CN106770427A - A kind of heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material - Google Patents
A kind of heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000000470 constituent Substances 0.000 title claims abstract description 24
- 238000004458 analytical method Methods 0.000 title claims abstract description 17
- 230000002441 reversible effect Effects 0.000 claims abstract description 29
- 238000001938 differential scanning calorimetry curve Methods 0.000 claims abstract description 19
- 230000009477 glass transition Effects 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 14
- 229920002521 macromolecule Polymers 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001595 flow curve Methods 0.000 claims abstract description 4
- 230000035772 mutation Effects 0.000 claims abstract description 4
- 229910052594 sapphire Inorganic materials 0.000 claims description 12
- 239000010980 sapphire Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 9
- 238000010309 melting process Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 9
- 238000011160 research Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000013102 re-test Methods 0.000 description 2
- 238000002076 thermal analysis method Methods 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- G01N25/04—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
- G01N25/005—Investigating or analyzing materials by the use of thermal means by investigating specific heat
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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 present invention provides a kind of heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material, conventional formula is respectively adopted and step-by-step movement heats up and sample is heated, StepScan DSC curves are resolved into a reversible specific heat capacity curve and a Non reversing heat flow curve, glass transition position is determined by the discontinuous mutation of specific heat capacity on reversible specific heat capacity curve, the melting enthalpy on specific heat capacity increment and DSC curve during further according to glass transition, determines the content of half hitch polycrystalline macromolecule different phase component.The present invention can be separated glass transition by SSDSC technologies from dynamic process, obtain the parameters such as reversible specific heat capacity and glass transition temperature and melting enthalpy in sample temperature-rise period, the glass transition temperature of hypocrystalline macromolecular material can not only be obtained, the reversible specific heat capacity corresponding to different temperatures can also accurately be obtained, the content of crystalline state in half hitch polycrystalline macromolecule sample, flowing unformed shape and hard unformed shape different phase can be calculated according to specific heat capacity and melting enthalpy simultaneously.
Description
Technical field
The present invention relates to a kind of hypocrystalline macromolecular material, and in particular to one kind determines each phase of hypocrystalline macromolecular material
The method of constituent content.
Background technology
According to the regularity that molecule space is arranged, macromolecular material can be divided into crystalline polymers and unformed macromolecule.One
As for, most of crystalline polymers materials due to when strand is piled into crystal, the end of chain and the part meeting such as point of tangling
Be ostracised outside crystalline region, thus whole strand can only partially crystallizable, the crystal for being formed is not perfect enough, that is, form hemicrystalline
Macromolecule.Glass transition is a kind of common phenomenon of half hitch polycrystalline macromolecule, be amorphous molecule in temperature field, mechanical state exists
Transformation between glassy state and elastomeric state, it can reflect macromolecular material sub-chain motion state and other structures.
Heat analysis are the physical property of measurement of species and a class technology of temperature relation under programed temperature.It is
A kind of research very effective analysis means of high molecular phase change.Differential scanning calorimetry (Differential Scanning
Calorimetry, DSC) it is a kind of thermoanalysis technology, it is the hot-fluid of measurement sample and reference substance under programed temperature
Difference or difference power and temperature or the relation of time.And step-scan means of differential scanning calorimetry (StepScan Differential
Scanning Calorimetry, SSDSC) technology be in the linear temperature program speed of traditional DSC superposition one stepping shape
The Sasser of formula, realizes the modulation to temperature, can be finally reversible (mainly glass transition, melting by SSDSC Curve Resolutions
Deng) with irreversible two parts such as (mainly solidification, enthalpy be lax and crystallization), it is hereby achieved that more accurate specific heat capacity and glass
Glass transition temperature.In the research test of hypocrystalline macromolecular material, SSDSC technologies are used by people to the reversible of research material
With irreversible change, the research of the phase constituent content (crystalline state and unformed shape etc.) of material is not carried out further.Therefore,
We will enter with the reversible specific heat of SSDSC this thermoanalysis technology measure hypocrystalline macromolecular materials and with this in the present invention
The calculating of row phase constituent content.
The content of the invention
Goal of the invention：The purpose of the present invention is to solve the shortcomings of the prior art, there is provided one kind determines half hitch polycrystalline macromolecule
The heat analysis method of each phase constituent content of material, conveniently obtains total hot-fluid, the reversible ratio of hypocrystalline macromolecular material
Thermal capacitance and glass transition temperature, and three kinds of phase components (crystalline state, flowing unformed shape and hard unformed shape) are calculated with this
Content.
Technical scheme：The invention provides a kind of heat analysis side for determining each phase constituent content of hypocrystalline macromolecular material
Method, comprises the following steps：
(1) accuracy and repeatability of DSC instruments are evaluated with standard substance sapphire；
(2) from 2~50mg hypocrystalline macromolecular materials as sample to be tested, conventional formula is respectively adopted and step-by-step movement heats up
Sample is heated, a DSC curve and a StepScan DSC curve are obtained respectively；
(3) StepScan DSC curves are resolved into a reversible specific heat capacity curve and a Non reversing heat flow curve, is led to
The discontinuous mutation of specific heat capacity on reversible specific heat capacity curve is crossed to determine glass transition position, during further according to glass transition
Specific heat capacity increment Delta CpWith the melting enthalpy Δ H on DSC curvem, determine the content of half hitch polycrystalline macromolecule different phase component.
Further, step (1) takes 40mg sapphires and carries out step-by-step movement intensification as standard sample, and experiment is obtained by terminating
One StepScan DSC curve, then by StepScan CpProgram is calculated and obtains sapphire specific heat capacity；Repeat above-mentioned reality
Test, contrast two groups of experimental results, the error between the specific heat capacitance and standard value that are obtained in curve is less than 2%.
Further, step (1) (2) is tested in an inert atmosphere, and flow is 15ml/min, the consumption of sample for 2~
50mg。
Further, step (2) routine heating schedule is the continuous warming in 25~300 DEG C, 10 DEG C/min of heating rate.
Further, step (2) step-by-step movement heating schedule is heated up in 25~300 DEG C, 2~10 DEG C of heating rate/
Min, often raises 1~5 DEG C of 1~10min of isothermal.
Further, when the final temperature of sample heating is higher than 135 DEG C, the step-by-step movement heats up and distinguish at whole story temperature
1~20min of isothermal.
Further, step (3) includes following calculating process：
1. StepScan C are passed throughpStepScan DSC curves are resolved to a reversible specific heat capacity curve and can not by program
Backheating flow curve；
2. sample from start melt t1Terminate t with to melting2, the whole melting process to DSC curve is integrated, accumulates
The area for dividing is the high molecular melting enthalpy Δ H of hypocrystallinem：
In formula, QsIt is the heat of sample, Q0It is the heat of baseline；
3. according to Δ HmWith the melting enthalpy Δ H of 100% crystalline polymersfValue just can obtain crystalline state XCConstituent content：
4. calculated by discontinuous Sudden change region on reversible specific heat capacity curve, sample can be obtained vitrifying turn occurs
Specific heat capacity increment Delta C during changep；
5. according to Δ CpWith half hitch polycrystalline macromolecule the unformed shape that glassy transition is 100% specific heat capacity increment Delta Cp0
Value just can obtain flowing unformed shape XMAConstituent content：
6. according to XCAnd XMAJust can obtain hard unformed shape XRAConstituent content：
XRA=1-XC-XMA (4)。
Beneficial effect：The present invention provides a kind of quick, convenient, accurate heat analysis method of testing, can by SSDSC technologies
Separated from dynamic process (such as solidify, crystallization and volatilize) with by glass transition, in obtaining sample temperature-rise period
Reversible specific heat capacity and the parameter such as glass transition temperature and melting enthalpy, can not only obtain the glass of hypocrystalline macromolecular material
Glass transition temperature, can also accurately obtain the reversible specific heat capacity corresponding to different temperatures, and also can according to specific heat capacity and
Melting enthalpy calculates the content of crystalline state in half hitch polycrystalline macromolecule sample, flowing unformed shape and hard unformed shape different phase.
Additionally, in order to accurately determine the high molecular specific heat capacity of hypocrystalline, need can be judged whether according to the probable ranges of its specific heat capacity
Carry out testing front and rear temperature isothermal operation, for the research of macromolecular material provides a kind of test new method.
Brief description of the drawings
Fig. 1 is sapphire specific heat capacity-temperature curve；
Fig. 2 is the specific heat capacity-temperature curve after sapphire isothermal；
Fig. 3 is the temperature curve of specific heat capacity one that PLA is tested twice；
Fig. 4 is the temperature curve of hot-fluid one that PLA is tested twice.
Specific embodiment
Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
Embodiment：
Embodiment 1：A kind of heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material, concrete operations are such as
Under：
(1) standard substance sapphire 40mg is weighed, is placed in aluminum cup and is added a cover and be compacted with blank panel, in 15ml/min
Under nitrogen, StepScan intensifications are carried out in 25~175 DEG C, 5 DEG C/min of heating rate often raises 1 DEG C of isothermal 1min, obtains
SSDSC curves.
(2) data analysis is carried out by SSDSC curves, the reversible specific heat capacity obtained in the range of 25~175 DEG C is bent
Line, specific heat capacitance on empirical curve is compared with sapphire standard specific heat capacitance.
(3) method according to step (1) and (2) carries out a SSDSC and repeats experiment again, show that a reversible specific heat capacity is bent
Line；By standard curve and this two reversible specific heat capacity Drawing of Curve in Fig. 1.As shown in figure 1, sapphire is tested by SSDSC
The two reversible specific heat capacity curve repeatability for measuring very well, and also can be good at overlapping with its standard specific heat capacity curve, and this two
The secondary sapphire specific heat capacity of retest is no more than 0.8% with its standard specific heat capacity worst error, less than 2%, illustrates that SSDSC is surveyed
The specific heat capacitance for obtaining is very accurate, credible, and repeatability is very well.
(4) hypocrystalline homopolymers PLA sample 12.80mg are weighed, is placed in aluminum cup and is added a cover and be compacted, in 15ml/
Under min nitrogen, conventional DSC experiments are carried out respectively in the range of 25~175 DEG C, programming rate is 10 DEG C/min；And
StepScan is tested, and heating rate is 5 DEG C/min, often raises 1 DEG C of isothermal 1min, respectively obtains DSC curve and SSDSC curves.
(5) by the StepScan C in Pyris Manager DSC operation interfacespProgram enters line number to SSDSC curves
According to analysis, a reversible specific heat capacity curve is just can obtain, it is all at 25~175 DEG C that the numerical value on these curves all show it
Specific heat capacitance, determines glass transition position, it is possible to by formula (4) by the mutation of specific heat capacity on reversible specific heat capacity curve
~(6) carry out three kinds of calculating of phase content.
(6) method according to step (4) carries out a SSDSC experiment again；Repeat step (5), a reversible ratio of getting back
Hold curve；This two reversible specific heat capacity curves and two DSC curves are drawn in figures 3 and 4 respectively.Such as Fig. 3, PLA samples lead to
Cross SSDSC two reversible specific heat capacity curves measuring of experiment to can be good at overlapping, illustrate the reappearance of SSDSC technologies also very
It is good.
Three kinds of calculating of phase component (crystalline state, flowing unformed shape and hard unformed shape), specific as follows in PLA：
1. understood according to formula (1), to the whole melting process of DSC curve in Fig. 4, (sample is from starting to melt 11.9min
Terminate 13.2min with to melting) it is integrated, the area for being integrated as melting enthalpy Δ Hm；
2. respectively by Δ HmWith Δ HF, PLA=93Jg-1Bring into formula (2) and just can obtain crystalline state XCConstituent content；
3. Fig. 3 is reversible specific heat capacity curve, by StepScan C in Pyris Manager DSC operation interfacespProgram
Calculating can obtain specific heat capacity increment Delta C during sample generation glass transitionp；
4. again by Δ CpWith Δ CPo, PLA=0.61Jg-1·℃-1Bringing into formula (3) just can obtain flowing unformed shape
XMAConstituent content；
5. it is last again by XCAnd XMASubstitute into formula (4) and just can obtain hard unformed shape XRA, specific data are shown in Table 1：
Three kinds of contents of phase component of the PLA of table 1
Embodiment 2：It is roughly the same with embodiment 1, except that when step (1) carries out StepScan experiments, starting to exist
25 DEG C carry out isothermal 15min, finally in 175 DEG C of isothermal 15min again, by standard curve and the two reversible specific heat capacity curves for obtaining
Draw in fig. 2.As shown in Fig. 2 increasing isothermal step, measured sapphire after terminating with intensification before experiment intensification starts
Reversible specific heat capacity equally there is repeatability and accuracy, this sapphire specific heat capacity of retest twice and its standard well
Specific heat capacity worst error is 0.8%, less than the conventional DSC method 2% that document is reported.And from the point of view of experimental result, although
Embodiment 1 is consistent with the worst error of embodiment 2, but in the non-isothermal in Fig. 1 whole story position, the specific heat capacity under lower temperature
Value almost overlaps, but curve tail there occurs deviation；After the isothermal of whole story position, curve tail is essentially coincided Fig. 2, illustrates that it compares
Error is minimum at relatively high temperatures for thermal capacitance value.Therefore, in the whole story position isothermal of stepping temperature elevating range, it is more beneficial for Instrument measuring
The specific heat capacity of higher temperature.
A certain numerical value in using claims technical scheme parameter area is tested all can reach the effect above,
Therefore embodiment part is no longer repeated.
Claims (7)
1. it is a kind of determine each phase constituent content of hypocrystalline macromolecular material heat analysis method, it is characterised in that：Including following
Step：
(1) accuracy and repeatability of DSC instruments are evaluated with standard substance sapphire；
(2) from 2~50mg hypocrystalline macromolecular materials as sample to be tested, conventional formula is respectively adopted and step-by-step movement heats up to sample
Product are heated, and a DSC curve and a StepScan DSC curve are obtained respectively；
(3) StepScan DSC curves are resolved into a reversible specific heat capacity curve and a Non reversing heat flow curve, by can
The discontinuous mutation of specific heat capacity determines glass transition position on inverse specific heat capacity curve, specific heat during further according to glass transition
Hold increment Delta CpWith the melting enthalpy Δ H on DSC curvem, determine the content of half hitch polycrystalline macromolecule different phase component.
2. the heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material according to claim 1, it is special
Levy and be：Step (1) takes 40mg sapphires and carries out step-by-step movement intensification as standard sample, and experiment obtains one by terminating
StepScan DSC curves, then by StepScan CpProgram is calculated and obtains sapphire specific heat capacity；Above-mentioned experiment is repeated, it is right
Than two groups of experimental results, the error between the specific heat capacitance obtained in curve and standard value is less than 2%.
3. the heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material according to claim 1, it is special
Levy and be：Step (1) (2) is tested in an inert atmosphere, and flow is 15ml/min.
4. the heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material according to claim 1, it is special
Levy and be：It is the continuous warming in 25~300 DEG C, 10 DEG C/min of heating rate that step (2) routinely heats up.
5. it is according to claim 1 and 2 determine each phase constituent content of hypocrystalline macromolecular material heat analysis method, its
It is characterised by：Step (2) step-by-step movement heats up to be heated up in 25~300 DEG C, and 2~10 DEG C/min of heating rate often raises 1
~5 DEG C of 1~10min of isothermal.
6. the heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material according to claim 5, it is special
Levy and be：When the final temperature of sample heating is higher than 135 DEG C, the step-by-step movement heat up distinguish at the whole story temperature isothermal 1~
20min。
7. the heat analysis method for determining each phase constituent content of hypocrystalline macromolecular material according to claim 1, it is special
Levy and be：Step (3) includes following calculating process：
1. StepScan C are passed throughpStepScan DSC curves are resolved to a reversible specific heat capacity curve and can not backheating by program
Flow curve；
2. sample from start melt t1Terminate t with to melting2, the whole melting process to DSC curve is integrated, integrated
Area is the high molecular melting enthalpy Δ H of hypocrystallinem：
In formula, QsIt is the heat of sample, Q0It is the heat of baseline；
3. according to Δ HmWith the melting enthalpy Δ H of 100% crystalline polymersfValue just can obtain crystalline state XCConstituent content：
4. calculated by discontinuous Sudden change region on reversible specific heat capacity curve, when can obtain sample generation glass transition
Specific heat capacity increment Delta Cp；
5. according to Δ CpWith half hitch polycrystalline macromolecule the unformed shape that glassy transition is 100% specific heat capacity increment Delta Cp0Value is just
Flowing unformed shape X can be obtainedMAConstituent content：
6. according to XCAnd XMAJust can obtain hard unformed shape XRAConstituent content：
XRA=1-XC-XMA。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108538416A (en) * | 2018-04-09 | 2018-09-14 | 西京学院 | A method of Nuclear Reactor Neutron Flux Density is measured based on reversible specific heat capacity method |
| CN109297997A (en) * | 2017-07-24 | 2019-02-01 | 北京化工大学 | A method of measurement polymer crystallinity, mesomorphic degree and unformed degree |
| CN109696455A (en) * | 2019-03-01 | 2019-04-30 | 北京食品科学研究院 | A method of quality stability in prediction mango powder glassy state storage |
| CN112098452A (en) * | 2020-09-10 | 2020-12-18 | 中国科学院金属研究所 | Method for calibrating content of cristobalite in ceramic core |
| CN112745568A (en) * | 2020-12-07 | 2021-05-04 | 国高材高分子材料产业创新中心有限公司 | Polymer-based multiple-melting-temperature standard substance and preparation method and application thereof |
| WO2021110075A1 (en) * | 2019-12-03 | 2021-06-10 | 中广核三角洲（太仓）检测技术有限公司 | Method for detecting pp content in hdpe by means of differential scanning calorimetry |
| CN114235736A (en) * | 2021-11-30 | 2022-03-25 | 中汽研汽车检验中心（天津）有限公司 | Qualitative and quantitative analysis method for PP-PET (polypropylene-polyethylene terephthalate) blending material for automobile |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109297997A (en) * | 2017-07-24 | 2019-02-01 | 北京化工大学 | A method of measurement polymer crystallinity, mesomorphic degree and unformed degree |
| CN109297997B (en) * | 2017-07-24 | 2020-09-04 | 北京化工大学 | Method for measuring crystallinity, mesomorphism and amorphous degree of polymer |
| CN108538416A (en) * | 2018-04-09 | 2018-09-14 | 西京学院 | A method of Nuclear Reactor Neutron Flux Density is measured based on reversible specific heat capacity method |
| CN108538416B (en) * | 2018-04-09 | 2019-08-20 | 西京学院 | A method of Nuclear Reactor Neutron Flux Density is measured based on reversible specific heat capacity method |
| CN109696455A (en) * | 2019-03-01 | 2019-04-30 | 北京食品科学研究院 | A method of quality stability in prediction mango powder glassy state storage |
| WO2021110075A1 (en) * | 2019-12-03 | 2021-06-10 | 中广核三角洲（太仓）检测技术有限公司 | Method for detecting pp content in hdpe by means of differential scanning calorimetry |
| CN112098452A (en) * | 2020-09-10 | 2020-12-18 | 中国科学院金属研究所 | Method for calibrating content of cristobalite in ceramic core |
| CN112745568A (en) * | 2020-12-07 | 2021-05-04 | 国高材高分子材料产业创新中心有限公司 | Polymer-based multiple-melting-temperature standard substance and preparation method and application thereof |
| CN114235736A (en) * | 2021-11-30 | 2022-03-25 | 中汽研汽车检验中心（天津）有限公司 | Qualitative and quantitative analysis method for PP-PET (polypropylene-polyethylene terephthalate) blending material for automobile |
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