper slice after metal spraying;
and (3) placing the cut piece of the wrapper subjected to metal spraying under an optical microscope or a scanning electron microscope for testing to obtain the size of the fiber cross-section structure.
Further, the alloy coating agent is formed by mixing metal simple substance powder, and comprises, by weight, 42-50% of bismuth, 15-17% of tin, 5-10% of cadmium, 23-38% of indium, 0-2% of zinc and 0-5% of gallium.
Further, the thickness of the wrap slices is 3-6mm.
Further, during the metal spraying treatment, the metal spraying current is 8-10mA, and the metal spraying time is 45-62 seconds.
Further, after the test is completed, the method further comprises the following steps:
slicing the tested wrappage and placing the rest wrappage after slicing treatment in a container capable of being heated, filling nitrogen, heating to be molten, and filtering the monofilament fibers in a molten state to obtain the reusable alloy wrapping agent.
The fiber wrapping device comprises a cylindrical shell, wherein an upper end sealing cover is arranged at the top of the shell, a lower end sealing cover is arranged at the bottom of the shell, a fixing ring used for fixing one end of a monofilament fiber to be tested is arranged on the inner side of the lower end sealing cover, a hole capable of enabling the other end of the monofilament fiber to be tested to pass through is formed in the upper end sealing cover, and a fixing hook used for fixing the other end of the monofilament fiber to be tested is connected to the shell through a bracket;
after the monofilament fiber to be tested is straightened through the fixing ring and the fixing hook, nitrogen is utilized to exhaust air in the shell, a prefabricated molten alloy wrapping agent is added into the shell, after the alloy wrapping agent is cooled to be solidified, a wrapping object is formed, and after one end, connected with the fixing hook, of the monofilament fiber to be tested is sheared off, the wrapping object is pushed out of the shell through the push rod.
Further, the fixing ring is arranged at the center of the lower end cover, the hole is arranged at the center of the upper end cover, and the fixing hook is arranged right above the hole.
Further, the lower end sealing cover is connected with the shell through a buckle, and the upper end sealing cover is connected with the shell through a buckle.
Further, the shell is made of metal.
Further, the inner side of the shell is provided with a lining, and the lining is made of polytetrafluoroethylene or polypropylene.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the method takes the alloy material with low melting point and high hardness as the alloy wrapping agent, and compared with the traditional resin or other wrapping agents, the method has the characteristics of fast wrapping speed because the solidification and melting processes are only controlled by temperature; secondly, the alloy material with low melting point and high hardness is used as the alloy wrapping agent, and the alloy wrapping agent can be melted by adopting hot water bath, so that the operation and the wrapping are convenient; in addition, the method adopts the alloy wrapping agent, the hardness after wrapping and the tightness after wrapping can be ensured, so that the whole wrapping object and the monofilament fiber to be measured are not easy to deform during slicing, the appearance and the structure of the fiber section can be reflected more truly, and the method has the characteristic of more accurate test results.
Further, the thickness of the wrapper slice is 3-6mm, so that the slicing is not suitable for slicing, and the measurement accuracy is improved.
Further, after the test is finished, the alloy wrapping agent can be recycled, and three wastes are not generated, so that compared with the method for discarding the slice and the residual wrapping object of the slice after the resin wrapping, the method has the characteristics of environment friendliness.
Further, the fiber wrapping device adopted by the invention has the advantages of simple structure, convenient operation and capability of rapidly and conveniently completing fiber wrapping.
Further, the upper end sealing cover is provided with a hole which can enable the other end of the monofilament fiber to be measured to pass through, so that the monofilament fiber to be measured can be guaranteed to pass through, and the balance of gas pressure inside and outside the fiber wrapping device can be guaranteed when the molten alloy wrapping agent is added and cooled and solidified.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic view of a fiber wrapping device used in the present invention;
FIG. 2 is a schematic structural view of a push rod;
FIG. 3 is a diagram of the metallographic reflection type optical microscope test of example 1;
FIG. 4 is a diagram of comparative example 1 showing a metallographic reflex optical microscope;
wherein, 1, the lower end is covered; 2. a fixing ring; 3. a housing; 4. a lining; 5. a cover at the upper end; 6. a fixed hook; 7. a push rod.
Detailed Description
In order that those skilled in the art may better understand the present invention, a further detailed description of the present invention will be provided with reference to the accompanying drawings, which are intended to illustrate, but not to limit, the present invention.
It should be noted that the terms "comprises" and "comprising," along with any variations thereof, in the description and claims of the present invention are intended to cover a non-exclusive inclusion, such as a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or apparatus.
The invention uses low-melting-point high-hardness alloy material as a wrapping agent to wrap and cut the fiber, and adopts an optical microscope or a scanning electron microscope to observe the cross-section structure of the fiber, and comprises the following steps:
straightening the monofilament fiber to be measured, immersing the monofilament fiber into a prefabricated molten alloy wrapping agent, and cooling until the alloy wrapping agent is solidified to form a wrapping object;
slicing the wrapper to obtain a wrapper slice;
carrying out metal spraying treatment on the wrapper slice to obtain a wrapper slice after metal spraying;
and (5) placing the cut piece of the wrapper subjected to metal spraying under an optical microscope or a scanning electron microscope for testing to obtain the fiber section structure.
More specifically, the process of the present invention is as follows:
1. preparation of alloy wrapper
The low-melting-point high-hardness alloy material is prepared by mixing common low-melting-point low-radiation low-chemical-activity metal simple substance powder, wherein the metal simple substance powder comprises four or more of bismuth, tin, cadmium, zinc, gallium and indium, and the preparation process comprises the following steps: under the nitrogen environment, mixing four or more metal simple substance powders according to a preset mass ratio, and heating to melt to obtain the alloy wrapping agent, wherein the metal simple substance powders comprise tin, bismuth, cadmium and indium, and the weight percentages of the metal simple substance powders are respectively 15-17 wt% of tin, 42-50 wt% of bismuth, 5-10 wt% of cadmium, 23-38 wt% of indium, 0-2wt% of zinc and 0-5wt% of gallium.
2. Fixing of the monofilament fiber to be measured
Taking high-performance monofilament fiber to be measured about 10cm, fixing one end of the high-performance monofilament fiber to be measured at a fixing ring 2 of a fiber wrapping device shown in fig. 1, fixing the other end of the high-performance monofilament fiber to be measured at a fixing hook 6 of the fiber wrapping device, and guaranteeing that the monofilament fiber to be measured is in a straightened state, wherein the fixing hook 6 is connected to the side face of the shell 3 through a bracket, the bracket comprises an L-shaped rod connected to the side face of the shell 3, a cross rod is connected to the L-shaped rod, the free end of the cross rod is connected with the fixing hook 6, the L-shaped rod is connected with the cross rod through a detachable triangular fixing frame, when the triangular fixing frame is installed between the L-shaped rod and the cross rod, the cross rod and a vertical rod of the L-shaped rod are supported by 90 degrees, and after the triangular fixing frame is detached, the fixing hook 6 is folded to one side of the vertical rod of the L-shaped rod along with the cross rod.
The shell 3 of this fibre parcel device is hollow cylindric container, and the bottom of lower extreme closing cap 1 and shell 3 adopts the buckle to be connected, and solid fixed ring 2 sets up the inboard central point of lower extreme closing cap 1 for fixed fibrous lower extreme of single silk that awaits measuring, shell 3 be metal material such as stainless steel or carbon steel, be convenient for heat conduction fast, inside lining 4 sets up in the inboard of shell 3, adopts materials such as polytetrafluoroethylene, polypropylene, and the buckle is connected with the top of shell 3 to upper end closing cap 5. The middle of the upper end sealing cover 5 is provided with a hole with the diameter larger than that of the monofilament fiber to be measured, so that the monofilament fiber to be measured can pass through, the balance of the gas pressure inside and outside can be ensured during heating and cooling, and the push rod 7 shown in fig. 2 is mainly used for pushing out the cooled wrapper from the fiber wrapping device.
3. Wrap of monofilament fibers to be tested
The fiber wrapping device is vertically fixed on a fixed table, an upper end sealing cover 5 is arranged on the fixed table, after the monofilament fiber to be measured is fixed and a lower end sealing cover 1 is sealed, the upper end sealing cover 5 is opened, nitrogen is filled into a shell 3 for 2 minutes, then molten alloy wrapping agent is added, the adding amount is 4/5 of the maximum capacity of the fiber wrapping device, the upper end sealing cover 5 is covered, and the alloy wrapping agent is cooled to room temperature to solidify. The method comprises the steps of cutting off the part where the monofilament fiber to be detected is connected with the fixed hook 6 by scissors, folding the fixed hook 6, opening the upper end sealing cover 5 and the lower end sealing cover 1, and pushing out a wrapping object from top to bottom by using the push rod 7, wherein the wrapping object is a cylindrical solid with the diameter of about 5mm and the length of 30 mm.
4. Slicing of wrappers
The cutting method is perpendicular to the axial direction of the cylindrical solid by 90 degrees, the cutting blade is used for cutting the wrapping material, the obtained wrapping material has no obvious deformation, no cutting tailing phenomenon and obvious boundary, and the section of the wrapping material is in the same focal plane under the objective lens.
The thickness of the sliced wrapper is 3-6mm, and when the sliced wrapper is too thin, the sliced wrapper is easy to cut off, so that measurement is inaccurate, and when the sliced wrapper is too thick, measurement is inconvenient.
5. Testing of the cross section of monofilament fibers to be tested
Carrying out metal spraying treatment on the wrapper slice, wherein the metal spraying parameters are as follows: the metal spraying current is 8-10mA, and the metal spraying time is 45-62 seconds. And (3) placing the cut piece of the wrapper subjected to metal spraying under an optical microscope or a scanning electron microscope for testing, and determining the cross-sectional morphology, the cross-sectional area and the like of the monofilament fiber to be tested.
6. Recovery of alloy wrappers
Slicing the tested wrappage and the rest wrappage after slicing are placed in a heatable container, nitrogen is filled in, the heating is carried out to a temperature above the melting point for melting, and then monofilament fibers in the wrapped slice and the rest wrappage are filtered while the wrapped slice is hot, so that the reusable wrappage is obtained, and the wrappage can be used for the next fiber cross-section morphology test.
The invention is described in further detail below in connection with examples:
example 1
A rapid and accurate test method for a high-performance fiber cross-section structure comprises the following steps:
and taking para-aramid fiber with fineness of 1000 denier and length of about 10cm, and fixing one end of the para-aramid fiber at the fixing ring 2 of the fiber wrapping device shown in fig. 1, and fixing the other end of the para-aramid fiber at the fixing hook 6 of the fiber wrapping device to ensure that the para-aramid fiber is in a straightened state.
The fiber wrapping device is vertically fixed on an iron stand, an upper end sealing cover 5 is arranged, after the upper end sealing cover 5 is fixed and the lower end sealing cover 1 is sealed, the upper end sealing cover 5 is opened, nitrogen is filled for 2 minutes, then molten alloy wrapping agent is added to 4/5 of the maximum capacity of the fiber wrapping device, the alloy wrapping agent comprises 15 weight percent of tin, 42 weight percent of bismuth, 5 weight percent of cadmium and 38 weight percent of indium in percentage by weight, then the upper end sealing cover 5 is covered, and the alloy wrapping agent is cooled to room temperature until the alloy wrapping agent is solidified. The para-aramid fiber is cut off from the fixed hook 6 by scissors, the fixed hook 6 is folded, the upper end sealing cover 5 and the lower end sealing cover 1 are opened, and the wrapper is pushed out of the fiber wrapping device from top to bottom by the push rod 7, wherein the wrapper is a cylindrical solid with the diameter of about 5mm and the length of 30 mm.
The cutting method is perpendicular to the direction of a cylindrical solid shaft by 90 degrees, the wrapping material is cut by a sharp blade, the thickness of the obtained wrapping material slice is 4mm, the cross section of the wrapping material slice has no obvious deformation, no cutting tailing phenomenon, obvious boundary and the cross section is in the same focal plane under the objective lens. And (3) carrying out metal spraying treatment on the wrapper slice, wherein the metal spraying current is 10mA, the metal spraying time is 60 seconds, placing the wrapper slice after metal spraying under a metallographic reflection optical microscope to test the appearance of the fiber, and calculating the area of the fiber section.
After the test is finished, slicing the wrapping and placing the remaining wrapping after slicing in a round bottom flask, filling nitrogen, placing the flask in a hot water bath for melting, taking out the fiber, recovering to obtain the reusable alloy wrapping agent, and preserving the alloy wrapping agent in a nitrogen seal for the next test.
Example 2
A rapid and accurate test method for a high-performance fiber cross-section structure comprises the following steps:
and taking meta-aramid fiber with the fineness of 1200 denier and the length of about 10cm, and fixing one end of the meta-aramid fiber at the fixing ring 2 of the fiber wrapping device shown in fig. 1, and fixing the other end of the meta-aramid fiber at the fixing hook 6 of the fiber wrapping device to ensure that the meta-aramid fiber is in a straightened state.
The fiber wrapping device is vertically fixed on an iron stand, an upper end sealing cover 5 is arranged, after the upper end sealing cover 5 is fixed and the lower end sealing cover 1 is sealed, the upper end sealing cover 5 is opened, nitrogen is filled for 2 minutes, then molten alloy wrapping agent is added to 4/5 of the maximum capacity of the fiber wrapping device, the alloy wrapping agent comprises, in percentage by weight, 17% by weight of tin, 44% by weight of bismuth, 10% by weight of cadmium, 23% by weight of indium, 1% by weight of zinc and 5% by weight of gallium, then the upper end sealing cover 5 is covered, and the temperature is reduced and cooled to room temperature until the alloy wrapping agent is solidified. The para-aramid fiber is cut off from the fixed hook 6 by scissors, the fixed hook 6 is folded, the upper end sealing cover 5 and the lower end sealing cover 1 are opened, and the wrapper is pushed out of the fiber wrapping device from top to bottom by the push rod 7, wherein the wrapper is a cylindrical solid with the diameter of about 5mm and the length of 30 mm.
The cutting method is perpendicular to the 90-degree direction of the cylindrical solid shaft, the wrapping material is cut by a sharp blade, the thickness of the obtained wrapping material slice is 3mm, the cross section of the wrapping material slice has no obvious deformation, no cutting tailing phenomenon, obvious boundary and the cross section is in the same focal plane under the objective lens. And (3) carrying out metal spraying treatment on the wrapper slice, wherein the metal spraying current is 8mA, the metal spraying time is 45 seconds, placing the wrapper slice after metal spraying under a metallographic reflection optical microscope to test the appearance of the fiber, and calculating the area of the fiber section.
After the test is finished, slicing the wrapping and placing the remaining wrapping after slicing in a round bottom flask, filling nitrogen, placing the flask in a hot water bath for melting, taking out the fiber, recovering to obtain the reusable alloy wrapping agent, and preserving the alloy wrapping agent in a nitrogen seal for the next test.
Example 3
A rapid and accurate test method for a high-performance fiber cross-section structure comprises the following steps:
and taking T600 carbon fiber with the length of about 10cm, fixing one end of the T600 carbon fiber at the fixing ring 2 of the fiber wrapping device shown in fig. 1, and fixing the other end of the T600 carbon fiber at the fixing hook 6 of the fiber wrapping device to ensure that the T600 carbon fiber is in a straightened state.
The fiber wrapping device is vertically fixed on an iron stand, an upper end sealing cover 5 is arranged, after the upper end sealing cover 5 is fixed and the lower end sealing cover 1 is sealed, the upper end sealing cover 5 is opened, nitrogen is filled for 2 minutes, then molten alloy wrapping agent is added to 4/5 of the maximum capacity of the fiber wrapping device, the alloy wrapping agent comprises, by weight, 16% of tin, 50% of bismuth, 5% of cadmium, 23% of indium, 2% of zinc and 4% of gallium, then the upper end sealing cover 5 is covered, and the temperature is reduced and cooled to room temperature until the alloy wrapping agent is solidified. The para-aramid fiber is cut off from the fixed hook 6 by scissors, the fixed hook 6 is folded, the upper end sealing cover 5 and the lower end sealing cover 1 are opened, and the wrapper is pushed out of the fiber wrapping device from top to bottom by the push rod 7, wherein the wrapper is a cylindrical solid with the diameter of about 5mm and the length of 30 mm.
The cutting method is perpendicular to the 90-degree direction of the cylindrical solid shaft, the wrapping material is cut by a sharp blade, the thickness of the obtained wrapping material slice is 6mm, the cross section of the wrapping material slice has no obvious deformation, no cutting tailing phenomenon, obvious boundary and the cross section is in the same focal plane under the objective lens. And (3) carrying out metal spraying treatment on the wrapper slice, wherein the metal spraying current is 9mA, the metal spraying time is 62 seconds, placing the wrapper slice after metal spraying under a scanning electron microscope to test the appearance of the fiber, and calculating the area of the fiber section.
After the test is finished, slicing the wrapping and placing the remaining wrapping after slicing in a round bottom flask, filling nitrogen, placing the flask in a hot water bath for melting, taking out the fiber, recovering to obtain the reusable alloy wrapping agent, and preserving the alloy wrapping agent in a nitrogen seal for the next test.
Comparative example 1
The method of GB/T29762-2013 'determination of diameter and cross-sectional area of carbon fiber' is used for testing, para-aramid fiber with fineness of 1000 denier and length of about 3cm is adopted, domestic epoxy resin 618 is adopted for wrapping, then a sharp blade is used for slicing the para-aramid fiber perpendicular to the axial direction of the fiber by 90 degrees after the resin is solidified, a polishing machine is used for polishing, sand paper and alumina powder are used for polishing the polished surface until a very smooth surface is formed, the morphology is tested by an optical microscope, and the cross-sectional area of the fiber is calculated.
Comparative example 2
Testing by referring to GB/T29762-2013 method of measuring diameter and cross-sectional area of carbon fiber, taking meta-aramid fiber with fineness of 1200 denier and length of about 3cm, wrapping with domestic epoxy resin 618, solidifying the resin, slicing with a sharp blade perpendicular to the axial direction of the fiber by 90 degrees, polishing with a polishing machine, polishing the polished surface with sand paper and alumina powder until a very smooth surface is formed, testing the morphology with an optical microscope, and calculating the cross-sectional area of the fiber.
Comparative example 3
The method of GB/T29762-2013 'determination of diameter and cross-sectional area of carbon fiber' is referred to for testing, T600 carbon fiber with the length of about 3cm is taken, domestic epoxy resin 618 is adopted for wrapping, then a sharp blade is used for slicing the resin perpendicular to the axial direction of the fiber by 90 degrees after the resin is solidified, a polishing machine is used for polishing, sand paper and alumina powder are used for polishing the polished surface until a very smooth surface is formed, the appearance is tested by an optical microscope, and the cross-sectional area of the fiber is calculated.
The results of the fiber morphology and cross-sectional area tests obtained in the above examples and comparative examples are shown in the following table:
the fiber diameter and the fiber cross-sectional area measured in the comparative examples are smaller than those of the comparative examples, because the cross-section obtained by the alloy wrapping agent and the cutting method adopted in the comparative examples is round, the cross-section obtained by the wrapping agent adopted in the comparative examples and the fiber cross-section obtained by the pulling action generated in the cutting process is a diagonal round cross-section, and the measured fiber diameter and the fiber cross-sectional area are larger, and as can be seen from the results, the measured fiber interface structure is more accurate in result and the test duration is shortened by 70% compared with that of the conventional method when the method is adopted for testing.
Fig. 3 is a metallographic reflection type optical microscope test chart of example 1, and fig. 4 is a metallographic reflection type optical microscope test chart of comparative example 1, and it can be seen from fig. 3 and 4 that after the alloy wrapping agent of the present invention is used to wrap high-performance fibers and slice the fibers, the photographed fiber section can better show the round section and skin-core structure of the fibers, no fiber tailing or deformation occurs, while the fiber section of fig. 4 has a tailing phenomenon, that is, the fiber edge has an obvious burr phenomenon, and the original appearance of the fiber section cannot be displayed. Therefore, the method can reflect the appearance and structure of the fiber section more truly, and the test result is more accurate.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of protection thereof, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: various changes, modifications, or equivalents may be made to the particular embodiments of the invention by those skilled in the art after reading the present disclosure, but such changes, modifications, or equivalents are within the scope of the invention as defined in the appended claims.

Claims (10)

1. A rapid and accurate test method for a high-performance fiber cross-section structure is characterized by comprising the following steps:
adopting a fiber wrapping device, straightening monofilament fibers to be measured, immersing the monofilament fibers into a prefabricated molten alloy wrapping agent, and cooling until the alloy wrapping agent is solidified to form a wrapper;
slicing the wrapper to obtain a wrapper slice;
carrying out metal spraying treatment on the wrapper slice to obtain a wrapper slice after metal spraying;
and (3) placing the cut piece of the wrapper subjected to metal spraying under an optical microscope or a scanning electron microscope for testing to obtain the size of the fiber cross-section structure.
2. The rapid and accurate testing method for the cross-sectional structure of the high-performance fiber according to claim 1, wherein the alloy wrapping agent is formed by mixing metal simple substance powder, and comprises, by weight, 42% -50% of bismuth, 15% -17% of tin, 5% -10% of cadmium, 23% -38% of indium, 0-2% of zinc and 0-5% of gallium.
3. The method for rapid and accurate testing of a high performance fiber cross-sectional structure of claim 1, wherein the thickness of the wrap slice is 3-6mm.
4. The method for rapidly and accurately testing the cross-sectional structure of the high-performance fiber according to claim 1, wherein the metal spraying current is 8-10mA and the metal spraying time is 45-62 seconds during the metal spraying treatment.
5. The method for rapid and accurate testing of a high performance fiber cross-sectional structure of claim 1, further comprising the steps of, after the testing is completed:
slicing the tested wrappage and placing the rest wrappage after slicing treatment in a container capable of being heated, filling nitrogen, heating to be molten, and filtering the monofilament fibers in a molten state to obtain the reusable alloy wrapping agent.
6. The fiber wrapping device used in the rapid and accurate testing method of the high-performance fiber cross-section structure according to claim 1, characterized in that the fiber wrapping device comprises a cylindrical shell (3), an upper end sealing cover (5) is arranged at the top of the shell (3), a lower end sealing cover (1) is arranged at the bottom of the shell (3), a fixing ring (2) for fixing one end of a to-be-tested monofilament fiber is arranged on the inner side of the lower end sealing cover (1), a hole capable of enabling the other end of the to-be-tested monofilament fiber to pass through is formed in the upper end sealing cover (5), and a fixing hook (6) for fixing the other end of the to-be-tested monofilament fiber is connected to the shell (3) through a bracket;
after the monofilament fiber to be tested is straightened through the fixing ring (2) and the fixing hook (6), air in the shell (3) is discharged by utilizing nitrogen, a prefabricated molten alloy wrapping agent is added into the shell (3), after the alloy wrapping agent is cooled to be solidified, a wrapping object is formed, and after one end, connected with the fixing hook (6), of the monofilament fiber to be tested is sheared off, the wrapping object is pushed out of the shell (3) by utilizing the push rod (7).
7. Fiber wrapping device according to claim 6, characterized in that the securing ring (2) is arranged in the central position of the lower end cap (1), the hole is arranged in the central position of the upper end cap (5), and the securing hook (6) is arranged directly above the hole.
8. The fiber package according to claim 6, wherein the lower end cap (1) is snap-connected to the housing (3) and the upper end cap (5) is snap-connected to the housing (3).
9. A fibre-wrapping apparatus according to claim 6, characterized in that the housing (3) is of metallic material.
10. The fiber wrapping device according to claim 6, characterized in that an inner liner (4) is arranged on the inner side of the outer shell (3), and the inner liner (4) is made of polytetrafluoroethylene or polypropylene.
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