KR100340585B1 - One-dimensional light diffusion apparatus and method for controlling the same - Google Patents

Abstract

PURPOSE: Provided are a one-dimensional light diffusion apparatus by which it is possible to analyse microstructures of new materials such as polymers, inorganic materials, metals, etc. and a method for controlling the same. CONSTITUTION: The apparatus includes a laser generator(1), a neutral density filter(2) for controlling an output intensity of laser beams from the laser generator(1) to a predetermined value; a polarizer(3) for polarizing the laser beams; a supporter(4) for supporting a heating plate(5); the heating plate(5) on which a sample film(6) is placed; a rotating plate(7) for adjusting the movement of material by heating; a micro-step-motor(8) for rotating the rotating plate(7); a temperature sensor(9); a power source(10); an analyzer(12); a photomultiplier tube(11); a computer motor drive(13); a temperature controller(14); a screw terminal(15); a direct port(16); an analogue/digital board(17); a host computer(18).

Description

1-dimensional light scattering device and control method

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a one-dimensional light scattering device and a control method thereof, and in particular, a polymer, an inorganic material, a metal, and the like, which are used when making a blend or a composite material. 1D light scattering device and a method of controlling the same for enabling non-destructive analysis of a micro-structure of a new material by using a laser beam and optics parts will be.

In general, the structure of a material is a direct factor influencing the physical properties required by the application environment. Therefore, if proper structural analysis is not accompanied, property control of the material is not properly performed, and thus a suitable material cannot be developed. For this reason, an optical microscope (OM), a scanning electron microscop (SEM), a transmission electron microscope (TEM), and the like have been developed and used.

However, these microscopes can observe the structure of a material from a few nanometers to several tens of micrometers, but most of the material's structure—here, only the qualitative knowledge of particle size or crystal size is known. In the case of a scanning electron microscope, since the material is used by cryogenical fracture, the material may be damaged and only the surface may be observed.

Accordingly, non-destructive and quantitative structural analysis apparatuses are being developed, and X-ray scattering and diffraction and Neuton scatterng are used in the submicrometer region.

However, the structure in the region of more than a submicrometer to several tens of micrometers is almost dependent on the optical microscope which is a qualitative method. Although the structure in this area, that is, the visible light region, is very important in the development of crystalline and optical materials, there was a problem that this quantified data could not be obtained.

The present invention has been made to solve the above problems.

Accordingly, an object of the present invention is a microstructure for new materials such as polymers, inorganic materials, and metals used in making blends or composites. SUMMARY OF THE INVENTION An object of the present invention is to provide a one-dimensional light scattering apparatus and a method of controlling the same, which can be analyzed non-destructively by using a laser (laser beam) and optical parts (Micro-structure).

As a technical means for achieving the above object, the one-dimensional light scattering device of the present invention comprises a laser device for generating a laser beam as a visual light source;

A neutral density filter for adjusting a predetermined output intensity of the laser beam from the laser device;

A polarizer for polarizing the laser beam through the neutral density filter;

A support for supporting the heating plate in a predetermined posture and position;

A heating plate on which the sample film is placed while being supported by the support;

Rotating plate for adjusting the behavior of the material according to the temperature;

A microstep motor for rotating the rotating plate under control of the host computer;

A temperature sensor for outputting temperature information of sensing the temperature of the heating plate to a screw terminal;

A power supply for supplying power to each device respectively;

An analyzer for controlling the polarization form of the scattered light through the sample film;

A photo multiplier tube for detecting the scattered light controlled by the analyzer and outputting the scattered light to a slew terminal;

A computer drive controlling an attitude and a position of the photomultiplier tube under the control of a host computer;

A silver controller for controlling the temperature of the heating plate according to the control of the host computer;

A screw terminal for amplifying the weak signal from the temperature sensor and the photomultiplier tube to a predetermined level and outputting the weak signal to the host computer;

A serial port for serial communication of data between the computer drive or the thermostat and a host computer;

An analog / digital board for converting an analog signal from the screw terminal into a digital signal;

It is characterized in that it comprises a host computer that controls the computer drive and temperature controller through the serial port, receives data from the analog / digital board, and processes and analyzes the data according to the embedded program.

The method of controlling a one-dimensional light scattering device comprising a laser device for generating the laser beam, a heating plate on which a sample film is placed, a photomultiplier tube for detecting scattered light, a plurality of accessory peripherals, and a host computer

A first step of operating the primary light source device and checking a state of each device;

A second step of accepting a selection of one of the flow point measuring mode and the particle size measuring mode after the first step;

A third step of receiving information about a sample and a measurement condition according to a built-in program corresponding to the selected mode, and accepting an experiment selection of an isothermal experiment and an elevated temperature experiment in the selected mode;

A fourth step of initializing the temperature controller after the specific experiment is selected in the third step, and initializing the microstep motor at a temperature corresponding to the start of the experiment after receiving a proper temperature for starting the specific experiment;

A fifth step of receiving a desired scattering angle, mounting a sample film on a hot stage, moving a detector to a measurement position, and collecting data on the mounted sample for a predetermined time;

In the sixth step, after the set time has elapsed, the sixth step of storing the collected data and performing data analysis according to a built-in program of the corresponding mode is performed.

Hereinafter, with reference to the accompanying drawings a preferred embodiment of the one-dimensional light scattering apparatus according to the present invention will be described.

3 is an overall configuration diagram of the one-dimensional light scattering device according to the present invention, wherein the one-dimensional light scattering device of the present invention comprises a laser device 1 for generating a laser beam as a light source for the entrance, and a laser beam from the laser device 1 A neutral density filter 2 for adjusting a predetermined output intensity of the light source, a polarizer 3 for polarizing a laser beam through the neutral density filter 2, and a heating plate 5 in a predetermined posture and position A support plate 4, a heating plate 5 on which the sample film 6 is placed while being supported by the support unit 4, a rotating plate 7 for adjusting the behavior according to the temperature of the material, and a host computer 18. To the microstep motor 8 for rotating the rotating plate 7 according to the control of the controller, a temperature sensor 9 for outputting temperature information of the temperature of the heating plate 5 to the screw terminal 15, and to each device. It consists of a power supply 10 for supplying each of the necessary power.

In addition, the analyzer 12 for controlling the polarization of the scattered light through the sample film, the photomultiplier tube 11 for detecting the scattered light controlled by the analyzer 12 and outputting to the screw terminal 15, and the host The computer 13 drives the position and position of the photomultiplier tube 11 under the control of the computer 18, and the temperature of the heating plate 5 under the control of the host computer 18. And a screw terminal 15 for amplifying a weak signal from the temperature controller 14, the temperature sensor 9 and the photomultiplier tube 11 to a predetermined level, and outputting the amplified signal to the host computer 18. A serial port 15 for serial communication between the computer drive 13 or the temperature controller 14 and the host computer 18, and an analog / digital signal for converting an analog signal from the screw terminal 15 into a digital signal. Digital Board ( 17) and control the computer drive 13 and the temperature controller 14 through the serial port 16, and receives data from the analog / digital board 17 to process and analyze according to the built-in program It comprises a host computer 18.

4 is a flow chart showing a control method of the one-dimensional light scattering device for measuring the flow point according to the present invention, Figure 5 is a flow chart showing a control method of the one-dimensional light scattering device for measuring the particle size according to the present invention, 6 is an exemplary graph showing a flow point measurement result according to the present invention. 7 is an exemplary graph showing particle size measurement results according to the present invention.

Thus, the operation and effect according to the present invention will be described in detail below based on the accompanying drawings.

FIG. 1 shows a schematic diagram of scattering angle-scattering intensity when two-dimensional scattering images of phase-separated material (a) and crystallized material (b) and one-dimensional slicing are performed. When scattering the phase-separated material, the scattered image (Scattered image) appears because the scattered light (Scattered light) is polarized in the same direction as the incident light (Incident light).

However, when scattering the crystallized material, the scattered image has the same polarization state as the incident light (Vv pattern) or polarization action due to the crystal alignment plane, resulting in a different polarization state. ) Is applied to data analysis.

Slicing is a one-dimensional light scattering device that provides scattering angle-scattering intensity data for each material and ultimately determines the size of the particles or crystals that make up the material from the scattering angle that represents the maximum scattering intensity. have.

In equations (1) and (2), q is the scattering vector, θ is the scattering angle, λ is the wavelength of incident light, and d is the size of the average particle.

2 shows a schematic diagram of the process of nonuniformity and change of scattering intensity due to the change of phase due to the change of time, composition and temperature. Therefore, one-dimensional light scattering devices can be used to investigate the starting point of a non-uniform structure (cloud point to normal point) from this scattering intensity change at a specific scattering angle. In general, when it is necessary to control the particle size or crystal size of the material, appropriate conditions can be found from the structural analysis data obtained by light scattering.

3 shows a hardware assembly drawing of the one-dimensional light scattering device. The incident light source mainly uses a helium-neon laser (1) having a wavelength of 632.8 mm, and when the laser output is strong, a neutral density filter is used to protect the detector and to prevent saturation of the scattered light. Filter) 2 is used. A polarizer 3 is attached to polarize the incident light, and an analyzer 12 is attached to control the polarization pattern of the scattered light, and the polarization is adjusted at a desired angle.

On the other hand, in order to establish the behavior according to the temperature of the material, the heating stage 5 and the supporting plate 4 should be installed, and the thermocouple 9 is attached to the heating stage. Program the desired temperature and snooze using a Temperature Controller (14). In this heating stage, the sample film 6 is properly positioned for each mode. The microstep motor (8), rotary table (7) and the control device Compumotor Driver / Indexer (113) to the desired scattering angle and scattering angle Let's "sweep".

Detection of the scattered light is to fix the highly sensitive Photomultiplier Tube (11) to the sweeping rod (sweeping rod) to detect the scattered light at each scattering angle (voltage within 10 Volt) ) Are digitized using an analog / digital board (17) and screw terminal (15). The Temperature Controller 14 and the Compumotor Driver / Indexer 13 control using RS 232C, a serial port built into the computer. All control and data storage and interpretation were configured to be a program (1DLS CON) written using the Turbo C language.

4 shows an algorithm for controlling and fixing a one-dimensional light scattering device in the case of cloud point measurement. First, preheat the host computer, detector, laser, etc. by turning it on to stabilize. Here, stabilization is performed by executing "Check !, c" in the configured program, and it is easy to find out the proper stabilization time by checking whether the Detect signal in the dark state changes.

After preheating the system, select "flow point measurement" in "measurement mode selection". Then, after inputting simple information about the sample to be measured and "Test Condition", the execution mode to be experimented is selected from the temperature rising or isothermal running mode.

Then initialize the "Temperature Controller" and enter the values of the temperature variables corresponding to the selected run. In the case of isothermal experiments, wait until the desired temperature is reached. In the case of elevated temperature experiments, wait until the start temperature ("Start" temperature) is reached. When the temperature is reached, the "Microstep Motor" is initialized, the desired scattering angle is input and the detector is moved.

The sample film is placed on a heating stage and starts receiving data. In this case, a graphic display may be used to monitor changes in scattered light. When the calculated time (in case of isothermal experiment) or final temperature (in case of elevated temperature experiment), data input and graph stop, and a message indicating the end of the experiment appears. Subsequently, the detector, which has moved to a specific scattering angle, returns to the origin (scattering angle = 0 degrees).

The stored "ASC11 TEXT / NUMBER DATA" is obtained through an off-line analysis to obtain a final "Cloud point".

5 shows the algorithm for controlling and measuring the one-dimensional light end device in the case of measuring the particle size. Preheating and stabilization are the same as the description with reference to FIG.

After the preheating of the system is completed, select "particle size measurement" in "selection of measurement mode". After inputting simple information about the sample to be measured and "Test Condition", the execution mode to be experimented is selected from the temperature rising or isothermal running mode.

Then initialize the "Temperature Controller" and enter the values of the temperature variables corresponding to the selected RUN. In the case of isothermal experiments, wait until the desired temperature is reached, and in the case of elevated temperature experiments, until the temperature reaches "Start".

When the temperature is reached, the "Microstep Motor" is initialized, the desired scattering angle is input, the sample is placed on the "Heating Stage", and the scattering light according to the scattering angle along with the movement of the detector. Start receiving data.

When the detector reaches the input scattering angle, it returns to the initial position (scattering angle = 0 degrees) to stop storing data. This detector's "sweeping" process of "Moving-Homing" is performed according to the programmed time interval, and the scattered light data according to the scattering angle is a graphic display (Graphic Disply) Is monitored.

When the calculated time (in the case of isothermal experiment) or the final temperature (in the case of elevated temperature experiment), the data and graphs stop, and a message indicating the end of the experiment appears. The stored "ASC11 TEXT / NUMBER DATA" is off-line analyzed to obtain the final "Particle size".

6 shows an example of performing a cloud point measurement using a one-dimensional light scattering device. In the case of isothermal and elevated temperature experiments, the graphs are similar in form, so an example of elevated temperature experiments is shown.

In the graphic display, the Y axis represents scattered light intensity and the X axis represents temperature change.

The information about the experiment is displayed in the lower left part of the graph, and the current measured temperature and the calculated temperature are displayed on the upper right side of the graph to check whether the temperature is well controlled. The number and duration of data, and the value of scattered light, are displayed numerically on the graph.

On the other hand, the "F1" key was set to "Hot Break" function in preparation for the safety and the accident of the experiment. Ultimately, the "Cloud Point" you want to know is the part where the value increases without the change of the scattered light intensity.

7 shows an example of measuring the particle size using a one-dimensional light scattering device. In the case of isothermal and elevated temperature experiments, the graphs are similar in form.

In addition, in the graphic display, the Y axis represents scattered light intensity and the X axis represents temperature change. The information about the experiment is shown in the lower left part of the graph, and the scattering angle and the intensity of the scattered light due to the sweep in the upper right part of the graph can be known numerically. The type of experiment (isothermal experiment), number of data, elapsed time and temperature are displayed numerically on the graph. The average size of the particles can be obtained by inserting the scattering angle at which the intensity of the scattered light is maximum into Equations (1) and (2).

As described above, the present invention provides a microstructure for new materials such as polymer, inorganic material, and metal used in making a blend or a composite material. By using (Micro-structure) laser beam and optical parts, there is a special effect that can be analyzed non-destructively.

The above description is only a description of one embodiment of the present invention, the present invention is capable of various changes and modifications within the scope of the configuration.

1 is an explanatory diagram showing scattering intensity according to scattering angle when two-dimensional image of scattered light and one-dimensional slicing of the image.

2 is an explanatory diagram showing the change of material structure and the scattering strength according to the change of external environment such as time, temperature and composition.

3 is an overall configuration diagram of a one-dimensional light scattering device according to the present invention.

Figure 4 is a flow chart showing a control method of the one-dimensional light scattering device for measuring the flow point in accordance with the present invention.

5 is a flowchart showing a control method of the one-dimensional light scattering device for measuring the particle size according to the present invention.

6 is an exemplary graph showing a flow point measurement result according to the present invention.

7 is an exemplary graph showing a particle size measurement results according to the present invention.

Explanation of symbols on the main parts of the drawings

1: laser device 2: neutral density filter

3: polarizer 4: support

5: heating plate 6: sample film

7: rotating plate 8: microstep motor

9: temperature sensor 10: power supply

11 Photomultiplier tube 12 Analyzer

13 computer drive 14 temperature controller

15 SCURU terminal 16: Serial port

17: analog / digital board 18: host computer

19: Cleaning direction

Claims (2)

A laser device 1 for generating a laser beam as a light source of entrance; A neutral density filter (2) for adjusting a predetermined output intensity of the laser beam from the laser device (1); A polarizer (3) for polarizing the laser beam through the neutral density filter (2); A support (4) for supporting the heating plate (5) in a predetermined posture and position; A heating plate 5 supported by the support 4 on which the sample film 6 is placed; A rotating plate 7 for adjusting the behavior according to the temperature of the material; A microstep motor 8 for rotating the rotating plate 7 under the control of the host computer 18; A temperature sensor 9 for outputting temperature information of the temperature of the heating plate 5 to the screw terminal 15; A power supply 10 for supplying power to each device respectively; An analyzer 12 for controlling the polarization pattern of the scattered light through the sample film; A photomultiplier tube 11 for detecting the scattered light controlled by the analyzer 12 and outputting the scattered light to the screw terminal 15; A computer drive 13 for adjusting the posture and the position of the photomultiplier tube 11 under the control of a host computer 18; A temperature controller (14) for controlling the temperature of the heating plate (5) under the control of the host computer (18); A screw terminal (15) for amplifying a weak signal from the temperature sensor (9) and the photomultiplier tube (11) to a predetermined level and outputting the signal to the host computer (18); A serial port 16 for serial communication of data between the computer drive 13 or the temperature controller 14 and the host computer 18; An analog / digital board 17 for converting an analog signal from the screw terminal 15 into a digital signal; The host computer 18 controls the computer drive 13 and the temperature controller 14 through the serial port 16, receives data from the analog / digital board 17, and processes and analyzes the data according to an embedded program. 1D light scattering device characterized in that it comprises a). A laser device 1 for generating a laser beam, a heating plate 5 on which the sample film 6 is placed, a photomultiplier tube 11 for detecting scattered light, a plurality of accessory peripherals and a host computer 18 The control method of the one-dimensional light scattering apparatus comprising A first step of operating the primary light source device and checking a state of each device; A second step of accepting a selection of one of the flow point measuring mode and the particle size measuring mode after the first step; A third step of receiving information about a sample and a measurement condition according to a built-in program corresponding to the selected mode, and accepting an experiment selection of an isothermal experiment and an elevated temperature experiment in the selected mode; A fourth step of initializing the temperature controller after the specific experiment is selected in the third step, and initializing the microstep motor at a temperature corresponding to the start of the experiment after receiving a proper temperature for starting the specific experiment; A fifth step of receiving a desired scattering angle, mounting a sample film on a hot stage, moving a detector to a measurement position, and collecting data on the mounted sample for a predetermined time; And a sixth step of storing the collected data and performing data analysis according to a program of a corresponding mode embedded therein after the set time has elapsed in the sixth step.