CN106645006A - Method for measuring activation energy of hydroxy in oxy glass - Google Patents
Method for measuring activation energy of hydroxy in oxy glass Download PDFInfo
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- CN106645006A CN106645006A CN201710038857.6A CN201710038857A CN106645006A CN 106645006 A CN106645006 A CN 106645006A CN 201710038857 A CN201710038857 A CN 201710038857A CN 106645006 A CN106645006 A CN 106645006A
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- total oxygen
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- 239000011521 glass Substances 0.000 title claims abstract description 88
- 230000004913 activation Effects 0.000 title claims abstract description 41
- 125000002887 hydroxy group Chemical group [H]O* 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims description 38
- 229910052760 oxygen Inorganic materials 0.000 claims description 38
- 230000000930 thermomechanical effect Effects 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004611 spectroscopical analysis Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 abstract description 8
- 238000001228 spectrum Methods 0.000 abstract description 5
- 230000003595 spectral effect Effects 0.000 abstract 2
- 239000005329 float glass Substances 0.000 description 25
- 238000002485 combustion reaction Methods 0.000 description 16
- 230000008859 change Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 229910008051 Si-OH Inorganic materials 0.000 description 4
- 229910002808 Si–O–Si Inorganic materials 0.000 description 4
- 229910006358 Si—OH Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000006124 Pilkington process Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000005483 Hooke's law Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
- G01N3/18—Performing tests at high or low temperatures
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0266—Cylindrical specimens
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0298—Manufacturing or preparing specimens
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0676—Force, weight, load, energy, speed or acceleration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0688—Time or frequency
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0694—Temperature
Abstract
The invention relates to a method for measuring the activation energy of hydroxy in an oxy glass. The method comprises the following steps: S1: making a sample into a glass rod with preset size; S2: performing temperature relaxation spectrum measurement on the glass rod by utilizing a dynamic thermodynamics analyzer, and obtaining a temperature relaxation spectral graph; S3: according to the temperature relaxation spectral graph, obtaining corresponding activation energy of the glass rod. The method for measuring the activation energy of the oxy glass, provided by the invention, can be applied to characterize the influence of the hydroxy in the oxy glass to a glass structure; the method is simple, convenient and quick, the stability and the credibility is high.
Description
Technical field
The present invention relates to microstructure determination techniques field, and in particular to a kind of measurement side of total oxygen glass hydroxyl activation energy
Method.
Background technology
The microstructure of glass is closely bound up with the macro property of glass, therefore, for glass industry researcher and
The information of reflection glass microstructure how efficiently, stably and is credibly obtained for producers, always one urgently solves
Problem certainly.
All-oxygen combustion float glass process is the new popular method for currently manufacturing special glass.Compared to common air-breathing float glass process
Glass, all-oxygen combustion float glass has some preferable performances, for example, can reduce atmosphere pollution, energy reducing energy consumption, improve
Melting rate, glass melting quality are high and melting furnace structure designs simple, active time length etc..When glass is molded, water meeting and glass
Glass surface reacts, depolymerization silicon-oxy tetrahedron, causes the fracture of Si-O-Si keys, so as to cause the short texture of inside glass,
Be conducive to the migration of cation.Compared with air-breathing float glass, the steam of total oxygen melting furnaces is higher, therefore the silica four of depolymerization
Face body will be more, and the Si-OH keys of formation are more, therefore the hydroxy radical content in all-oxygen combustion float glass is more, interior microscopic
Structure is also different.
Up to now, hydroxyl is measured still rare to effective laboratory facilities of all-oxygen combustion glass Effects on Microstructure.Mesh
Before, scientists generally adopt enthalpy change measuring method (for example, differential scanning calorimetry), by the absworption peak for determining glass material
Area, carries out formula calculating, so as to obtain reacting the activation energy of inside glass structure change.Studies have shown that, traditional enthalpy change
Measuring method cannot accurately obtain activation energy of the hydroxyl to inside glass structure influence, and efficiently, stably and credibly obtain
Desired glass hydroxyl microstructure information.
The content of the invention
To solve the deficiencies in the prior art, the invention provides a kind of measuring method of total oxygen glass hydroxyl activation energy, bag
Include following steps：
S1：Sample is made into the glass bar of predefined size；
S2：Temperature relaxation spectrometry is carried out to glass bar using dynamic thermo-mechanical analsis instrument, temperature relaxation spectrogram is obtained；
S3：The corresponding activation energy of glass bar is obtained according to temperature relaxation spectrogram.
Wherein, step S3 includes：
S31：The corresponding ln τ～T of glass bar is obtained according to temperature relaxation spectrogram-1Curve；
S32：According to Arrhenius crow equation, to ln τ～T-1Curve matching, obtains the corresponding activation energy of glass bar.
Wherein, in step S31, obtained by the peak temperature in quasi- α relaxation regions in temperature relaxation spectrogram
To the corresponding ln τ～T of glass bar-1Curve.
Wherein, in step S1, the length of glass bar is between 20-40cm, diameter between 2-4cm.
Wherein, in step S2, the amplitude of dynamic thermo-mechanical analsis instrument is between 5-15 μm.
Wherein, in step S2, the heating rate of dynamic thermo-mechanical analsis instrument is between 0.5-1.5 DEG C/min.
Wherein, in step S2, the operating temperature of dynamic thermo-mechanical analsis instrument is between 50-590 degree Celsius.
Wherein, in step S2, the measure frequency of dynamic thermo-mechanical analsis instrument is between 0.1-15.0Hz.
It is micro- that the measuring method of the total oxygen glass hydroxyl activation energy that the present invention is provided can effectively obtain total oxygen glass hydroxyl
Structural information is seen, and it is simple and efficient, good stability, with a high credibility.
Description of the drawings
Fig. 1：The sine wave stress diagram of sample is applied under a certain environment；
Fig. 2：The identical waveform strain figure produced after sample is excited under a certain environment；
Fig. 3：The phase angle schematic diagram of viscoelastic body；
Fig. 4 a：The temperature relaxation spectrogram of all-oxygen combustion float glass；
Fig. 4 b：The temperature relaxation spectrogram of air-breathing float glass；
Fig. 5：The Arrhenius equation fitted figures of all-oxygen combustion float glass and air-breathing float glass.
Specific embodiment
Further understand to have to technical scheme and beneficial effect, coordinate accompanying drawing to describe in detail below
Technical scheme and its beneficial effect of generation.
Dynamic thermomechanical Mechanical Method be measurement sample under periodic vibration, the mechanical property that changes with temperature or frequency and viscous
The technology of elastic energy, the research of the relation between the relation being substantially carried out between deformation and power and strain and stress.
Fig. 1 is the sine wave stress diagram that sample is applied under a certain environment；Fig. 2 is under same environment corresponding with Fig. 1
The identical waveform strain figure that sample is produced after being excited；As Figure 1-Figure 2, it is assumed that apply a sinusoidal wave stress to sample
(or strain), then sample can produce the strain (or stress) of same waveform after being excited, and different samples have it is different stagnant
Time afterwards.
Stress/strain=modulus, modulus can be divided into storage modulus and loss modulus again.The mechanical performance and microcosmic of material
Structure is responded to its stress (or strain)/lag time or storage modulus or loss modulus is corresponding has close relationship.Example
Such as, absolute solid elastomers, for example, meet the spring of Hooke's law, deformation can all be saved as energy, lossless, phase
Parallactic angle is 0 degree, and loss modulus is 0.Absolute liquid, such as Newtonian fluid, are converted to flowing, it is impossible to energy storage, phase place deformation
Angle is 90 degree, and elastic modelling quantity is 0.
And majority of material is all viscoelastic body, as shown in figure 3, for the phase angle schematic diagram of viscoelastic body, its phase place
Angle is between 0 degree to 90 degree.
The present invention by measured using dynamic thermomechanical Mechanical Method total oxygen glass temperature relaxation spectrum (i.e. modulus with temperature and
The response of frequency change) obtaining the activation energy of total oxygen glass, so as to obtain inside glass microstructure information.
The invention provides a kind of measuring method of total oxygen glass hydroxyl activation energy, comprises the steps：
S1：Sample is made into the glass bar of predefined size；
S2：Temperature relaxation spectrometry is carried out to glass bar using dynamic thermo-mechanical analsis instrument, temperature relaxation spectrogram is obtained；
S3：The corresponding activation energy of glass bar is obtained according to temperature relaxation spectrogram.
Preferably, step S3 includes：
S31：The corresponding ln τ～T of glass bar is obtained according to temperature relaxation spectrogram-1Curve；
S32：According to Arrhenius crow equation, to ln τ～T-1Curve matching, obtains the corresponding activation energy of glass bar.
Preferably, in step S31, by the peak temperature in quasi- α relaxation regions in temperature relaxation spectrogram
Obtain the corresponding ln τ～T of glass bar-1Curve.
Therefore, the present invention mainly utilizes dynamic thermomechanical mechanics, the activation energy of total oxygen glass is measured, so as to obtain
Internal mechanical performance change and microstructure information that the hydroxyl of total oxygen glass causes.Its specific theoretical foundation is：Glass
Structural relaxation is relevant with surface silicon-oxy tetrahedron or Si-OH keys, the concentration of Si-O-Si keys.The increase of hydroxyl concentration can make glass
The Si-O-Si bond fissions of material internal system, generate more Si-OH keys, because the bond energy of Si-O-Si keys is than Si-OH key
Bond energy be eager to excel, therefore structural relaxation change to be overcome activation energy reduction.Therefore, by the activation of measure total oxygen glass
Can, you can learn the hydroxyl concentration in glass, and then further learn the microstructure information of glass.
(i.e. modulus is with temperature and frequency by the temperature relaxation spectrum of dynamic thermo-mechanical analsis instrument measurement total oxygen glass for the present invention
The response of change) obtaining the activation energy of glass, the method for testing is simple and efficient, good stability, with a high credibility.So that glass row
The researcher of industry and manufacturing enterprise can accurately and efficiently obtain the microstructure information of glass material.
Preferably, in step S1, the length of glass bar between 20-40cm, diameter between 2-4cm glass bar.Tool
When body is implemented, the length of glass bar can be set to any value between 20cm or 40cm or 20-40cm, diameter can be set to 2cm or
Any value between 4cm or 2-4cm.
Preferably, in step S2, the amplitude of dynamic thermo-mechanical analsis instrument is between 5-15 μm.When being embodied as, dynamic
The amplitude of thermodynamic analyzer can be set to any value between 5 μm or 15 μm or 5-15 μm.
Preferably, in step S2, the heating rate of dynamic thermo-mechanical analsis instrument is between 0.5-1.5 DEG C/min.Specifically
During enforcement, the heating rate of dynamic thermo-mechanical analsis instrument can be set to 0.5 DEG C/min or 1.5 DEG C/min or 0.5-1.5 DEG C/min
Between any value.
Preferably, in step S2, the operating temperature of dynamic thermo-mechanical analsis instrument is between 50-590 degree Celsius.It is concrete real
Shi Shi, the operating temperature of dynamic thermo-mechanical analsis instrument can be set between 50 degrees Celsius or 590 degrees Celsius or 50-590 degree Celsius
Any value.
Preferably, in step S2, the measure frequency of dynamic thermo-mechanical analsis instrument is between 0.1-15.0Hz.It is embodied as
When, the measure frequency of dynamic thermo-mechanical analsis instrument can be set to any value between 0.1Hz or 15.0Hz or 0.1-15.0Hz.
Present invention can be suitably applied to the measure of the activation energy of various special glasss, it is thus possible to obtain the interior of various special glasss
Portion's mechanical performance and microstructure information, such as air-breathing float glass, all-oxygen combustion float glass and extraordinary soda-lime-silica glass
Deng being particularly suited for the all-oxygen combustion float glass harsh to condition determination requirement.
Below only by taking air-breathing float glass and all-oxygen combustion float glass as an example, the total oxygen glass of present invention offer is illustrated
The specific implementation method of the measuring method of glass hydroxyl activation energy：
S1：Sample is founded and grows into 30cm, the glass bar of a diameter of 3cm or so, in the present embodiment, selected sample
It is divided to two classes, respectively all-oxygen combustion float glass and air-breathing float glass.
S2：The temperature relaxation spectrum of glass sample is measured using dynamic thermo-mechanical analsis instrument DMA (U.S. TA, Q800)：
First, DMA is opened into preheating half an hour, position correction is carried out respectively and (three-point bending) fixture is calibrated；
Secondly, experimental arrangement parameter is set：Elect Mode as DMA Multi-Frequency-Strain, Test is elected as
Temp Ramp/Frequency Sweep, Clamp elect 3-PointBending as, and the size of input sample, input amplitude is 10
μm, heating rate is 1 DEG C/min, makes temperature be warming up to 590 degrees Celsius from 50 degrees Celsius, operating frequency is followed successively by 0.1,0.2,
0.5th, 1.0,2.0,5.0 and 10.0Hz；
Finally, Measure is clicked on, after the numerical stability of the modulus shown on computer screen, clicks on start button and start
Carry out temperature relaxation spectrometry.
The all-oxygen combustion float glass and the temperature of air-breathing float glass that Fig. 4 a and Fig. 4 b are respectively finally measured relaxes
Henan spectrogram；As shown in Fig. 4 a and Fig. 4 b, measured glass sample there occurs that certain structure is relaxed in the temperature range of measurement
Henan.
Wherein, in Fig. 4 a and Fig. 4 b, seven curves of lower section represent respectively from the bottom to top all-oxygen combustion float glass and sky
G of the combustion-supporting float glass of gas under 10.0Hz, 5.0Hz, 2.0Hz, 1.0Hz, 0.5Hz, 0.2Hz, 0.1Hz "/Gmax curves, on
Seven curves of side, from top to bottom represent respectively all-oxygen combustion float glass and air-breathing float glass 10.0Hz,
G ' under 5.0Hz, 2.0Hz, 1.0Hz, 0.5Hz, 0.2Hz, 0.1Hz/Gmax curves.
S31：By the peak temperature (being shown in Table 1) in quasi- α relaxation regions in the temperature relaxation spectrum for obtaining, phase is obtained
Ln τ～the T for answering-1Curve, as shown in figure 5, the all-oxygen combustion float glass and air-breathing float glass for the present invention
Arrhenius equation fitted figures；
As shown in Figure 5, hydroxy radical content is different, ln τ～T-1The slope of curve changes, so as to predictive of hydroxy radical content meeting shadow
Ring the activation energy of glass structure relaxation.
The empirical value of the all-oxygen combustion float glass of table 1. and air-breathing float glass
S32：According to Arrhenius crow (Arrhenius) equation, to ln τ～T-1Curve matching, obtains glass bar corresponding
Activation energy；
Specifically, Arrhenius crow (Arrhenius) equation is：
Wherein, τ is the relaxation time, τ0For pre-exponential factor, Δ H is activation energy, and k is Boltzmann constant；
Fig. 2 is fitted using Origin, corresponding activation energy Δ H is obtained.
S4：The hydroxyl concentration of measurement glass bar, obtains the relation between the hydroxyl concentration of glass bar and activation energy, so as to test
The reliability of the measuring method of the present invention is demonstrate,proved.
2 are specifically shown in Table, the hydroxyl concentration and its activation energy Δ H of measured glass sample is which show, can by table 2
Know：Hydroxyl concentration is bigger in glass sample, and activation energy is less, and this result is coincide with the theory relation of hydroxyl concentration and activation energy
(concrete theory analysis as detailed above statement), therefore, the measuring method result of the glass activation energy that the present invention is provided be it is reliable,
Realize the accurate measurement to all-oxygen combustion float glass.
The glass sample hydroxyl concentration of table 2. and Arrhenius equation model parameters
Note:Sample hydroxyl concentration is obtained by ft-ir measurement
Although the present invention is illustrated using above-mentioned preferred embodiment, so it is not limited to the protection model of the present invention
Enclose, any those skilled in the art carry out various changes within without departing from the spirit and scope of the present invention with respect to above-described embodiment
It is dynamic still to belong to the scope that the present invention is protected with modification, therefore protection scope of the present invention is by being defined that claims are defined.
Claims (8)
1. a kind of measuring method of total oxygen glass hydroxyl activation energy, it is characterised in that comprise the steps：
S1：Sample is made into the glass bar of predefined size；
S2：Temperature relaxation spectrometry is carried out to glass bar using dynamic thermo-mechanical analsis instrument, temperature relaxation spectrogram is obtained；
S3：The corresponding activation energy of glass bar is obtained according to temperature relaxation spectrogram.
2. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that the step S3 bag
Include：
S31：The corresponding ln τ～T-1 curves of glass bar are obtained according to temperature relaxation spectrogram；
S32：According to Arrhenius crow equation, to ln τ～T-1 curve matchings, the corresponding activation energy of glass bar is obtained.
3. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 2, it is characterised in that：In step S31,
The corresponding ln τ～T-1 curves of glass bar are obtained by the peak temperature in quasi- α relaxation regions in temperature relaxation spectrogram.
4. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that：In step S1,
The length of glass bar is between 20-40cm, diameter between 2-4cm.
5. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that：In step S2,
The amplitude of dynamic thermo-mechanical analsis instrument is between 5-15 μm.
6. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that：In step S2,
The heating rate of dynamic thermo-mechanical analsis instrument is between 0.5-1.5 DEG C/min.
7. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that：In step S2,
The operating temperature of dynamic thermo-mechanical analsis instrument is between 50-590 degree Celsius.
8. the measuring method of total oxygen glass hydroxyl activation energy as claimed in claim 1, it is characterised in that：In step S2,
The measure frequency of dynamic thermo-mechanical analsis instrument is between 0.1-15.0Hz.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107478798A (en) * | 2017-06-30 | 2017-12-15 | 浙江大学 | A kind of method for measuring block metallic glass structures relaxation activation energy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1780723A (en) * | 2003-03-03 | 2006-05-31 | 莫尔德弗洛爱尔兰有限公司 | Apparatus and methods for predicting properties of processed material |
| CN103926213A (en) * | 2014-04-17 | 2014-07-16 | 中国计量学院 | Terahertz spectrum detection device and method for heat stability of solid protein |
| CN105866167A (en) * | 2016-03-24 | 2016-08-17 | 中国华能集团公司 | Method for characterizing and analyzing grain boundary characteristics of nickel-based/ferronickel-based high-temperature alloy on basis of internal friction |
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2017
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| CN1780723A (en) * | 2003-03-03 | 2006-05-31 | 莫尔德弗洛爱尔兰有限公司 | Apparatus and methods for predicting properties of processed material |
| CN103926213A (en) * | 2014-04-17 | 2014-07-16 | 中国计量学院 | Terahertz spectrum detection device and method for heat stability of solid protein |
| CN105866167A (en) * | 2016-03-24 | 2016-08-17 | 中国华能集团公司 | Method for characterizing and analyzing grain boundary characteristics of nickel-based/ferronickel-based high-temperature alloy on basis of internal friction |
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| Z.WANG, ET AL: "Evolution of hidden localized flow during glass-to-liquid transition in metallic glass", 《NATURE COMMUNICATIONS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107478798A (en) * | 2017-06-30 | 2017-12-15 | 浙江大学 | A kind of method for measuring block metallic glass structures relaxation activation energy |
| CN107478798B (en) * | 2017-06-30 | 2020-06-16 | 浙江大学 | Method for measuring relaxation activation energy of bulk metal glass structure |
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| CN106645006B (en) | 2019-11-01 |
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