CN109342402A - A kind of ceramic material method for measuring stress based on Raman spectrum - Google Patents
A kind of ceramic material method for measuring stress based on Raman spectrum Download PDFInfo
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- CN109342402A CN109342402A CN201811515453.2A CN201811515453A CN109342402A CN 109342402 A CN109342402 A CN 109342402A CN 201811515453 A CN201811515453 A CN 201811515453A CN 109342402 A CN109342402 A CN 109342402A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
Abstract
The present invention discloses a kind of ceramic material method for measuring stress based on Raman spectrum, different size of pressure is applied to multiple ceramic samples by acquisition and generates different Raman spectrograms, determine the crest location of Raman spectrogram, the Raman stress coefficient that ceramic material can be obtained according to the frequency shift amount relational graph of stress and Raman spectrogram crest location can calculate the internal stress size of the unknown ceramic sample of internal stress using the corresponding Raman spectrum main peak frequency shift amount of the unknown ceramic sample of Raman stress coefficient and internal stress.This method also proposed a kind of device that can apply constant stress to ceramic material, it can guarantee obtaining for ceramic sample Raman stress coefficient X, to can directly calculate the size of unknown stress according to the corresponding Raman spectrum main peak frequency shift amount of the unknown ceramic sample of internal stress, it is easy to operate, it is widely used in brittle ceramic materials, and vulnerable to external interference, the precision of measurement does not can be improved in Raman spectrum.
Description
Technical field
The present invention relates to ceramic material mechanical meaurement fields, answer more particularly to a kind of ceramic material based on Raman spectrum
Force measuring method.
Background technique
In the prior art, XRD mensuration is commonly used to measure ceramic-like materials stress.XRD mensuration is by material
Material carries out X-ray diffraction, analyzes its diffracting spectrum, obtains the ingredient of material, the structure or form of material internal atom or molecule
Etc. information research means.
The basic principle of XRD measurement stress are as follows: change inside sample there are when stress, the spacing of lattice of crystal can be generated
Become, causes x-ray diffraction angle to change, enter with the available stress of Elasticity formula with X-ray in conjunction with Bragg diffraction equation
The relation formula of firing angle, the angle of diffraction: σψ=KM, whereinWork as test
When diffraction surfaces are constant, K value is definite value, and M is (2 θ)-sin2The slope of ψ straight line.X-ray incidence angle available one is varied multiple times
2 θ of the angle of diffraction of series, it can thus be concluded that slope M and the stress value in sample is finally calculated.
Since XRD mensuration needs to be varied multiple times X-ray incidence angle, so that this method measurement process is complicated, and because X
Ray diffraction peaks peak intensity is weaker, and vulnerable to external interference, so that measurement accuracy is inaccurate.
Summary of the invention
The object of the present invention is to provide a kind of ceramic material method for measuring stress based on Raman spectrum reaches operation letter
Just, the effect of measurement accuracy is improved.
To achieve the above object, the present invention provides following schemes:
A kind of ceramic material method for measuring stress based on Raman spectrum, which comprises
Obtain the Raman spectrogram for the ceramic sample not stressed, the Raman spectrogram for the ceramic sample not stressed described in determination
Peak position；
Different size of power is applied to multiple ceramic samples, obtains the ceramic sample for applying the different size of power
Raman spectrogram, determine the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power；
According to the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power and it is described not
The Raman frequency shift amount of the peak position of the Raman spectrogram of the ceramic sample of stress and the corresponding different size of power, meter
Calculate the Raman stress coefficient of the ceramic sample；
Ceramic sample identical as the ceramic sample material but that internal stress is unknown is selected, it is unknown to obtain the internal stress
Ceramic sample Raman spectrogram determines the peak position of the unknown ceramic sample Raman spectrogram of the internal stress；
According to the peak position of the unknown ceramic sample Raman spectrogram of the stress and the ceramic sample not stressed
Raman spectrogram peak position Raman frequency shift amount and the ceramic sample Raman stress coefficient, calculate it is described in answer
The value of the unknown ceramic sample internal stress of power.
Optionally, described to obtain the Raman spectrogram of ceramic sample not stressed, determine described in the ceramic sample that does not stress
The peak position of Raman spectrogram specifically include:
The ceramic sample is placed in and is answered in force retaining device, force retaining device is answered described in adjustment, makes the ceramics examination
Sample stress is zero, and the length x of the spring of force retaining device is answered described in record0；
By under the object lens probe for answering force retaining device to be placed in Raman spectrum tester, the Raman spectrum is set and is surveyed
The excitation wavelength for trying instrument is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, obtain it is described not by
The Raman spectrogram of the ceramic sample of power；
The peak position ω of the Raman spectrogram for the ceramic sample not stressed described in determination0。
Optionally, force retaining device is answered described in the adjustment, makes the specific steps of the ceramic sample stress zero are as follows: is full
The foot spring is freely without deformation state.
Optionally, described that different size of power is applied to multiple ceramic samples, it is described different size of to obtain application
The Raman spectrogram of the ceramic sample of power determines the Raman spectrogram of the ceramic sample for applying the different size of power
Peak position specifically includes:
By the ceramic sample be placed in it is described answer in force retaining device, force retaining device is answered described in adjustment, to multiple institutes
It states ceramic sample and applies the different size of power, the length x of the spring of force retaining device is answered described in recordi；
By under the object lens probe for answering force retaining device to be placed in the Raman spectrum tester, the Raman light is set
The excitation wavelength for composing tester is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, applied
The Raman spectrogram of the ceramic sample of the different size of power；
Determine the peak position ω of the Raman spectrogram of the ceramic sample for applying the different size of poweri。
Optionally, the main peak position of the Raman spectrogram according to the ceramic sample for applying the different size of power
It sets big with the Raman frequency shift amount of the peak position of the Raman spectrogram of the ceramic sample not stressed and the corresponding difference
Small power, the Raman stress coefficient for calculating the ceramic sample specifically include:
According to Hooke's law Δ Fi=k Δ xiForce retaining device is answered to apply the ceramic sample described in calculating stressed
Size, wherein Δ FiFor the stress value of the ceramic sample, k is the stiffness factor of the spring, Δ xiFor the deformation of the spring
Amount, Δ xi=x0-xi, wherein x0Indicate the length of the spring when ceramic sample does not stress, xiExpression states ceramics to described
Sample applies the length of spring when different size power；
According to formula σi=Δ Fi/ S calculates the stress of the ceramic sample, wherein σiIndicate the stress of the ceramic sample
Size, S indicate the size of the forced area of the ceramic sample；
Measure the Raman spectrogram of the ceramic sample for applying the different size of power peak position and it is described not
The Raman frequency shift amount Δ ω of the peak position of the Raman spectrogram of the ceramic sample of stressi；
Using the stress of the ceramic sample as horizontal axis, rectangular coordinate system is established using the Raman frequency shift amount as the longitudinal axis, in institute
The stress intensity point corresponding with the Raman frequency shift amount for drawing the ceramic sample in vertical rectangular coordinate system is stated, determines the point
Corresponding straight line calculates the slope of the straight line, determines that the slope is the Raman stress coefficient X of the ceramic sample.
Optionally, the selection is identical as the ceramic sample material but ceramic sample that internal stress is unknown, described in acquisition
The unknown ceramic sample Raman spectrogram of internal stress, determines the main peak position of the unknown ceramic sample Raman spectrogram of the internal stress
It sets and specifically includes:
Select a ceramic sample identical as the ceramic sample material but that internal stress is unknown；
The unknown ceramic sample of the internal stress is placed under the object lens probe of the Raman spectrum tester, institute is set
The excitation wavelength for stating Raman spectrum tester is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1,
Obtain the Raman spectrogram of the unknown ceramic sample of the internal stress；
Determine the peak position ω of the Raman spectrogram of the unknown ceramic sample of the internal stressx。
Optionally, the peak position of the ceramic sample Raman spectrogram unknown according to the internal stress and it is described not by
The Raman frequency shift amount of the peak position of the Raman spectrogram of the ceramic sample of power and the Raman stress coefficient of the ceramic sample,
The value for calculating the unknown ceramic sample internal stress of the internal stress specifically includes:
The unknown ceramic sample of the internal stress is placed in the lower setting institute of object lens probe of the Raman spectrum tester
The excitation wavelength for stating Raman spectrum tester is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1,
Obtain the Raman spectrogram of the unknown ceramic sample of the internal stress；
Measure the peak position and the ceramics not stressed of the Raman spectrogram of the unknown ceramic sample of the internal stress
The Raman frequency shift amount Δ ω of the peak position of the Raman spectrogram of samplex=| ωx-ω0|, wherein ωxFor the internal stress
The peak position of the Raman spectrogram of unknown ceramic sample, ω0For the Raman spectrogram of the ceramic sample not stressed
Peak position；
According to formulaThe size of the unknown stress of the unknown ceramic sample of the internal stress is calculated, wherein X is described
The Raman stress coefficient of ceramic sample.
Optionally, it needs to carry out silicon wafer correction before obtaining Raman spectrogram.
A kind of ceramic material stress measurement system based on Raman spectrum, including force retaining device and Raman spectrum is answered to test
Instrument, described to answer force retaining device include: spring, screw rod, nut, equal power piece and matrix, and the screw rod is fixed on the matrix,
The nut, the equal power piece and the spring are sequentially sleeved on the screw rod, the spring, the equal power piece and the nut
On same level axis, one end of the spring is contacted with the equal power piece, and the other end and the ceramic sample of the spring connect
Touching；Rotating the nut makes the equal power piece compress the spring generation deformation, and the spring answers ceramic sample application
Power is arranged under the object lens probe for answering force retaining device to be placed in the Raman spectrum tester Raman spectrum and surveys
The excitation wavelength for trying instrument is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, applied described in
The Raman spectrogram of the ceramic sample of power utilizes the ceramic material stress measurement described in any of the above-described based on Raman spectrum
Method measures the stress of the ceramic material.
The specific embodiment provided according to the present invention, the invention discloses following technical effects: the present invention passes through acquisition pair
Multiple ceramic samples apply different size of pressure and generate different Raman spectrograms, determine the wave crest position of Raman spectrogram
It sets, the Raman stress coefficient of ceramic material can be obtained according to the frequency shift amount relational graph of stress and Raman spectrogram crest location,
It can be calculated in unknown using the corresponding Raman spectrum main peak frequency shift amount of the unknown ceramic sample of Raman stress coefficient and internal stress
The stress intensity of the ceramic sample of stress.This method also proposed a kind of device that can apply constant stress to ceramic material, energy
Enough guarantee obtaining for ceramic sample Raman stress coefficient X, thus according to the corresponding Raman spectrum of the unknown ceramic sample of internal stress
Main peak frequency shift amount can directly calculate the size of unknown internal stress, easy to operate, be widely used in brittle ceramic materials, and draw
Vulnerable to external interference, the precision of measurement does not can be improved in graceful spectrum.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the flow chart of the ceramic material method for measuring stress provided in an embodiment of the present invention based on Raman spectrum；
Fig. 2 is the frequency shift amount relational graph of stress provided in an embodiment of the present invention and Raman spectrogram crest location；
Fig. 3 is the ceramic material stress measurement system schematic diagram provided in an embodiment of the present invention based on Raman spectrum.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The object of the present invention is to provide a kind of ceramic material method for measuring stress based on Raman spectrum, according to ceramic style
Stress-Raman frequency shift measures out the Raman stress coefficient X of ceramic style, then corresponding using Raman stress coefficient and unknown stress
The frequency shift amount of Raman spectrum main peak can calculate the stress intensity of ceramic sample.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
Embodiment
As shown in Figure 1, the ceramic material method for measuring stress provided in this embodiment based on Raman spectrum includes:
Step 101: obtaining the Raman spectrogram for the ceramic sample not stressed, the drawing for the ceramic sample not stressed described in determination
The peak position of graceful spectrogram.
In the present embodiment, specifically using the master of the Raman spectrogram for the ceramic sample not stressed described in following steps determination
Peak position.
The ceramic sample is placed in and is answered in force retaining device, force retaining device is answered described in adjustment, makes the ceramics examination
Sample stress is zero, and the length x of the spring of force retaining device is answered described in record0；
By under the object lens probe for answering force retaining device to be placed in Raman spectrum tester, the Raman spectrum is set and is surveyed
The excitation wavelength for trying instrument is 532nm, may be set to be 355nm, and the range that the excitation wavelength is arranged is 100-1000cm-1,
The Raman spectrogram for the ceramic sample not stressed described in acquisition；
The peak position ω of the Raman spectrogram for the ceramic sample not stressed described in determination0=660.397cm-1。
By limiting the range of optical maser wavelength as 100-1000cm-1, can quickly obtain Raman spectrogram.
In a step 101, answer force retaining device described in adjustment, make the ceramic sample stress zero the specific steps are,
The nut that force retaining device is answered described in rotation guarantees equal power piece not compressed spring, is in spring freely without deformation state.
Step 102: different size of power being applied to multiple ceramic samples, obtains and applies the different size of power
The Raman spectrogram of ceramic sample determines the main peak of the Raman spectrogram of the ceramic sample for applying the different size of power
Position.
In the present embodiment, the ceramic sample for applying the different size of power specifically is determined using following steps
The peak position of Raman spectrogram.
By the ceramic sample be placed in it is described answer in force retaining device, force retaining device is answered described in adjustment, to the pottery
Porcelain sample applies five different size of power, and the length x of the spring of force retaining device is answered described in record1~x5, according to Hooke's law
The deformation quantity Δ x of Δ F=k Δ x and spring calculates the power of ceramic style being subject to；Wherein k is the coefficient of elasticity of spring, Δ x
=x0-xi, i=1 ... 5, x0Indicate the length of spring when ceramic sample does not stress, xiIndicate different big to ceramic sample application is stated
The length of spring when small stress.
By under the object lens probe for answering force retaining device to be placed in Raman spectrum tester, the Raman spectrum is set and is surveyed
The excitation wavelength for trying instrument is 532nm, may be set to be 355nm, and the range that the excitation wavelength is arranged is 100-1000cm-1,
Obtain the Raman spectrogram for applying the ceramic sample of the different size of power；
Determine the peak position ω of the Raman spectrogram of the ceramic sample for applying the five different size of poweri, i
=1 ... 5.
It selects the ceramic sample of five same types to apply different size of stress, applies not compared to same ceramic sample
With the stress of size, more representative of the characteristic of this kind of ceramic samples, so that measurement method is more accurate.
Step 103: according to the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power
With the Raman frequency shift amount and the corresponding different size of the peak position of the Raman spectrogram of the ceramic sample not stressed
Power, calculate the Raman stress coefficient of the ceramic sample.
In the present embodiment, the Raman stress coefficient of the ceramic sample is specifically calculated using following steps.
According to Hooke's law Δ Fi=k Δ xiForce retaining device is answered to apply the ceramic sample described in calculating stressed
Size, wherein Δ FiFor the stress value of the ceramic sample, k is the stiffness factor of the spring, Δ xiFor the deformation of the spring
Amount, Δ xi=x0-xi, i=1 ... 5, wherein x0Indicate the length of the spring when ceramic sample does not stress, xiIt indicates to institute
State the length that ceramic sample applies spring when different size power；
According to formula σi=Δ Fi/ S, i=1 ... 5 calculates the stress of the ceramic sample, wherein σiIndicate the ceramics examination
The stress intensity of sample, S indicate the size of the forced area of the ceramic sample；
Measure the Raman spectrogram of the ceramic sample for applying the different size of power peak position and it is described not
The Raman frequency shift amount Δ ω of the peak position of the Raman spectrogram of the ceramic sample of stressi；
As shown in Fig. 2, being established using the stress σ of the ceramic sample as horizontal axis by the longitudinal axis of the Raman frequency shift amount Δ ω
Rectangular coordinate system, the stress intensity that the ceramic sample is drawn in the vertical rectangular coordinate system are corresponding with the Raman frequency shift amount
Point, determine the corresponding straight line of the point, calculate the slope of the straight line, determine the slope be the ceramic sample Raman
Stress coefficient X=7.9 × 10-5(cm-1/Pa)。
When drawing the stress intensity of the ceramic sample with the corresponding straight line of the corresponding point of Raman frequency shift amount, Ying Bao
The more points of card are located on straight line, and meet the two sides that point not on straight line is uniformly just distributed in straight line, guarantee Raman stress
The accuracy of coefficient X.
Step 104: the ceramic sample that selection is identical as the ceramic sample material but internal stress is unknown is obtained and is answered in described
The unknown ceramic sample Raman spectrogram of power, determines the peak position of the unknown ceramic sample Raman spectrogram of the internal stress.
In the present embodiment, the Raman spectrogram of the unknown ceramic sample of the internal stress is specifically determined using following steps
Peak position.
A ceramic sample x identical with the ceramic sample material is selected, ceramic sample x is put into Muffle furnace and is heated
It is air-cooled after keeping the temperature a hour to 800 DEG C, obtain the unknown ceramic sample x of internal stress；
The unknown ceramic sample x of the internal stress is placed under the object lens probe of the Raman spectrum tester, setting
The excitation wavelength of the Raman spectrum tester is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-
1000cm-1, obtain the Raman spectrogram of the unknown ceramic sample x of the internal stress；
Determine the peak position ω of the Raman spectrogram of the unknown ceramic sample x of the internal stressx。
The method that ceramic material internal stress changes has stress, temperature change etc., and the present invention is to change to make pottery by temperature change
The internal stress of ceramic material, but the mode for changing internal stress is not limited to change temperature.
Step 105: not stressed according to the peak position of the unknown ceramic sample Raman spectrogram of the internal stress with described
Ceramic sample Raman spectrogram peak position Raman frequency shift amount and the ceramic sample Raman stress coefficient, meter
Calculate the value of the unknown ceramic sample stress of the internal stress.
In the present embodiment, the value of the unknown stress of ceramic sample x is specifically calculated using following steps.
Measure the peak position and the ceramics not stressed of the Raman spectrogram of the unknown ceramic sample x of the internal stress
The Raman frequency shift amount Δ ω of the peak position of the Raman spectrogram of samplex=| ωx-ω0|=10.225cm-1；
According to formulaThe size of the internal stress of the unknown ceramic sample x of the internal stress is calculated,Wherein X is the Raman stress coefficient of the ceramic sample.
Ceramic material method for measuring stress provided by the invention based on Raman spectrum, utilizes the Raman stress of ceramic sample
Coefficient X and Raman frequency shift amount can directly calculate the internal stress of ceramic sample, easy to operate.
In the ceramic material method for measuring stress based on Raman spectrum, obtain every time ceramic style Raman spectrogram it
Before, the accuracy of measurement method can be improved in all progress silicon wafer corrections.
As shown in figure 3, the ceramic material stress measurement system based on Raman spectrum includes answering force retaining device 6 and Raman light
Tester 7 is composed, answering force retaining device 6 includes: spring 1, equal power piece 2, nut 3, screw rod 4 and matrix 5, and screw rod 4 is fixed on 5 body of base
On, nut 3, equal power piece 2 and spring 1 are sequentially sleeved on screw rod 4, spring 1, equal power piece 2 and nut 3 on same level axis,
One end of spring 1 is contacted with equal power piece 2, and the other end of spring 1 is contacted with ceramic style；Rotating nuts 3 make equal power piece 2 compress bullet
Spring 1 generates deformation, and spring 1 applies stress, the object that force retaining device 6 will be answered to be placed in Raman spectrum tester 7 to ceramic sample
Under mirror probe, the excitation wavelength of setting Raman spectrum tester 7 is 355nm or 532nm, and the range that excitation wavelength is arranged is 100-
1000cm-1, the Raman spectrogram for applying the ceramic style of the power is obtained, using any of the above-described described based on Raman spectrum
Ceramic material method for measuring stress measures the internal stress of the ceramic material.
Ceramic material stress measurement system based on Raman spectrum include it is a kind of can to ceramic material apply constant stress
Device can guarantee obtaining for ceramic sample Raman stress coefficient X, easy to operate, be widely used in brittle ceramic materials.
For the system disclosed in the embodiment, since it is corresponded to the methods disclosed in the examples, so the ratio of description
Relatively simple, reference may be made to the description of the method.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art, foundation
Thought of the invention, there will be changes in the specific implementation manner and application range.In conclusion this specification appearance is not answered
It is interpreted as limitation of the present invention.
Claims (9)
1. a kind of ceramic material method for measuring stress based on Raman spectrum, which is characterized in that the described method includes:
Obtain the Raman spectrogram for the ceramic sample not stressed, the master of the Raman spectrogram for the ceramic sample not stressed described in determination
Peak position；
Different size of power is applied to multiple ceramic samples, obtains the drawing for applying the ceramic sample of the different size of power
Graceful spectrogram determines the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power；
It is not stressed according to the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power with described
Ceramic sample Raman spectrogram peak position Raman frequency shift amount and the corresponding different size of power, calculate institute
State the Raman stress coefficient of ceramic sample；
Ceramic sample identical as the ceramic sample material but that internal stress is unknown is selected, the unknown ceramics of the internal stress are obtained
Sample Raman spectrogram determines the peak position of the unknown ceramic sample Raman spectrogram of the internal stress；
According to the peak position of the unknown ceramic sample Raman spectrogram of the internal stress and the ceramic sample not stressed
The Raman frequency shift amount of the peak position of Raman spectrogram and the Raman stress coefficient of the ceramic sample, calculate the internal stress
The value of unknown ceramic sample internal stress.
2. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that described to obtain
The Raman spectrogram for the ceramic sample that must do not stressed, determine described in the peak position of the Raman spectrogram of ceramic sample that does not stress
It specifically includes:
The ceramic sample is placed in and is answered in force retaining device, force retaining device is answered described in adjustment, make the ceramic sample by
Power is zero, and the length x of the spring of force retaining device is answered described in record0；
By under the object lens probe for answering force retaining device to be placed in Raman spectrum tester, the Raman spectrum tester is set
Excitation wavelength be 355nm or 532nm, be arranged the excitation wavelength range be 100-1000cm-1, do not stress described in acquisition
The Raman spectrogram of ceramic sample；
The peak position ω of the Raman spectrogram for the ceramic sample not stressed described in determination0。
3. the ceramic material method for measuring stress according to claim 2 based on Raman spectrum, which is characterized in that the tune
Force retaining device is answered described in whole, makes the specific steps of the ceramic sample stress zero are as follows: meets the spring for freely without change
Shape state.
4. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that described right
Multiple ceramic samples apply different size of power, obtain the Raman spectrum for applying the ceramic sample of the different size of power
Figure determines that the peak position of the Raman spectrogram of the ceramic sample for applying the different size of power specifically includes:
By the ceramic sample be placed in it is described answer in force retaining device, force retaining device is answered described in adjustment, to multiple potteries
Porcelain sample applies the different size of power, and the length x of the spring of force retaining device is answered described in recordi；
By under the object lens probe for answering force retaining device to be placed in the Raman spectrum tester, the Raman spectrum is set and is surveyed
The excitation wavelength for trying instrument is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, applied described in
The Raman spectrogram of the ceramic sample of different size of power；
Determine the peak position ω of the Raman spectrogram of the ceramic sample for applying the different size of poweri。
5. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that described
According to the peak position and the ceramics not stressed of the Raman spectrogram of the ceramic sample for applying the different size of power
The Raman frequency shift amount of the peak position of the Raman spectrogram of sample and the corresponding different size of power, calculate the ceramics
The Raman stress coefficient of sample specifically includes:
According to Hooke's law Δ Fi=k Δ xiForce retaining device is answered to apply stressed size to the ceramic sample described in calculating,
Wherein Δ FiFor the stress value of the ceramic sample, k is the stiffness factor of the spring, Δ xiFor the deformation quantity of the spring, Δ
xi=x0-xi, wherein x0Indicate the length of the spring when ceramic sample does not stress, xiThe ceramic sample of stating is applied in expression
The length of spring when adding different size power；
According to formula σi=Δ Fi/ S calculates the stress of the ceramic sample, wherein σiIndicate the stress intensity of the ceramic sample,
S indicates the size of the forced area of the ceramic sample；
The peak position for measuring the Raman spectrogram of the ceramic sample for applying the different size of power does not stress with described
Ceramic sample Raman spectrogram peak position the Raman frequency shift amount Δ ωi；
Using the stress of the ceramic sample as horizontal axis, rectangular coordinate system is established using the Raman frequency shift amount as the longitudinal axis, described vertical
The stress intensity point corresponding with the Raman frequency shift amount that the ceramic sample is drawn in rectangular coordinate system determines that the point corresponds to
Straight line, calculate the slope of the straight line, determine the slope be the ceramic sample Raman stress coefficient X.
6. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that the choosing
Ceramic sample identical as the ceramic sample material but that internal stress is unknown is selected, the unknown ceramic sample of the internal stress is obtained and draws
Graceful spectrogram determines that the peak position of the unknown ceramic sample Raman spectrogram of the internal stress specifically includes:
Select a ceramic sample identical as the ceramic sample material but that internal stress is unknown；
The unknown ceramic sample of the internal stress is placed under the object lens probe of the Raman spectrum tester, the drawing is set
The excitation wavelength of graceful spectral investigator is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, obtain
The Raman spectrogram of the unknown ceramic sample of the internal stress；
Determine the peak position ω of the Raman spectrogram of the unknown ceramic sample of the internal stressx。
7. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that described
According to the peak position of the unknown ceramic sample Raman spectrogram of the internal stress and the Raman light of the ceramic sample not stressed
The Raman frequency shift amount of the peak position of spectrogram and the Raman stress coefficient of the ceramic sample, it is unknown to calculate the internal stress
The value of ceramic sample internal stress specifically includes:
The unknown ceramic sample of the stress is placed in the object lens probe lower setting Raman of the Raman spectrum tester
The excitation wavelength of spectral investigator is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1, obtain institute
State the Raman spectrogram of the unknown ceramic sample of stress；
Measure the peak position and the ceramic sample not stressed of the Raman spectrogram of the unknown ceramic sample of the internal stress
Raman spectrogram peak position the Raman frequency shift amount Δ ωx=| ωx-ω0|, wherein ωxIt is unknown for the internal stress
Ceramic sample Raman spectrogram peak position, ω0For the main peak of the Raman spectrogram of the ceramic sample not stressed
Position；
According to formulaThe size of the unknown stress of the unknown ceramic sample of the internal stress is calculated, wherein X is the ceramics
The Raman stress coefficient of sample.
8. the ceramic material method for measuring stress according to claim 1 based on Raman spectrum, which is characterized in that drawn
It needs to carry out silicon wafer correction before graceful spectrogram.
9. a kind of ceramic material stress measurement system based on Raman spectrum, including force retaining device and Raman spectrum is answered to test
Instrument, which is characterized in that described to answer force retaining device include: that spring, screw rod, nut, equal power piece and matrix, the screw rod are fixed on
In described matrix, the nut, the equal power piece and the spring are sequentially sleeved on the screw rod, the spring, the equal power
Piece and the nut are on same level axis, and one end of the spring is contacted with the equal power piece, the other end of the spring
It is contacted with ceramic sample；Rotating the nut makes the equal power piece compress the spring generation deformation, and the spring is to the pottery
Porcelain sample applies stress, and by under the object lens probe for answering force retaining device to be placed in the Raman spectrum tester, institute is arranged
The excitation wavelength for stating Raman spectrum tester is 355nm or 532nm, and the range that the excitation wavelength is arranged is 100-1000cm-1,
Obtain the Raman spectrogram for applying the ceramic sample of the power, using as described in claim any one of 1-7 based on Raman
The ceramic material method for measuring stress of spectrum measures the stress of the ceramic material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811515453.2A CN109342402A (en) | 2018-12-12 | 2018-12-12 | A kind of ceramic material method for measuring stress based on Raman spectrum |
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| CN110514332A (en) * | 2019-09-29 | 2019-11-29 | 福州大学 | A kind of stress test calibration experiment platform and its experimental method |
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| CN110514332A (en) * | 2019-09-29 | 2019-11-29 | 福州大学 | A kind of stress test calibration experiment platform and its experimental method |
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