Capillary rheometer

Abstract: In a capillary rheometer including: a furnace (20) comprising a plurality of furnace zones (22a-d) and having a sample bore (23e) with a capillary (25a) connected to the lower end thereof; a plurality of heaters (22h) for heating the furnace zones (22a-d) thereby to heat a sample in the sample bore; and a plunger (6) for extruding the heated sample through the capillary; a plurality of temperature sensors (31,32a,32d) are provided for detecting the temperatures of the furnace zones, and the temperature characteristics of the furnace zones related to the temperature of the inner wall of the sample bore are obtained and stored in a controller (61). With a set objective temperature level to which the sample in the sample bore is to be heated, the controller determines on the basis of the stored temperature characteristics data the temperature of each of the furnace zones corresponding to the set objective temperature level, and controls the heaters so that the temperature detected by each of the temperature sensors coincides with the determined temperature of the corresponding one of the furnace zones. A temperature measuring rod (50) is also provided, which is adapted for insertion into the sample bore to accurately measure the temperature of the inner wall of the sample bore.

Description: BACKGROUND OF THE INVENTION This invention relates to an extrusion type capillary rheometer for measuring the rheological properties, such as, flow property, viscosity and molecular weight distribution of materials such as plastics, ceramics and rubber, comprising a temperature measuring device for measuring the temperature of the sample bore of the rheometer. Japanese Unexamined Utility Model Publication No. 59-101196 (Appln. No. 57-202566) discloses a rheometer of this type which comprises an electric furnace provided with a bore for a sample to be inserted into and a capillary connected to the lower end of the sample bore. The body of the furnace is sectioned into a plurality of zones, which are provided with individual heaters to heat the sample in the sample bore, and individual temperature sensors for detecting the temperatures of the respective furnace zones. One of the furnace zones is selected as a reference zone, and a controller controls the heater of the reference zone by a control signal so as to keep the zone at a predetermined temperature, and applies the control signal to the temperature controllers for the other furnace zones thereby to keep the temperature distribution of the whole furnace uniform. Then a plunger is inserted into the sample bore to extrude the heated sample out of the furnace through the capillary to thereby measure the rheological properties of the sample by the speed of movement of the plunger. Japanese Unexamined Utilty Model Publication No. 3-40550 (Appln. No. 1-101648) discloses a rheometer in which a separate barrel formed with a sample bore is disposed in the central portion of an electric furnace provided with heaters so as to make assemblage and maintenance of the furnace easy. There are problems, however, to be solved in these known arrangements. Since there is a difference in temperature between the furnace zones and the inside of the sample bore, in the arrangement that the temperatures of the zones are merely controlled so as to coincide with the reference temperature, it is impossible to make the temperature distribution of the sample itself uniform because of thermal interference between the different furnace zones. In the arrangement that a separate barrel is disposed in the furnace, if the barrel is of a single body, a similar thermal interference occurs to prevent the temperature distribution in the sample from becoming uniform. Furtheron, in the document US-A-4 587 837 a capillary rheometer is described which comprises a barrel for receiving the sample, the barrel being surrounded by electrical bandheaters which are controlled in response to temperatures measured by thermocouples arranged in pocket holes in the wall of the barrel. The sample is extruded through a capillary arranged at the lower end of the barrel in response to a gas pressure exerted on the molten sample. However, since the thermocouples are arranged in pocket holes, and a certain thickness of the wall is always required for reasons of mechanical stability, the measured temperatures have a deviation from the actual value of the temperatures at the inner wall of the barrel. Consequently, there always remains a considerable uncertainty of the measured results. From the document EP-A-0 089 130 an extruder cylinder is known which is provided with temperature sensors arranged in pocket holes of the wall thereof, and a method for calculating the actual inner wall temperature of the extruder is described. The inner wall temperature, however, is a function of a plurality of different apparatus and ambient parameters so that a calculation is cumbersome and already adversly affected by any slight changes of these parameters. Consequently, since the temperature of the inner wall surface or of the sample is uncertain, this uncertainty remains also for the measured results. Therefore, it is the object of the invention to provide a capillary rheometer in which the handling and the measuring accuracy is improved. The object is achieved with a capillary rheometer having the features of claim 1. When a setting means is operated to set an objective value of the temperature of the inner wall of the sample bore, a heater controlling means determines the temperatures of the furnace zones corresponding to the objective temperature on the basis of the temperature characteristics data stored in a storing means, and controls the heaters so that the temperatures detected by the temperature sensors in the furnace zones coincide with the determined temperatures to thereby maintain the temperature of the inner wall of the sample bore and consequently that of the sample uniformly at the set objective temperature. In a preferred embodiment, inside the furnace there is provided a hollow cylindrical barrel, in which a tubular inner liner is fitted. The inner liner is divided into a plurality of sections along the length thereof to thereby suppress mutual thermal interference on the inner surface of the barrel between the furnace zones and to improve the uniformity of temperature distribution in the sample. The invention provides a temperature measuring rod for use in the rheometer to measure the temperature of the sample bore of the rheometer. In a preferred embodiment, the rod comprises a cylindrical stem adapted for insertion into the sample bore defined by the inner liner of the barrel of the rheometer so as to be able to be pulled out therefrom, and a plurality of temperature sensors provided on the outer surface of the stem at those positions thereof which correspond to the furnace zones when the rod is inserted into the sample bore of the rheometer. When the rod is inserted into the sample bore, the temperature sensors on the outer surface of the stem contact the inner wall surface of the sample bore at the positions corresponding to the furnace zones to measure the temperatures thereof accurately. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a block diagram of a control system of a rheometer constructed in accordance with the invention; Fig. 2 is a front view, partially in vertical section, of the rheometer mounted on a material testing machine; Fig. 3 is a sectional view of the furnace included in the rheometer of the invention; Fig. 4(a) is a sectional view of a part of the furnace with a temperature measuring rod of the invention inserted into the sample bore of the rheometer; Fig. 4 (b) is an axial end view of the temperature measuring rod; Fig. 4(c) is a perspective view of part of the temperature measuring rod; and Fig. 5 is a graph showing some of the temperature characteristic lines of the furnace zones stored in the control system of Fig. 1. PREFERRED EMBODIMENT OF THE INVENTION Referring to the drawings, first to Fig. 2, there is shown a part of a material testing machine including a table 1, a crosshead 2 carried by a spaced pair of columns, not shown, so as to be vertically movable, and a load cell 3 provided on the crosshead for detecting the load imposed on a sample to be tested. A load rod 4 is connected to the load cell 3, extends vertically downward through the crosshead 2, and carries at its lower end a connector 5 to which a plunger 6 for extruding a sample is connected. The table 1 supports a gate-shaped support 7, from which an electric furnace 20 hangs. As shown in detail in Fig. 3, the furnace 20 comprises an upper furnace portion 21 fixed on the upper side of the support 7, a lower main furnace portion 22 fixed on the under side of the support 7, and a central barrel 23 extending concentrically through the upper and lower furnace portions 21 and 22 so as to connect the two portions into a single furnace. The barrel 23 comprises an outer tubular member 23a and an inner liner 23b closely fitted into the outer tubular member 23a. The upper furnace portion 21 is provided at its central portion with a semi-spherical bearing 21a, into which the upper end of the outer tubular member 23a is screwed, so that the barrel hangs from the bearing 21a to extend through the furnace. The inner liner 23b defines an axial bore 23e into which a sample to be tested is to be inserted. A plug 25 formed with a capillary 25a is fitted into the lower end of the sample bore 23e and secured by a nut 24 screwed to the lower end of the barrel 23 so that the sample bore 23e communicates with the capillary 25. In the illustrated embodiment, the inner liner 23b is made up of an upper liner section 23c and a lower liner section 23d, which are separately formed and shrinkfitted into the outer tubular member 23a of the barrel 23 so as to form a continuous liner. The arrangement that the two separate liner sections are combined in the outer tubular member 23a not only makes it easy to form the sample bore 23e and improve the accuracy of its inner diameter but also enables suppression of thermal interference between the upper and lower furnace zones 22d and 22c on the opposite sides of the border between the upper and the lower liner sections 23c and 23d, as will be described in detail hereinafter. The upper furnace portion 21 has an upper, a lower and a circumferential wall 21b of thermal insulator, which define an inner annular space filled with cement 21c, with a pair of concentric Nichrome ring heaters 21d embedded in the cement 21c. The upper furnace portion 21 is formed with a radial hole 21e, into which a temperature sensor 31 is inserted. The sensor 31 is provided at its forward end with a thermocouple or thermistor. The lower furnace portion 22 comprises a hollow cylindrical casing 22e and four annular members 22f of cement piled up one upon another in the casing 22e. Each of the annular members 22f is formed with a central through hole of an inner diameter greater than the outer diameter of the previously described barrel 23. The holes of the annular members 22f are axially aligned to form a central bore, in which the barrel 23 is disposed, with an air space 30 formed between the inner circumferential surface of the central bore and the outer circumferential surface of the barrel 23. A plurality of annular members 22g of thermal insulator are provided, one in each of the top and bottom portions of the hollow cylindrical casing 22e as well as between each adjacent two of the annular members 22f of cement. The annular members 22g of thermal insulator have their inner circumferential edges projecting radially inwardly into the air space 30 as far as adjacent the outer circumferential surface of the barrel 23. In each of the annular cement members 22f and adjacent the inner circumferential surfaces thereof there are embeded four Nichrome ring heaters 22h vertically equidistantly spaced part from each other. The sample in the bore 23e is heated by the ring heaters 22h through the barrel 23. Those sections of the lower furnace portion 22 which correspond to the four annular cement members 22f will be referred to as the furnace zones 22a, 22b, 22c and 22d from the bottom upward. Each of the furnace zones 22a to 22d is provided with a radial bore 22i, into which a temperature sensor 32a to 32d is inserted as far as the forward end thereof passes through a corresponding radial bore formed in the barrel 23a to contact the outer circumferential surface of the inner liner 23b for detection of the temperature of the liner 23b. The temperature sensors 32a to 32d are provided at their respective front ends with a thermocuple or thermistor. Fig. 4 shows a temperature measuring rod 50 adapted for insertion into the sample bore 23e of the barrel 23. The rod 50 comprises a stem 50a formed on the outer circumferential surface thereof with a plurality, say, five axially extending parallel grooves 51 arranged at equiangular positions about the circumference of the stem, and a plurality, say, four circumferential grooves 52 spaced a suitable distance apart from each other axially of the stem. Temperature sensors 33, 34a, 34b, 34c and 34d are fitted in the axial grooves 51, respectively, and secured therein by a tungsten wire 35 wound in each of the circumferential grooves 52. The temperature sensors 33 and 34a to 34d have such lengths that when the temperature measuring rod 50 is inserted into the sample bore 23e of the barrel 23, the respective forward ends of the temperature sensors 33 and 34a to 34d contact those portions of the wall surface of the sample bore 23e which correspond to the upper furnace portion 21 and the furnace zones 22a to 22d of the lower furnace portion 22, respectively, so as to measure the temperatures of those surface portions of the sample bore. Fig. 1 shows a system for controlling the temperature of the furnace. The system comprises a controller 61 which includes a memory 61a and a central processing unit not shown. The temperature sensors 31 and 32a to 32d are connected to the controller 61 so that the output signals from the sensors 31 and 32a to 32d corresponding to the detected temperatures are applied to the controller 61. Also connected to the controller 61 are circuits 62 and 63a to 63d for energizing the ring heaters 21a and 21h for the upper furnace portion 21 and the four furnace zones 22a to 22d of the lower furnace portion 22, respectively. A switch SW₁ for setting an objective temperature to which a sample to be tested is to be heated is also connected to the controller 61, to which the temperature sensors 33 and 34a to 34d of the measuring rod 50 are connectable. The memory 61a stores the temperature characteristics of those portions of the barrel 23 which correspond to the upper furnace portion 21 and the furnace zones 22a to 22d, related to the temperature of the inner wall of the sample bore 23e. The temperature characteristics are obtained in a manner to be described below in detail. When a sample is to be tested, the controller 61 controls the energizing circuits 62 and 63a to 63d in accordance with the stored temperature characteristics data to thereby control the temperature of the sample at a required level. As previously mentioned, the temperature measuring rod 50 provided with the temperature sensors 33 and 34a to 34d is inserted into the sample bore 23e of the barrel 23, so that the temperature sensor 33 contacts the inner wall surface of that portion of the bore 23e which corresponds to the upper furnace portion 21 while the temperature sensors 34a to 34d contact the inner wall surface of those portions of the bore 23e which correspond to the furnace zones 22a to 22d, respectively, of the lower furnace portion 22. Then the heater energizing ciruicts 62 and 63a to 63d are actuated to energize the ring heaters 21a and 22h until the outputs from all of the temperature sensors 33 and 34a to 34d indicate, say, 100°C, whereupon the temperatures detected by the temperature sensor 31 in the upper furnace portion 21 and the temperature sensors 32a to 32d in the furnace zones 22c to 22d of the lower furnace portion 22, that is, the temperatures in the five different portions of the inner liner 23b of the barrel 23 for the set temperature of 100°C, are read and stored in the memory 61a. In a similar manner, the energizing circuits 62 and 63a to 63d are so controlled that the temperatures detected by all of the sensors 33 and 34a to 34d of the temperature measuring rod 50 become, say, 150°C, and the temperatures then detected by the sensors 31 and 32a to 32d for the set temperature of 150°C are recorded. The above operation is repeated with the energizing circuits 62 and 63a to 63d being so controlled that the temperatures detected by all of the sensors 33 and 34a to 34d of the temperature measuring rod 50 become 200°C, 250°C, ..., respectively, and the temperatures detected by the sensors 31 and 32a to 32d for each of the set temperatures of 200°C, 250°C, ...being stored in the memory 61a. From the data obtained in the above manner charcteristic lines are plotted as shown in Fig. 5, wherein the set temperature T detected by the sensors 33 and 34a to 34d of the temperature measuring rod 50 is taken along the abscissa, and the temperature t detected by each of the sensors 31 and 32a to 32d is taken along the ordinate. In particular, the temperatures t detected by one of the sensors 31 and 32a to 32d, say, the sensor 31 are plotted for the set temperatures T of 100°C, 150°C, 200°C, 250°C, ... to obtain a characteristic line L₁. In a similar manner, the temperatures t detected by each of the other sensors 32a to 32d are plotted for the set temperatures T of 100°C, 200°C, 250°C, ... to obtain similar characteristic lines L₂, L₃, L₄ and L₅, only one of which is shown at L₂ in Fig. 5 for simplicity of illustration. These characteristic lines are stored in the memory 61a of the controller 61. In operation, a sample to be tested is put in the sample bore 23e of the barrel 23, and the switch SW₁ is oporated to set an objective temperature T to which the sample is to be heated. The controller 61 determines the temperatures t corresponding to the set objective temperature T for the five furnace zones on the basis of the above-mentioned five characteristic lines stored in the memory 61a, and then controls the ring heaters 21d and 22h through the energizing circuits 62 and 63a to 63c, respectively, so that the temperatures detected by the temperature sensors 31 and 32a to 32d coincide with the determined temperatures t for the five furnace zones, respectively. In this manner, it is possible to cause the temperature of the inner wall surface of the sample bore 23e of the barrel 23 and consequently that of the sample itself in the bore 23e to uniformly coincide with the objective temperature T . Then the crosshead 2 is driven to push the plunger 6 into the sample bore 23e to impose a predetermined load on the sample, which is extruded outside through the capillary 25a. The viscosity of the sample is calculated from the speed of the plunger driven in the above-mentioned manner for measurement of the fluidity of the sample. In addition to the above-mentioned advantage that the temperature of the sample can be maintained uniformly at the set level, this embodiment has the following advantages. First, since the inner liner 23b of the barrel 23 is divided into the upper and lower sections 23c and 23d, thermal interference in the inner surface of the barrel between at least the furnace zones 22c and 22d can be suppressed to thereby improve the uniformity of the temperature distribution of the sample. Secondly, since the insulation ring 22g is interposed between each adjacent two of the annular members 22f of cement constitutting the furnace zones 22a to 22d can be suppressed to thereby improve the uniformity of the temperature distribution of the sample. Since the Nichrome ring heaters are used, the maximum temperature that is controllable can be higher than with the band heaters used in the invention disclosed in Japanese Unexamined Utility Model Publication No. 59-101196. In the above embodiments, the memory 61a constitutes storing means; the switch SW₁ constitutes temperature setting means; and the controller 62 and the energizing circuits 63a to 63c constitute heater controlling means. In the above embodiments, the inner liner 23b of the barrel 23 is divided into two sections. It may be divided into three or more sections. For example, the inner liner may be divided into five sections corresponding to the upper furnace portion 21 and the four furnace zones 22a to 22d of the lower furnace portion 22. This will suppress thermal interference in the inner surface of the barrel 23 between the furnace zones to thereby improve the uniformity of the temperature distribution in the sample being tested. The number of the furnace zones is not limited to four as in the illustrated embodiment. The arrangement of the control system is not limited to that shown in Fig. 1, either. In the apparatus of the invention, the memory 61a stores the temperature characteristics of the furnace zones related to the temperature of the inner wall of the sample bore in the furnace, and on the basis of the stored temperature characteristics data a control temperature to which each of the furnace zones is to be heated so as to attain the objective temperature in the sample bore is determined, whereupon the ring heaters are so controlled that the temperatures of the furnace zones coincide with the determined control temperature. This makes it possible to keep the temperature of the inner wall of the sample bore and consequently that of the sample therein uniform and at a required level. Since the barrel 23 comprises a hollow cylindrical body and an inner liner fitted therein, which is divided into a plurality of sections in the axial direction thereof, it is possible to prevent thermal interference in the inner wall of the barrel between the furnace zones to thereby improve the uniformity of temperature distribution of the sample. Since the temperature measuring rod to be inserted into the sample bore is provided on its circumferential surface with a plurality of sensors at different positions along the length of the rod, the temperature of the inner wall surface of the sample bore at different portions thereof corresponding to the furnace zones can be detected by merely inserting the rod into the sample bore only once and without troublesome operations. In the illustrated embodiment, although the sensors 32a to 32d are so arranged that the sensing elements contact the outer circumferential surface of the inner liner 23b of the barrel 23, they need not necessarily contact the inner liner. In a capillary rheometer including: a furnace comprising a plurality of furnace zones and having a sample bore with a capillary connected to the lower end thereof; a plurality of heaters for heating the furnace zones to thereby heat a sample in the sample bore; and a plunger for extruding the heated sample through the capillary; a plurality of temperature sensors are provided for detecting the temperatures of the furnace zones, and the temperature characteristics of the furnace zones related to the temperature of the inner wall of the sample bore are obtained and stored in a controller. With a set objective temperature level to which the sample in the sample bore is to be heated, the controller determines on the basis of the stored temperature characteristics data the temperatue of each of the furnace zones corresponding to the set objective temperature level, and controls the heaters so that the temperature detected by each of the temperature sensors coincides with the determined temperature of the corresponding one of the furnace zones. By means of a temperature measuring rod which is adapted for insertion into the sample bore the temperature of the inner wall of the sample bore can be accurately measured.

Claims: A capillary rheometer comprising a furnace (20) divided into a plurality furnace zones (21, 22a, 22b, 22c, 22d) surrounding a central barrel (23) having a sample bore (23e) communicating with a capillary (25) connected to the lower end thereof, said sample bore (23e) receiving a sample to be tested, at least one heater (21d, 22h) in each furnace zone (21, 22a, 22b, 22c, 22d) so as to heat said sample received in said sample bore (23e), a plunger (6) for imposing a load on said sample received in said sample bore (23e) so as to forcedly extrude said sample through said capillary (25), a controller (61) for controlling each of said heaters (21d, 22h) in response to an output signal of a temperature sensor (31, 32a, 32b, 32c, 32d) arranged in each of said furnace zones (21, 22a, 22b, 22c, 22d), and a setting means (SW1) for setting an objective sample temperature ( T ), characterized by insulating layers (22g) interposed between each of said heaters (21d, 22h) so as to thermically decouple same, and a temperature measuring rod (50) adapted to be inserted into said sample bore (23e), said rod (50) having temperature sensors (33, 34a, 34b, 34c, 34d) arranged to measure the actual temperature of the wall surface of the sample bore (23e) which corresponds to each of said furnace zones (21, 22a, 22b, 22c, 22d) after insertion of said rod (50) into said sample bore (23e), wherein the actual temperatures are stored in a memory (61a) of said controller (61) for correcting the values (t) measured with said temperature sensors (31, 32a, 32b, 32c, 32d) arranged in each furnace zone (21, 22a, 22b, 22c, 22d) in order to determine and maintain a temperature (t) of said heaters (21d, 22h) which corresponds to a set objective temperature ( T ) for the sample. A capillary rheometer according to claim 1, wherein said sample bore (23e) is provided with an inner liner (23b) surrounding the sample bore (23e), said inner liner (23b) being divided into a plurality of sections along the length thereof, so as to interrupt heat conduction along an axial direction of said sample bore (23e). A capillary rheometer according to claim 1 or 2, wherein temperature measuring rod (50) comprises a cylindrical stem being provided on the outer circumferential surface thereof with a plurality of axially extending parallel grooves (51) in which said temperature sensors (33, 34a, 34b, 34c, 34d) comprising elongated members having a temperature sensing element attached to the tip thereof are fitted so that each of said sensing elements is placed at those portions of the wall surface of said sample bore (23e) which correspond to said furnace zones when said measuring rod (50) is inserted into said sample bore.

Inventors: TAKANO SUSUMU, TAKANO, SUSUMU
Applicants: SHIMADZU CORP, SHIMADZU CORPORATION
Application year: 1991
Main classification: G01N11
IPC codes: G01N33, G01N11, G01N25, F27D11