JP3261339B2 - Pore distribution measuring device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention belongs to the technical field of a pore distribution measuring device for measuring the distribution of a porous sheet or the like.

[0002]

The pore distribution in the membrane has been conventionally determined by a gas adsorption method utilizing the adsorption temperature curve of helium nitrogen gas in the sample pore, a mercury intrusion method in which mercury is injected into the sample pore, There is a method of directly observing the pores with an optical electron microscope, but the operation for the measurement and the data processing for obtaining the distribution are troublesome, all of which require a long time for the measurement, and the measurement is quick. Was impossible. In addition, those which were formed inside the film and did not appear on the surface (voids) could not be measured.

[0003] On the other hand, in a normal scattering type particle size distribution meter, scattering due to macro distortion or scratches on the film, and the scattered light and reflected light of the film surface itself are much larger than the scattered light of the pore distribution. The distribution information was hidden and measurement was not possible.

[0004] The present invention has been made in view of such circumstances,
It is an object of the present invention to provide a pore distribution measuring device capable of quickly and accurately measuring pore distribution in a membrane even if it does not appear on the surface.

[0005]

According to the present invention, means for solving the above-mentioned problems are constituted as follows. That is, in the invention described in claim 1, the film to be measured sandwiched between the pair of light-transmissive parallel flat plates is irradiated from the light source to the film to be measured .
It is characterized by irradiating light , measuring the intensity distribution of scattered light generated by the pores of the film, and calculating the pore distribution based on the measurement result, thereby obtaining the pore distribution of the film. I have.

According to the second aspect of the present invention, the film to be measured contained in a container made of a translucent material is
The film is immersed in a liquid having a refractive index substantially equal to the material of the film, and the film is irradiated with light from a light source, and the intensity distribution of scattered light generated by the pores of the film is measured. It is characterized in that the pore distribution of the membrane is obtained by calculating the pore distribution based on the calculated pore distribution.

The sample can be fixed straight by sandwiching the sample film itself between two parallel flat plates, and when the film itself is greatly contaminated or distorted or when the film is thick, the material of the film is almost the same. By immersing in a liquid having the same light refractive index, reflection and scattered light from the film surface can be reduced.

On the other hand, by performing calculations based on the measurement results in accordance with a calculation program using a conversion coefficient matrix which is set and stored in advance, the pore distribution of the membrane can be obtained in a short time.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an embodiment of the pore distribution measuring device of the present invention will be described in detail. FIG. 1 shows the entire configuration of the apparatus. Reference numeral 1 denotes a light source such as a laser light source for generating parallel light, reference numerals 2 and 3 denote reflecting mirrors, 4 denotes a beam expander, 5 denotes a sample holding device, and 6 (6 _1). To 6 _n ) are scattered light detectors including a condenser lens and a photodiode, and 7.
Is a condenser lens, 8 is an array type detector, 9 is a multiplexer, 10 is an AD converter, 11 is an input / output unit, and 12 is a CPU.

The above-mentioned sample holding means 5 is provided in FIGS.
In the sample holding means 5 shown in FIG. 2, a film (or sheet) S serving as a sample is sandwiched between two flat plates 51 and 52 made of a translucent material. 531
Bolts 54, 55 provided on a frame 53 having
By sandwiching the sample 51 and 52 from both sides of the sample S, the sample S can be fixed straight, and the occurrence of reflection and scattering from the film surface can be easily suppressed. is there. When the frame 53 is formed of a translucent material, the opening 531 and one of the flat plates 51 can be omitted. Further, when a separate holder is provided in the measuring apparatus, a film S serving as a sample may be sandwiched between the two flat plates 51 and 52 (see FIG. 4).

In the sample holding means 5 shown in FIG. 3, a container having a thin rectangular shape and an open top is made of a transparent material such as a film or glass.
56 is formed, the film S is inserted into the internal space 57, and a liquid having the same optical refractive index as the film S is injected into the internal space 57 so that the film S is immersed in the liquid. By immersion in such a liquid, the film S
Reflection and scattered light from the surface can be more effectively reduced. In the case where the film S is thick, although not shown, the film S is placed in a cell containing a liquid having the same optical refractive index as the film S.
And the scattered light can be measured.

The film S held by the sample holding means 5 as described above is irradiated with parallel light from the light source 1 and scattered light scattered from pores in the film S is collected by a condenser lens 7 and an array type detector. The intensity distribution of the scattered light is measured by the scattered light detector 6 and the scattered light detector 6 disposed therearound. On the other hand, the CPU 12 has a film S
A calculation program using a conversion coefficient matrix for converting from the uniform data of the pore distribution obtained from these scattered light intensities to the pore distribution is set and stored, and the measured value of the intensity distribution of the scattered light described above is stored. It is possible to calculate and calculate the pore distribution based on the information at once. According to such a pore size distribution measuring device, light is also radiated to vacancies existing inside the film S that does not appear on the surface, causing scattering, so that these can also be detected.

On the other hand, unnecessary scattered light may be detected due to distortion or scratches of the film itself. In such a case, when the pore distribution calculation is performed, the data of the target minute pore distribution is large. The scattering angle data used in the pore distribution calculation is selected so as not to be hidden by the pore data. For example, a pore distribution of several μm or less was determined,
When the flaw m is detected, the pore distribution calculation is performed only on the scattered light data of ten degrees or more, and information such as the flaw on the film S is used as noise so as not to use unnecessary data. to erase.

[0014]

As described above, according to the pore distribution measuring apparatus of the present invention, a non-self-supporting film is sandwiched between translucent parallel flat plates and fixed straight, and the film is fixed to the film from a light source. of
By irradiation with light to measure the intensity distribution of scattered light generated by the pores of the membrane, since obtaining the pore distribution from the particle size distribution obtained on the basis of the measurement result, without performing troublesome pretreatment, Further, it is possible to easily and quickly measure the pore distribution of the membrane even if it does not appear on the surface without using consumable articles.

Further, by immersing a film to be measured contained in a container made of a translucent material in a liquid having a refractive index substantially equal to the material of the film and measuring the film, contamination and distortion of the film itself can be achieved. Is large, reflected light and scattered light from the film surface can be reduced.

[Brief description of the drawings]

FIG. 1 is a configuration diagram showing one embodiment of a pore distribution measuring device of the present invention.

FIG. 2 is a sectional view showing an example of the sample holding device.

FIG. 3 is a perspective view showing another example of the sample holding device.

FIG. 4 is a perspective view showing another example of the sample holding device.

[Explanation of symbols]

 1: light source, 51, 52: parallel plate, 56: container, S: film.

Claims (2)

(57) [Claims] A film to be measured sandwiched between a pair of light-transmitting parallel flat plates is irradiated with light from a light source,
A pore distribution measuring device for measuring the intensity distribution of the scattered light generated by the pores of the film and calculating the pore distribution based on the measurement result to obtain the pore distribution of the film. . 2. A film to be measured contained in a container made of a translucent material is immersed in a liquid having a refractive index substantially equal to the material of the film, and the film is irradiated with light from a light source. Measuring the intensity distribution of the scattered light generated by the pores of the film, and calculating the pore distribution based on the measurement result, thereby obtaining the pore distribution of the film. Distribution measuring device.