CN113447483A - Method for testing fiber length in short fiber composite plastic - Google Patents
Method for testing fiber length in short fiber composite plastic Download PDFInfo
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- CN113447483A CN113447483A CN202110714178.2A CN202110714178A CN113447483A CN 113447483 A CN113447483 A CN 113447483A CN 202110714178 A CN202110714178 A CN 202110714178A CN 113447483 A CN113447483 A CN 113447483A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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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
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
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- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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Abstract
The invention belongs to the field of fiber length measurement, and particularly relates to a method for testing the fiber length of short fiber composite plastic. The method specifically comprises the following steps: calcining a sample to be detected in inert gas, dissolving the calcined pure fiber in viscous liquid, drying to obtain pure fiber, and detecting under a microscope. The method is an improvement on the basis of the traditional combustion method, the combustion process is carried out in inert gas, viscous liquid is used for tackifying the combusted fibers, so that the fibers are effectively dispersed, the fiber dispersibility obtained by the method is better, more accurate data can be reflected by testing a small amount of data, the method is simple and easy to operate, and the test equipment has strong universality.
Description
Technical Field
The invention belongs to the field of fiber length measurement, and particularly relates to a method for testing the fiber length of short fiber composite plastic.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The short fiber reinforced composite material is a composite material with the widest application, particularly relates to the aspect of replacing steel with plastics, has the advantages of more obvious light weight application trend, large specific strength and specific modulus, simple forming process, secondary processing and the like, and the performance of the fiber length in the fiber reinforced composite material is the core of the whole material, but no uniform fiber length testing standard and method exists at present.
The method has two problems, namely, the first method is that the composite material is contacted with air in the calcining process, so that the carbon fiber is easily decomposed and damaged, and the test result is inaccurate, and the second method is that the fiber has different lengths and lower viscosity, so that the longer fiber and the shorter fiber are subjected to uneven phenomena such as layering and the like in the process of stirring and dispersing in water to a culture dish, so that the statistical result has larger deviation from the actual result; the other method is a dissolution method, namely the composite material is dissolved in a solvent, and after filtration, the fiber is taken down from the filter paper and placed on a glass slide for observation. A method for taking out the copper net includes such steps as adding short fibres to the solution of silica sol, stirring, preparing prefabricated part, removing a layer of fibres, putting it in acetone solution, taking out the short fibres, taking out them by microscope, taking out the fibres, and low-power observation by SEM. The disadvantage of this method is that sampling is very occasional. The indirect method is to calculate and estimate the specific length of the fiber on two closely spaced cross sections, but the measured result has high dispersion and cannot accurately reflect the actual length of the fiber.
Therefore, the existing methods for measuring the fiber length in the short fiber composite material have various defects, which affect the accuracy of the detection result, and a new method for realizing the accurate measurement of the fiber length is urgently needed to be researched.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a method for testing the fiber length in short fiber composite plastic, which is an improvement on the basis of the traditional combustion method, the combustion process is carried out in inert gas, viscous liquid is used for tackifying the combusted fiber to realize effective dispersion of the fiber, the fiber obtained by the method has better dispersibility, more accurate data can be reflected by a small amount of data, the method is simple and easy to operate, and the test equipment has strong universality.
In order to achieve the purpose, the invention relates to the following technical scheme:
a method for testing the length of fibres in short-fibre composite plastics includes calcining the specimen in inertial gas, dissolving the calcined pure fibres in viscous liquid, drying to obtain pure fibres, and detecting under microscope.
One or more embodiments of the present invention have at least the following effects:
(1) the invention carries out the combustion process in the inert gas, and can avoid the air from participating in the calcination to damage the fiber;
(2) the invention adopts the viscous liquid to disperse and dissolve the burnt pure fiber, and can weaken the layering phenomenon of long fiber and short fiber (powder fiber) through the viscosity of the dispersion liquid, so that the fiber distribution in the whole system is more uniform, and the detection process is more accurate.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a photograph of the alcohol-diluted fibers of example 1;
FIG. 2 is a photograph of example 1 after addition of a viscous solution.
FIG. 3 is a photograph taken under a microscope in example 1;
FIG. 4 is a photograph taken under a microscope in example 2;
FIG. 5 is a photograph of an observation under a microscope in comparative example 1.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background art, various defects exist in the existing methods for measuring the fiber length in the short fiber composite material, which affect the accuracy of the detection result, and it is urgently needed to explore a new method for realizing the accurate measurement of the fiber length.
In order to solve the technical problems, the invention provides a method for testing the fiber length in short fiber composite plastic, which comprises the steps of calcining a sample to be tested in inert gas, dissolving pure fibers obtained after calcination in viscous liquid, drying to obtain pure fibers, and detecting under a microscope.
The existing combustion method is characterized in that a sample to be tested is generally calcined at a certain temperature so that a resin matrix is fully decomposed and then placed in a culture dish after being diluted and dispersed by water, and the method mainly has the defects of two aspects.
Therefore, the invention is improved aiming at the existing combustion method, firstly, the calcining atmosphere is replaced by inert gas, the fiber damage caused by the air participating in the calcining is avoided, secondly, the existing 'aqueous dispersion liquid' is replaced by 'viscous liquid', the fiber is suspended in the viscous liquid by increasing the viscosity of the dispersion liquid, the layering phenomenon of long fiber and short fiber (powder fiber) is weakened, the fiber distribution in the whole system is more uniform, and the detection process is more accurate.
In one or more embodiments of the present invention, the viscous liquid is a mixture of a solvent and a thickener.
The solvent is one or more of water, ethanol, acetone or dichloromethane.
The thickening agent is polyethylene glycol, xanthan gum, cellulose and carbomer resin, preferably carbomer resin.
The xanthan gum and the cellulose can be only used for aqueous solution and have low volatilization speed, and the carbomer resin is used as the thickening agent, so that the purposes can be achieved by selecting various solvents and only adding 0.2-5 percent of the carbomer resin.
The Carbomer resin (Carbomer) is a polymer formed by chemically crosslinking acrylic acid or acrylic ester and allyl ether, comprises polyacrylic acid (homopolymer) and long-chain alkanol acrylate polymer (copolymer), commonly used labels comprise Carbopol910, 934P, 940, 941, 954, 980, 1342, Ultrez 20/21 and the like, and the molecular structure of the Carbomer resin contains 52-68% of acid groups, so that the Carbomer resin has certain acidity and hydrophilic performance, and can be dissolved in water, ethanol and glycerol. The carbomer resin has the functions of thickening, suspending, stabilizing a system and the like. Proper amount of carbomer resin is mixed with the solvent, so that the solvent can be significantly tackified, the calcined fiber can be uniformly dispersed and stably suspended in the solvent, the layering of the fiber is avoided, and the accuracy of the fiber length measurement is improved.
When carbomer resin is used as the thickening agent, the solvent needs to be adjusted to a pH in the range of 6-8 using an alkaline neutralizing agent. The reason is that: the carbomer resin contains acid groups, carboxyl groups of the carbomer resin neutralized by alkaline are ionized, and a coiled molecular chain stretches to be in a great expansion state due to the mutual repulsion of negative charges, so that the original volume is increased to about 1000 times, and the carbomer resin has a thickening effect.
Further, the alkaline neutralizing agent is one or more of sodium hydroxide, potassium bicarbonate or triethanolamine.
Further, when carbomer resin is used as the thickener, additional glycerin is required to be mixed with the above solvent because: a small amount of glycerin is added into the system, the carbomer resin is not separated out along with the volatilization of the solvent in the process of drying and removing the solvent, and moreover, the carbomer resin is dissolved in the glycerin to form a layer of transparent colloidal film on the surface of a vessel, so that the observation and the measurement of the fiber length under a subsequent microscope are not influenced. In addition, glycerol can provide hydroxyl groups, and carbomer molecules act as carboxyl donors and can combine with one or more hydroxyl groups to form hydrogen bonds for further thickening.
Furthermore, the mass ratio of the solvent to the glycerol is 100: 5.
Further, the mass ratio of the solvent to the thickener is 1000:1-1000: 10.
Further, the mass ratio of the solvent to the pure fiber is 1000: 1.
Furthermore, the pure fiber is mixed with the solvent and then added with the thickening agent to form viscous liquid dissolved with the pure fiber.
In one or more embodiments of the present invention, the calcination process is performed in a tube furnace, and a ceramic crucible is used to hold a sample to be tested for calcination;
the existence of water can influence the calcination effect, so that the ceramic crucible needs to be dehydrated for 15-20min under the conditions of 500-600 ℃, is taken out and then placed in a drying dish to be cooled to room temperature, and then is placed in a sample to be detected;
further, after the tube furnace is kept at the constant temperature for 5-6min, the temperature is increased to 540-. At this calcination temperature, the resin matrix in the composite plastic can be sufficiently decomposed to separate the fibers in the composite plastic.
Further, when the temperature of the tube furnace is reduced to below 300 ℃, the crucible is taken out, placed in a drying dish and cooled to room temperature, and then pure fibers are remained in the crucible.
In one or more embodiments of the present invention, the inert gas includes any one of nitrogen, argon; the flow rate of the inert gas into the tube furnace is 150-250 ml/min.
In one or more embodiments of the invention, the process of dissolving pure fiber in viscous liquid is performed in a culture dish, the culture dish is placed on a heating plate at 60-70 ℃, and the detection is performed after the solvent is completely volatilized;
further, the detection process is carried out under a 40-50 times microscope, and 6 points are randomly selected for statistical observation.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
Putting a ceramic crucible into a tube furnace, dehydrating for 15min at 500 ℃, taking out, and placing in a drying dish to cool to room temperature;
secondly, putting a proper amount of samples to be measured (blocks, strips and granules) into the dried crucible, and putting the crucible into a tube furnace;
thirdly, adjusting the atmosphere of the tube furnace to be nitrogen, keeping the temperature constant for 5min at the flow rate of 150ml/min, heating to 550 ℃ at the speed of 50 ℃/min, keeping the temperature constant for 30min, stopping heating, and naturally cooling;
fourthly, when the temperature of the tube furnace is reduced to below 300 ℃, taking out the crucible, placing the crucible in a drying dish, and cooling to room temperature, wherein pure fibers are left in the crucible;
fifthly, taking 0.02g of fiber in the crucible, placing the fiber in a culture dish, adding 20g of alcohol and 1g of glycerol, stirring the mixture evenly and lightly, wherein the picture after stirring is shown in figure 1, part of the fiber floats in the solution, and part of the fiber is deposited on the bottom of the dish;
sixthly, 0.02g of carbomer Ultrez 20 is added into the mixed solution of the alcohol and the fiber, the mixture is gently stirred until the mixture is completely mixed, an alkaline neutralizer is added to adjust the pH value of the solution to 6-8, the solution forms transparent viscous liquid, the picture of the solution is shown in figure 2, and the fiber is uniformly suspended in the liquid;
seventhly, placing the culture dish on a heating plate at the temperature of 60 ℃, and heating until liquid substances are completely volatilized;
placing the culture dish under a 50-time microscope for observation, and randomly selecting 6 points for statistical observation.
Example 2
Putting a ceramic crucible into a tube furnace, dehydrating for 15min at 500 ℃, taking out, and placing in a drying dish to cool to room temperature;
secondly, putting a proper amount of samples to be measured (blocks, strips and granules) into the dried crucible, and putting the crucible into a tube furnace;
thirdly, adjusting the atmosphere of the tube furnace to be nitrogen, keeping the temperature constant for 5min at the flow rate of 250ml/min, heating to 550 ℃ at the speed of 50 ℃/min, keeping the temperature constant for 30min, stopping heating, and naturally cooling;
fourthly, when the temperature of the tube furnace is reduced to below 300 ℃, taking out the crucible, placing the crucible in a drying dish, and cooling to room temperature, wherein pure fibers are left in the crucible;
fifthly, taking 0.02g of fibers in the crucible, putting the fibers in a culture dish, adding 20g of alcohol and 1g of glycerol, and slightly and uniformly stirring;
sixthly, adding 0.2g of carbomer 940 into the mixed solution of the solvent and the fiber, slightly stirring the mixture until the mixture is completely mixed, adding an alkaline neutralizer into the mixture to adjust the pH of the solution to be 6-8 so that the solution forms transparent viscous liquid, and uniformly suspending the fiber in the liquid;
seventhly, placing the culture dish on a heating plate at the temperature of 60 ℃, and heating until liquid substances are completely volatilized;
placing the culture dish under a 50-time microscope for observation, and randomly selecting 6 points for statistical observation.
Example 3
Putting a ceramic crucible into a tube furnace, dehydrating for 15min at 500 ℃, taking out, and placing in a drying dish to cool to room temperature;
secondly, putting a proper amount of samples to be measured (blocks, strips and granules) into the dried crucible, and putting the crucible into a tube furnace;
thirdly, adjusting the atmosphere of the tube furnace to be nitrogen, keeping the flow rate at 150-;
fourthly, when the temperature of the tube furnace is reduced to below 300 ℃, taking out the crucible, placing the crucible in a drying dish, and cooling to room temperature, wherein pure fibers are left in the crucible;
fifthly, taking 0.02g of fibers in the crucible, putting the fibers in a culture dish, adding 20g of alcohol, and slightly and uniformly stirring;
sixthly, adding 0.2g of polyethylene glycol into the mixed solution of the solvent and the fiber, and slightly stirring the mixture until the mixture is completely mixed to ensure that the solution forms transparent viscous liquid, and the fiber is uniformly suspended in the liquid;
seventhly, placing the culture dish on a heating plate at the temperature of 60 ℃, and heating until liquid substances are completely volatilized;
placing the culture dish under a 50-time microscope for observation, and randomly selecting 6 points for statistical observation.
Comparative example 1
Putting a ceramic crucible into a tube furnace, dehydrating for 15min at 500 ℃, taking out, and placing in a drying dish to cool to room temperature;
secondly, putting a proper amount of samples to be measured (blocks, strips and granules) into the dried crucible, and putting the crucible into a muffle furnace;
thirdly, taking out the crucible after burning for 1 hour at the temperature of 600 ℃, placing the crucible in a drying dish, and cooling to room temperature, wherein pure fibers are remained in the crucible;
fourthly, placing 0.02g of fibers in the crucible into a culture dish, adding 20g of alcohol, and stirring the mixture lightly and uniformly;
fifthly, placing the culture dish on a heating plate at 60 ℃, and heating until liquid substances are completely volatilized;
sixthly, placing the culture dish under a 50-fold microscope for observation, and randomly selecting 6 points for statistical observation.
Fiber length testing:
example 1 data
When the fiber length is shot under a microscope, six point photos are shown in fig. 1, the fiber length in 6 pictures in fig. 3 is counted (table 1), the total length is calculated, the fiber length is respectively counted according to three sections of 0-0.3, 03-0.5 and more than 0.5, and the percentage of the fiber length of the sections in the total length is calculated, so that the average fiber length in each picture is good in consistency and the fiber distribution is uniform. Wherein, FIGS. 3a, b, c, d, e, f correspond to data of 1-1, 1-2, 1-3, 1-4, 1-5, 1-6 in Table 1, respectively.
Table 1 example 1 mean fiber length calculation data
As can be seen from the data in table 1, the average fiber length and the ratio of the fiber length in each interval to the total length in the 6 observation points selected in example 1 are not different, which indicates that the fiber length data in each observation point are similar and the overall fiber distribution is uniform.
Example 2 data
When the fiber length is shot under a microscope, six point photos are shown in fig. 2, the fiber length in 6 pictures in fig. 4 is counted (table 2), the total length is calculated, the fiber length is respectively counted according to three sections of 0-0.3, 03-0.5 and more than 0.5, and the percentage of the fiber length of the sections in the total length is calculated, so that the average fiber length in each picture is good in consistency and the fiber distribution is uniform. Wherein, FIGS. 4a, b, c, d, e, f correspond to the data of 2-1, 2-2, 2-3, 2-4, 2-5, 2-6 in Table 2, respectively.
Table 2 example 2 mean fiber length calculation data
As can be seen from the data in table 2, the average fiber length and the ratio of the fiber length in each interval to the total length in the 6 observation points selected in example 2 are not different, which indicates that the fiber length data in each observation point are similar and the overall fiber distribution is uniform.
Comparative example 1
When the fiber length is shot under a microscope, the pictures of six points are shown in fig. 3, the fiber length in 6 pictures in fig. 5 is counted (table 3), the total length is calculated, the fiber length is respectively counted according to three sections of 0-0.3, 03-0.5 and more than 0.5, and the percentage of the fiber length of the sections in the total length is calculated, so that the average fiber length in each picture is good in consistency and uniform in fiber distribution. Wherein, FIGS. 5a, b, c, d, e, f correspond to data of 1-1, 1-2, 1-3, 1-4, 1-5, 1-6 in Table 3, respectively.
Table 3 comparative example 1 mean fiber length calculation data
As can be seen from the data in Table 3, the average fiber length and the ratio of the fiber length in each interval to the total length in the 6 observation points selected in comparative example 1 are greatly different, which indicates that the fiber length data in each observation point are greatly different and the overall distribution of the fibers is not uniform.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for testing the fiber length in short fiber composite plastic is characterized in that: calcining a sample to be detected in inert gas, dissolving pure fibers obtained after calcination in viscous liquid, drying to obtain pure fibers, and detecting under a microscope.
2. The method of claim 1, wherein: the viscous liquid is a mixed liquid of a solvent and a thickening agent;
preferably, the solvent is one or more of water, ethanol, acetone or dichloromethane;
more preferably, the thickening agent is polyethylene glycol, xanthan gum, cellulose and carbomer resin, and preferably carbomer resin.
3. The method of claim 2, wherein: when carbomer resin is used as a thickening agent, an alkaline neutralizing agent is needed to adjust the pH of the solvent to be within the range of 6-8;
further, the alkaline neutralizing agent is one or more of sodium hydroxide, potassium bicarbonate or triethanolamine.
4. The method of claim 3, wherein: when carbomer resin is used as a thickening agent, glycerin is additionally added to be mixed with a solvent;
further, the mass ratio of the solvent to the glycerol is 100: 5.
5. The method of claim 2, wherein: the mass ratio of the solvent to the thickening agent is 1000:1-1000: 10;
further, the mass ratio of the solvent to the pure fiber is 1000: 1;
furthermore, the pure fiber is mixed with the solvent and then added with the thickening agent to form viscous liquid dissolved with the pure fiber.
6. The method of claim 1, wherein: the calcining process is carried out in a tubular furnace, and a ceramic crucible is adopted to contain a sample to be tested for calcining;
furthermore, the ceramic crucible needs to be dehydrated for 15-20min at the temperature of 500-600 ℃, taken out, placed in a drying dish to be cooled to room temperature, and then placed in a sample to be tested.
7. The method of claim 6, wherein: the calcination conditions were: keeping the temperature of the tube furnace constant for 5-6min, heating to 540-560 ℃ at the speed of 50 ℃/min, keeping the temperature constant for 30-35min, stopping heating, and naturally cooling;
when the temperature of the tube furnace is reduced to below 300 ℃, the crucible is taken out, placed in a drying dish and cooled to room temperature, and then pure fibers are remained in the crucible.
8. The method of claim 1, wherein: the inert gas comprises any one of nitrogen and argon; the flow rate of the inert gas into the tube furnace is 150-250 ml/min.
9. The method of claim 1, wherein: the process of dissolving pure fiber in viscous liquid is carried out in a culture dish, the culture dish is placed on a heating plate at 60-70 ℃, and the detection is carried out after the solvent is completely volatilized.
10. The method of claim 9, wherein: the detection process is carried out under a microscope of 40-50 times, and 6 points are randomly selected for statistical observation.
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