JPH0833341B2 - Simple container type crystal observation device - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a simple container type crystal observing apparatus, and in particular, to a crystal shape, a growth process, a annihilation process, etc. of a crystal under a pressure load condition, especially under high pressure. The present invention relates to a simple container type crystal observing device for observing physical changes.

(Prior Art) It is extremely important to understand the physical change of the crystal such as the shape of the crystal, the growth process, the annihilation process under the pressure load when manufacturing or using a chemical substance under pressure.

For example, in the pressure crystallization method, which is attracting attention as a technique for separating and purifying a target component from a mixture, it is an essential requirement to grasp the physical change of the crystal as described above. The pressure crystallization method is a separation and purification technique in which crystals of a target component are separated from other components and precipitated from a liquid or slurry mixture by the action of high pressure to obtain a high-purity product. Because there is. That is, it is necessary that the pressure for crystallizing / growing the crystal and the pressure condition for forming a good crystal are known in advance.

In order to understand the physical change of the crystal under such pressure load condition, the crystal observation under pressure is performed.

FIG. 3 shows a typical example of a simple container type crystal observing apparatus (simple container type optical cell) which has been conventionally used for observing crystals under the pressure as described above. As shown in this figure, the conventional simple container type crystal observing apparatus has a pressure resistant simple container (3) having optical windows (1) and (2) made of light transmissive bodies on opposite side views, and the pressure resistant simple container (3). A simple container type crystal observation device having a pressure increasing means (4) for increasing the pressure in the simple container is used. A pipe (5) for injecting a sample (observation target) is connected to the pressure increasing means (4). The pressure increasing means (4) and the pressure resistant simple container (3) are connected by pressure resistant piping (6). The pressure in the container (3) is measured by a pressure gauge (19) of any type connected to the pressure resistant pipe (6).

Crystal observation by this simple container type crystal observation apparatus is performed as follows. That is, the sample is injected from the pipe (5) into the pressure increasing means (4) and filled in the sample chamber (7) of the pressure resistant simple container (3) through the pressure resistant pipe (6). on the other hand,
The light source (8) illuminates the optical window (2) with light.

In this way, light passes through the optical window (2) and irradiates the sample, so that the state of the sample can be observed from outside the optical window (1). This observation is done with the naked eye or by a microscope.

Next, the pressure increasing means (4) pressurizes the sample in the pressure resistant simple container, that is, the sample chamber (7), and observes the state of the sample. As crystallization progresses with the progress of pressurization,
Observe the crystal shape and growth process under pressure. Also, the pressure is reduced to observe the disappearance process of crystals.

(Problems to be Solved by the Invention) However, the conventional simple container type crystal observing apparatus as described above has various problems as described below.

That is, since the sample is injected into the pressure increasing means and filled in the pressure resistant simple container through the pressure resistant pipe, there is a problem that a large amount of sample is required. That is, at least an amount capable of filling all of the pressure increasing means, the pressure resistant piping and the pressure resistant simple container is necessary.

Of course, the samples for crystal observation are often new substances,
In that case, it is difficult to make a large amount of sample. In addition, even if it is not a new substance, there are cases where there is only a small amount of sample. Therefore, requiring a large amount of sample as described above is a very serious problem.

Further, the pressure resistant pipe has a small inner diameter in order to ensure the pressure resistance, and particularly for high pressure, it is extremely thin. Therefore, when the sample is a solid, the sample cannot be injected into the pressure resistant simple container. In the case of a slurry containing solids, there is a drawback that it is extremely difficult to inject a sample because of its high viscosity.

In particular, when the melting point of the sample is relatively high, a slight temperature decrease during or after the injection of the sample in the liquid state,
Alternatively, the increase in pressure causes the sample to solidify in the pressure-resistant pipe or the like, resulting in blockage in the pipe. As a result, even if the pressure is increased by the pressure increasing means, the pressure is not transmitted, so that the sample in the pressure resistant simple container cannot be adjusted to a predetermined pressure. There is also a problem that it becomes difficult to measure the accurate pressure of the sample.

In order to prevent the solidification, it is sufficient to heat the pressure resistant pipe or the like, but the sample to be observed may be overheated. In this case, the physical properties change depending on the sample, and accurate crystal observation cannot be performed. Therefore, the above heating is extremely difficult because it is necessary to perform strict temperature control so as not to overheat the sample to be observed. or,
The pressure gauge may also be heated, and accurate pressure measurement may not be possible.

Furthermore, after observation, it is necessary to completely clean the inside of the pressure increasing means, the pressure resistant simple container and the pressure resistant piping before injecting the next observation sample, but since there are many cleaning parts, it takes a long time. It costs. In particular, since the inside of the pressure resistant pipe has a small diameter, complete cleaning is not easy and it takes a very long time. Further, since the final stage of the cleaning is performed using the next observation sample as the cleaning liquid, there is a problem that a large amount of the sample is required.

The present invention has been made by paying attention to such a situation, and its purpose is to solve the above-mentioned problems of the conventional crystal observation apparatus (simple container type crystal observation apparatus) and to reduce the amount of sample. Well, the sample can be placed on the simple container type crystal observation device relatively easily and in a short time, the pressure of the sample can be constantly adjusted to the predetermined value, and the sample temperature can be set to the predetermined temperature without heating the pressure resistant piping. An object of the present invention is to provide a simple container type crystal observing device which can be held and which can relatively easily perform complete cleaning of the simple container type crystal observing device.

In addition to the above, the conventional simple container type crystal observation device is
As shown in the figure, the optical window is cylindrical and the optical window pedestal is flat, so that the thickness from the optical window lower surface (or upper surface) to the optical window pedestal upper surface (or lower surface) is increased in order to provide pressure resistance. It is relatively large. Therefore, the distance between the microscope and the sample becomes relatively large, so the microscope magnification cannot be increased,
Therefore, the crystal cannot be seen in a large scale. Therefore, it was an issue to make the microscope magnification higher.

(Means for Solving the Problems) In order to achieve the above object, the present invention provides a simple container type crystal observing apparatus having the following configuration.

That is, the simple container type crystal observing device according to claim 1 is a pressure resistant simple container having an optical window made of a light-transmitting body on a side surface thereof, and a pressure increasing medium for increasing the pressure of a fluid pressure medium in the pressure resistant simple container. A simple container type crystal observing device having a pressure means, wherein the pressure resistant simple container is formed of a stretchable small container and the optical window, and a sample is sealed, via the fluid pressure medium. A simple container type crystal observation apparatus is characterized in that a sample chamber pressurized by the pressure increasing means is arranged.

A simple container type crystal observing apparatus according to claim 2, wherein a pressure resistant simple container having an optical window made of a light-transmitting body on a side surface thereof, and a pressure increasing means for increasing the pressure of the fluid pressure medium in the pressure resistant simple container. A simple container type crystal observation device having
The pressure-resistant simple container is formed of a stretchable small container in which a light-transmissive window is provided on at least a side surface facing the optical window, and a sample is sealed, and the pressure boosting is performed via the fluid pressure medium. It is a simple container type crystal observation device characterized in that a sample chamber pressurized by means is arranged.

In the simple container type crystal observing apparatus according to claim 3, the optical window is a hemispherical body, and the circular surface of the bottom portion of the hemispherical body is arranged to face the pressure resistant simple container. The simple container type crystal observation apparatus described in 1.

(Operation) As described above, the simple container type crystal observing apparatus according to the present invention (the crystal observing apparatus according to claim 1) includes a pressure resistant simple container having an optical window made of a light-transmitting body on a side surface thereof. A simple container type crystal observing device having a pressure increasing means for increasing the pressure of a fluid pressure medium in the pressure resistant simple container, wherein the elastic small container and the optical window are provided in the pressure resistant simple container. The sample chamber is formed and sealed with the sample, and the sample chamber is pressurized by the pressure increasing means via the fluid pressure medium. That is, in a pressure-resistant simple container having an optical window made of a light-transmitting body on the side surface, a sample chamber formed of a stretchable small container and the optical window, and a sample is sealed,
The sample chamber pressurized by the pressure increasing means is arranged via the fluid pressure medium.

Therefore, the pressure increasing means can pressurize the sample chamber through the fluid pressure medium, and when such pressurization is performed, the small container forming a part of the sample chamber has elasticity. , The pressure in the sample chamber may be equal to the pressure of the fluid pressure medium. That is, when the fluid pressure medium is injected into the pressure resistant simple container through the pressure resistant pipe by the pressure increasing means and then the fluid pressure medium is pressurized to a predetermined pressure, the small container in the sample chamber has elasticity. Therefore, the pressure in the sample chamber can be equal to the pressure of the fluid pressure medium. Therefore, the sample in the sample chamber can be pressurized to the predetermined pressure. Further, for the same reason as above, even when the pressure is reduced to a predetermined pressure after pressurization, the sample can be reduced to the predetermined pressure.

On the other hand, since the optical window forming the sample chamber (hereinafter referred to as the optical window A) has a light-transmitting property, when the light is irradiated from the outside of the optical window A toward the sample chamber, the state of the sample is observed. You can In addition to the optical window A, an optical window (hereinafter referred to as another optical window) can be provided on the side surface of the pressure resistant simple container.
In this case, if the small container is made entirely light-transmissive, or if at least a side surface facing the other optical window is provided with a light-transmissive window, light is transmitted through the optical window A (or other optical window). And the sample can be observed from the other optical window (or optical window A).

Further, as described above, since the sample is sealed in the sample chamber, the sample is not contaminated by the fluid pressure medium and the predetermined purity of the sample can be maintained.

Therefore, the sample state under a predetermined pressure can be observed without contaminating the sample.

Regarding the required amount of the sample, the volume of the sample chamber is naturally smaller than the volume of the pressure-resistant simple container, so that the sample may be extremely small compared with the case of the conventional simple container type crystal observing apparatus described above. Moreover, the volume of the sample can be very small if the volume of the sample chamber is set to the minimum necessary.

The sample can be placed in the simple container type crystal observing device by placing the sample in a small container outside the pressure resistant simple container and then incorporating the sample in the pressure resistant simple container. Therefore, even in the case of a solid or slurry-like sample which has been a problem in the conventional injection method, the sample can be arranged in a short time like a liquid.

Further, when the melting point of the sample is high, it is possible to solve the problem that the sample is solidified in the pressure resistant pipe or the like to be clogged and the sample cannot be adjusted to a predetermined pressure. This is because the sample is in the sample chamber, while a pressure medium that is hard to solidify can be used in the pressure resistant pipe and the like. Further, since the solidification is prevented in this way, the accurate pressure of the sample can be measured, and the heating of the pressure resistant pipe becomes unnecessary. Therefore, there is no concern that the physical properties of the sample will change due to heating, and the accuracy of the pressure gauge will not deteriorate due to heating.

Further, since the sample is sealed in the sample chamber formed by the small container and the optical window A, the cleaning before the injection of the next sample for observation may be performed on the optical window A and the small container. If the small container is replaced, only the optical window A needs to be washed. Therefore, cleaning is relatively easy and can be performed in a short time.

As described above, the simple container type crystal observing device according to claim 2 has a pressure-resistant simple container having an optical window made of a light-transmitting body on a side surface thereof, and at least a light-transmitting window on a side surface facing the optical window. A sample chamber, which is formed by the elastic small container provided and in which the sample is sealed, is arranged to be pressurized by the pressure increasing means via the fluid pressure medium.

With this configuration, the same operation and effect as those of the device according to the first aspect can be obtained. In addition, since the sample is sealed in the sample chamber formed by only the small container, the cleaning before the next injection of the sample for observation may be performed only on the small container. , The cleaning time can always be shortened. Further, if the small container is replaced, it becomes unnecessary to wash. When light is irradiated from outside the optical window of the pressure resistant simple container (hereinafter referred to as optical window B) toward the sample chamber, the light passes through the optical window B and the light transmissive window of the small container. Upon hitting the sample, the sample state can be observed through the optical window B. In addition to the optical window B, an optical window can be provided on the side surface of the pressure resistant simple container. In this case, if the small container is made entirely light-transmissive, or if a light-transmissive window is also provided on the side surface facing another optical window, the optical window B (or another optical window) The sample can be observed through another optical window (or optical window B).

Incidentally, in the simple container type crystal observation apparatus according to the present invention,
With respect to the material and shape of the optical window, any material can be used as long as it has optical transparency and required strength, and for example, hemispherical or cylindrical sapphire, hard glass, hard plastic, etc. can be used. However, the optical window is hemispherical,
It is desirable that the circular surface at the bottom of the hemispherical body is arranged so as to face the pressure-resistant simple container. By doing so, it becomes possible to make the thickness from the lower surface (or upper surface) of the optical window to the upper surface (or lower surface) of the optical window pedestal necessary for providing the required compressive strength relatively small. This is because the distance between and can be made relatively short, and the microscope magnification can be increased. That is, it becomes possible to see the crystal greatly enlarged.

With respect to the stretchable small container, not all the parts of the small container need to be stretchable, and it is sufficient that each of the stretchable small containers has stretchability in the necessary portion, and as a result, the small container can stretch. For example, the one as shown in FIG. 2 can be used. That is, FIG. 2 is a view showing a sample chamber formed by a small container having a bottomed cylindrical shape and a cylindrical light-transmissive window (16). As shown in FIG. A small container is constituted by 17) and a light-transmissive bottom member (18) joined to the cylindrical body (17). This small container expands and contracts in the cylindrical body (17) according to the external pressure. The bottom member (18) may be non-light transmissive.

The small container according to the second aspect of the invention is required to have the light-transmissive window as described above in addition to the elasticity as described above, but it is not necessary to make the whole light-transmissive. For example, as shown in FIG. 4, the bottom member (18) is joined to the lower part of the elastic cylindrical body (17), and the upper part (side surface facing the optical window B) is provided with a light-transmissive disc (as a light-transmissive disc). It may be a combination of 20). The bottom member (18) and the cylindrical body (17) may be light transmissive or non-light transmissive.

The material of the stretchable portion may be, for example, silicone rubber or polyethylene, and is not particularly limited as long as it has stretchability. Further, in the case of the device according to claim 1, the shape of the small container may be, for example, a shallow rectangular parallelepiped with a flange, a hemispherical shape, or the like, or a part having a bellows may be used. In the case of the described device, a rectangular parallelepiped or a spherical device can be used, and the device is not particularly limited.

(Example) Example 1 FIG. 1 shows a partially cutaway side view of a simple container type crystal observation apparatus according to Example 1. As shown in FIG. 1, this device has a pressure resistant simple container (3) part, a pressure increasing means (4) part for increasing the pressure in the container (3), and a pressure resistant property for connecting both of them. It consists of a pipe (6) part.

A pipe (5) for injecting a fluid pressure medium is connected to the pressure increasing means (4).

Regarding the pressure-resistant simple container (3), (1) and (2) are sapphire optical windows provided on opposite side surfaces of the container (3). Both of the optical windows (1) and (2) are hemispherical bodies, and are arranged so that the circular surface of the bottom of the hemispherical body faces the pressure-resistant simple container. The optical windows (1) and (2) are supported by an optical window pedestal (12), and the pedestal (12) is screwed to a pressure resistant simple container (14). (13) is a seal member (O
Ring). The central portion of the spherical surface of the hemispherical body and its vicinity are flat. The reason for flattening is that the sample becomes more clearly observed.

(10) is a stretchable small container (small container made of silicone rubber) having light transmittance as a whole, and its flange portion is fixed to the end of the optical window (1) and its vicinity by a small container holder (11). Has been done. As a result, an airtight sample chamber (9) is formed by the small container (10) and the optical window (1). A sample is sealed in the sample chamber (9). In addition, in the figure (1
9) is a pressure gauge.

Crystal observation was performed as follows using such a crystal observation apparatus. That is, the fluid pressure medium is increased in pressure increasing means (4).
And the inside (7) of the pressure resistant simple container (3) is filled through the pressure resistant pipe (6). Meanwhile, the optical window (2) was irradiated with light from the light source (8) to start observation of the state of the sample. This observation was performed by an optical microscope (not shown) arranged outside the optical window (1).

Then, the fluid pressure medium (1
5) was pressed to pressurize the sample. This way,
It was observed that the small container gradually contracted as the pressurization proceeded. Further, when crystals were observed to be precipitated from the liquid sample and the deposition pressure was measured, the measured values were similar to those measured by the conventional method (method by the conventional simple container type crystal observing device).

Example 2 A different point from Example 1 is that the optical window is only (1) and does not have the optical window (2), and that the elastic small container (10) does not have light transmittance. The light source (8) arranged outside the optical window (1) radiated light, and the state of the sample was observed by a reflection type optical microscope arranged outside the optical window (1). Others are the same as in the first embodiment. As a result, the same crystal observation as in Example 1 could be performed, and the same deposition pressure value was obtained.

Example 3 FIG. 5 shows a partially cutaway side view of a simple container type crystal observation apparatus according to Example 3. As shown in FIG. 5, the difference from the first embodiment is that the optical window of the device is only (1), and the sample chamber (9) is a stretchable small container (10) having a light transmitting property as a whole. The light source (8) arranged outside the optical window (1) irradiates light, and the sample state is observed by a reflection type optical microscope arranged outside the optical window (1). It is a thing. Others are the same as in the first embodiment. As a result, the same crystal observation as in Example 1 could be performed.

(Effects of the Invention) According to the simple container type crystal observing apparatus of the present invention, a small amount of sample is required as compared with the conventional simple container type crystal observing apparatus, and the sample can be arranged in the simple container type crystal observing apparatus. It is relatively easy and can be done in a short time, the pressure of the sample can always be adjusted to a predetermined value, and the sample temperature can be maintained at a predetermined temperature without the need for heating the pressure resistant piping. Complete cleaning can be made relatively easy.

In addition to the above, there is also an effect that the distance between the microscope for observation and the sample can be shortened, and the microscope magnification (observation magnification) can be increased.

[Brief description of drawings]

FIG. 1 is a partially cutaway side view of a simple container type crystal observing apparatus according to Example 1, FIG. 2 is a view showing a sample chamber formed by a bottomed cylindrical small container and a cylindrical optical window, and FIG. FIG. 4 is a side view showing a typical example of a conventional simple container type crystal observing device, FIG. 4 is a view showing an example of a small container, and FIG. 5 is a partially broken side view of the simple container type crystal observing device according to Example 3. It is a figure. (1), (2) ... optical window, (3) ... pressure resistant simple container, (4) ... pressure increasing means, (5) ... piping, (6) ...
Pressure resistant piping, (7) …… Sample chamber of pressure resistant simple container,
(8) …… Light source, (9) …… Sample chamber, (10) …… Small container, (11) …… Small container holder, (12) …… Optical window pedestal,
(13) …… Seal member, (14) …… Pressure-proof simple container, (1
5) …… Pressure medium, (16) …… Cylindrical light-transmissive window, (1
7) ...... Stretchable cylinder, (18) ...... Light transmissive bottom member, (19) ...... Pressure gauge, (20) ...... Light transmissive disc.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-1-99014 (JP, A) Actual development Sho 53-153981 (JP, U)

Claims (3)

[Claims] 1. A simple container type crystal observing apparatus having a pressure resistant simple container having an optical window made of a light transmitting body on its side surface, and a pressure increasing means for increasing the pressure of a fluid pressure medium in the pressure resistant simple container. In the pressure-resistant simple container, the sample is formed of a stretchable small container and the optical window, and the sample is sealed and pressurized by the pressure increasing means via the fluid pressure medium. A simple container-type crystal observation device characterized by arranging a chamber. 2. Crystal observation of a simple container type having a pressure-resistant simple container having an optical window made of a light-transmitting body on a side surface thereof, and a pressure increasing means for increasing the pressure of a fluid pressure medium in the pressure-resistant simple container. A device, which is formed of a stretchable small container in which a light-transmissive window is provided on at least a side surface facing the optical window in the pressure-resistant simple container, and a sample is sealed to store the fluid pressure medium. A simple container type crystal observing device characterized in that a sample chamber pressurized by the pressure increasing means is arranged via the pressure increasing means. 3. The simple container type crystal observing apparatus according to claim 1, wherein the optical window is in a hemispherical state, and the circular surface of the bottom of the hemispherical body is arranged to face the pressure resistant simple container. .