CN108195860A - A kind of test method of fiber lattice parameter - Google Patents
A kind of test method of fiber lattice parameter Download PDFInfo
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- CN108195860A CN108195860A CN201711410853.2A CN201711410853A CN108195860A CN 108195860 A CN108195860 A CN 108195860A CN 201711410853 A CN201711410853 A CN 201711410853A CN 108195860 A CN108195860 A CN 108195860A
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- 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
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Abstract
The invention discloses a kind of test method of fiber lattice parameter, the fiber is aramid fiber, carbon fiber and oxidization fiber fiber, this method are：First, the specimen holder of cube structure is made, specifies the test surfaces that one of outer surface is specimen holder；2nd, glue is coated in the dorsal surface of specimen holder, the dorsal surface of the specimen holder is opposite with test surfaces position, then winds around fibre bundle on specimen holder side by side, after glue drying, obtains sample to be tested；3rd, the sample to be tested being located on test surfaces is tested using X-ray diffraction method, obtains 2 θ of the angle of diffraction of fiber, finally calculate the lattice parameter of the interplanar distance, i.e. fiber of fiber.The present invention solve the problems, such as fiber be difficult to grind, conventional test methodologies accuracy it is relatively low, as a result accurately and securely property is high, and the test result coefficient of dispersion of fiber lattice parameter reduces by more than 10%, and sample preparation is easy to operate, the sample preparation time shorten to 10min from 2h, suitable for mass sample preparation.
Description
Technical field
The invention belongs to fibre structure parameter testing technical fields, and in particular to a kind of test side of fiber lattice parameter
Method.
Background technology
Carbon fiber (carbon fiber, abbreviation CF) is a kind of high intensity of phosphorus content more than 95%, high modulus fibre
New fiber materials.Carbon fiber quality is lighter than metallic aluminium, but intensity is higher than steel, and with axial strength and modulus
Height, density is low, higher than performance, no creep, and superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, and coefficient of thermal expansion is small and has
Anisotropy, good corrosion resistance, many excellent performances such as good electrical and thermal conductivity performance and electromagnetic wave shielding, in defence and military and
Civilian aspect is all used widely.
Industrialized production carbon fiber by raw material route can be divided into polyacrylonitrile (PAN) base carbon fibre, asphalt base carbon fiber and
Viscose-based carbon fiber three categories, the high-performance polyacrylonitrile carbon fiber as made from polyacrylonitrile fibre precursor, production technology compared with
Other methods are simple, and yield accounts for about more than 90% global carbon fiber total output.The skill flow of polyacrylonitrile carbon fiber is：Poly- third
Alkene nitrile precursor → pre-oxidation → carbonization → graphitization → is surface-treated → batches → carbon fiber.Wherein Pre oxidation is 200 DEG C
~300 DEG C, carburizing temperature is 1000 DEG C~2000 DEG C, and graphitization temperature is 2500 DEG C~3000 DEG C, because for the treatment of of different temperature
The oxidization fiber fiber or carbon fiber of acquisition are changed significantly with processing temperature change, are had due to fine structure difference, fibre property
Necessity characterizes fibre structure number, and one of crucial structural parameters are fiber lattice parameter.
By taking C/C larynxs lining as an example, carbon fiber and its oxidization fiber fiber are that multidimensional braiding larynx serves as a contrast molding key raw material, and carbon is fine
Dimension performance is directly related to the final performance of larynx lining, in order to improve the stability of material property and study the differentiation of fibre property,
It needs to be measured the carbon fiber lattice parameter of oxidization fiber fiber, different temperatures preparation, to analyze between different batches fiber
Difference existing for lattice structure, while the difference of C/C larynxs lining preparation process high temperature treatment temperature, it is also desirable to carry out carbon fiber crystalline substance
Lattice parametric measurement, difference existing for lattice structure between fiber caused by analyze different process.
In addition, aramid fiber (full name aromatic polyamide fibre) is a kind of high intensity, high-modulus, low-density and wearability
The tec fiber of good organic composition also usually requires to carry out lattice parameter measure in engineer application.
At present when X-ray diffraction method measures lattice parameter, generally use powder diffraction method, i.e., by buck into certain
The powder of granularity, it is smooth to be closely pressed on specimen mounting, by X-ray diffractometer acquire diffraction data after by data processing system
System directly obtains 2 θ of the angle of diffraction, then calculate fiber interplanar distance, i.e. lattice parameter by bragg's formula.Spread out for X ray
Method is penetrated, the smooth degree of sample directly affects the accuracy of 2 θ angular datas, therefore the sample to be tested of X-ray diffraction method generally will
It asks smooth closely knit, ensures that specimen surface is maintained at sample holder plane on same horizontal plane as possible, to obtain satisfied test
As a result, effective method for making sample becomes the key of test.
Traditional method for making sample is to be cut short fiber to be measured, and ground with agate mortar with scissors, due to oxidization fiber fiber,
Carbon fiber, aramid fiber characteristic caused by, be ground into that powder difficulty is quite big, and carbon fiber oxidization fiber and aramid fiber are difficult
It is ground into the powder of diffraction test request, fiber can only be worn into relatively thin cotton-shaped, and cotton-shaped sample is laid on specimen holder,
It is placed on diffractometer and tests, in terms of diffraction spectrogram, the intensity of diffraction maximum is weaker, accurately can not directly analyze 2 θ angles.This is
Since cotton-shaped sample can only be loosely laid on specimen holder naturally very much, compactness is not caused enough.
Invention content
The technical problems to be solved by the invention are in view of the above shortcomings of the prior art, to provide a kind of fiber lattice
The test method of parameter.The test method winds method for making sample by fiber, solves fiber existing for tradition grinding method for making sample
It is difficult to grind, the problem of test accuracy is relatively low, diffraction peak intensity is weaker.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of test method of fiber lattice parameter,
The fiber is aramid fiber, carbon fiber and oxidization fiber fiber, which is characterized in that this method includes the following steps：
Step 1: making the specimen holder of cube structure, an outer surface for specifying the specimen holder is test surfaces；
Step 2: the dorsal surface coating glue of the specimen holder made in step 1, the dorsal surface of the specimen holder and survey
Examination face position is opposite, then winds around fibre bundle on specimen holder side by side, after glue drying, obtains sample to be tested；
When the fibre bundle is carbon fiber or oxidization fiber fiber, the specimen holder that makes in step 1 for bakelite specimen holder or
Graphite sample frame, when the fibre bundle is aramid fiber beam, the specimen holder made in step 1 is bakelite specimen holder；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested on test surfaces in step 2, fibre is obtained
2 θ of the angle of diffraction of dimension finally calculates the lattice parameter of fiber.
A kind of test method of above-mentioned fiber lattice parameter, which is characterized in that the size of specimen holder described in step 1
For 50mm × 20mm × 10mm, test surfaces of the surface of one of 50mm × 10mm as specimen holder are specified.
A kind of test method of above-mentioned fiber lattice parameter, which is characterized in that the specific mistake wound described in step 2
Cheng Wei：One end of fibre bundle is placed on tensioner, the other end of fibre bundle is fixed on the dorsal surface of specimen holder, the fiber
Beam is wound around on specimen holder successively along clockwise direction, and the tension of the fibre bundle is 5N~15N during winding.
The test method of a kind of fiber lattice parameter stated, which is characterized in that specimen holder described in step 2 is bakelite sample
Product frame is epoxy glue solution coated in the glue on specimen holder.
The test method of above-mentioned a kind of fiber lattice parameter, which is characterized in that the epoxy glue solution is by epoxy resin
E51, triethylene tetramine and polyamide are according to 100:(2~4):The mass ratio of (30~40) is made.
The test method of above-mentioned a kind of fiber lattice parameter, which is characterized in that specimen holder described in step 2 is graphite
Specimen holder is phenolic aldehyde glue coated in the glue on graphite sample frame.
The test method of above-mentioned a kind of fiber lattice parameter, which is characterized in that the phenolic aldehyde glue is by boron bakelite resin
Alcoholic solution and White Carbon black according to 100:The mass ratio of (0.2~1.5) is made, and the alcoholic solution of the boron bakelite resin is by boron
Phenolic resin is dissolved in alcohol and is made, and the mass ratio of the boron bakelite resin and alcohol is 1:1.
The test method of above-mentioned a kind of fiber lattice parameter, which is characterized in that the process of the dry phenolic aldehyde glue is：
The graphite sample for being closely wound fibre bundle is placed in heat-treatment furnace, is first heated up with the heating rate of 9 DEG C/h~11 DEG C/h
To 75 DEG C~85 DEG C, 1h~2h is kept the temperature, is then warming up to 115 DEG C~125 DEG C with the heating rate of 18 DEG C/h~22 DEG C/h, heat preservation
1h~2h is further continued for being warming up to 160 DEG C~170 DEG C with the heating rate of 18 DEG C/h~22 DEG C/h, keeps the temperature 1h~3h, last natural
Cooling.
The test method of above-mentioned a kind of fiber lattice parameter, which is characterized in that it is being tested using X-ray diffraction method
Before, first the sample to be tested is heat-treated.
Compared with the prior art, the present invention has the following advantages：
What the 1st, the method being wrapped in fiber on specimen holder in test method of the invention solved that fiber is difficult to grind asks
Topic, the consistency of sample preparation is high, realizes the accurate test of oxidization fiber fiber, carbon fiber, aramid fiber lattice parameter, coefficient of dispersion
It is substantially reduced.
2nd, test method sample preparation of the present invention is easy to operate, and the sample preparation time shortens, particularly with the oxidization fiber fiber sample preparation time
It is shorten to 10 minutes from original sample preparations in 2 hours, substantially increases the efficiency of fiber lattice parametric measurement.
3rd, relative to existing polishing sample preparation, the present invention may be adapted to carry out mass sample preparation, and sample obtained exists
When being tested on diffractometer, for being difficult to the fiber ground, the diffraction spectrogram diffraction peak intensity that winding method obtains spreads out with respect to powder method
It penetrates peak intensity to be substantially higher, is easy to calculate 2 θ angles.
4th, sample to be tested is made by fiber solidifying in the present invention on specimen holder, and sample to be tested can be heat-treated, with
The lattice parameter of fiber at a temperature of acquisition different heat treatment, for studying the heat treatment under different temperatures to fiber lattice parameter
It influences.
5th, diffraction data is acquired in testing, and forms XRD spectra by data processing system, and diffraction is obtained by analysis
2 θ of angle, then lattice parameter can be calculated by bragg's formula d=n λ/2sin θ, wherein d is interplanar distance, and λ is incident X-rays
Wavelength, θ are Bragg angle, and n is integer, referred to as reflects series, understand that the accuracy of lattice parameter is depended primarily on from formula
The precision of sin θ, i.e., depending on 2 θ of the angle of diffraction.XRD spectra shows that different method for making sample directly affect the standard of 2 θ data of the angle of diffraction
True property, so as to influence lattice parameter characterization reliability.The 2 θ angles of diffraction are apparent on the XRD spectra that the present invention measures, than existing powder
The precision of last diffraction approach is more preferable.
Technical scheme of the present invention is described in further detail below by drawings and examples.
Attached drawing table explanation
Fig. 1 is the XRD spectra for the 12K polyacrylonitrile carbon fibers that the embodiment of the present invention 1 measures.
Fig. 2 is the XRD spectra of 12K polyacrylonitrile carbon fibers that existing powder diffraction method measures.
Fig. 3 is the XRD spectra for the 12K PAN-based stabilized fiber fibers that the embodiment of the present invention 2 measures.
Fig. 4 is the XRD spectra of 12K PAN-based stabilized fiber fibers that existing powder diffraction method measures.
Fig. 5 is the XRD spectra for the 3K PAN-based stabilized fiber fibers that the embodiment of the present invention 3 measures.
Fig. 6 is the XRD spectra of 3K PAN-based stabilized fiber fibers that existing powder diffraction method measures.
Fig. 7 is the XRD spectra of the 6K PAN-based stabilized fiber fibers after the heat treatment that the embodiment of the present invention 4 measures.
Fig. 8 is the XRD spectra of the 6K PAN-based stabilized fiber fibers after the heat treatment that existing powder diffraction method measures.
Fig. 9 is the XRD of the 1K polyacrylonitrile carbon fibers after the heat treatment that the embodiment of the present invention 5 measures
Spectrogram.
Figure 10 is the 1K polyacrylonitrile carbon fibers after the heat treatment that existing powder diffraction method measures
XRD spectra.
Figure 11 is the XRD spectra for the aramid fiber that the embodiment of the present invention 6 measures.
Specific embodiment
Embodiment 1
Step 1: using bakelite specimen holder of the size that bakelite makes for 50mm × 20mm × 10mm, bakelite sample is specified
Measuring surface of the surface of one 50mm × 10mm of frame as bakelite specimen holder；
Step 2: the dorsal surface coating epoxy glue solution of the bakelite specimen holder made in step 1, the bakelite specimen holder
Dorsal surface it is opposite with measuring surface position, then 12K polyacrylonitrile carbon fibers are wound around side by side on bakelite specimen holder, and
Uniformly without stock phenomenon is twisted, winding rear surface is smooth, after epoxy glue solution spontaneously dries, obtains sample to be tested for arrangement；The epoxy glue
Liquid is by epoxy resin E51, triethylene tetramine and polyamide according to 100:4:40 mass ratio is made；
The detailed process of the winding is：One end of 12K polyacrylonitrile carbon fibers is placed on tensioner, 12K polypropylene
The other end of nitrile carbon fiber is fixed on the dorsal surface of bakelite specimen holder, and the 12K polyacrylonitrile carbon fibers are along clockwise direction
It winds around successively on bakelite specimen holder, the tension of the fibre bundle is 15N during winding；It is described to be wrapped on bakelite specimen holder
Adjacent two fibre bundles between gap cannot occur；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtain
To 2 θ of the angle of diffraction of 12K polyacrylonitrile carbon fibers, 12K polyacrylonitrile is calculated finally by bragg's formula d=n λ/2sin θ
The lattice parameter of the interplanar distance d, i.e. 12K polyacrylonitrile carbon fibers of carbon fiber.Wherein λ is incident X-rays wavelength (i.e. CuKa waves
A length of 0.15406nm)；θ is Bragg angle (°), and n is to reflect the integer (the present embodiment n=1) that series and n are >=1.
The lattice parameter of 12K polyacrylonitrile carbon fibers tested using embodiment 1 and existing powder diffraction method, Fig. 1 are real
The XRD spectra of the 12K polyacrylonitrile carbon fibers of the measurement of example 1 is applied, Fig. 2 is the 12K polyacrylonitrile that existing powder diffraction method measures
The XRD spectra of carbon fiber；2 θ of the angle of diffraction of sample can be directly obtained by Fig. 1 and Fig. 2, is respectively adopted in each method identical
Raw fibre produces 5 samples, measures 2 θ of the angle of diffraction of 5 samples respectively, and utilize bragg's formula counting lattice parameter, and count
The coefficient of dispersion of lattice parameter that two kinds of test methods are tested is calculated, so as to evaluate the accuracy of measuring method.Embodiment 1 and existing
There is the measurement result of the lattice parameter of 12K polyacrylonitrile carbon fibers that powder diffraction method measures as shown in table 1.
1 embodiment 1 of table and existing powder diffraction method measure the interplanar distance of 12K polyacrylonitrile carbon fibers
As known from Table 1, the interplanar distance average value for the 12K polyacrylonitrile carbon fibers that the present embodiment is calculated is
0.3481nm, the interplanar distance average value for the carbon fiber that existing powder diffraction method measures is 0.3481nm, passes through comparison, this reality
Applying the coefficient of dispersion of the interplanar distance for the carbon fiber that example is calculated reduces 17.8%, illustrates that the method through the present embodiment can
With the lattice parameter of the interplanar distance, i.e. 12K polyacrylonitrile carbon fibers of more accurate characterization 12K polyacrylonitrile carbon fibers.
Embodiment 2
Step 1: using graphite sample frame of the size that graphite makes for 50mm × 20mm × 10mm, one of them is specified
Measuring surface of the surface of 50mm × 10mm as graphite sample frame；
Step 2: the dorsal surface coating phenolic aldehyde glue of the graphite sample frame made in step 1, the graphite sample frame
Dorsal surface it is opposite with measuring surface position, then 12K PAN-based stabilized fibers fibre bundle is wound around on specimen holder side by side,
And arrangement is uniformly without stubborn stock phenomenon, then the graphite sample for being closely wound 12K PAN-based stabilized fiber fibre bundles is placed on heat
In treatment furnace, 85 DEG C first are warming up to the heating rate of 11 DEG C/h, 1h is kept the temperature, is then warming up to the heating rate of 22 DEG C/h
125 DEG C, 1h is kept the temperature, then 170 DEG C are warming up to the heating rate of 22 DEG C/h, keep the temperature 1h, obtain treating test sample after last natural cooling
Product；The phenolic aldehyde glue is by the alcoholic solution of boron bakelite resin with White Carbon black according to 100:1.5 mass ratio is made, the boron phenol
The alcoholic solution of urea formaldehyde, which is dissolved in by boron bakelite resin in alcohol, to be made, and the mass ratio of the boron bakelite resin and alcohol is 1:
1.5；A concentration of 50wt% of the alcohol；
The detailed process of the winding is：One end of 12K PAN-based stabilized fiber fibre bundles is placed on tensioner, 12K
The other end of PAN-based stabilized fiber fibre bundle is fixed on the dorsal surface of specimen holder, the 12K PAN-based stabilized fibers fiber
Beam is wound around on graphite sample frame successively along clockwise direction, and the tension of the carbon fiber is 5N during winding；The winding
Gap cannot occur between adjacent two carbon fibers on graphite sample frame；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtain
To 2 θ of the angle of diffraction of 12K PAN-based stabilized fiber fibers, 12K poly- third is calculated finally by bragg's formula d=n λ/2sin θ
The lattice parameter of the interplanar distance d, i.e. 12K PAN-based stabilized fibers fiber of alkene nitrile oxidization fiber fiber.Wherein λ is incident X-rays
Wavelength (i.e. CuKa wavelength is 0.15406nm)；θ is Bragg angle (°), and n is to reflect integer (the present embodiment that series and n are >=1
N=1).
The lattice parameter of 12K PAN-based stabilized fiber fibers tested using embodiment 2 and existing powder diffraction method, Fig. 3
It is the XRD spectra for the 12K PAN-based stabilized fiber fibers that embodiment 2 measures, Fig. 4 is the 12K that existing powder diffraction method measures
The XRD spectra of PAN-based stabilized fiber fiber can directly obtain 2 θ of the angle of diffraction of sample by Fig. 3 and Fig. 4, divide in each method
Not Cai Yong identical raw fibre produce 5 samples, respectively measure 5 samples 2 θ of the angle of diffraction, and using bragg's formula calculate
Lattice parameter, and the coefficient of dispersion of lattice parameter that two kinds of test methods are tested is calculated, so as to evaluate the accurate of measuring method
Property, the measurement result such as table for the lattice parameter of 12K PAN-based stabilized fiber fibers that embodiment 1 and existing powder diffraction method measure
Shown in 1.
The lattice parameter of 12K PAN-based stabilized fiber fibers tested using embodiment 2 and existing powder diffraction method, Fig. 3
It is the 12K PAN-based stabilized fiber fiber winding method XRD spectras of embodiment 2, Fig. 4 is measured by existing powder diffraction method
12K PAN-based stabilized fiber fiber XRD spectras, can directly obtain 2 θ of the angle of diffraction of sample by Fig. 3 and Fig. 4, in each method
Identical raw fibre is respectively adopted and produces 5 samples, measures 2 θ of the angle of diffraction of 5 samples respectively, and utilize bragg's formula meter
Lattice parameter is calculated, and calculates the coefficient of dispersion of lattice parameter that two kinds of test methods are tested, so as to evaluate the standard of measuring method
The measurement result of the lattice parameter of 12K PAN-based stabilized fiber fibers that true property, embodiment 1 and existing powder diffraction method measure is such as
Shown in table 2.
2 embodiment 2 of table and existing powder diffraction method measure the interplanar distance of 12K PAN-based stabilized fiber fibers
As shown in Table 2, the interplanar distance average value of 12K PAN-based stabilized fiber fibers that the present embodiment is calculated is
0.3540nm, the interplanar distance average value that existing powder diffraction method measures are 0.3541nm, and by comparison, this example calculation obtains
To the coefficient of dispersion of interplanar distance of carbon fiber reduce 16.3%, illustrate that the method through the present embodiment can be more accurate
Characterize the lattice parameter of the interplanar distance, i.e. 12K PAN-based stabilized fibers fiber of 12K PAN-based stabilized fiber fibers.
Embodiment 3
Step 1: using bakelite specimen holder of the size that bakelite makes for 50mm × 20mm × 10mm, one of them is specified
Measuring surface of the surface of 50mm × 10mm as bakelite specimen holder；
Step 2: the dorsal surface coating epoxy glue solution of the bakelite specimen holder made in step 1, the bakelite specimen holder
Dorsal surface it is opposite with measuring surface position, 3K PAN-based stabilized fibers fibre bundle is then wound around into bakelite specimen holder side by side
On, and arrange uniformly without stock phenomenon is twisted, after glue spontaneously dries, obtain sample to be tested；The epoxy glue solution is by epoxy resin
E51, triethylene tetramine and polyamide are according to 100:2:30 mass ratio is made；
The detailed process of the winding is：One end of 3K PAN-based stabilized fiber fibre bundles is placed on tensioner, 3K gathers
The other end of acrylonitrile oxidization fiber fibre bundle is fixed on the dorsal surface of bakelite specimen holder, the 3K PAN-based stabilized fibers fiber
Beam is wound around on bakelite specimen holder successively along clockwise direction, of 3K PAN-based stabilized fibers fibre bundle during winding
Power is 5N；Coincidence between the adjacent two 3K PAN-based stabilized fiber fibre bundles being wrapped on bakelite specimen holder cannot go out
Existing gap；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtain
To 2 θ of the angle of diffraction of 3K PAN-based stabilized fiber fibers, 3K polypropylene is calculated finally by bragg's formula d=n λ/2sin θ
The lattice parameter of the interplanar distance d, i.e. 3K PAN-based stabilized fibers fiber of nitrile oxidization fiber fiber.Wherein λ is incident X-rays wavelength
(i.e. CuKa wavelength is 0.15406nm)；θ is Bragg angle (°), and n is to reflect integer (the present embodiment n=that series and n are >=1
1)。
The lattice parameter of 3K PAN-based stabilized fiber fibers tested using embodiment 3 and existing powder diffraction method, Fig. 5 are
The XRD spectra for the 3K PAN-based stabilized fiber fibers that the present embodiment measures, Fig. 6 is the 3K poly- third that existing powder diffraction method measures
The XRD spectra of alkene nitrile oxidization fiber fiber can directly obtain 2 θ of the angle of diffraction of sample by Fig. 5 and Fig. 6, be adopted respectively in each method
5 samples are produced with identical raw fibre, measure 2 θ of the angle of diffraction of 5 samples respectively, and utilize bragg's formula counting lattice
Parameter, and the coefficient of dispersion of lattice parameter that two kinds of test methods are tested is calculated, it is real so as to evaluate the accuracy of measuring method
It is as shown in table 3 to apply the measurement result of the lattice parameter of 3K PAN-based stabilized fiber fibers that example 1 and existing powder diffraction method measure.
3 embodiment 3 of table and existing powder diffraction method measure the interplanar distance of 3K PAN-based stabilized fiber fibers
As shown in Table 3, the average value of the interplanar distance of 3K PAN-based stabilized fiber fibers that the present embodiment is calculated is
0.3489nm, the average value of the interplanar distance of 3K PAN-based stabilized fiber fibers that existing powder diffraction method measures are
0.3490nm, by comparison, the coefficient of dispersion of the interplanar distance of 3K PAN-based stabilized fiber fibers that the present embodiment is calculated
Reduce 14.0%, illustrate the method through the present embodiment can more accurate characterization 3K PAN-based stabilized fibers fiber crystal face
The lattice parameter of spacing, i.e. 3K PAN-based stabilized fibers fiber.
Embodiment 4
Step 1: using graphite sample frame of the size that graphite makes for 50mm × 20mm × 10mm, one of them is specified
Measuring surface of the surface of 50mm × 10mm as graphite sample frame；
Step 2: the dorsal surface coating phenolic aldehyde glue of the graphite sample frame made in step 1, the graphite sample frame
Dorsal surface it is opposite with measuring surface position, then 6K PAN-based stabilized fibers fibre bundle is wound around on specimen holder side by side,
And arrangement is uniformly without stubborn stock phenomenon, then the graphite sample for being closely wound 6K PAN-based stabilized fiber fibre bundles is placed on hot place
It manages in stove, is first warming up to 80 DEG C with the heating rate of 10 DEG C/h, keep the temperature 1.5h, be then warming up to the heating rate of 20 DEG C/h
120 DEG C, 1.5h is kept the temperature, then 165 DEG C are warming up to the heating rate of 20 DEG C/h, keep the temperature 2h, obtained after last natural cooling to be measured
Sample；The phenolic aldehyde glue is by the alcoholic solution of boron bakelite resin with White Carbon black according to 100:0.2 mass ratio is made, the boron
The alcoholic solution of phenolic resin, which is dissolved in by boron bakelite resin in alcohol, to be made, and the mass ratio of the boron bakelite resin and alcohol is
1:1, a concentration of 75wt% of the alcohol；
The detailed process of the winding is：One end of 6K PAN-based stabilized fiber fibre bundles is placed on tensioner, 6K gathers
The other end of acrylonitrile oxidization fiber fibre bundle is fixed on the dorsal surface of graphite sample frame, the 6K PAN-based stabilized fibers fiber
Beam is wound around on graphite sample frame successively along clockwise direction, of 6K PAN-based stabilized fibers fibre bundle during winding
Power is 15N；Coincidence between the adjacent two 6K PAN-based stabilized fiber fibre bundles being wrapped on graphite sample frame cannot
There is gap；
Step 3: sample to be tested described in step 2 is warming up to 1500 DEG C with the rate of 50 DEG C/h from room temperature and keeps the temperature 2 hours,
It is tested after Temperature fall using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtains heat
2 θ of the angle of diffraction of 6K PAN-based stabilized fibers fiber after processing calculates 6K finally by bragg's formula d=n λ/2sin θ and gathers
The interplanar distance d of acrylonitrile oxidization fiber fiber, that is, the lattice parameter of the 6K PAN-based stabilized fiber fibers after being heat-treated.Wherein λ
For incident X-rays wavelength (i.e. CuKa wavelength is 0.15406nm)；θ is Bragg angle (°), n be reflect series and n be >=1 it is whole
Number (the present embodiment n=1).
The lattice of 6K PAN-based stabilized fiber fibers is joined after the heat treatment tested using embodiment 4 and existing powder diffraction method
Number, Fig. 7 are the XRD spectras of the 6K PAN-based stabilized fiber fibers after the heat treatment that embodiment 4 measures, and Fig. 8 is existing powder
The XRD spectra of 6K PAN-based stabilized fiber fibers after the heat treatment that diffraction approach measures, sample can be directly obtained by Fig. 7 and Fig. 8
2 θ of the angle of diffraction of product is respectively adopted identical raw fibre in each method and produces 5 samples, measures the diffraction of 5 samples respectively
2 θ of angle, and bragg's formula counting lattice parameter is utilized, and calculate the discrete system of lattice parameter that two kinds of test methods are tested
Number, so as to evaluate the accuracy of measuring method, 6K polyacrylonitrile is pre- after the heat treatment that embodiment 1 and existing powder diffraction method measure
The measurement result of the lattice parameter of oxygen silk fiber is as shown in table 4.
4 embodiment 4 of table and existing powder diffraction method measure the interplanar distance of 6K PAN-based stabilized fiber fibers after heat treatment
The average value of the interplanar distance of 6K PAN-based stabilized fibers fiber is after the heat treatment that the present embodiment is calculated
0.3482nm, the average value of the interplanar distance of 6K PAN-based stabilized fibers fiber after the heat treatment that existing powder diffraction method measures
For 0.3483nm, by comparison, the interplanar distance of 6K PAN-based stabilized fibers fiber after the heat treatment that the present embodiment is calculated
Coefficient of dispersion reduce 15.5%, illustrate through the present embodiment method can more accurate characterization heat treatment after 6K polypropylene
The lattice parameter of the interplanar distance, i.e. 6K PAN-based stabilized fibers fiber of nitrile oxidization fiber fiber.
Embodiment 5
Step 1: using graphite sample frame of the size that graphite makes for 50mm × 20mm × 10mm, one of them is specified
Measuring surface of the surface of 50mm × 10mm as graphite sample frame；
Step 2: the dorsal surface coating phenolic aldehyde glue of the graphite sample frame made in step 1, the graphite sample frame
Dorsal surface it is opposite with measuring surface position, then 1K polyacrylonitrile carbon fibers beam is wound around on specimen holder side by side, and arrange
Row are uniformly without stock phenomenon is twisted, then the graphite sample for being closely wound fibre bundle is placed in heat-treatment furnace, first with the liter of 9 DEG C/h
Warm rate is warming up to 75 DEG C, keeps the temperature 2h, is then warming up to 115 DEG C with the heating rate of 18 DEG C/h, keeps the temperature 2h, then with 18 DEG C/h's
Heating rate is warming up to 160 DEG C, keeps the temperature 3h, sample to be tested is obtained after last natural cooling；The phenolic aldehyde glue is by boron phenolic tree
The alcoholic solution of fat is with White Carbon black according to 100:1 mass ratio is made, and the alcoholic solution of the boron bakelite resin is by boron phenolic tree
Fat is dissolved in alcohol and is made, and the mass ratio of the boron bakelite resin and alcohol is 1:1, a concentration of 90wt% of alcohol；
The detailed process of the winding is：One end of 1K polyacrylonitrile carbon fiber beams is placed on tensioner, 1K polypropylene
The other end of nitrile carbon fiber bundle is fixed on the dorsal surface of graphite sample frame, and the 1K polyacrylonitrile carbon fibers beam edge is square clockwise
To winding around successively on graphite sample frame, the tension of the 1K polyacrylonitrile carbon fibers beam is 10N during winding；It is described to twine
Gap cannot occur in the coincidence being wound between adjacent two 1K polyacrylonitrile carbon fiber beams on graphite sample frame；
Step 3: sample to be tested described in step 2 is warming up to 1500 DEG C with the rate of 50 DEG C/h from room temperature and keeps the temperature 2 hours,
It is tested after Temperature fall using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtains heat
2 θ of the angle of diffraction of 1K polyacrylonitrile carbon fibers after processing calculates 1K polypropylene finally by bragg's formula d=n λ/2sin θ
The interplanar distance d of nitrile carbon fiber, that is, the lattice parameter of the 1K polyacrylonitrile carbon fibers after being heat-treated.Wherein λ is incident X-rays wave
Long (i.e. CuKa wavelength is 0.15406nm)；θ is Bragg angle (°), and n is to reflect integer (the present embodiment n that series and n are >=1
=1).
The lattice parameter of 1K polyacrylonitrile carbon fibers after the heat treatment tested using embodiment 5 and existing powder diffraction method,
Fig. 9 is the XRD spectra of the 1K polyacrylonitrile carbon fibers after the heat treatment that embodiment 5 measures, and Figure 10 is existing powder diffraction method
The XRD spectra of 1K polyacrylonitrile carbon fibers after the heat treatment measured can directly obtain the angle of diffraction of sample by Fig. 9 and Figure 10
2 θ are respectively adopted identical raw fibre in each method and produce 5 samples, measure 2 θ of the angle of diffraction of 5 samples respectively, and utilize
Bragg's formula counting lattice parameter, and the coefficient of dispersion of lattice parameter that two kinds of test methods are tested is calculated, so as to evaluate
The lattice of 1K polyacrylonitrile carbon fibers after the heat treatment that the accuracy of measuring method, embodiment 1 and existing powder diffraction method measure
The measurement result of parameter is as shown in table 5.
5 embodiment 5 of table and existing powder diffraction method measure the interplanar distance of 1K polyacrylonitrile carbon fibers after heat treatment
As shown in Table 5, the present embodiment be calculated heat treatment after 1K polyacrylonitrile carbon fibers interplanar distance average value
The average value of the interplanar distance of 1K polyacrylonitrile carbon fibers is after the heat treatment obtained for 0.3493nm, existing powder diffraction method
0.3492nm, by comparison, the interplanar distance of 1K polyacrylonitrile carbon fibers is discrete after the heat treatment that the present embodiment is calculated
Coefficient has dropped 21.6%, illustrate through the present embodiment method can more accurate characterization heat treatment after 1K polyacrylonitrile carbon fibers
Interplanar distance, i.e. 1K polyacrylonitrile carbon fibers lattice parameter.
Embodiment 6
Step 1: using bakelite specimen holder of the size that bakelite makes for 50mm × 20mm × 10mm, one of them is specified
Measuring surface of the surface of 50mm × 10mm as bakelite specimen holder；
Step 2: the dorsal surface coating epoxy glue solution of the bakelite specimen holder made in step 1, the bakelite specimen holder
Dorsal surface it is opposite with measuring surface position, then aramid fiber is wound around on specimen holder side by side, and arrange uniformly without twist
Stock phenomenon, after epoxy glue solution spontaneously dries, sample to be tested is obtained in the measuring surface of bakelite specimen holder；The epoxy glue solution is by ring
Oxygen resin E51, triethylene tetramine and polyamide are according to 100:3:35 mass ratio is made；
The detailed process of the winding is：One end of aramid fiber is placed on tensioner, the other end of aramid fiber is consolidated
It being scheduled on the dorsal surface of bakelite specimen holder, the aramid fiber is wound around on bakelite specimen holder successively along clockwise direction,
The tension of the aramid fiber is 10N during winding；Coincidence between adjacent two aramid fibers being wrapped on specimen holder
Gap cannot occur；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested in measuring surface in step 2, obtain
To 2 θ of the angle of diffraction of aramid fiber, the interplanar distance d of aramid fiber is calculated finally by bragg's formula d=n λ/2sin θ,
That is the lattice parameter of aramid fiber.Wherein λ is incident X-rays wavelength (i.e. CuKa wavelength is 0.15406nm)；θ is Bragg angle
(°), the integer (the present embodiment n=1) that n is reflection series and n is >=1.
Using the lattice parameter of the aramid fiber of above method test, Figure 11 is the XRD for the aramid fiber that embodiment 6 measures
Spectrogram can directly obtain 2 θ of the angle of diffraction of sample by Figure 11, and identical raw fibre is respectively adopted and produces 5 samples, surveys respectively
2 θ of the angle of diffraction of 5 samples is measured, and utilizes bragg's formula counting lattice parameter, and calculates the crystalline substance that two kinds of test methods are tested
The coefficient of dispersion of lattice parameter, so as to evaluate the accuracy of measuring method, the aramid fiber that embodiment 1 and existing powder diffraction method measure is fine
The measurement result of the lattice parameter of dimension is as shown in table 6.
6 embodiment 6 of table winding diffraction approach measures the interplanar distance of aramid fiber
As shown in Table 6, the average value of the interplanar distance for the aramid fiber that the present embodiment is calculated is 0.5436nm, due to
Aramid fiber is difficult the powder for being ground into test request, and existing powder diffraction method can not obtain the interplanar distance of aramid fiber.This
The coefficient of dispersion of the interplanar distance for the aramid fiber that embodiment is calculated is 0.0154%, illustrates that the method through the present embodiment can
To meet aramid fiber material lattice parameter testing requirement.
The above is only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art substantially makees above example, still fall within technical solution of the present invention
Protection domain in.
Claims (9)
1. a kind of test method of fiber lattice parameter, the fiber is aramid fiber, carbon fiber and oxidization fiber fiber, feature
It is, this method includes the following steps：
Step 1: making the specimen holder of cube structure, an outer surface for specifying the specimen holder is test surfaces；
Step 2: the dorsal surface coating glue of the specimen holder made in step 1, the dorsal surface and test surfaces of the specimen holder
Position is opposite, then winds around fibre bundle on specimen holder side by side, after glue drying, obtains sample to be tested；
When the fibre bundle is carbon fiber or oxidization fiber fiber, the specimen holder made in step 1 is bakelite specimen holder or graphite
Specimen holder, when the fibre bundle is aramid fiber beam, the specimen holder made in step 1 is bakelite specimen holder；
Step 3: being tested using X-ray diffraction method being located at the sample to be tested on test surfaces in step 2, fiber is obtained
2 θ of the angle of diffraction finally calculates the lattice parameter of fiber.
A kind of 2. test method of fiber lattice parameter according to claim 1, which is characterized in that sample described in step 1
The size of product frame is 50mm × 20mm × 10mm, specifies test surfaces of the surface of one of 50mm × 10mm as specimen holder.
3. the test method of a kind of fiber lattice parameter according to claim 1, which is characterized in that twined described in step 2
Around detailed process be：One end of fibre bundle is placed on tensioner, the other end of fibre bundle is fixed on the dorsal surface of specimen holder
On, the fibre bundle is wound around on specimen holder successively along clockwise direction, during winding the tension of the fibre bundle for 5N~
15N。
A kind of 4. test method of fiber lattice parameter according to claim 1, which is characterized in that sample described in step 2
Product frame is bakelite specimen holder, is epoxy glue solution coated in the glue on specimen holder.
5. a kind of test method of fiber lattice parameter according to claim 4, which is characterized in that the epoxy glue solution by
Epoxy resin E51, triethylene tetramine and polyamide are according to 100:(2~4):The mass ratio of (30~40) is made.
A kind of 6. test method of fiber lattice parameter according to claim 1, which is characterized in that sample described in step 2
Product frame is graphite sample frame, is phenolic aldehyde glue coated in the glue on graphite sample frame.
7. a kind of test method of fiber lattice parameter according to claim 6, which is characterized in that the phenolic aldehyde glue by
The alcoholic solution of boron bakelite resin is with White Carbon black according to 100:The mass ratio of (0.2~1.5) is made, the wine of the boron bakelite resin
Smart solution, which is dissolved in by boron bakelite resin in alcohol, to be made, and the mass ratio of the boron bakelite resin and alcohol is 1:1.
A kind of 8. test method of fiber lattice parameter according to claim 6, which is characterized in that the dry phenol glue
The process of liquid is：The graphite sample for being closely wound fibre bundle is placed in heat-treatment furnace, first with the liter of 9 DEG C/h~11 DEG C/h
Warm rate is warming up to 75 DEG C~85 DEG C, keeps the temperature 1h~2h, then with the heating rate of 18 DEG C/h~22 DEG C/h be warming up to 115 DEG C~
125 DEG C, 1h~2h is kept the temperature, is further continued for being warming up to 160 DEG C~170 DEG C with the heating rate of 18 DEG C/h~22 DEG C/h, heat preservation 1h~
3h, last natural cooling.
9. the test method of a kind of fiber lattice parameter according to claim 6, which is characterized in that spread out using X ray
It penetrates before method test, first the sample to be tested is heat-treated.
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