CN111610149A - Crystallization melting furnace and high polymer optical polarization-resolving instrument - Google Patents
Crystallization melting furnace and high polymer optical polarization-resolving instrument Download PDFInfo
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- 229920000642 polymer Polymers 0.000 title claims abstract description 101
- 230000003287 optical effect Effects 0.000 title claims abstract description 92
- 238000002844 melting Methods 0.000 title claims abstract description 64
- 230000008018 melting Effects 0.000 title claims abstract description 63
- 238000002425 crystallisation Methods 0.000 title abstract description 57
- 230000008025 crystallization Effects 0.000 title abstract description 57
- 238000010438 heat treatment Methods 0.000 claims abstract description 82
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000919 ceramic Substances 0.000 claims abstract description 57
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 7
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 37
- 229910052710 silicon Inorganic materials 0.000 claims description 37
- 239000010703 silicon Substances 0.000 claims description 37
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- 230000028161 membrane depolarization Effects 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/21—Polarisation-affecting properties
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
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Abstract
The invention relates to the technical field of polymer crystallization speed measurement, in particular to a crystallization melting furnace and a polymer optical depolarizer. The crystallization melting furnace comprises a shell, a through hole is formed in the shell, and the shell is internally provided with: the device comprises a sliding device, a ceramic heating device and a liquid nitrogen cooling pipeline are arranged in the sliding device, a sample groove is formed in the surface of the sliding device, a glass slide loaded with a high polymer sample is detachably and fixedly arranged in the sample groove, and a light transmission hole is formed in the sample groove of the sliding device; adjustment means are provided for moving the slide means in the X and Y directions. The high polymer optical depolarizer comprises the crystallization melting furnace. According to the invention, the heating time and temperature of the ceramic heating device are controlled, and the control valve is controlled to be opened and closed, so that the temperature of the crystallization melting furnace can be controlled in a very short time, and the automatic control of the melting and crystallization processes is realized.
Description
Technical Field
The invention relates to the technical field of polymer crystallization speed measurement, in particular to a crystallization melting furnace and a polymer optical depolarizer.
Background
The existing optical depolarizer melting furnace and crystallization furnace are two separated furnace bodies, and the melting furnace and crystallization furnace are controlled to have different working temperatures by a control element. For example, in the patent application No. 201711098593X filed by the present applicant, when the high polymer optical depolarizer is operated, it is necessary to melt a high polymer sample placed on a slide in a remelting furnace, then take out the slide and place it on a crystallization furnace for optical detection. The high polymer optical depolarizer is very inconvenient and has poor user experience because the melting and crystallization are carried out in two separate steps.
Disclosure of Invention
In view of the above, the present invention provides a crystallization melting furnace and a high polymer optical depolarizer, and aims to facilitate the measurement of the crystallization speed of high polymer.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
a crystal melting furnace comprising a casing having a through hole formed therein, wherein: the device comprises a sliding device, wherein a ceramic heating device and a liquid nitrogen cooling pipeline are arranged in the sliding device, the liquid nitrogen cooling pipeline is annularly arranged around the ceramic heating device and is connected with a liquid nitrogen source, a control valve is arranged on a pipeline for connecting the liquid nitrogen cooling pipeline and the liquid nitrogen source, a sample groove is arranged on the surface of the sliding device, a glass slide loaded with a high polymer sample is detachably and fixedly arranged in the sample groove, and a light hole is arranged at the sample groove of the sliding device; and the adjusting device is used for enabling the sliding device to move along X and Y directions, the X and Y directions are mutually perpendicular directions so as to adjust the visual field position of the high polymer sample, and when the sliding device moves, the light holes are all in the visual field range of the through holes.
In the above crystal melting furnace, the adjusting device comprises an X-axis adjusting device and a Y-axis adjusting device, wherein the X-axis adjusting device comprises a first screw rod and a first elastic member, and the Y-axis adjusting device comprises a second screw rod and a second elastic member; the sliding device comprises a first side face, a second side face, a third side face and a fourth side face, the first side face and the third side face are two opposite side faces, the second side face and the fourth side face are two opposite side faces, the first side face and the first side face are oppositely arranged, the second side face and the second side face are oppositely arranged, the third side face and the third side face are oppositely arranged, and the fourth side face are oppositely arranged; external threads are arranged on the first screw rod and the second screw rod, through holes are arranged on the first side wall and the second side wall of the shell, internal threads are arranged in the through holes, and the external threads are matched with the internal threads; a first groove is formed in the first side face of the sliding device, one end of the first spiral rod is arranged in the first groove, a second groove is formed in the second side face of the sliding device, and one end of the second spiral rod is arranged in the second groove; one end of the first elastic piece is fixedly connected with the third side face of the sliding device, and the other end of the first elastic piece is fixedly connected with the third side wall of the shell; one end of the second elastic piece is fixedly connected with the fourth side face of the sliding device, the other end of the second elastic piece is fixedly connected with the fourth side face of the shell, and the fourth side face are two opposite faces.
A high polymer optical depolarizer, comprising in its housing: the optical detection device comprises a signal light source, a color filter structure, a polarizer, a crystal melting furnace, a semi-transparent and semi-reflective mirror and a first silicon photocell which are sequentially arranged along the same straight line, wherein after a light signal sent by the signal light source passes through the color filter and the polarizer and passes through a light hole of the crystal melting furnace, one part of the light signal passes through the semi-transparent and semi-reflective mirror to be a transmitted light signal, the other part of the light signal is reflected by the semi-transparent and semi-reflective mirror to be a reflected light signal, the first silicon photocell receives the transmitted light signal of the semi-transparent and semi-reflective mirror, the first silicon photocell converts the transmitted light signal into a first electric signal, and the crystal melting furnace is the crystal melting furnace; the signal light source brightness control device comprises a second silicon photocell and a feedback circuit module, the feedback circuit module is connected with the signal light source, the second silicon photocell receives a reflected light signal of the semi-transparent semi-reflective mirror, the second silicon photocell is perpendicular to the reflected light signal, the second silicon photocell converts the reflected light signal into a second electric signal, and the feedback circuit module adjusts the brightness of the signal light source according to the intensity of the second electric signal.
In the above optical depolarizer for high polymer, the optical depolarizer for high polymer further comprises a temperature control device, and the temperature control device is electrically connected to the ceramic heating device; the temperature control device is provided with: a first set temperature element containing a first set temperature for heating of the ceramic heating device, the first set temperature being 250 ℃ to 300 ℃; a second set temperature element containing a second set temperature for heating of the ceramic heating device, the second set temperature being 100 ℃ to 150 ℃; the ceramic heating device is heated at a first set temperature or at a second set temperature.
In the high polymer optical depolarizer, a temperature increase button and a temperature decrease button are arranged on the housing, the temperature increase button and the temperature decrease button are pressure trigger buttons, a set temperature signal of the temperature control module is increased by 0.1-1 ℃ each time the temperature increase button is triggered, and the set temperature signal of the temperature control module is decreased by 0.1-1 ℃ each time the temperature decrease button is triggered;
in the above optical depolarizer for high polymer, the temperature controller further comprises a temperature signal collecting element, a temperature adjusting element and a temperature signal transmitting element, the temperature signal collecting element is configured to collect the temperature increase signal and the temperature decrease signal, the temperature adjusting element is configured to calculate a first set temperature and a second set temperature according to the temperature increase signal and the temperature decrease signal, and the temperature signal transmitting element transmits the first set temperature and the second set temperature signal to the ceramic heating device.
In the above high polymer optical depolarizer, a display unit is further disposed on the housing, the display unit is connected to the temperature control device, the temperature control device provides a first set temperature and a second set temperature signal to the display unit, and the display unit can display the first set temperature and the second set temperature signal.
In the above optical depolarizer for high polymer, the optical depolarizer for high polymer further comprises an automatic control device, the automatic control device is connected to the temperature control device and the control valve, a time distribution element is disposed in the automatic control device, and a first time period, a second time period and a third time period are disposed in the time distribution element, wherein: in a first time period, the control valve is in a closed state, and the ceramic heating device heats according to a first set temperature; in a second time period, the control valve is in an open state, and the ceramic heating device is in a non-heating state; and in a third time period, the control valve is in a closed state, and the ceramic heating device heats according to a second set temperature.
In the above high polymer optical depolarizer, the high polymer optical depolarizer further includes a displacement control device, the displacement control device sends a first adjustment signal and a second adjustment signal to the adjustment device, and respectively adjusts a first bidirectional rotating motor and a second bidirectional rotating motor of the adjustment device, the first bidirectional rotating motor is connected to the first screw rod, and the second bidirectional rotating motor is connected to the second screw rod.
In the above-mentioned high polymer optical depolarizer, the high polymer optical depolarizer further includes a data conversion device, and the data conversion device converts the first electrical signal into the transmitted light intensity of the digital signal.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the crystal melting furnace provided by the embodiment of the invention, the ceramic heating device and the liquid nitrogen cooling pipeline are arranged in the sliding device, and the temperature of the crystal melting furnace can be adjusted and controlled within a very short time by controlling the heating time and temperature of the ceramic heating device and controlling the opening and closing of the control valve.
According to the crystallization melting furnace provided by the embodiment of the invention, after the high polymer sample is placed on the crystallization melting furnace, the melting and crystallization processes can be realized without manually moving the position of the high polymer sample, so as to obtain crystallization data.
According to the high polymer optical depolarizer provided by the embodiment of the invention, a user only needs to place a glass slide loaded with a sample to be detected on the sliding device, and the high polymer optical depolarizer can detect the crystallization data of the sample to be detected, that is to say, the high polymer optical depolarizer of the embodiment can simplify the step of obtaining the crystallization data of the sample to be detected, and user experience of the user is greatly improved.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic view of a crystal melting furnace according to an embodiment of the present invention;
fig. 2 is a schematic structural view of a sliding apparatus provided in an embodiment of the present invention;
fig. 3 is a schematic structural diagram of an optical depolarizer for high polymer according to an embodiment of the present invention.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Examples of the Crystal melting furnace
As shown in fig. 1 and 2, the crystal melting furnace includes a casing having a through hole formed therein, and the casing includes: the device comprises a sliding device 1, wherein a ceramic heating device 11 and a liquid nitrogen cooling pipeline 12 are arranged in the sliding device 1, the liquid nitrogen cooling pipeline 12 is arranged around the ceramic heating device 11 in a surrounding manner, the liquid nitrogen cooling pipeline 12 is connected with a liquid nitrogen source, a control valve is arranged on a pipeline connecting the liquid nitrogen cooling pipeline 12 and the liquid nitrogen source, a sample groove is formed in the surface of the sliding device 1, a glass slide 10 loaded with a high polymer sample is detachably and fixedly arranged in the sample groove, and a light hole 13 is formed in the sample groove of the sliding device 1; and an adjusting device for moving the sliding device 1 along X and Y directions, wherein the X and Y directions are mutually vertical directions to adjust the visual field position of the high polymer sample, and the light holes 13 are all in the visual field range of the through holes when the sliding device 1 moves.
The ceramic heating device 11 and the liquid nitrogen cooling pipeline 12 are arranged in the sliding device 1, and the temperature of the crystal melting furnace can be adjusted and controlled in a very short time by controlling the heating time and temperature of the ceramic heating device 11 and controlling the opening and closing of the control valve.
In specific implementation, the working process of the crystallization melting furnace comprises the following stages: 1) a melting stage, wherein the crystallization melting furnace is heated according to a first set temperature, and the first set temperature is 250-300 ℃; 2) in the rapid cooling stage, the control valve is in an open state, and the liquid nitrogen source introduces liquid nitrogen into the liquid nitrogen cooling pipeline 12 until the temperature reaches the room temperature or a second set temperature; 3) and a crystallization stage, wherein the crystallization melting furnace is heated according to a second set temperature, and the second set temperature is 100-150 ℃.
The numerical value and the time length of the first set temperature can be set; the numerical value and the time length of the second set temperature can be set; the time for introducing the liquid nitrogen into the liquid nitrogen cooling pipeline 12 can be set, and the time for introducing the liquid nitrogen in the embodiment is 2-5 s.
The diameter of the through hole is larger than the diameter of the light-transmitting hole 13. In the embodiment, the diameter of the light transmission hole 13 is 2.5mm-3.0mm, the diameter of the through hole is 10mm-20mm, and the light transmission hole 13 is in the range of the through hole, so that light can penetrate through the crystal melting furnace. Preferably, the light-transmitting hole 13 is located at the center of the sliding device 1 and the ceramic heating device 11.
The heating device in the present embodiment includes a ceramic heating element, and specifically, the ceramic heating element is a heat generating body formed by co-sintering a ceramic material and a metal material. The ceramic heating element is a high-efficiency heater with uniform heat distribution and a metal alloy with excellent heat conductivity, so that the temperature of a hot surface is ensured to be uniform, and hot spots and cold spots of equipment are eliminated. The ceramic heating elements are divided into two types, namely a PTC ceramic heating element and an MCH ceramic heating element. The materials used in these two products are completely different, but the finished product is similar to ceramic, and is therefore collectively referred to as a "ceramic heating element". The device has the advantages of reliable work, long service life, firmness, durability, energy conservation, flexible installation, high temperature resistance, quick heat transfer, good insulation, no limitation of model and specification size in manufacturing and the like. The voltage can be from 36V, 110V, 180V, 220V, 380V according to the wiring mode of user's demand, and the highest power load is 6.5W per square, and energy consumption can be reduced by 30% compared with the traditional electric heater. Compared with the prior art, the high polymer optical depolarizer of this embodiment adopts miniature ceramic heating device 11 as the heating element, compares with conventional heating wire heating element, because the volume is little, consequently has advantages such as heat capacity is less, rise/cooling rate is fast, the temperature is even, oxidation resistant high temperature resistant, long service life and energy-efficient for the high polymer optical depolarizer of this embodiment's volume is less, thickness is thin.
The shell comprises a first side wall 31, a second side wall 32, a third side wall 33 and a fourth side wall 34, the sliding device comprises a first side surface, a second side surface, a third side surface and a fourth side surface, the first side surface and the third side surface are two opposite side surfaces, the second side surface and the fourth side surface are two opposite side surfaces, the first side wall 31 and the first side surface are oppositely arranged, the second side wall 32 and the second side surface are oppositely arranged, the third side wall 33 and the third side surface are oppositely arranged, and the fourth side wall 34 and the fourth side surface are oppositely arranged. In order to realize the adjustment device to adjust the position of the sliding device 1, the adjustment device comprises an X-axis adjustment device and a Y-axis adjustment device, wherein the X-axis adjustment device comprises a first screw rod 21 and a first elastic element 23, and the Y-axis adjustment device comprises a second screw rod 22 and a second elastic element 24; a first groove 14 is formed in a first side surface of the sliding device 1, one end of the first screw rod 21 is arranged in the first groove 14, and when the first screw rod 21 rotates, one end of the first screw rod 21 rotates in the first groove 14; a second groove 15 is formed in the second side surface of the sliding device 1, one end of the second screw rod 22 is placed in the second groove 15, and when the second screw rod 22 rotates, one end of the second screw rod 22 rotates in the second groove 15; one end of the first elastic element 23 is fixedly connected with the third side surface of the sliding device 1, and the other end of the first elastic element 23 is fixedly connected with the third side wall 33 of the casing; one end of the second elastic element 24 is fixedly connected with the fourth side of the sliding device 1, and the other end of the second elastic element 24 is fixedly connected with the fourth side wall 34 of the housing; the first screw rod 21 and the second screw rod 22 are provided with external threads, the first side wall 31 and the second side wall 32 of the shell are provided with through holes, internal threads are arranged in the through holes, and the external threads are in threaded fit with the internal threads.
Thus, the adjustment of the slide device 1 in the X-axis direction is achieved by rotating the first screw 21, and the adjustment of the slide device 1 in the Y-axis direction is achieved by rotating the second screw 22. The X-axis direction and the Y-axis direction are mutually perpendicular directions.
Through the crystallization melting furnace provided by the embodiment, after a high polymer sample is placed on the crystallization melting furnace, the melting and crystallization processes can be realized without manually moving the position of the high polymer sample.
High Polymer optical depolarizer example 1
In this embodiment, as shown in fig. 3, an optical depolarizer for high polymer is provided, in a housing of the optical depolarizer for high polymer,: an optical detection device, which comprises a signal light source 41, a color filter structure 42, a polarizer 43, a crystal melting furnace 44, a half-mirror 45 and a first silicon photocell 46, which are arranged in sequence along the same straight line, wherein after an optical signal emitted by the signal light source 41 passes through the color filter and the polarizer 43 and passes through the light-transmitting hole 13 of the crystal melting furnace 44, a part of the optical signal passes through the half-mirror 45 to be a transmitted optical signal, and the other part of the optical signal is reflected by the half-mirror 45 to be a reflected optical signal, the first silicon photocell 46 receives the transmitted optical signal of the half-mirror 45, the first silicon photocell 46 converts the transmitted optical signal into a first electrical signal, and the crystal melting furnace 44 is the crystal melting furnace 44 in the above embodiment; the brightness control device of the signal light source 41 comprises a second silicon photocell 47 and a feedback circuit module, the feedback circuit module is connected with the signal light source 41, the second silicon photocell 47 receives a reflected light signal of the half mirror 45, the second silicon photocell 47 is perpendicular to the reflected light signal, the second silicon photocell 47 converts the reflected light signal into a second electric signal, and the feedback circuit module adjusts the brightness of the signal light source 41 according to the intensity of the second electric signal.
Wherein, the light emitted by the signal light source 41 is irradiated onto the high polymer sample to be measured of the crystallization melting furnace 44 after passing through the color filter structure 42 and the polarizer 43; the first silicon photo cell 46 is used for converting the light transmitted through the half mirror 45 into a first electric signal; the second silicon photo cell 47 is used to convert the light reflected by the half mirror 45 into a second electrical signal.
Openings are provided in the housing to facilitate the polymer sampleTaking and placing. During the concrete implementation, will the back is opened to the opening, will place the fixed setting on slider 1 of the sample that awaits measuring on slide 10, warp adjusting device adjusts the sample that awaits measuring is just right the light trap 13 sets up, the sample that awaits measuring heats the melting back at first settlement temperature through crystal melting furnace 44, and the control valve is opened, and liquid nitrogen gets into liquid nitrogen cooling pipeline 12, and is right crystal melting furnace 44 and surrounding space cool down to the second settlement temperature rapidly, then crystal melting furnace 44 keeps warm under the second settlement temperature, the sample that awaits measuring begins the crystallization. And collecting the electrical signal parameters and the second set temperature from the first silicon photocell 46 and the second silicon photocell 47, converting the electrical signal parameters and the heating temperature parameters into digital signals, and transmitting the digital signals to a computer to obtain the crystallization data and curve of the high polymer sample. The sample crystallization data comprises a depolarization light intensity versus time curve and isothermal crystallization parameters in different isothermal crystallization processes (
Isothermal crystallization curve for t), half crystallization time (1/t)1/2Curve for T), crystallization rate constant and alfamel index: (
The afzel index plot for log t).
The light-transmitting holes 13 are arranged to transmit polarized light through the polymer sample in the crystal melting furnace 44.
Wherein, when the crystallization melting furnace 44 is heated at the second set temperature, the initial time of the crystallization induction period of the high polymer sample is defined as the transmitted light intensity I0(ii) a After the crystallization of the high polymer sample begins, the light intensity is continuously increased until the light intensity is finally constant, and the transmitted light intensity is I∞. Thereby obtaining a depolarized light intensity-time curve. Changing the temperature of the second set temperature, and taking another high polymer sample to perform isothermal crystallization curves at other temperatures (e.g., 122.5 ℃, 125 ℃, 127.5 ℃ and 130 ℃).
Specifically, in the embodiment of the present invention, the signal acquisition and conversion device 49 is used for acquiring the electrical signal parameters from the first silicon photocell 46 and the second silicon photocell 47 and the heating temperature parameter of the crystal melting furnace 44.
The optical polymer depolarizer of this embodiment does not need to remove the slide 10 to move the position of the sample to be measured after the polymer sample is placed on the crystal melting furnace 44. The present embodiment achieves both crystallization and melting functions by controlling the crystallization-melting furnace 44 to different temperatures at different time periods.
The high polymer optical depolarizer provided in this embodiment realizes the adjustment of the sliding device 1 in the X-axis direction by rotating the first screw rod 21, and realizes the adjustment of the sliding device 1 in the Y-axis direction by rotating the second screw rod 22. So as to adjust the position of the visual field of the polymer sample to be measured, and the light can be irradiated on the polymer sample to be measured through the light-transmitting hole 13.
The high polymer optical depolarizer provided by this embodiment converts an optical signal into an electrical signal by using the silicon photocell, and the silicon photocell has a small volume, thereby reducing the volume of the optical depolarizer as a whole. In addition, the silicon photocell also has the advantages of good stability, corrosion resistance, durability, no pollution and the like, so that the measurement performance and the environmental protection performance of the optical depolarizer of the embodiment are improved.
In the optical depolarizer for high polymer provided in this embodiment, after the high polymer starts to crystallize, since the crystalline phase and the amorphous phase have different refractive indexes, scattered light is generated at the interface between the two phases, and as the crystallization process proceeds, the transparency of the sample is continuously decreased, so that the experimental curve deviates from the actual crystallization condition. The deviation caused by scattering can be eliminated through the multi-stage control feedback device, specifically, the second silicon photocell 47 converts the electric signal into an electric signal, and then the voltage of the signal light source 41 is automatically increased through the multi-stage control feedback device, so that the light intensity penetrating through the sample in the crystallization process is linearly increased all the time, and the experimental error is effectively reduced. The high polymer optical depolarizer provided by the embodiment of the invention converts an optical signal into an electric signal by adopting the silicon photocell, so that the volume of the optical depolarizer is reduced as a whole. In addition, the silicon photocell also has the advantages of good stability, corrosion resistance, durability, no pollution and the like, so that the measurement performance and the environmental protection performance of the high polymer optical depolarizer provided by the embodiment of the invention are improved.
Through the high polymer optical depolarizer that this embodiment provided, the user only need place the slide 10 that has the sample that awaits measuring with the loading slide 1 is last, high polymer optical depolarizer can automated inspection sample's crystallization data, that is to say, this embodiment the high polymer optical depolarizer can simplify the step of obtaining the sample's that awaits measuring crystallization data, improves user's user experience greatly.
High Polymer optical depolarizer example 2
The difference between the high polymer optical depolarizer provided in this embodiment and the high polymer optical depolarizer in embodiment 1 is that this embodiment further designs components related to temperature control, display and adjustment, so as to improve the user experience.
The high polymer optical depolarizer further comprises a temperature control device 51, wherein the temperature control device 51 is electrically connected with the ceramic heating device 11; the temperature control module is used for setting the temperature heated by the ceramic heating device 11. The temperature control device 51 is provided with: a first set temperature element containing a first set temperature for heating the ceramic heating device 11, the first set temperature being 250 to 300 ℃; a second set temperature element containing a second set temperature for heating the ceramic heating device 11, the second set temperature being 100 to 150 ℃; the ceramic heating device 11 is heated at a first set temperature or at a second set temperature. The numerical value of the first set temperature is specifically set according to the melting temperature of different high polymer samples to be detected. And the numerical value of the second set temperature is specifically set according to the crystallization temperatures of different high polymer samples to be detected.
Further, the temperature control device 51 is PID closed-loop control; the temperature control device 51 compares the set temperature signal with the temperature signal of the heating device acquired by the temperature sensor in real time and then corrects the temperature signal; specifically, if the temperature signal of the heating device acquired in real time is the same as the constant temperature signal, no correction is required, and if the temperature signal of the heating device acquired in real time is different from the constant temperature signal, the set temperature signal displayed by the first display unit is corrected to the temperature signal of the heating device acquired in real time.
A temperature increase button and a temperature decrease button are arranged on the shell, the temperature increase button and the temperature decrease button are pressure trigger buttons, a set temperature signal of the temperature control module is increased by 0.1-1 ℃ each time the temperature increase button is triggered, and the set temperature signal of the temperature control module is decreased by 0.1-1 ℃ each time the temperature decrease button is triggered;
the set temperature signal includes a first set temperature and a second set temperature. A modified first set temperature when the temperature increase button and the temperature decrease button are triggered during the melting phase; a second set temperature modified upon activation of the temperature increase button and the temperature decrease button during the crystallization phase.
In this embodiment, the temperature setting of the ceramic heating device 11 is realized by the temperature increase button and the temperature decrease button, the temperature increase button and the temperature decrease button are arranged on the operation surface 50 of the housing, and the angle formed by the operation surface 50 and the lower bottom surface of the housing is 20-60 degrees, so that the user can conveniently operate and observe the high polymer optical depolarizer.
Since the approximate melting point and crystallization temperature of the polymer sample are known values, when the optical depolarizer is used, the set temperature signal can be set to the melting point value or slightly smaller than the melting point value, and during heating, the melting condition of the polymer sample is judged by the first electric signal, and if the first electric signal is unchanged, the temperature increasing button is operated to increase the heating temperature of the ceramic heating device 11 until the polymer sample is melted.
Specifically, in order to realize the relationship between the pressure signals of the temperature increase button and the temperature decrease button and the temperature setting of the ceramic heating device 11, the temperature control device 51 is further provided with a temperature signal acquisition element, a temperature adjustment element and a temperature signal transmission element, the temperature signal acquisition element is used for acquiring the temperature increase signal and the temperature decrease signal, the temperature adjustment element is used for calculating a first set temperature and a second set temperature according to the temperature increase signal and the temperature decrease signal, and the temperature signal transmission element is used for transmitting the first set temperature and the second set temperature signal to the ceramic heating device 11.
The high polymer optical depolarizer further comprises an automatic control device, the automatic control device is connected with the temperature control device 51 and the control valve, a time distribution element is arranged in the automatic control device, a first time period, a second time period and a third time period are arranged in the time distribution element, wherein: in a first time period, the control valve is in a closed state, and the ceramic heating device 11 heats according to a first set temperature; in a second time period, the ceramic heating device 11 is in a non-heating state, the control valve is in an opening state, and liquid nitrogen is introduced into the liquid nitrogen cooling pipeline to cool the ceramic heating device 11; in a third time period, the control valve is in a closed state, and the ceramic heating device 11 heats according to a second set temperature.
The high polymer optical depolarizer further comprises a data conversion device, wherein the data conversion device converts the first electric signal into a digital signal according to the intensity of transmitted light
The high polymer optical depolarizer further comprises a signal acquisition and conversion device 49, wherein the signal acquisition and conversion device 49 is electrically connected with the first silicon photocell 46, and is used for converting the first electric signal into a digital signal and transmitting the digital signal to a computer, so that computer software can obtain crystallization speed data of a high polymer sample. The signal acquisition and conversion device 49 comprises a multi-channel acquisition card. The signal acquisition and conversion device 49 is also used for acquiring the temperature in the crystallization and melting furnace 44.
The high polymer optical depolarizer further comprises a multi-stage control feedback device, wherein the multi-stage control feedback device is respectively connected with the second silicon photocell 47 and the light source, and is used for automatically adjusting the light intensity of the second electric signal intensity control signal light source 41. The multi-stage control feedback arrangement includes a high power compensation circuit 48; the high-power compensation circuit 48 is connected to the second silicon photocell 47, connected to the light source, and compares the second electrical signal with a reference voltage to control the light intensity of the signal light source 41. The multi-stage control feedback device can well eliminate the deviation caused by scattering through the arrangement, so that the light intensity of the signal light source 41 is linearly improved all the time in the crystallization process of the high polymer field sample, and the experimental error is effectively reduced.
In order to adjust the position of the high polymer sample on the ceramic heating device 11, the control mode of the ceramic heating device 11 is designed as follows:
scheme 1: an adjusting knob is arranged on a shell of the optical depolarizer and comprises a first knob and a second knob, the first knob controls the sliding device 1 to move in the X direction, and the second knob controls the sliding device 1 to move in the Y direction. The slide 10 is moved in the X direction and the Y direction by the slide device 1, so that the high polymer sample can be positioned in a suitable field of view. Specifically, in the manner of providing the first screw rod 21 and the second screw rod 22, the first knob is the other end (the end not disposed in the first groove 14) of the first screw rod 21, and the second knob is the other end of the second screw rod 22.
Scheme 2: the high polymer optical depolarizer further comprises a displacement control device, wherein the displacement control device sends a first adjusting signal and a second adjusting signal to the adjusting device, and respectively and correspondingly adjusts a first bidirectional rotating motor and a second bidirectional rotating motor of the adjusting device, the first bidirectional rotating motor is connected with the first screw rod 21, and the second bidirectional rotating motor is connected with the second screw rod 22. Control buttons are arranged on the shell, and the number of the control buttons is four, and a first adjusting (+, -) signal and a second adjusting (+, -) signal are respectively and correspondingly generated. The first conditioning (+) signal controls movement of the slide 10 in a first direction of the X-direction, and the first conditioning (-) signal controls movement of the slide 10 in a second direction of the X-direction, wherein the first direction of the X-direction and the second direction of the X-direction are opposite directions. Likewise, the second conditioning (+) signal control and the second conditioning (-) signal control the movement of the slide 10 in the Y direction.
The position of the high polymer sample can be conveniently adjusted through the two schemes, so that the observed sample wafer is in the best visual field observation position.
In summary, the high polymer optical depolarizer provided by the embodiment of the present invention is provided with a sliding device 1 for accommodating the sample slide, and an adjusting device for moving the sliding device 1 along the X-axis direction and/or the Y-axis direction, so as to adjust the position of the sample, so that the sample slide to be observed microscopically is in the best viewing position. In addition, the high polymer optical depolarizer and the micro melting point measuring instrument provided by the embodiment of the invention adopt the micro ceramic heating device 11 as a heating body, and have the effects of small heat capacity, high temperature rise/fall rate, uniform temperature, oxidation resistance, high temperature resistance, long service life, high efficiency and energy saving due to small volume.
The sample carrying sheet is a glass sheet, specifically, after a high polymer sample to be detected is placed on the glass slide 10, a cover glass is placed and pressed on the sample, and under the action of gravity, the cover glass can enable the sample to be uniformly dispersed.
In this embodiment, in order to facilitate the resetting of the motor, the next operation is performed. The adjusting device also comprises a motor resetting device which is used for resetting the first motor and the second motor to the original position.
Further, in order to observe the set temperature value of the ceramic heating device 11 conveniently, a display unit is further arranged on the housing, the display unit is connected with the temperature control device 51, the temperature control device 51 provides a first set temperature signal and a second set temperature signal to the display unit, and the display unit can display the first set temperature signal and the second set temperature signal.
Further, the high polymer optical depolarizer also comprises a switch module, and the switch module is used for controlling the communication between the high polymer optical depolarizer and a power supply.
Further, the color filter structure 42 is formed by bonding two color filters; wherein, the outer diameter of the color filter is 10mm +/-0.1 mm, and the thickness of the color filter is 1.5mm +/-0.1 mm. The present embodiment can improve the color filtering effect by arranging the color filter structure 42 as described above.
After the high polymer starts to crystallize, because the crystalline phase and the amorphous phase have different refractive indexes, scattered light is generated at the interface of the two phases, and the transparency of a sample is continuously reduced along with the progress of the crystallization process, so that the experimental curve deviates from the actual crystallization condition. Converting the optical signal into a second electrical signal by the second silicon photocell 47; the multi-stage control feedback device comprises a high-power compensation circuit 48; the second electrical signal is compared with a reference voltage, and light source brightness adjustment is performed according to the comparison result to control the light emission intensity of the signal light source 41 and indicate light source voltage indication. The light source voltage is automatically increased through the light source voltage adjusting circuit, so that the light intensity penetrating through the sample in the crystallization process is linearly improved all the time, the experimental error is reduced, and the stability of instrument measurement and the accuracy of data acquisition are ensured.
In summary, it is readily understood by those skilled in the art that the advantageous modes described above can be freely combined and superimposed without conflict.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. A crystal melting furnace, comprising a casing having a through hole formed therein, wherein:
the device comprises a sliding device, wherein a ceramic heating device and a liquid nitrogen cooling pipeline are arranged in the sliding device, the liquid nitrogen cooling pipeline is annularly arranged around the ceramic heating device and is connected with a liquid nitrogen source, a control valve is arranged on a pipeline for connecting the liquid nitrogen cooling pipeline and the liquid nitrogen source, a sample groove is arranged on the surface of the sliding device, a glass slide loaded with a high polymer sample is detachably and fixedly arranged in the sample groove, and a light hole is arranged at the sample groove of the sliding device;
and the adjusting device is used for enabling the sliding device to move along X and Y directions, the X and Y directions are mutually perpendicular directions so as to adjust the visual field position of the high polymer sample, and when the sliding device moves, the light holes are all in the visual field range of the through holes.
2. A crystal melting furnace according to claim 1,
the adjusting device comprises an X-axis adjusting device and a Y-axis adjusting device, wherein the X-axis adjusting device comprises a first screw rod and a first elastic piece, and the Y-axis adjusting device comprises a second screw rod and a second elastic piece;
the sliding device comprises a first side face, a second side face, a third side face and a fourth side face, the first side face and the third side face are two opposite side faces, the second side face and the fourth side face are two opposite side faces, the first side face and the first side face are oppositely arranged, the second side face and the second side face are oppositely arranged, the third side face and the third side face are oppositely arranged, and the fourth side face are oppositely arranged;
external threads are arranged on the first screw rod and the second screw rod, through holes are arranged on the first side wall and the second side wall of the shell, internal threads are arranged in the through holes, and the external threads are matched with the internal threads;
a first groove is formed in the first side face of the sliding device, one end of the first spiral rod is arranged in the first groove, a second groove is formed in the second side face of the sliding device, and one end of the second spiral rod is arranged in the second groove;
one end of the first elastic piece is fixedly connected with the third side face of the sliding device, and the other end of the first elastic piece is fixedly connected with the third side wall of the shell;
one end of the second elastic piece is fixedly connected with the fourth side face of the sliding device, the other end of the second elastic piece is fixedly connected with the fourth side face of the shell, and the fourth side face are two opposite faces.
3. The optical depolarizer for high polymer features that inside its casing:
an optical detection device, which comprises a signal light source, a color filter structure, a polarizer, a crystal melting furnace, a semi-transparent and semi-reflective mirror and a first silicon photocell, which are sequentially arranged along the same straight line, wherein after an optical signal sent by the signal light source passes through the color filter and the polarizer and passes through a light hole of the crystal melting furnace, one part of the optical signal passes through the semi-transparent and semi-reflective mirror to be a transmitted optical signal, the other part of the optical signal is reflected by the semi-transparent and semi-reflective mirror to be a reflected optical signal, the first silicon photocell receives the transmitted optical signal of the semi-transparent and semi-reflective mirror, the first silicon photocell converts the transmitted optical signal into a first electrical signal, and the crystal melting furnace is the crystal melting furnace as claimed in claim 1 or 2;
the signal light source brightness control device comprises a second silicon photocell and a feedback circuit module, the feedback circuit module is connected with the signal light source, the second silicon photocell receives a reflected light signal of the semi-transparent semi-reflective mirror, the second silicon photocell is perpendicular to the reflected light signal, the second silicon photocell converts the reflected light signal into a second electric signal, and the feedback circuit module adjusts the brightness of the signal light source according to the intensity of the second electric signal.
4. The optical depolarizer of claim 3, further comprising a temperature control device, said temperature control device being electrically connected to said ceramic heating device;
the temperature control device is provided with:
a first set temperature element containing a first set temperature for heating of the ceramic heating device, the first set temperature being 250 ℃ to 300 ℃;
a second set temperature element containing a second set temperature for heating of the ceramic heating device, the second set temperature being 100 ℃ to 150 ℃;
the ceramic heating device is heated at a first set temperature or at a second set temperature.
5. The optical depolarizer of high polymer of claim 4,
the temperature control module is characterized in that a temperature increasing button and a temperature reducing button are arranged on the shell, the temperature increasing button and the temperature reducing button are pressure trigger buttons, a set temperature signal of the temperature control module is increased by 0.1-1 ℃ each time the temperature increasing button is triggered, and the set temperature signal of the temperature control module is reduced by 0.1-1 ℃ each time the temperature reducing button is triggered.
6. The optical depolarizer of high polymer of claim 5,
the temperature control device is also provided with a temperature signal acquisition element, a temperature adjusting element and a temperature signal sending element, wherein the temperature signal acquisition element is used for acquiring the temperature increase signal and the temperature decrease signal, the temperature adjusting element is used for calculating a first set temperature and a second set temperature according to the temperature increase signal and the temperature decrease signal, and the temperature signal sending element sends the first set temperature and the second set temperature signal to the ceramic heating device.
7. The optical depolarizer of high polymer of claim 4,
still be equipped with the display element on the shell, the display element with temperature control device connects, temperature control device to the display element provides first settlement temperature and second settlement temperature signal, the display element can show first settlement temperature and second settlement temperature signal.
8. The optical depolarizer of high polymer of claim 4,
the high polymer optical depolarizer further comprises an automatic control device, the automatic control device is connected with the temperature control device and the control valve, a time distribution element is arranged in the automatic control device, a first time period, a second time period and a third time period are arranged in the time distribution element, wherein:
in a first time period, the control valve is in a closed state, and the ceramic heating device heats according to a first set temperature; in a second time period, the control valve is in an open state, and the ceramic heating device is in a non-heating state; and in a third time period, the control valve is in a closed state, and the ceramic heating device heats according to a second set temperature.
9. The optical depolarizer of claim 3, wherein the optical depolarizer of the polymer,
the high polymer optical depolarizer further comprises a displacement control device, the displacement control device sends a first adjusting signal and a second adjusting signal to the adjusting device, and correspondingly adjusts a first bidirectional rotating motor and a second bidirectional rotating motor of the adjusting device respectively, the first bidirectional rotating motor is connected with the first screw rod, and the second bidirectional rotating motor is connected with the second screw rod.
10. The optical depolarizer of claim 3, wherein the optical depolarizer of the polymer,
the high polymer optical depolarizer further comprises a data conversion device, and the data conversion device converts the first electric signal into transmission light intensity of a digital signal.
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Application publication date: 20200901 |