CN106596246A - Method for measuring thermodynamic property of polymer material - Google Patents
Method for measuring thermodynamic property of polymer material Download PDFInfo
- Publication number
- CN106596246A CN106596246A CN201610992150.4A CN201610992150A CN106596246A CN 106596246 A CN106596246 A CN 106596246A CN 201610992150 A CN201610992150 A CN 201610992150A CN 106596246 A CN106596246 A CN 106596246A
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- Prior art keywords
- modulus
- fighting
- macromolecular material
- sample
- metal tube
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Classifications
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- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
-
- 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
- G01N2203/0226—High temperature; Heating means
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a method for measuring the thermodynamic property of a polymer material. A low internal friction metal tube is used as a carrier, the powdered polymer material is directly loaded into an empty cavity of the metal tube or the granular polymer material is sucked into the empty cavity of the metal tube after being molten to prepare a sample, then the internal friction and modulus of the sample is measured in a twisting, stretching or bending mode, and Tg, Tm or other thermodynamic parameters of the material are analyzed through an internal friction and temperature curve and a modulus and temperature curve. Compared with the prior art, the method can measure the Tg, Tm or other thermodynamic parameters of the polymer material in a wider temperature range, and avoids the problem that when the temperature is extremely high, instrument measurement is beyond a normal measurement range due to the change of material properties and when the temperature is extremely low, because an instrument needs to output more acting force, the instrument is damaged.
Description
Technical field
It is the present invention relates to the technical field of material property detection more particularly to a kind of for measuring macromolecular material thermodynamics
The method of performance.
Background technology
Bar of the conventional macromolecular material thermodynamic parameter measuring method typically to pressurizeing, cooling down, be cut into
Shape sample applies cyclic stress, measures the real-time change process of its ess-strain, and according to stress, the amplitude of strain curve and
Phase relation calculates modulus and Internal friction, and the thermodynamics of material is obtained with temperature and frequency variation curve by modulus and in-fighting
Parameter.But because macromolecular material is being heated to TgRuckbildung occurs after (material glass transition temperature), it is impossible to
Restoring force is provided, it is normal beyond instrument even if this causes the active force for applying very little that big plastic deformation also can be produced to sample
Measurement range, so the measuring method of routine is typically at most only able to detect macromolecular material Tg.But in actual applications, accurately
The T of measurement macromolecular materialgAnd Tm(Material Melt temperature) and some other thermodynamic data pair determine Process Technology of Polymer shaping work
Skill parameter is extremely important.By taking extrusion molding as an example, when extrusion temperature is higher, material decomposes to be accelerated, and causes material property to occur
Change；When extrusion temperature is low, material flowability is too poor, needs instrument to export bigger extrusion force, and this can damage screw rod and chamber
Body, reduces its service life.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided one kind is used to measure macromolecular material thermodynamics
The method of performance, to solve to exceed caused by changing because of material property when temperature is too high the normal measurement range of measuring instrument, with
And temperature needs measuring instrument to export the technical problem of the damage caused by bigger active force to instrument when too low.
The technical problem to be solved employs the following technical solutions to realize：
A kind of method for measuring macromolecular material thermodynamic property, it is characterised in that methods described is with low in-fighting gold
Category pipe is carrier, macromolecular material to be measured is fitted in the cavity of metal tube and prepares sample, then by reversing, stretching or bending die
Formula determines the in-fighting of sample and modulus, and finally by analysis in-fighting-temperature curve and modulus-temperature curve material is obtained
Tg、TmAnd other thermodynamic parameters, wherein, described in-fighting metal tube is Internal friction 10-3Magnitude and following metal tube.
Further, the macromolecular material to be measured is powder or graininess, when for powder when, by macromolecule to be measured
Material is directly loadable in the cavity of metal tube, and two ends are shut；When for graininess when, will macromolecular material to be measured melt after fill
In entering the cavity of metal tube, and two ends are shut.
Further, the external diametrical extent of the low in-fighting metal tube be 1-5mm, wall thickness range be 0.1-0.5mm, length model
Enclose for 3-10cm.
Further, the assay method of the in-fighting of the sample and modulus includes two ways：
1. sample reversed using forced vibration measurement pattern, stretched and flexural deformation, passed by stress and strain
The reinforcing of sensor Real-time Collection material and oscillating curve, are obtained by calculating the quotient of amplitudes and both angle of lags of ess-strain
Modulus and Internal friction, the measuring principle of which is：Under forced vibration measurement pattern, a cycle that signal generator occurs
Property sinusoidal force signal force sample to do periodic sinusoidal vibration, it is σ=σ that now strain gauge measurement obtains stress curve0Sin (ω t- α), strain transducer measurement obtains strain curve ε=ε0Sin (ω t- α-φ), wherein φ represent strain signal with
The phase angle difference of excitation signal, thus calculates elastic modulus E or G=σ/ε, Internal friction Q-1=tan φ；
2. sample is reversed or flexural deformation using free damping pattern, it is bent by the strain decay of capturing material
Line, the logarithmic decrement of calculated amplitude and frequency obtain modulus and Internal friction, and the measuring principle of which is：Survey in free damping
Under amount pattern, signal generator sends a defection signal makes sample reverse to setting strain amplitude value ε0, then make sample
Free damping campaign, and measure its strain attenuation curve ε=ε0e-δωtSin (ω t), according to deflecting force σ and strain value ε, calculates
Go out elastic modulus G=σ/ε, Internal friction is calculated according to the amplitude of multiple vibration periodsIts
Middle φ represents the phase angle difference of strain signal and excitation signal, AnAnd An+mIt is respectively the amplitude of the n-th and n-th+m vibration.
Further, the Tg、TmAnd the preparation method of other thermodynamic parameters is：By changing measurement temperature and frequency
In-fighting and the modulus for obtaining macromolecular material is bent with temperature and the change curve of frequency, i.e. in-fighting-temperature curve and modulus versus temperature
Line, according to the most fast position of the position of Internal Friction Peak and modulus change in in-fighting-temperature curve and modulus-temperature curve material is obtained
Tg, Tm value and other thermodynamic parameter values.
The present invention has compared to existing technology advantages below：The invention provides a kind of be used to measure macromolecular material heating power
The method for learning performance, the method can determine macromolecular material T in more wide temperature rangeg、TmAnd other thermodynamic parameters, keep away
Exempt to need instrument when too low beyond the normal measurement range of instrument, and temperature caused by changing because of material property when temperature is too high
Damage caused by the bigger active force of output to instrument.
Description of the drawings
Fig. 1 is the sample preparation schematic diagram of graininess macromolecular material；
Fig. 2 is the sample preparation schematic diagram of powder macromolecular material；
Fig. 3 is that sample is carried out into torsional deflection processing detection process schematic, and in figure, 1 is stationary fixture, and 2 is sample, 3
For vertical pendulum bar, 4 is mirror, and 5 is yaw bar pendulum, and 6 is yaw bar, and 7 is strain gauge, and 8 is excitation variable winding, and 9 is permanent magnet,
10 is light source, and 11 is photocell；
Fig. 4 is that sample is draw textured into processing detection process schematic, and in figure, 1 is stationary fixture, and 2 is sample, 3
For vertical pendulum bar, 4 is displacement transducer, and 5 is strain gauge, and 6 is stepper motor；
Fig. 5 is that sample is curved into deformation process detection process schematic diagram, and in figure, 1 is stationary fixture, and 2 is sample, 3
For vertical pendulum bar, 4 is displacement transducer, and 5 is strain gauge, and 6 is stepper motor；
Fig. 6 is stress curve and strain curve under forced vibration measurement pattern；
Fig. 7 is the vibration attenuation curve under free damping pattern；
Fig. 8 is the in-fighting-temperature curve and modulus-temperature curve of empty metal tube；
Fig. 9 is the in-fighting-temperature curve and modulus-temperature curve of polystyrene.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following enforcements
Example.
Embodiment 1
A kind of method for measuring macromolecular material thermodynamic property is present embodiments provided, is comprised the following steps：
(1) by Internal friction 10-3Magnitude and following, external diametrical extent is that 1-5mm, wall thickness range are low for 0.1-0.5mm's
In-fighting cuts in metallic pipe into length for 3-10cm short tube, as the container of macromolecular material to be measured.
(2) using graininess or powder macromolecular material as macromolecule raw material to be measured；When using granular material,
Needs are heated after fusing and are directly sucked in the cavity body of metal tube, and then both-end is shut, and used as sample to be tested, it was prepared
Journey is as shown in Figure 1；When using dusty material, first metal tube one end is shut, after by powder from the other end load metal tube
Cavity body in, be compacted, shut, used as sample to be tested, its preparation process is as shown in Figure 2.
(3) as in Figure 3-5, sample to be tested both-end is clamped on the stationary fixture being horizontally mounted, or both-end is fixed
Fix at one end on the moveable fixture of the other end, dynamic force is applied to sample to facilitate.By variable-frequency motor or exciting
Device is curved deformation to the sample center that both-end is fixed, or the sample that one end moveable jaw is fixed is reversed, drawn
Deformation is stretched, range of strain is 1-10 μm, and frequency range is 0.1-10Hz.
(4) sample reversed using forced vibration measurement pattern, stretched and flexural deformation, passed by stress and strain
The reinforcing of sensor Real-time Collection material and oscillating curve, are obtained by calculating the quotient of amplitudes and both angle of lags of ess-strain
Modulus and Internal friction, as a result as shown in Figure 6；Or, sample is reversed using free damping pattern or flexural deformation, pass through
The strain attenuation curve of capturing material, the logarithmic decrement of calculated amplitude and frequency obtain in-fighting and modulus value, as a result such as Fig. 7 institutes
Show.
(5) by change measurement temperature and frequency obtain macromolecular material in-fighting and modulus with temperature and frequency change
Curve, i.e. in-fighting-temperature curve and modulus-temperature curve, according to Internal Friction Peak in in-fighting-temperature curve and modulus-temperature curve
Position and the most fast position of modulus change obtain the T of materialg、TmValue and other thermodynamic parameter values.
As shown in figure 8, be using said method determine be not charged with macromolecular material to be measured empty metal tube in-fighting-
Temperature curve and modulus-temperature curve (blank assay), as can be seen from Figure 8, the in-fighting-temperature of the metal tube of low in-fighting is bent
Line and modulus-temperature curve tendency are steady, without special peak value or the position for significantly changing, illustrate using low in-fighting metal tube
As container is determined, the thermodynamic parameter measurement result of macromolecular material is not made significant difference, with certain feasibility.
As shown in figure 9, being the in-fighting-temperature curve and mould of the polystyrene polymeric material determined using said method
Amount-temperature curve, it can be seen in figure 9 that polystyrene has two Internal Friction Peaks in the range of measurement temperature, while according to modulus
Mutation analysis：110 DEG C or so of Internal friction peak should be the change of the Internal friction caused due to the glass transition of polystyrene
Change, the change of 240 DEG C or so Internal frictions should cause because polystyrene melts.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not restricted to the described embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes and improvements
Both fall within scope of the claimed invention.The claimed scope of the invention is by appending claims and its equivalent circle.
It is fixed.
Claims (7)
1. a kind of method for measuring macromolecular material thermodynamic property, it is characterised in that methods described is with low in-fighting metal
Manage as carrier, macromolecular material to be measured be fitted in the cavity of metal tube and prepare sample, then by reversing, stretching or beam mode
In-fighting and the modulus of sample are determined, the T of material is obtained finally by analysis in-fighting-temperature curve and modulus-temperature curveg、Tm
And other thermodynamic parameters.
2. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
State low in-fighting metal tube for Internal friction 10-3Magnitude and following metal tube.
3. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
Macromolecular material to be measured is stated for powder or graininess, when for powder when, macromolecular material to be measured is directly loadable into into metal tube
Cavity in, and two ends are shut；When for graininess when, will macromolecular material to be measured melt after be fitted in the cavity of metal tube,
And shut at two ends.
4. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
The external diametrical extent for stating low in-fighting metal tube is 1-5mm, wall thickness range is 0.1-0.5mm, length range is 3-10cm.
5. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
The assay method of the in-fighting and modulus of stating sample is：Sample is reversed, stretched and is bent using forced vibration measurement pattern
Deformation, the reinforcing and oscillating curve by stress and strain sensor Real-time Collection material, by the amplitude for calculating ess-strain
Ratio and both angle of lags obtain modulus and Internal friction.
6. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
The assay method of the in-fighting and modulus of stating sample is：Sample is reversed using free damping pattern or flexural deformation, passed through
The strain attenuation curve of capturing material, the logarithmic decrement of calculated amplitude and frequency obtain modulus and Internal friction.
7. a kind of method for measuring macromolecular material thermodynamic property according to claim 1, it is characterised in that institute
State Tg、TmAnd the preparation method of other thermodynamic parameters is：The in-fighting of macromolecular material is obtained by changing measurement temperature and frequency
With modulus with temperature and the change curve of frequency, i.e. in-fighting-temperature curve and modulus-temperature curve, according to in-fighting-temperature curve
The position most fast with the position of Internal Friction Peak in modulus-temperature curve and modulus change obtains the T of materialg、TmValue and other thermodynamics
Parameter value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610992150.4A CN106596246A (en) | 2016-11-11 | 2016-11-11 | Method for measuring thermodynamic property of polymer material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610992150.4A CN106596246A (en) | 2016-11-11 | 2016-11-11 | Method for measuring thermodynamic property of polymer material |
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| CN106596246A true CN106596246A (en) | 2017-04-26 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108344766A (en) * | 2018-02-23 | 2018-07-31 | 洛阳师范学院 | One organic molecular species photoelectric material thermodynamic property test method |
| CN112484946A (en) * | 2020-10-28 | 2021-03-12 | 哈尔滨电机厂有限责任公司 | Method for testing inherent frequency of multi-rubber die-pressing main insulation |
| CN114088579A (en) * | 2021-11-17 | 2022-02-25 | 广东莱尔新材料科技股份有限公司 | Viscosity detection equipment and method for hot-melt extrusion material containing filler resin |
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| CN103308546A (en) * | 2013-05-24 | 2013-09-18 | 西安交通大学 | Phase change function measuring method of shape-stabilized phase change material |
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| CN101924182A (en) * | 2009-06-12 | 2010-12-22 | 中国科学院化学研究所 | Method for measuring glass transition temperature of polymer |
| JP2012025830A (en) * | 2010-07-22 | 2012-02-09 | Mitsubishi Chemical Holdings Corp | Composite resin composition having vibration-damping property, and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108344766A (en) * | 2018-02-23 | 2018-07-31 | 洛阳师范学院 | One organic molecular species photoelectric material thermodynamic property test method |
| CN112484946A (en) * | 2020-10-28 | 2021-03-12 | 哈尔滨电机厂有限责任公司 | Method for testing inherent frequency of multi-rubber die-pressing main insulation |
| CN114088579A (en) * | 2021-11-17 | 2022-02-25 | 广东莱尔新材料科技股份有限公司 | Viscosity detection equipment and method for hot-melt extrusion material containing filler resin |
| CN114088579B (en) * | 2021-11-17 | 2024-03-26 | 广东莱尔新材料科技股份有限公司 | Viscosity detection apparatus and method for hot melt extrusion containing filler resin |
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Application publication date: 20170426 |