CN106596246A - Method for measuring thermodynamic property of polymer material - Google Patents
Method for measuring thermodynamic property of polymer material Download PDFInfo
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- 238000002844 melting Methods 0.000 abstract description 3
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- 239000004793 Polystyrene Substances 0.000 description 5
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- 229920002223 polystyrene Polymers 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
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- 239000008187 granular material Substances 0.000 description 3
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- 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
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- 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
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Abstract
本发明公开了一种用于测量高分子材料热力学性能的方法，该方法以低内耗金属管为载体，将粉末状高分子材料直接装入金属管的空腔体中或将颗粒状高分子材料熔化后吸入金属管的空腔体中制备试样，然后通过扭转、拉伸或弯曲模式测定试样的内耗和模量，并通过分析内耗‑温度曲线和模量‑温度曲线来获得材料Tg、Tm及其他热力学参数。与现有技术相比，该方法能够在更宽温度范围内测定高分子材料Tg、Tm及其他热力学参数，避免了温度过高时因材料性能改变导致的超出仪器正常测量范围，以及温度过低时需要仪器输出更大的作用力导致的对仪器的损伤。
The invention discloses a method for measuring the thermodynamic properties of polymer materials. The method uses a metal tube with low internal friction as a carrier, and directly packs powdery polymer materials into the hollow body of the metal tube or puts granular polymer materials After melting, suck it into the hollow body of the metal tube to prepare the sample, then measure the internal friction and modulus of the sample by torsion, tension or bending mode, and obtain the material T g by analyzing the internal friction-temperature curve and modulus-temperature curve , T m and other thermodynamic parameters. Compared with the existing technology, this method can measure the Tg , Tm and other thermodynamic parameters of polymer materials in a wider temperature range, avoiding the normal measurement range of the instrument caused by the change of material properties when the temperature is too high, and the temperature When it is too low, the instrument needs to output more force to cause damage to the instrument.
Description
技术领域technical field
本发明涉及材料性能检测的技术领域，尤其涉及一种用于测量高分子材料热力学性能的方法。The invention relates to the technical field of material performance detection, in particular to a method for measuring thermodynamic properties of polymer materials.
背景技术Background technique
常规的高分子材料热力学参数测量方法通常是对加热加压、冷却、切割制成的条状试样施加周期性应力，测量其应力应变的实时变化过程，并根据应力、应变曲线的振幅及相位关系计算出模量和内耗值，通过模量和内耗随温度和频率变化曲线获得材料的热力学参数。但由于高分子材料在被加热到Tg(材料玻璃化转变温度)以后会出现软化现象，无法提供恢复力，这导致即便施加很小的作用力也会对试样产生大的塑性形变，超出仪器正常测量范围，所以常规的测量方法一般最多只能检测到高分子材料Tg。但在实际应用中，准确测量高分子材料的Tg和Tm(材料熔化温度)及其他一些热力学数据对确定高分子加工成型工艺参数非常重要。以挤出成型为例，当挤出温度偏高时，材料分解加快，导致材料性能发生变化；挤出温度偏低时，材料流动性太差，需要仪器输出更大的挤出力，这会损伤螺杆及腔体，降低其使用寿命。The conventional measurement method of thermodynamic parameters of polymer materials is usually to apply periodic stress to the strip sample made by heating, pressing, cooling, and cutting, and measure the real-time change process of stress and strain, and according to the amplitude and phase of the stress and strain curve The modulus and internal friction are calculated according to the relationship, and the thermodynamic parameters of the material are obtained through the curve of the modulus and internal friction with temperature and frequency. However, since the polymer material will soften after being heated to Tg (glass transition temperature of the material), it cannot provide restoring force, which leads to a large plastic deformation of the sample even if a small force is applied, exceeding the instrument The normal measurement range, so conventional measurement methods generally can only detect the T g of polymer materials at most. However, in practical applications, accurate measurement of T g and T m (material melting temperature) and other thermodynamic data of polymer materials is very important for determining the parameters of polymer processing and molding. Taking extrusion molding as an example, when the extrusion temperature is too high, the material decomposes faster, resulting in changes in material properties; Damage the screw and cavity and reduce its service life.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足，提供了一种用于测量高分子材料热力学性能的方法，以解决温度过高时因材料性能改变导致的超出测量仪器的正常测量范围，以及温度过低时需要测量仪器输出更大的作用力导致的对仪器的损伤的技术问题。The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for measuring the thermodynamic properties of polymer materials to solve the problem of exceeding the normal measurement range of the measuring instrument caused by the change of the material properties when the temperature is too high, and the temperature is too high. When it is low, it is a technical problem that the measuring instrument needs to output a greater force to cause damage to the instrument.
本发明所要解决的技术问题采用以下技术方案来实现：The technical problem to be solved by the present invention adopts the following technical solutions to realize:
一种用于测量高分子材料热力学性能的方法，其特征在于，所述方法以低内耗金属管为载体，将待测高分子材料装入金属管的空腔中制备试样，再通过扭转、拉伸或弯曲模式测定试样的内耗和模量，最后通过分析内耗-温度曲线和模量- 温度曲线来获得材料的Tg、Tm及其它热力学参数，其中，所述的内耗金属管为内耗值在10-3量级及以下的金属管。A method for measuring the thermodynamic properties of polymer materials, characterized in that the method uses a metal tube with low internal friction as a carrier, and puts the polymer material to be tested into the cavity of the metal tube to prepare a sample, and then twists, Tensile or bending mode measures the internal friction and modulus of the sample, and finally obtains the T g , T m and other thermodynamic parameters of the material by analyzing the internal friction-temperature curve and the modulus-temperature curve, wherein the internal friction metal pipe is Metal pipes with an internal friction value of 10 -3 and below.
进一步地，所述待测高分子材料为粉末状或颗粒状，当为粉末状时，将待测高分子材料直接装入金属管的空腔中，并将两端封死；当为颗粒状时，将待测高分子材料熔化后装入金属管的空腔中，并将两端封死。Further, the polymer material to be tested is in the form of powder or granules, and when it is in the form of powder, the polymer material to be tested is directly packed into the cavity of the metal tube, and both ends are sealed; when it is in the form of granules , the polymer material to be tested is melted and put into the cavity of the metal tube, and the two ends are sealed.
进一步地，所述低内耗金属管的外径范围为1-5mm、壁厚范围为0.1-0.5mm、长度范围为3-10cm。Further, the low internal friction metal pipe has an outer diameter ranging from 1-5 mm, a wall thickness ranging from 0.1-0.5 mm, and a length ranging from 3-10 cm.
进一步地，所述试样的内耗和模量的测定方法包括两种方式：Further, the determination method of the internal friction and modulus of the sample includes two ways:
①采用强迫振动测量模式对样品进行扭转、拉伸和弯曲变形，通过应力和应变传感器实时采集材料的加力和振动曲线，通过计算应力应变的振幅比值以及两者滞后角获得模量和内耗值，该方式的测量原理为：在强迫振动测量模式下，信号发生器发生的一个周期性正弦施力信号迫使试样做周期性正弦振动，此时应力传感器测量获得应力曲线为σ＝σ0sin(ωt-α)，应变传感器测量获得应变曲线ε＝ε0sin(ωt-α-φ)，其中φ代表应变信号与激发信号的相角差，由此计算出弹性模量E或G＝σ/ε，内耗值Q-1＝tanφ；① Use the forced vibration measurement mode to perform torsion, tension and bending deformation on the sample, collect the force and vibration curves of the material in real time through the stress and strain sensors, and obtain the modulus and internal friction by calculating the amplitude ratio of the stress and strain and the lag angle between the two , the measurement principle of this method is: in the forced vibration measurement mode, a periodic sinusoidal force signal generated by the signal generator forces the sample to do periodic sinusoidal vibration, and the stress curve obtained by the stress sensor measurement is σ=σ 0 sin (ωt-α), the strain sensor measures the strain curve ε=ε 0 sin(ωt-α-φ), where φ represents the phase angle difference between the strain signal and the excitation signal, and thus calculates the elastic modulus E or G=σ /ε, internal friction value Q -1 = tanφ;
②采用自由衰减模式对样品进行扭转或弯曲变形，通过采集材料的应变衰减曲线，计算振幅的对数衰减率和频率获得模量和内耗值，该方式的测量原理为：在自由衰减测量模式下，信号发生器发出一个偏转信号使样品扭转至设定应变振幅值ε0，然后使样品作自由衰减运动，并测量其应变衰减曲线ε＝ε0e-δωtsin(ωt),根据偏转力σ与应变值ε，计算出弹性模量G＝σ/ε，根据多个振动周期的振幅值计算出内耗值其中φ代表应变信号与激发信号的相角差，An和An+m分别是第n和第n+m次振动的振幅。② Use the free decay mode to twist or bend the sample, collect the strain decay curve of the material, calculate the logarithmic decay rate and frequency of the amplitude to obtain the modulus and internal friction value, the measurement principle of this method is: in the free decay measurement mode , the signal generator sends out a deflection signal to twist the sample to the set strain amplitude ε 0 , then make the sample perform free decaying motion, and measure its strain decay curve ε=ε 0 e -δωt sin(ωt), according to the deflection force σ Calculate the elastic modulus G=σ/ε with the strain value ε, and calculate the internal friction value according to the amplitude values of multiple vibration cycles Where φ represents the phase angle difference between the strain signal and the excitation signal, and An and An +m are the amplitudes of the nth and n+mth vibrations, respectively.
进一步地，所述Tg、Tm及其它热力学参数的获得方法为：通过改变测量温度和频率获得高分子材料的内耗和模量随温度和频率的变化曲线，即内耗-温度曲线和模量-温度曲线，根据内耗-温度曲线和模量-温度曲线中内耗峰的位置和模量变化最快的位置获得材料的Tg、Tm值及其他热力学参数值。Further, the method for obtaining the Tg , Tm and other thermodynamic parameters is: by changing the measurement temperature and frequency to obtain the curve of internal friction and modulus of the polymer material with temperature and frequency, that is, internal friction-temperature curve and modulus -Temperature curve, according to the internal friction-temperature curve and the modulus-temperature curve, the position of the internal friction peak and the position where the modulus changes the fastest obtain the Tg, Tm value and other thermodynamic parameter values of the material.
本发明相比现有技术具有以下优点：本发明提供了一种用于测量高分子材料热力学性能的方法，该方法能够在更宽温度范围内测定高分子材料Tg、Tm及其他热力学参数，避免了温度过高时因材料性能改变导致的超出仪器正常测量范围，以及温度过低时需要仪器输出更大的作用力导致的对仪器的损伤。Compared with the prior art, the present invention has the following advantages: the present invention provides a method for measuring the thermodynamic properties of polymer materials, which can measure T g , T m and other thermodynamic parameters of polymer materials in a wider temperature range , to avoid the damage to the instrument caused by the change of material properties when the temperature is too high, and the damage to the instrument caused by the instrument outputting a greater force when the temperature is too low.
附图说明Description of drawings
图1是颗粒状高分子材料的试样制备过程示意图；Fig. 1 is the schematic diagram of the sample preparation process of granular polymer material;
图2是粉末状高分子材料的试样制备过程示意图；Fig. 2 is the schematic diagram of the sample preparation process of powdery polymer material;
图3是将试样进行扭转变形处理检测过程示意图，图中，1为固定夹具，2为试样，3为竖摆杆，4为镜子，5为横摆杆摆锤，6为横摆杆，7为应力传感器，8为激发线圈，9为永磁体，10为光源，11为光电池；Figure 3 is a schematic diagram of the test process of torsion deformation treatment of the sample. In the figure, 1 is the fixed fixture, 2 is the sample, 3 is the vertical swing rod, 4 is the mirror, 5 is the pendulum of the swing rod, and 6 is the swing rod , 7 is a stress sensor, 8 is an excitation coil, 9 is a permanent magnet, 10 is a light source, and 11 is a photocell;
图4是将试样进行拉伸变形处理检测过程示意图，图中，1为固定夹具，2为试样，3为竖摆杆，4为位移传感器，5为应力传感器，6为步进马达；Fig. 4 is a schematic diagram of the test process of stretching and deforming the sample. In the figure, 1 is a fixed fixture, 2 is a sample, 3 is a vertical swing rod, 4 is a displacement sensor, 5 is a stress sensor, and 6 is a stepping motor;
图5是将试样进行弯曲变形处理检测过程示意图，图中，1为固定夹具，2为试样，3为竖摆杆，4为位移传感器，5为应力传感器，6为步进马达；Fig. 5 is a schematic diagram of the detection process of bending and deforming the sample. In the figure, 1 is a fixed fixture, 2 is a sample, 3 is a vertical swing rod, 4 is a displacement sensor, 5 is a stress sensor, and 6 is a stepping motor;
图6是强迫振动测量模式下的应力曲线和应变曲线；Fig. 6 is the stress curve and the strain curve under the forced vibration measurement mode;
图7是自由衰减模式下的振动衰减曲线；Fig. 7 is the vibration attenuation curve under the free attenuation mode;
图8是空的金属管的内耗-温度曲线和模量-温度曲线；Fig. 8 is the internal friction-temperature curve and the modulus-temperature curve of empty metal tube;
图9是聚苯乙烯的内耗-温度曲线和模量-温度曲线。Figure 9 is the internal friction-temperature curve and modulus-temperature curve of polystyrene.
具体实施方式detailed description
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below. This embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following implementation example.
实施例1Example 1
本实施例提供了一种用于测量高分子材料热力学性能的方法，包括以下步骤：This embodiment provides a method for measuring the thermodynamic properties of polymer materials, comprising the following steps:
(1)将内耗值在10-3量级及以下的，外径范围为1-5mm、壁厚范围为0.1-0.5mm的低内耗金属管切割成长度为3-10cm的短管，作为待测高分子材料的容器。(1) Cut the low internal friction metal pipe with an internal friction value of 10 -3 and below, an outer diameter range of 1-5mm, and a wall thickness range of 0.1-0.5mm into short pipes with a length of 3-10cm, as the waiting Containers for measuring polymer materials.
(2)以颗粒状或粉末状高分子材料作为待测高分子原材料；当使用颗粒状材料时，需要将其加热熔化后直接吸入金属管的空腔体中，然后双端封死，作为待测试样，其制备过程如图1所示；当使用粉末状材料时，先将金属管一端封死，后将粉末从另一端装入金属管的空腔体中、压实、封死，作为待测试样，其制备过程如图2所示。(2) Granular or powdery polymer materials are used as the polymer raw materials to be tested; when granular materials are used, they need to be heated and melted and then sucked directly into the cavity of the metal tube, and then sealed at both ends, as the material to be tested. The preparation process of the test sample is shown in Figure 1; when using powdered materials, first seal one end of the metal tube, then put the powder into the cavity of the metal tube from the other end, compact and seal, As the sample to be tested, its preparation process is shown in Figure 2.
(3)如图3-5所示，待测试样双端夹持固定在水平安装的固定夹具上，或双端固定在一端固定另一端可移动的夹具上，以方便对试样施加动态作用力。通过变频电机或激振器对双端固定的试样中心进行弯曲变形，或者对一端可动夹具所固定的试样进行扭转、拉伸变形，应变范围为1-10μm，频率范围为0.1-10Hz。(3) As shown in Figure 3-5, both ends of the sample to be tested are clamped and fixed on a fixed fixture installed horizontally, or both ends are fixed on a fixture with one end fixed and the other end movable, so as to facilitate dynamic application of the sample. force. Bending and deforming the center of the sample fixed at both ends by means of frequency conversion motor or vibrator, or torsion and stretching deformation of the sample fixed by a movable fixture at one end, the strain range is 1-10μm, and the frequency range is 0.1-10Hz .
(4)采用强迫振动测量模式对样品进行扭转、拉伸和弯曲变形，通过应力和应变传感器实时采集材料的加力和振动曲线，通过计算应力应变的振幅比值以及两者滞后角获得模量和内耗值，结果如图6所示；或者，采用自由衰减模式对样品进行扭转或弯曲变形，通过采集材料的应变衰减曲线，计算振幅的对数衰减率和频率获得内耗和模量值，结果如图7所示。(4) Use the forced vibration measurement mode to perform torsion, tension and bending deformation on the sample, collect the force and vibration curves of the material in real time through the stress and strain sensors, and obtain the modulus and The internal friction value, the result is shown in Figure 6; or, the sample is torsionally or flexibly deformed in the free decay mode, and the internal friction and modulus are obtained by calculating the logarithmic decay rate and frequency of the amplitude by collecting the strain decay curve of the material, and the results are as follows Figure 7 shows.
(5)通过改变测量温度和频率获得高分子材料的内耗和模量随温度和频率的变化曲线，即内耗-温度曲线和模量-温度曲线，根据内耗-温度曲线和模量-温度曲线中内耗峰的位置和模量变化最快的位置获得材料的Tg、Tm值及其他热力学参数值。(5) Obtain the curve of internal friction and modulus of polymer material with temperature and frequency by changing the measurement temperature and frequency, that is, internal friction-temperature curve and modulus-temperature curve, according to the internal friction-temperature curve and modulus-temperature curve The position of the internal friction peak and the position of the fastest modulus change obtain the T g , T m values and other thermodynamic parameters of the material.
如图8所示，为利用上述方法测定的未装有待测高分子材料的空的金属管的内耗-温度曲线和模量-温度曲线(空白实验)，从图8中可以看出，低内耗的金属管的内耗-温度曲线和模量温度曲线走势平稳，没有特别的峰值或大幅变化的位置，说明利用低内耗金属管作为测定容器，对高分子材料的热力学参数测量结果无显著影响，具有一定的可行性。As shown in Figure 8, it is the internal friction-temperature curve and the modulus-temperature curve (blank experiment) of the empty metal tube that is not equipped with the macromolecular material to be measured by the above-mentioned method, as can be seen from Figure 8, low The internal friction-temperature curve and modulus-temperature curve of the internal friction metal tube have a stable trend, and there are no special peaks or large changes in position, indicating that the use of low internal friction metal tubes as the measurement container has no significant impact on the measurement results of thermodynamic parameters of polymer materials. It has certain feasibility.
如图9所示，为利用上述方法测定的聚苯乙烯高分子材料的内耗-温度曲线和模量-温度曲线，从图9中可以看出，聚苯乙烯在测量温度范围内有两个内耗峰，同时根据模量的变化分析：110℃左右的内耗值峰应是由于聚苯乙烯的玻璃化转变而引起的内耗值的变化，240℃左右内耗值的变化应是由于聚苯乙烯熔化而引起的。As shown in Figure 9, it is the internal friction-temperature curve and modulus-temperature curve of the polystyrene polymer material determined by the above method. As can be seen from Figure 9, polystyrene has two internal friction curves in the measurement temperature range. At the same time, according to the change of modulus, the peak of internal friction at around 110°C should be due to the change of internal friction due to the glass transition of polystyrene, and the change of internal friction at around 240°C should be due to the melting of polystyrene. caused.
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.
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