CN109297997A - A method of measurement polymer crystallinity, mesomorphic degree and unformed degree - Google Patents
A method of measurement polymer crystallinity, mesomorphic degree and unformed degree Download PDFInfo
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- CN109297997A CN109297997A CN201710607146.6A CN201710607146A CN109297997A CN 109297997 A CN109297997 A CN 109297997A CN 201710607146 A CN201710607146 A CN 201710607146A CN 109297997 A CN109297997 A CN 109297997A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- 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
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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- 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
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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Abstract
The invention discloses a kind of methods of measurement polymer crystallinity, mesomorphic degree and unformed degree.It include: the crystallinity of (1) measurement polymer；(2) (crystallization+mesomorphic) degree of polymer is measured；(3) it according to step (1) and step (2) data, calculates: mesomorphic degree=C of polymerKnot+Jie%-CKnot%；Unformed degree=1-C of polymerKnot+Jie%-CKnot%.The present invention, which changes the methods of traditional DSC and WAXD only, can measure the history of crystalline polymer crystallinity.In conjunction with DMTA result not only available crystallinity as a result, the result of mesomorphic degree can also be obtained.Also by the crystallization of vulcanization crosslinking technology controlling and process natural rubber and gutta-percha, the crystal region being destroyed is transformed into mesomorphous region first, then can just be transformed into amorphous region explanation simultaneously.
Description
Technical field
The present invention relates to technical field of polymer materials, further say, are to be related to a kind of measurement polymer crystallinity, be situated between
The method of brilliant degree and unformed degree.
Background technique
The crystallization property of polymer plays key effect for the application performance of polymer, and traditional two-phase crystal model is theoretical
Think polymer be mutually constituted by crystalline phase with unformed, and crystallinity be characterize one of polymer crystallization performance it is extremely important
Thermodynamic parameter.The measurement of traditional crystallinity be all based on crystallization itself architectural characteristic or crystalline transition process occur
Physical change is measured, for example calculates crystallization using the crystal diffraction peak of WAXD measurement crystalline polymer and unformed peak
Degree, DSC calculate crystallinity by measuring the melting enthalpy of polymer.
With the progress of science and technology, it has been found that polymer is not only made of crystalline phase and amorphous phase, further includes
Mesomorphic phase of the structure between crystallization and amorphous state.Obviously, mesomorphic phase itself also closes polymer application performance very much
Key.Due to the mesomorphic phase both not no perfect regularity of crystalline phase, the also not no random coil state of unformed shape, therefore people are simultaneously
Have no idea to measure the presence of mesomorphic phase.
Summary of the invention
To solve the problem in the prior art, the present invention provides a kind of measurement polymer crystallinity, mesomorphic degree and
The method of unformed degree.During its principle is polymer glass transition, DMTA is can be used in the motion state of free segment
Characterization, movement degree are controlled not only by cerium sulphate crystal by mesomorphic.Therefore using the DMTA crystalline polymer measured
What tan δ peak area embodied is remaining free movement segment number after being controlled by crystallization and mesomorphic.Therefore, as long as knowing that this is poly- again
The tan δ peak area under 100% amorphous state of object is closed, the two subtracts each other, so that it may know the total of the polymer crystallinity and mesomorphic degree
With.And the crystallinity of the only polymer of WAXD and DSC measurement.Subtract WAXD's or DSC using the result of DMTA as a result,
As a result, can be obtained by the crystallinity of polymer, mesomorphic degree and unformed degree.
The object of the present invention is to provide a kind of methods of measurement polymer crystallinity, mesomorphic degree and unformed degree.The side
Method includes:
(1) crystallinity of polymer is measured；
(2) (crystallization+mesomorphic) degree of polymer is measured；
The tan δ peak area for measuring glass transition region under the unformed state of polymer 100%, uses ArCharacterization；Then it surveys
The tan δ peak area for determining glass transition region under polymer crystallization state, uses AaCharacterization；According to polymer by crystalline phase and nothing
The tow phase model of sizing phase composition is theoretical, (crystallization+mesomorphic) degree of the polymer are as follows:
In step (2), 1-10 DEG C/min of heating rate, test frequency 1-20Hz.
In step (2), obtaining 100% by way of liquid nitrogen is quickly cooled down quenching or in such a way that crosslinking inhibits crystallization
The polymer of amorphous state.
The crosslinking is carried out by way of sulfur cross-linking, peroxide cure and radiation vulcanization.
(3) it according to step (1) and step (2) data, calculates:
Mesomorphic degree=C of polymerKnot+Jie%-CKnot%
Unformed degree=1-C of polymerKnot+Jie%-CKnot%.
Wherein, preferably
In step (1), one of following two method is can be used in the crystallinity for measuring polymer；
A measure polymer Wide angle X-ray diffraction curve, by swarming technology obtain the polymer characteristic crystalline peak and
Unformed diffraction maximum, uses W respectivelycAnd WaCharacterization；Then the polymer uses the crystallinity of WAXD measurement are as follows:
B measures the heating melting curve of polymer, obtains the melting peak of the polymer, by integrating the available polymerization
The melting enthalpy of object, with Δ HfCharacterization；Melting enthalpy under known 100% crystalline state of polymer, with Δ HF100%Characterization；The polymerization
Object uses the crystallinity of DSC measurement are as follows:
Wherein, 1-10 DEG C/min of heating rate.
Following technical scheme specifically can be used in the present invention:
The method is needed using three kinds of test equipments, is Dynamic Mechanical Thermal respectively
Analysis (DMTA) and Differential Scanning Calorimetry (DSC) and Wide Angle X-ray
Diffraction(WAXD).Crystallinity, mesomorphic degree and the unformed degree of DMTA and DSC cooperation measurement polymer can be passed through.?
Crystallinity, mesomorphic degree and the unformed degree of DMTA and WAXD cooperation measurement polymer can be passed through.
The tan δ peak area that glass transition region under the unformed state of polymer 100% is measured using DMTA, uses ArTable
Sign.Then the tan δ peak area for measuring glass transition region under polymer crystallization state with DMTA again, uses AaCharacterization.Test temperature
Degree is arranged according to the glass transition temperature of polymer, and 1-10 DEG C/min of heating rate, test frequency 1-20Hz.According to polymerization
Object is theoretical by crystalline phase and the tow phase model of unformed phase composition, the crystallinity+mesomorphic degree of the polymer measured with DMTA are as follows:
Using the heating melting curve of DSC measurement polymer, the melting peak of the polymer is obtained, it is available by integrating
The melting enthalpy of the polymer, with Δ HfCharacterization.Melting enthalpy under known 100% crystalline state of polymer, with Δ HF100%Characterization.
Test temperature is arranged according to the crystalline melt temperature of polymer, and 1-10 DEG C/min of heating rate.The polymer is surveyed using DSC
Fixed crystallinity are as follows:
It is the theory of the triphase flow as composed by crystalline phase, mesomorphic phase and unformed phase according to polymer, is surveyed by DMTA
Fixed crystallinity not only includes crystalline portion, also includes mesogenic moiety.And the crystallinity that DSC is measured only includes crystallization unit
Point.Therefore, crystallinity, mesomorphic degree and the unformed degree of polymer can be measured with the method for DMTA combination DSC, specific as follows:
Crystallinity=CDSC%
Mesomorphic degree=CDMTA%-CDSC%
Unformed degree=1-CDMTA%-CDSC%
Using the Wide angle X-ray diffraction curve of WAXD measurement polymer, pass through the available polymer of swarming technology
Characteristic crystalline peak and unformed diffraction maximum, use W respectivelycAnd WaCharacterization.Test condition is specifically set according to the crystallization property of polymer
It sets.The then crystallinity of the polymer measured using WAXD are as follows:
The similarly mesomorphic degree and unformed degree of polymer are as follows:
Mesomorphic degree=CDMTA%-CWAXD%
Unformed degree=1-CDMTA%-CWAXD%
The polymer of 100% amorphous state can be obtained in such a way that liquid nitrogen is quickly cooled down quenching.Friendship can also be passed through
The mode of connection, such as sulfur cross-linking, peroxide cure and radiation vulcanization inhibit the mode of crystallization to obtain 100% amorphous
The polymer of state, then further according to the linear relationship of crosslink density and tan δ peak area, it is counter push away crystallized under different crosslink densities it is poly-
Close the tan δ peak area under 100% amorphous state of object.
The present invention " a method of measurement polymer crystallinity, mesomorphic degree and unformed degree ", change traditional DSC and
The methods of WAXD can only measure the history of crystalline polymer crystallinity.In conjunction with the result not only available crystallinity of DMTA
As a result, the result of mesomorphic degree can also be obtained.Also explanation passes through vulcanization crosslinking technology controlling and process natural rubber and gutta-percha simultaneously
Crystallization, the crystal region being destroyed is transformed into mesomorphous region first, then can just be transformed into amorphous region.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1
Measure the crystallinity of high density polyethylene (HDPE), mesomorphic degree and unformed degree.The sample of polyethylene is having a size of 25mm × 6mm
×2mm.Using tan δ~temperature curve of stretch mode measurement crystalline polyethylene.Test condition: it 1 DEG C/min of heating rate, surveys
Frequency 1Hz is tried, -150---140 DEG C of test temperature, tan δ~temperature curve of crystalline polyethylene is obtained at this time, then passes through product
Divide the tan δ peak area for calculating polyethylene under glass transition temperature.140 DEG C of holding is temperature-resistant, and the temperature is in melting temperature
More than (130 DEG C), and it is no more than 15 DEG C, polyethylene crystallization has melted at this time, but is in soft state, still keeps batten
Shape.Then it is passed through liquid nitrogen rapidly to quench the polyethylene specimen of softening, so that polyethylene specimen be made to be in 100% unformed shape
State.Using tan δ~temperature curve of stretch mode measurement amorphous state polyethylene.Test condition: 1 DEG C/min of heating rate,
Test frequency 1Hz, obtains tan δ~temperature curve of amorphous state polyethylene, then at this time by -150---140 DEG C of test temperature
Pass through the tan δ peak area of amorphous state polyethylene under integral calculation glass transition temperature.Then it is mentioned according to claim 2
The crystallinity of DMTA test is calculated for formula.
Utilize DSC test crystalline polyethylene heating melting curve.1 DEG C/min of heating rate, temperature range is from room temperature --
200℃.Then the crystallinity of DSC test is calculated using formula shown in claim 3.
Finally according to formula shown in claim, crystallinity (C%), the mesomorphic degree (M%) of high density polyethylene (HDPE) are settled accounts
With unformed degree (A%), it is shown in Table 1.
Crystallinity, mesomorphic degree and the unformed degree of 1 high density polyethylene (HDPE) of table
Embodiment 2
Measure the crystallinity of low temperature crystallization natural rubber, mesomorphic degree and unformed degree.The sample of natural rubber having a size of
25mm×6mm×2mm.It is crystallized 0,1,2,4,12 hour first with DMTA low temperature (- 25 DEG C) inducing natural rubber.Then using drawing
Stretch tan δ~temperature curve that mode measures natural rubber under different crystallization times.Test condition: it 3 DEG C/min of heating rate, surveys
Try frequency 3Hz.Then it by the tan δ peak area of natural rubber under integral calculation glass transition temperature, is then wanted according to right
2 provided publicities are asked to calculate the crystallinity of DMTA test.
It is crystallized 0,1,2,4,12 hour using DSC low temperature (- 25 DEG C) inducing natural rubber, then tests their liter respectively
Warm melting curve.1 DEG C/min of heating rate, temperature range is from -80--120 DEG C.Then formula meter shown in claim 3 is utilized
Calculate the crystallinity of DSC test.
Finally according to formula shown in claim, crystallinity (C%), mesomorphic degree (M%) and the nothing of natural rubber are settled accounts
Sizing degree (A%), is shown in Table 2.
Crystallinity, mesomorphic degree and the unformed degree of 2 low temperature induction natural rubber of table
Embodiment 3
Measure the crystallinity of natural rubber under low temperature crystallization difference crosslink density, mesomorphic degree and unformed degree.Natural rubber
Sample having a size of 25mm × 6mm × 2mm.The natural rubber under different crosslink densities is first formulated using traditional rubber processing
Sample, crosslinking agent use sulphur, 0,0.25,0.5,0.75,1,1.5,2 part of number.It is induced first with (- 25 DEG C) of DMTA low temperature
Natural rubber crystallizes 4 hours.Then tan δ~temperature curve of natural rubber under different crosslink densities is measured using stretch mode.
Test condition: 5 DEG C/min of heating rate, test frequency 10Hz.Then pass through natural rubber under integral calculation glass transition temperature
Then the tan δ peak area of glue calculates the crystallinity of DMTA test according to the provided publicity of claim 2.Under different crosslink densities
The tan δ peak area for crystallizing 100% amorphous state of natural rubber, can be extrapolated by the relationship of tan δ peak area and crosslink density
?.
It is crystallized 4 hours using natural rubber under the above-mentioned different crosslink densities of (- 25 DEG C) of DSC low temperature inductions, is then surveyed respectively
Try their heating melting curve.1 DEG C/min of heating rate, temperature range is from -80--120 DEG C.Then claim 3 is utilized
Shown formula calculates the crystallinity of DSC test.
Finally according to formula shown in claim, crystallinity (C%), mesomorphic degree (M%) and the nothing of natural rubber are settled accounts
Sizing degree (A%), is shown in Table 3.
Crystallinity, mesomorphic degree and the unformed degree of 3 low temperature induction natural rubber of table
Embodiment 4
Measure the crystallinity of gutta-percha under room temperature difference crosslink density, mesomorphic degree and unformed degree.The sample ruler of gutta-percha
Very little is 25mm × 6mm × 2mm.The natural rubber sample under different crosslink densities first is formulated using traditional rubber processing, is handed over
Join agent and uses DCP, number 0,1,2,4,6,8,10,12,14, part.It is close using the different crosslinkings of stretch mode measurement using DMTA
Spend tan δ~temperature curve of lower gutta-percha.Test condition, 10 DEG C/min of heating rate, test frequency 20Hz.Then pass through product
Grading mode calculates the tan δ peak area of gutta-percha under glass transition temperature, then according to the provided publicity meter of claim 2
Calculate the crystallinity of DMTA test.The tan δ peak area that 100% amorphous state of gutta-percha is crystallized under different crosslink densities, can pass through
The relationship of tan δ peak area and crosslink density is extrapolated and is obtained.
The diffraction pattern for testing them using WAXD is general.5 ° < 2 θ < 30 ° of scanning angle range, 5 °/minute of scanning speed.Then
The crystallinity of WAXD test is calculated using formula shown in claim 5.
Finally according to formula shown in claim 5, crystallinity (C%), mesomorphic degree (M%) and the nothing of natural rubber are settled accounts
Sizing degree (A%), is shown in Table 4.
Crystallinity, mesomorphic degree and the unformed degree of 4 low temperature induction natural rubber of table
Claims (7)
1. a kind of method of measurement polymer crystallinity, mesomorphic degree and unformed degree, it is characterised in that the described method includes:
(1) crystallinity of polymer is measured；
(2) (crystallization+mesomorphic) degree of polymer is measured；
The tan δ peak area for measuring glass transition region under the unformed state of polymer 100%, uses ArCharacterization；Then measurement is poly-
The tan δ peak area for closing glass transition region under object crystalline state, uses AaCharacterization；According to polymer by crystalline phase and unformed
The triphase flow of phase composition is theoretical, (crystallization+mesomorphic) degree of the polymer are as follows:
(3) it according to step (1) and step (2) data, calculates:
Mesomorphic degree=C of polymerKnot+Jie%-CKnot%
Unformed degree=1-C of polymerKnot+Jie%-CKnot%.
2. the method for measurement polymer crystallinity, mesomorphic degree and unformed degree as described in claim 1, it is characterised in that:
In step (1), the crystallinity of polymer is measured；
The Wide angle X-ray diffraction curve for measuring polymer obtains the characteristic crystalline peak of the polymer by swarming technology and without fixed
Type diffraction maximum, uses W respectivelycAnd WaCharacterization；The then crystallinity of the polymer are as follows:
。
3. the method for measurement polymer crystallinity, mesomorphic degree and unformed degree as described in claim 1, it is characterised in that:
In step (1), the crystallinity of polymer is measured；
The heating melting curve for measuring polymer, obtains the melting peak of the polymer, by integrating the available polymer
Melting enthalpy, with Δ HfCharacterization；Melting enthalpy under known 100% crystalline state of polymer, with Δ HF100%Characterization；The polymer
Crystallinity are as follows:
4. the method for measurement polymer crystallinity, mesomorphic degree and unformed degree as described in claim 1, it is characterised in that:
In step (2), 1-10 DEG C/min of heating rate, test frequency 1-20Hz.
5. the method for measurement polymer crystallinity, mesomorphic degree and unformed degree as claimed in claim 3, it is characterised in that:
1-10 DEG C/min of heating rate.
6. the method for measurement polymer crystallinity, mesomorphic degree and unformed degree as described in claim 1, it is characterised in that:
In step (2), obtaining 100% without fixed by way of liquid nitrogen is quickly cooled down quenching or in such a way that crosslinking inhibits crystallization
The polymer of form.
7. the method for measurement polymer crystallinity as claimed in claim 6, mesomorphic degree and unformed degree, it is characterised in that:
The crosslinking is carried out by way of sulfur cross-linking, peroxide cure and radiation vulcanization.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111398333A (en) * | 2020-04-13 | 2020-07-10 | 中国科学院金属研究所 | Differential thermal analysis method for measuring primary melting temperature of single crystal superalloy |
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