CN105372282A - Method for testing material softening point by using static thermal mechanical analyzer - Google Patents
Method for testing material softening point by using static thermal mechanical analyzer Download PDFInfo
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- CN105372282A CN105372282A CN201410408479.2A CN201410408479A CN105372282A CN 105372282 A CN105372282 A CN 105372282A CN 201410408479 A CN201410408479 A CN 201410408479A CN 105372282 A CN105372282 A CN 105372282A
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Abstract
The invention relates to a method for testing a material softening point by using a static thermal mechanical analyzer. According to the method, a static thermal mechanical analyzer is used, a material sample to be tested is placed on the clamper of the static thermal mechanical analyzer, the sample is clamped, a test is started according to the programming temperature, the tested curve of the sample size or probe position along with the temperature is recorded, the recording is stopping after the sample is softened, and the temperature of the tangent line intersection point at the base line extending line and the maximum descending slope in the tested curve is the softening point. According to the present invention, the thermoplastic material softening point testing can be conveniently performed; compared to the ring and ball softening method prescribed in the national standard, the method of the present invention has characteristics of no requirement of high temperature material melting and casting sample preparation, simple operation, no pollution and no toxicity and harm on human body; and the programming temperature control provides advantages of high precision and wide testing temperature range compared to the oil bath heating.
Description
Technical field
The present invention relates to a kind of method of static heat mechanical analyzer test material softening point, belong to analysis and testing technology method field.
Background technology
Temperature when softening point refers to that amorphous polymer starts deliquescing.It is not only relevant with the structure of superpolymer, and relevant with the size of its molecular weight, is the important indicator affecting materials hot working technique, mechanical property.The assay method of softening point is a lot, and assay method is different, and its result is often inconsistent, and comparatively conventional has dimension block-regulations and ball and ring method etc.Ball and ring method adopts asphalt softening point tester usually, carries out according to GB GB/T15332-94 " the mensuration ball and ring method of hot melt adhesive softening point ".Its ultimate principle and process are: in advance sample is melted in becket, after cooling, a steel ball are placed on sample, heat in water-bath or oil bath, and along with temperature raises, sample softens, and steel ball falls through sample, and temperature is now considered as softening point.The method is the method extensively adopted in commercial production and quality control, but there is following shortcoming: sample preparation bothers, complicated operation; Sample dosage is large, and during melting, the smell is awful, has infringement to eyes, respiratory tract, pollutes large; The temperature range of water-bath or oil bath is limited, and temperature control error is large, test repeatability difference etc.
For the test of national regulations extraneous softening point, there is a kind of method measuring heavy oil softening point of known Chinese patent, publication number CN1448709, publication date 2003-10-15, think in mink cell focus
13c's quantitatively can reflect its structure, thus affects its softening point.This invention by representative mink cell focus sample composition calibration set, to they
13c-nuclear magnetic resonance figure and corresponding softening point basic data mathematically carry out regretional analysis, set up calibration model, by
13c-nmr spectrum, calculates the softening point of unknown mink cell focus sample.Known Chinese patent method for measuring natural ganoine bitumen softening point, publication number 101256162, publication date 2008-09-03, by in the both matter pitch that softening point is lower quantitatively in mix the hard pitch of high softening-point, measure the softening point of the compounding zoarium of ginseng, utilize and return the softening point that the method calculated obtains hard pitch indirectly.The method can be applied to the high softening-point material beyond existing testing standard scope, but its making joining compounding zoarium is complicated, and the accuracy of autoregression extrapolation disposal route remains to be discussed.The method of known Chinese patent determination softening point or dropping point, publication number 102980908, publication date 2013-03-20, provides a kind of measurement mechanism, records the visual pattern that sample starts to drip, obtain softening point or dropping point in temperature-rise period.
Visible, thermoplastic especially high softening-point material softening temperature test there is certain difficulty, need be undertaken by the apparatus of complexity.
Summary of the invention
The object of the present invention is to provide a kind of method of static heat mechanical analyzer test material softening point, have easy and simple to handle, measuring accuracy is high, and sample dosage is few, and sample preparation is simple, the advantage that testing cost is low.
Technical scheme of the present invention is: adopt static heat mechanical analyzer, the sample of material to be tested is positioned on the fixture of static heat mechanical analyzer, clamping sample, test is started according to program temperature, record specimen size or probe positions are with the test curve of temperature, stop record after sample is softening, the base-line extension of test curve and the point of intersection of tangents temperature of descending slope maximum are softening point.
The sample of described material to be tested is positioned on the fixture of static heat mechanical analyzer through planchet.
The sample of described material to be tested is fluid at normal temperatures.
The sample of described material to be tested is solid at normal temperatures.
The sample of described material to be tested is thin slice, and thin slice is square sheet, and the length of side of thin slice is 2mm-10mm, and the thickness of thin slice is 3mm-5mm, and upper and lower both ends of the surface are parallel.
The fixture of described thermomechanical analyzer is dull and stereotyped compression clamp, acupuncture fixture.
The probe diameter of described fixture is 1mm-5mm.
Described clamping sample is for applying static stress clamping sample, and static stress size is 10-20mN.
Described clamping sample is for applying static stress clamping sample, and static stress size is 10-100mN, for the material that softening rear viscosity is larger, suitably can increase static stress size, but should more than 100mN.
Described program temperature is that initial temperature should lower than sample softening point more than 20 DEG C, and more than constant temperature 10min, with 10 DEG C/min ramp, when sample softens, probe declines and after stablize, stops heating up and taking out sample as early as possible, prevent softening after sample adhesion pop one's head in or pollution instrument.
The present invention adopts static heat mechanical analyzer, select the suitable test condition such as fixture, method of preparing sample, planchet, heating rate, sample heats up under program temperature controls, and when reaching softening temperature, specimen size is undergone mutation, by this change curve of instrument record.The present invention can carry out the test of thermoplastic softening point easily, compares the ball and ring method of national regulations, and material does not need through high-temperature fusion, cast sample preparation, simple to operation, pollution-free, to human non-toxic's evil; And temperature programmed control is higher than oil bath heating accuracy, Range of measuring temp is wide.Method of testing of the present invention can be applied on the thermomechanical analyzer of various model easily, expands its application function, and the present invention compared with prior art beneficial effect is:
(1) the inventive method temperature journey scope (-100 DEG C ~ 550 DEG C) is wider than ball and ring method (normal temperature ~ 180 DEG C), can test the material softening point beyond prior art test specification.In addition, the fusing point of crystalline material or the melt temperature of amorphous materials also can refer to this method and test.
(2) the inventive method temperature control is accurate, result favorable reproducibility, and test curve have recorded the change in size of sample softening process, more intuitively, is convenient to data analysis.
(3) sample preparation of the present invention is convenient, and raw material usage is little, simple to operate, pollutes little, nonhazardous, has extremely strong practicality and the feature of environmental protection.
Accompanying drawing explanation
Fig. 1 is the test curve of the embodiment of the present invention 1.
Fig. 2 is the test curve of the embodiment of the present invention 2.
Fig. 3 is the test curve of the embodiment of the present invention 3.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
The mensuration of phenolics 2407 softening point.By the thin slice of sample polishing into about 5mm × 5mm × 3mm on sand paper, put into planchet and put into instrument again, select the dull and stereotyped compression clamp of φ=3mm, apply 10mN static stress, at room temperature keep 10min, reading specimen height is 3.83mm, start to heat with the heating rate of 10 DEG C/min, be warming up to 95 DEG C, stop test, take out sample.Record probe positions-temperature curve 1, as shown in Figure 1, the tangent line 4 intersection point temperature of base-line extension 3 and descending slope maximum is as softening point, and the softening point that can calculate sample is 77.088 DEG C.In Fig. 1,1 is probe positions-temperature curve, and 2 is probe positions differential-temperature curve, and Probeposition is probe positions, and Derivativeprobeposition is probe positions differential, and Temperature is temperature.When the descending slope maximum of probe positions-temperature curve 1 is difficult to judge, auxiliary judgment can be carried out by the peak of probe positions differential-temperature curve 2.
Embodiment 2
Be fluid under tackifying resin TX(normal temperature) mensuration of softening point.Sample is poured in the circular sample ware of φ 5mm, deeply about 3mm.Planchet is put into instrument, keeps probe unsettled; Be cooled to-70 DEG C, and keep 10min; Fall probe, apply 10mN static stress, reading specimen height is 3.38mm.Start, with the heating of the heating rate of 10 DEG C/min, to be warming up to 30 DEG C, to stop test, take out sample.Record probe positions-temperature curve 1, as shown in Figure 2, the tangent line 4 intersection point temperature of base-line extension 3 and descending slope maximum is as softening point, and the softening point that can calculate sample is-17.83 DEG C.
Embodiment 3
The mensuration of HIPS plastic melt temperature.Sample is processed into the thin slice of φ 5mm × 3mm, put into planchet and put into instrument again, select the dull and stereotyped compression clamp of φ=3mm, apply 20mN static stress, at room temperature keep 10min, reading specimen height is 2.53mm, start to heat with the heating rate of 10 DEG C/min, be warming up to 280 DEG C, stop test, take out sample.Record specimen size-temperature curve 1, as shown in Figure 3, the tangent line 4 intersection point temperature of base-line extension 3 and descending slope maximum is as melt temperature, and the melt temperature that can calculate sample is 233.45 DEG C.SampleDimension is specimen size.
The above; be only the embodiment of the best of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
The content be not described in detail in this instructions belongs to the known technology of professional and technical personnel in the field.
Claims (10)
1. the method with static heat mechanical analyzer test material softening point, it is characterized in that: adopt static heat mechanical analyzer, the sample of material to be tested is positioned on the fixture of static heat mechanical analyzer, clamping sample, test is started according to program temperature, record specimen size or probe positions are with the test curve of temperature, and stop record after sample is softening, the base-line extension of test curve and the point of intersection of tangents temperature of descending slope maximum are softening point.
2. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: the sample of described material to be tested is positioned on the fixture of static heat mechanical analyzer through planchet.
3. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: the sample of described material to be tested is fluid at normal temperatures.
4. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: the sample of described material to be tested is solid at normal temperatures.
5. the method for static heat mechanical analyzer test material softening point according to claim 4, it is characterized in that: the sample of described material to be tested is thin slice, and thin slice is square sheet, the length of side of thin slice is 2mm-10mm, and the thickness of thin slice is 3mm-5mm.
6. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: the fixture of described thermomechanical analyzer is dull and stereotyped compression clamp, acupuncture fixture.
7. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: the probe diameter of described fixture is 1mm-5mm.
8. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: described clamping sample is for applying static stress clamping sample, and static stress size is 10-20mN.
9. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: described clamping sample is for applying static stress clamping sample, and static stress size is 10-100mN.
10. the method for static heat mechanical analyzer test material softening point according to claim 1, is characterized in that: described program temperature is that initial temperature should lower than sample softening point more than 20 DEG C, and more than constant temperature 10min, with 10 DEG C/min ramp.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535312A (en) * | 2018-04-13 | 2018-09-14 | 云南中烟工业有限责任公司 | A method of utilizing the headspace gas chromatography Accurate Determining rosin softening point of temperature programming |
| CN108844829A (en) * | 2018-07-02 | 2018-11-20 | 上海电缆研究所有限公司 | A kind of measuring method of copper and copper alloy softening temperature |
| CN110514689A (en) * | 2019-08-28 | 2019-11-29 | 湖北三江航天江河化工科技有限公司 | The test method of HTPB propellant glass transition temperature |
| CN113848152A (en) * | 2021-09-02 | 2021-12-28 | 山东东岳高分子材料有限公司 | Method for measuring melt viscosity of fluorine-containing polymer |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535312A (en) * | 2018-04-13 | 2018-09-14 | 云南中烟工业有限责任公司 | A method of utilizing the headspace gas chromatography Accurate Determining rosin softening point of temperature programming |
| CN108535312B (en) * | 2018-04-13 | 2021-02-02 | 云南中烟工业有限责任公司 | Method for accurately measuring softening point of rosin by utilizing programmed heating headspace gas chromatography |
| CN108844829A (en) * | 2018-07-02 | 2018-11-20 | 上海电缆研究所有限公司 | A kind of measuring method of copper and copper alloy softening temperature |
| CN110514689A (en) * | 2019-08-28 | 2019-11-29 | 湖北三江航天江河化工科技有限公司 | The test method of HTPB propellant glass transition temperature |
| CN110514689B (en) * | 2019-08-28 | 2022-09-06 | 湖北三江航天江河化工科技有限公司 | Method for testing glass transition temperature of butylated hydroxytoluene propellant |
| CN113848152A (en) * | 2021-09-02 | 2021-12-28 | 山东东岳高分子材料有限公司 | Method for measuring melt viscosity of fluorine-containing polymer |
| CN113848152B (en) * | 2021-09-02 | 2024-05-14 | 山东东岳高分子材料有限公司 | Method for measuring melt viscosity of fluorine-containing polymer |
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Application publication date: 20160302 |