CN101430267B - Test method and apparatus for rheological behavior of polymer composite material - Google Patents
Test method and apparatus for rheological behavior of polymer composite material Download PDFInfo
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- CN101430267B CN101430267B CN2008101439345A CN200810143934A CN101430267B CN 101430267 B CN101430267 B CN 101430267B CN 2008101439345 A CN2008101439345 A CN 2008101439345A CN 200810143934 A CN200810143934 A CN 200810143934A CN 101430267 B CN101430267 B CN 101430267B
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Abstract
The invention relates to a method for testing polymer composite material rheological characteristic and a device thereof. The invention can measure the rheological actions of polymer composite material during an extrusion molding process, a capillary extrusion process and an injection molding process under the function of physical field enhancement and also can measure the rheological action of the polymer composite material when processing condition and parameter are changed according to a specific program. The invention uses a servo motor, a ball screw, an excitation system and a digital intelligent servo system to control the rheological testing process of the polymer composite material exactly, and the invention can measure the rheological characteristic of high polymer complex liquid continuously and fast under different processing conditions during the process of a single experiment. The invention can quench fused mass sharply during the testing process and then samples and studies the rheological characteristic of polymer fused mass intuitively. The invention has the high accuracy and stability of measurement data and the wide application range of material and is fit for macromolecular material, a macromolecule blending system, a macromolecule filling system, other similar macromolecular liquid systems, etc.
Description
Technical field
The present invention relates to a kind of rheological behavior of polymer composite material method of testing and device thereof, particularly a kind of based on multi-functional and full electric type rheological behavior of polymer composite material method of testing and device thereof.
Background technology
The processing and forming of superpolymer blend or infill system relates to superpolymer complex fluid rheological behaviour problem.The Response Mechanism and the behavior of research superpolymer complex fluid, to how in process accurate their multi-level inner structure of control, give full play to the performance potential of superpolymer blend or packing material, obtain all even desirable institutional framework at last, to rationally being chosen to shape technological parameter, optimal design contour machining equipment, realizing high yield, high-quality, low consumption, significant undoubtedly.
Polymeric material is a kind of typical viscoelastic materials, and has non-Newton fluid characteristic usually.In this fluid, be nonlinear relationship between viscosity and the shear rate.After introducing added physical field, the viscosity of polymer melt was not only relevant with shear rate, temperature, pressure, but also relevant with type of the intensity that adds physical field, the mode of action, physical field etc.After promptly introducing the outfield in the forming polymer process, polymer melt has shown unique rheological characteristics.
At present, traditional polymer melt rheology method of testing mainly contains capillary rheology method of testing and rotation rheology method of testing, but they are the rheological behaviour of polymer melt under the invigoration effect of energy measurement physical field not, particularly when add physical field in polymer processing when a certain setting program changes, very large variation will take place in the rheological behaviour of polymer melt thereupon, and this is that conventional test methodologies and means can't be finished.
Application number is that 200510033364.0 Chinese patent has been introduced a kind of polymer capillary sinuous pulsation squeezing rheometer, and it can measure the rheological behaviour of polymkeric substance in kapillary under the sinuous pulsation effect.Application number is that 200510033367.4 Chinese patent has been introduced a kind of polymer vibration induced plastification extrusion rheological behavior detecting method and extremely installed, and it can measure the dynamic rheological property behavior of polymkeric substance in single spiro rod plasticizing extrusion.Application number is that 200510033385.2 Chinese patent has been introduced a kind of polymer dynamic injection rheological properties and behavior detection method and equipment, and it can measure the dynamic rheological property and the behavior of polymkeric substance in the process of injection molding.But foregoing invention does not realize extruding of polymer composites and the integrated design of injecting, the rheological behaviour that can not test polymeric material in extrusion and the injection process simultaneously; Foregoing invention can not accurately be controlled the rheometer test process of polymer composites, promptly can not measure the rheological characteristics of high polymer composite material under different processing conditionss continuously, apace in the single experiment process; Foregoing invention is the rheological behaviour under energy measurement non-sinusoidal (as serrate, the rectangle) panting action not, can not freely design the pattern, the mode of action and the action time that add physical field, can not measure other performances that difference adds goods under the physical field effect; Foregoing invention can not quench cooled and subdivision barrel, mouthful mould and mould, with in time, study the rheological behaviour of polymer melt intuitively, statically; Comparatively speaking, measuring accuracy of the present invention is higher, and the maximum shear speed of permission, maximum extrusion pressure, peak swing and maximum vibration frequency are bigger, to material adaptability broad.
Summary of the invention
One of purpose of the present invention is to provide a kind of method that can measure polymer composites rheological behaviour and product properties in the multi-state molding process accurately, continuously.
Two of purpose of the present invention just provides the device that polymer composites method of rheological behaviour and product properties in the multi-state molding process is measured in realization accurately, continuously.
The objective of the invention is to be achieved through the following technical solutions: it not only can truly measure the rheological behaviour of the extrusion molding process of polymer composites under the physical field invigoration effect, kapillary extrusion, process of injection molding, can also measure the rheological behaviour of polymer composites when processing conditions and parameter change by specific program simultaneously;
Central processing unit is by instruction control servo drive system and excitation system, servo drive system guarantees plunger rod free rectilinear motion up and down in barrel, excitation system guarantees the plunger vibration of bar, like this, central processing unit just can be by point-to-point speed, run duration and the vibration parameters of any adjustable column stopper rod of instruction; At least three sections heating systems, three sections pressure transducers, three sections temperature sensors are installed on the barrel, sensor is connected with central processing unit by data acquisition system (DAS), central processing unit can be monitored material temperature, pressure and other parameters in real time, and adjusted in due course; Material is heated fusion in barrel, when the barrel lower end is connected with capillary die, material is just extruded from capillary die under the effect of plunger rod, parameters such as the pressure by melt under the sensor measurement vibration parameters, temperature, extruded velocity just can draw the rheological characteristics of polymer composites under this vibration parameters like this; When the barrel lower end is connected with nozzle, and directly and the cast gate of injection molding when fitting tightly, polymer complex fluid is injected into mould molding under the powerful thrust of plunger rod, by measure parameters such as temperature, pressure, speed can obtain polymer composites under certain vibration parameters in the injection barrel, the rheological behaviour of die cavity mold filling process; Be processed with hollow pipe in the middle of the barrel wall thickness, cooling liquid or gas carry out quench cooled by pipeline to melt, and simultaneously, barrel is cut open from the centre, like this, will melt extrude the material quench cooled in the process after, open barrel and take out material and intuitively study.
A kind of device of realizing above-mentioned method of testing; contain barrel; plunger rod; cooling system; the temperature sensor Data Acquisition and Conversion System (DACS); temperature sensor; capillary die; pressure transducer; heating system; pressure sensor data is gathered and control system; servo drive system; excitation system and central processing unit; wherein; be processed with cooling duct on the barrel tube wall; three sections heating systems are installed on the barrel; be connected with three temperature sensors on the barrel respectively; temperature sensor is connected with central processing unit with control system by temperature data acquisition; three pressure transducers are installed on the barrel; pressure transducer is connected with central processing unit with control system by the pressure data collection; plunger rod and servo drive system; excitation system connects; servo drive system is connected with central processing unit respectively with excitation system; the barrel bottom is connected with capillary die or nozzle (nozzle fits tightly with mould), and the pressure and temperature sensor is connected with central processing unit by the Pressure/Temperature Data Acquisition and Conversion System (DACS) respectively.
The present invention can either simulate extrusioning experiment exactly, and the flow field of melt and the flow field in the middle of the actual production are just the same during also simulate injection experiment exactly, and test; Owing to adopt servomotor, ball-screw and digital intelligent servo drive system, the rheometer test process of polymer composites can be accurately controlled, the rheological characteristics of superpolymer complex fluid under different processing conditionss can be in the single experiment process, measured continuously, apace; Simultaneously, the present invention can also measure under the multiple physical field effect, and the rheological behaviour of physical field melt when changing continuously by specific program; Can study the rheological characteristics of melt under outer field action intuitively; Measurement data accuracy height of the present invention, high, the wide application range of material of stability are fit to macromolecular material, polymer blended system, macromolecule infill system and other are similar to high molecular fluid system etc.
The vibrational waveform that excitation system of the present invention produces is sine wave, sawtooth pattern ripple or square wave, and vibration frequency is regulated arbitrarily between 0～50Hz, and amplitude is regulated arbitrarily between 0～12mm.
The extruded velocity of plunger rod of the present invention is regulated arbitrarily between 0～1000mm/min, and the suffered shear rate of respective material is at 0～40000S
-1Control arbitrarily in the scope.
The maximum extrusion pressure of plunger rod of the present invention is 50KN, can satisfy the injection technique requirement.
The length-diameter ratio of capillary die of the present invention can select 10,15,20,30,40,50.
Below the capillary die of the present invention laser diameter measuring instrument is housed, thereby can conveniently studies the extrusion swelling phenomenon of polymer composites.
Servo drive system of the present invention adopts servomotor, ball-screw and digital intelligent servo drive system, and is easy to operate, the precision height..
Description of drawings
Fig. 1 is the structural representation of extruding of the present invention.
Fig. 2 is an injection structure synoptic diagram of the present invention.
Among the figure: 1, barrel; 2, plunger rod; 3, cooling system; 4, temperature sensor Data Acquisition and Conversion System (DACS); 5, first temperature sensor; 6, second temperature sensor; 7, three-temperature sensor; 8, the 4th temperature sensor; 9, capillary die; 10, laser diameter measuring instrument; 11, the 4th pressure transducer; 12, heating system; 13, the 3rd pressure transducer; 14, second pressure transducer; 15, pressure sensor data collection and control system; 16, first pressure transducer; 17, servo drive system; 18, excitation system; 19, central processing unit; 20, nozzle; 21, injection molding; 22, pressure transducer; 23, temperature sensor.
Embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with accompanying drawing.
The present invention not only can truly measure the rheological behaviour of the extrusion of polymer composites under the physical field invigoration effect, kapillary extrusion, process of injection molding, can also measure the rheological behaviour of polymer complex fluid when processing conditions and parameter change by specific program simultaneously;
Shear rate in the inventive method is at 0～40000S
-1Control arbitrarily in the scope can be provided with different shear rates in the different time periods, and realize freely switching between the different shear rate with in experimentation.
The vibrational waveform of plunger rod can be controlled automatically among the present invention, makes that vibrational waveform can be sine wave, sawtooth pattern ripple or square wave etc., and can freely select as required.
Can control time of vibration length, vibration zero-time, vibration concluding time or vibration number in the test process among the present invention arbitrarily, can freely determine as required; Can regulate vibration frequency and amplitude arbitrarily, frequency is regulated in 0～50Hz scope, and amplitude is regulated in 0～12mm scope.
The present invention can measure apparent viscosity, normal stress difference, slack time, elastic modulus and the viscous modulus etc. of material.The present invention can also measure the diameter of extruding object, thus research extrusion swelling phenomenon.The inventive method can be measured any polyblend system, superpolymer infill system and other flow-like materials, also can be applied to simultaneously some rheology of solution can measurement, material accommodation is extensive.
The inventive method has been introduced chilling subdivision barrel and mouthful modular system, promptly can when the equipment operate as normal, make the melt quench cooled, rheology state when making melt after curing, can keep operate as normal, thus barrel and mouthful mould can be opened, study the rheological behaviour of melt intuitively.
As shown in Figure 1, be processed with cooling duct 3 on barrel 1 tube wall, cooling liquid or gas are injected in cooling duct 3 the insides, can make polymer melt cooling curing immediately when extruding or injecting, barrel 1 can be cut open from the centre simultaneously, when polymer melt the inside adding trace particle, quench cooled just can directly be taken out sample after cutting barrel open, studies the rheological behaviour of polymer melt under the different situations intuitively.Three sections heating systems 12 are installed on the barrel 1, three sections heating systems are independently controlled, be connected with first temperature sensor 5, second temperature sensor 6, three-temperature sensor 7 respectively, temperature sensor is connected with central processing unit 19 with control system 4 by temperature data acquisition, temperature data and setting data that central processing unit 19 is come collection compare, send power and the contact-making switch that well heater is regulated in instruction immediately if data are variant, thereby reach the purpose of regulating temperature.The 3rd pressure transducer 13 is installed on the barrel 1 simultaneously, second pressure transducer 14, first pressure transducer 16, pressure transducer is connected with central processing unit 19 with control system 15 by the pressure data collection, central processing unit can obtain the force value of melt at any time by pressure transducer, and directly calculate the viscosity of melt by program design, simultaneously, central processing unit 19 can also be by decline rate that changes plunger rod 2 and the pressure that oscillation intensity is regulated melt, plunger rod 2 can be in the inner easy on and off motion of barrel, plunger rod 2 and servo drive system 17, excitation system 18 connects, digital intelligent servo drive system 17 orders about plunger rod 2 at the vertical direction rectilinear motion, excitation system 18 can order about plunger rod 2 and vibrate straight-line the generation simultaneously, servo drive system 17, excitation system 18 is connected with central processing unit 19 respectively, and central processing unit 19 can be controlled the point-to-point speed of plunger rod 2 by servo drive system 17 and excitation system 18 respectively, move the time in fact, vibration frequency and amplitude.Barrel 1 bottom is connected with capillary die 9, the length-diameter ratio of capillary die 9 can select 5,10,15,20,30,40,50 etc., capillary die 9 can be opened by subdivision, can directly take a sample to research from the inside, capillary die 9 is connected with the 4th pressure transducer 11, the 4th temperature sensor 8, and the pressure and temperature sensor is connected with central processing unit 9 by the Pressure/Temperature data acquistion and control system respectively.One laser diameter measuring instrument 10 is housed below the capillary die 9, is used for studying the extrusion swelling phenomenon of polymkeric substance.
As shown in Figure 2, when capillary die 9 is changed into nozzle 20, and injection molding 21 is installed below nozzle 20, just can be used for doing injection molding rheometer test.The 4th pressure transducer 11 and the 4th temperature sensor 8 are installed above the nozzle 20, so just can measure polymeric material in injection process, the pressure and temperature value of melt in nozzle 20, thus can calculate rheological property in the nozzle.Pressure transducer 22 and temperature sensor 23 are housed above the injection molding 21, same, by gathering the pressure and temperature of melt in the die cavity, just can measure the rheological behaviour of polymer composites in mold filling process.
Below introduce the polymer complex fluid physical field and strengthen rheometer test method embodiment.
(1) selects the rheological measurement device of extruding shown in Figure 1; (2) weighing LDPE pellet 50 grams, and with in its adding barrel; (3) start the heating system heating cylinder, three sections temperature of barrel are respectively 180 ℃, 190 ℃, 190 ℃; (4) insulation starts vibrator and servo drive system after 20 minutes, plunger rod is remained a constant speed in vibration move downward, and the setting vibration frequency is 10Hz, and amplitude is 0.2mm, and the vibrational waveform that makes plunger rod is sinusoidal vibration; (5) signals such as turn-on data acquisition system collecting temperature, pressure, displacement, speed, vibration parameters; (6) select apparatus embodiments 2～7, repeat (2) and went on foot for (5) step; (7) Data Post draws data such as apparent viscosity, elastic modulus.
Change vibration frequency and amplitude among the embodiment 1, all the other are with omiting;
With vibration frequency among the embodiment 1 and amplitude setting is zero, and all the other are with omiting;
Change the vibrational waveform among the embodiment 1 into zigzag wave, all the other are with omiting;
Change the waveform among the embodiment 1 into square wave, all the other are with omiting;
(1), (2), (3), (5), (6) are identical with method embodiment 1 with (7) step, the vibration parameters in (4) setting experimentation: 0～20 second, and amplitude 0.1mm, vibration frequency 5Hz; 20～40 seconds, amplitude 0.2mm, vibration frequency 10Hz; 40～60 seconds, amplitude 0.3mm, vibration frequency 15Hz; 60～80 seconds, amplitude 0.4mm, vibration frequency 20Hz; 80 seconds～finish amplitude 0.5mm, vibration frequency 25Hz.
Change the first step among the embodiment 1～6 into injection rheological measurement device shown in Figure 2, all the other are with omiting.
Among the embodiment 1～7 the 5th step back is increased by the 6th step: open quenching apparatus, make polymer melt cooled and solidified immediately, take a sample to research then; Former the 6th step changed for the 7th step into, and all the other are with omiting.
Claims (9)
1. the method for testing of a rheological behavior of polymer composite material, it is characterized in that: it not only can truly measure the extrusion molding process of polymer composites under the physical field invigoration effect, the rheological behaviour of process of injection molding, can also measure the rheological behaviour of polymer composites when processing conditions and parameter change by specific program simultaneously;
A), central processing unit is by instruction control servo drive system and excitation system, servo drive system guarantees plunger rod free rectilinear motion up and down in barrel, excitation system guarantees the plunger vibration of bar, like this, central processing unit just can be by point-to-point speed, run duration and the vibration parameters of any adjustable column stopper rod of instruction;
B), at least three sections heating systems, three sections pressure transducers, three sections temperature sensors are installed on the barrel, sensor is connected with central processing unit by data acquisition system (DAS), central processing unit can be monitored material temperature, pressure and other parameters in real time, and adjusted in due course;
C), material is heated fusion in barrel, when the barrel lower end is connected with capillary die, material is just extruded from capillary die under the effect of plunger rod, parameters such as the pressure by measuring melt under certain vibration parameters, temperature, extruded velocity, mouthful mould length-diameter ratio just can draw the rheological characteristics of polymer composites under this vibration parameters like this;
D), be processed with hollow pipe in the middle of the barrel wall thickness, cooling liquid or gas carry out quench cooled by pipeline to melt, simultaneously, barrel is cut open from the centre, like this, will melt extrude the material quench cooled in the process after, open barrel and take out material and intuitively study;
E), be connected with nozzle when the barrel lower end, and directly and the cast gate of injection molding when fitting tightly, polymer melt is injected into mould molding under the powerful thrust of plunger rod, by measure parameters such as temperature, pressure, speed can obtain polymer composites under certain vibration parameters in the injection barrel, the rheological behaviour of die cavity mold filling process.
2. according to the method for testing of the described a kind of rheological behavior of polymer composite material of claim 1, it is characterized in that the vibrational waveform that described excitation system produces is sine wave, sawtooth pattern ripple or square wave, vibration frequency is regulated arbitrarily between 0～50Hz, and amplitude is regulated arbitrarily between 0～12mm.
3. according to the method for testing of the described a kind of rheological behavior of polymer composite material of claim 1, it is characterized in that the extruded velocity of described plunger rod is regulated arbitrarily between 0～1000mm/min, the suffered shear rate of respective material is at 0～40000S
-1Control arbitrarily in the scope.
4. according to the method for testing of the described a kind of rheological behavior of polymer composite material of claim 1, it is characterized in that the maximum extrusion pressure of described plunger rod is 50KN.
5. device of realizing the method for testing of a kind of rheological behavior of polymer composite material as claimed in claim 1, contain barrel (1), plunger rod (2), cooling system (3), temperature sensor Data Acquisition and Conversion System (DACS) (4), first temperature sensor (5), second temperature sensor (6), three-temperature sensor (7), the 4th temperature sensor (8), capillary die (9), the 4th pressure transducer (11), heating system (12), the 3rd pressure transducer (13), second pressure transducer (14), first pressure transducer (16), pressure sensor data is gathered and control system (15), servo drive system (17), excitation system (18) and central processing unit (19), wherein, be processed with cooling duct on barrel (1) tube wall, three sections heating systems (12) are installed on the barrel (1), respectively with barrel (1) on first temperature sensor (5), second temperature sensor (6), three-temperature sensor (7) connects, temperature sensor is connected with central processing unit (19) with control system (4) by temperature data acquisition, i.e. the 3rd pressure transducer (13) of three pressure transducers is installed on the barrel (1), second pressure transducer (14), first pressure transducer (16), pressure transducer is connected with central processing unit (19) with control system (15) by the pressure data collection, plunger rod (2) and servo drive system (17), excitation system (18) connects, servo drive system (17) is connected with central processing unit (19) respectively with excitation system (18), barrel (1) bottom is connected with capillary die (9) or nozzle (20), and the 4th pressure transducer (11) is connected with central processing unit (19) by the Pressure/Temperature Data Acquisition and Conversion System (DACS) respectively with the 4th temperature sensor (8).
6. the proving installation of a kind of rheological behavior of polymer composite material according to claim 5 is characterized in that the length-diameter ratio of described capillary die (9) can select 5,10,15,20,30,40,50.
7. the proving installation of a kind of rheological behavior of polymer composite material according to claim 5 is characterized in that the independent respectively control of described three sections heating systems.
8. the proving installation of a kind of rheological behavior of polymer composite material according to claim 5 is characterized in that below the described capillary die (9) laser diameter measuring instrument (10) being housed.
9. the proving installation of a kind of rheological behavior of polymer composite material according to claim 5 is characterized in that described servo drive system (17) adopts servomotor, ball-screw and digital intelligent servo drive system..
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