JP2655917B2 - Crystal observation device - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a crystal observation apparatus, and more particularly, to a physical change of a crystal such as a crystal shape, a growth process, and an annihilation process under a pressure load condition, particularly under high pressure. The present invention relates to a crystal observation device for observing.

(Prior Art) It is extremely important to understand physical changes of a crystal such as a crystal shape, a growth process and an annihilation process under a pressure load condition when producing or using a chemical substance under pressure.
For example, in a pressure crystallization method, which is attracting attention as a separation and purification technique for precipitating a crystal of a target component from a mixture by high-pressure action to obtain a high-purity product, it is necessary to grasp the pressure conditions for crystal precipitation and growth in advance. This is a mandatory requirement.

In order to grasp the physical change of the crystal, a crystal observation under pressure is performed. A typical example of a conventional crystal observation apparatus used for the crystal observation is shown in FIG. 3 and will be described below with reference to FIG.

As shown in FIG. 3, the conventional crystal observation apparatus comprises a pressure-resistant container (3) having optical windows (1) and (2) made of a light transmitting body on opposite sides, and a container (3) provided with a pipe (6). And (3) a pressure increasing means (4) for increasing the pressure of the object to be observed (sample) in the container (7). The pressure of the sample is measured by a pressure gauge (19) arranged in the pipe (6).

The crystal observation by the above apparatus is performed as follows. First, a sample is injected from the pipe (5) into the pressure intensifying means (4), and filled in the pressure-resistant container (7) and the pipe (6) via the pipe (6). On the other hand, the sample is irradiated with light from the light source (8) through the optical window (2). In this way, the sample can be observed from outside the optical window (1) with the naked eye or a microscope.

Next, the sample in the container (7) is pressurized by the pressure increasing means (4) to observe the crystal shape, the growth process, and the like, and the pressure is reduced to observe the crystal extinction process.

(Problems to be Solved by the Invention) However, the above-mentioned conventional crystal observation apparatus has a problem that a large amount of the sample is required because the sample is filled as described above. Since the inside diameter is extremely small, there is a problem that a solid sample cannot be injected, and a high viscosity slurry sample is extremely difficult to be injected. In the case of a high melting point sample, a slight temperature decrease or pressure increase solidifies the sample in the pipe (6) and causes blockage in the pipe. In addition, there is a problem that accurate pressure measurement cannot be performed. Furthermore, when cleaning the inside of the apparatus after the observation and before the next sample injection, a pipe having a large number of cleaning portions and a small diameter (6)
There is also a problem that it takes a very long time because it is difficult to clean the inside.

In order to solve the above problems, the inventors of the present invention have repeated studies and have developed a pressure-resistant container of the above-mentioned conventional apparatus in which a sample chamber having further elasticity and light transmission is additionally provided (Japanese Patent Application No. 1-49074).
FIG. 2 shows an example of the development apparatus, and a typical example of a crystal observation method using the apparatus will be described below. First, a small sample chamber (10) in which a sample (9) is sealed is placed in a pressure-resistant container (7). Next, a pressure medium is injected into the container (3) through the pipe (6) by the pressurizing means (4), and when the pressure medium is pressurized to a predetermined pressure, the sample chamber (10) expands and contracts. Sample (9)
Is pressurized to a predetermined pressure. On the other hand, when light is emitted from the optical window (2) to the sample chamber (10) by the light source (8), the light illuminates the sample (9), and the state of the sample is observed from outside the optical window (1).

As described above, the above-described development apparatus can observe crystals under pressure under a small amount of the sample (9) sealed in the small sample chamber (10). Can be resolved. The pressure medium for pressurizing the sample chamber (10) is injected into the container (7) and the pipe (6) as described above instead of the sample in the case of the conventional apparatus. As a result, the problems such as blockage in the tube (6) and corrosion of the sample chamber (10) due to the medium do not arise newly. This is because a medium that does not cause such blockage or corrosion can be selectively used as the medium.

However, since the pressure medium is filled in the container (7) and the pipe (6), a large amount of the pressure medium is required in the same manner as a large amount of the sample is required in the conventional apparatus. Capacity) and a long time for pressurization / decompression. In addition, there is a possibility that the pressure medium may leak at the connection portion of the pipe (6), and there is a problem that maintenance for the leak is required. In addition to the demand for solving these problems, it is desired to further reduce the size of the crystal observation apparatus as a whole.

The present invention has been made in view of such circumstances, and its object is to solve all the problems with the conventional device as well as the above-mentioned development device, and at the same time, to solve the above problems, An object of the present invention is to provide a crystal observation apparatus in which the amount of the pressure medium can be reduced, the capacity of the pressure means can be reduced, or the pressure / decompression time can be shortened, and the possibility of leakage of the pressure medium is small. Things. Another object is to make the apparatus compact.

(Means for Solving the Problems) In order to achieve the above object, the present invention provides a crystal observation apparatus having the following configuration. That is, the crystal observation apparatus according to the present invention includes a pressure-resistant container having an optical window made of a light-transmitting body on a side surface, an elastic sample chamber disposed in the pressure-resistant container, What is claimed is: 1. A crystal observation apparatus comprising: a pressurizing means for a pressure medium for increasing a pressure, wherein said pressurizing means fits into a through hole provided in a side wall with easy pressure resistance and an inner peripheral portion of said through hole. A crystal observation device comprising a piston that moves forward and backward together and a drive mechanism that moves the piston forward and backward. In other words, this is a crystal observation apparatus using the pressurizing means configured as described above, instead of the pressurizing means of the development apparatus.

(Operation) As described above, the crystal observation apparatus according to the present invention
Instead of the pressurizing means of the development device, a pressurizing means configured as described above (hereinafter, referred to as a pressurizing means according to the present invention) is used. The pressurizing means according to the present invention comprises a through-hole provided in the side wall of the pressure-resistant container as described above, a piston fitted to the inner peripheral portion of the through-hole to advance and retreat, and a drive mechanism to advance and retreat the piston It is composed of

The pressurizing means according to the present invention can be used by injecting a pressure medium into the pressure-resistant container and the through-hole and using the piston by moving the piston forward and backward by the drive mechanism. The sample chamber can be expanded and contracted to pressurize the sample. When the piston is withdrawn after the pressurization, the pressure can be reduced. Other than the pressurizing means, it is the same as the case of the development device. Therefore, the crystal observation apparatus according to the present invention can solve all the problems of the conventional apparatus as in the development apparatus.

As described above, the pressure medium is injected into the pressure-resistant container and the through-hole, and only those portions need to be filled, so that the required amount of the pressure medium is surely reduced, so that the pressure means can be reduced in volume. Alternatively, the pressurization / decompression time can be shortened.

Further, the pressurizing means according to the present invention does not have a pipe (6) as in the example of the development device, that is, does not have a pipe connecting the pressurizing means and the pressure-resistant container. In the method according to the above, the possibility of leakage of the pressure medium is extremely reduced because the leakage of the pressure medium is basically unlikely to occur.

Further, since the pressurizing means according to the present invention does not have the pipe as described above, and the piston is disposed by being fitted into the through hole in the side wall of the pressure-resistant container, the means provided outside the pressure-resistant container is mainly used. Therefore, the entire structure of the crystal observation apparatus (including the pressurizing means) can be significantly reduced in size.

In the crystal observation apparatus according to the present invention, the sample chamber may be constituted by a small container and an optical window as shown in FIG. 2, or may be constituted only by a sealed small container. In any case, the small container constituting the sample chamber needs to have elasticity and optical transparency. However, it is not necessary that all the parts of the small container are filled, and it is sufficient if the small container can be expanded and contracted as a result and the sample can be irradiated with light from the optical window.

In order to provide the above-mentioned elasticity, for example, those made of silicone rubber or polyethylene may be used. Alternatively, metal having a bellows can be used. As the shape of the small container, for example, a rectangular parallelepiped, a hemisphere, a sphere, or the like can be used.

There may be only one optical window on the side of the pressure-resistant container,
Two may be provided as shown in FIGS. The material and shape of the optical window need only be those having light transmittance and necessary strength, and for example, hemispherical or cylindrical sapphire, hard glass, hard plastic and the like can be used. However, when it is desired to increase the pressure resistance or to make the distance between the microscope and the sample short, it is desirable to arrange the hemispherical optical window as shown in FIG.

(Example) Example 1 FIG. 1 shows a partially cutaway side view of a crystal observation apparatus according to Example 1. FIG. As shown in FIG. 1, the apparatus comprises a pressure-resistant container (3), a sample chamber (10) disposed in the container (7), and a pressure medium (15) for increasing the pressure in the container (7). ). The pressurizing means includes the container (3)
Through hole (16) provided in the side wall (14) of the
And a drive mechanism (20) for moving the piston (17) into and out of the inner periphery of the piston (17). Incidentally, (24) indicates a packing for a pressure medium.

The drive mechanism (20) includes an electric rotating means (23),
A worm speed reducer (22) interlocked with the speed reducer (22)
It consists of a feed screw (21) linked to 2) and a piston (1
A male screw (18) meshing with the female screw (25) of the screw (21) is provided in the large diameter portion of 7). When the rotating means (23) rotates at a high speed, the feed screw (21) rotates at a low speed, and the piston (17) is driven to advance or retreat.

Regarding the pressure-resistant container (3), (1) is a hemispherical sapphire optical window provided on the side surface of the container (3). The optical window (1) is supported by an optical window support (12), and the support (12) is screwed to a pressure-resistant container (14). still,
(13) is a seal member.

(10) is a stretchable sample chamber having light transmissivity as a whole, and the wall of the chamber (10) is formed of silicone rubber. The sample (9) is sealed in the chamber (10).

The following crystal observation was performed using such a crystal observation apparatus.
That is, first, the optical window (1) was irradiated with light from the light source (8), so that the inside of the container (7) and the sample (9) could be observed. Next, after injecting the pressure medium (15) into the pressure-resistant container (7) and the through hole (16), the rotating means (23) is rotated, the piston (17) is advanced, and the pressure medium (15) is discharged. The sample (9) was pressurized. In parallel with the pressurization, the state of the sample was observed with an optical microscope (not shown) arranged outside the optical window (1).

As a result of the above pressurization and observation, it was observed that the sample chamber (10) gradually shrunk with the progress of pressurization, and crystals were precipitated from the liquid sample. When the pressure at the time of such crystal precipitation was determined by measuring the pressure of a pressure medium, the measured values were the same as those measured by the conventional method.

Embodiment 2 Embodiment 2 is different from Embodiment 1 in that the rotating means (23) of the piston drive mechanism (20) is manually operated. Others are the same as in the first embodiment.

When pressure and observation were performed in the same manner as in Example 1 using such an apparatus, precipitation of crystals was observed, and the measured value of the pressure during crystal precipitation was the same as the measured value by the conventional method. .

Regarding the rotating means (23), the pressure control is more flexible in the case of the electric type used in the first embodiment than in the case of the manual type used in the second embodiment, and the pressure is increased at a constant pressure change speed. Get
Further, complicated pressure rise / fall control by a computer was also possible.

(Effects of the Invention) According to the crystal observation apparatus according to the present invention, as in the case of the above-described development apparatus in which a stretchable and light-transmitting sample chamber is provided in a pressure-resistant container, all the problems of the conventional apparatus are solved. And the amount of pressure medium required for pressurizing the sample for crystal observation can be reduced as compared with the case of the development device, so that the pressure means can be reduced in volume, or the pressure / decompression time can be reduced. Can be shortened, the possibility of leakage of the pressure medium becomes extremely small, and the whole crystal observation apparatus can be made much more compact.

[Brief description of the drawings]

FIG. 1 is a partially cutaway side view of a crystal observation apparatus according to Example 1, FIG. 2 is a partially cutaway side view of a development apparatus provided with an elastic and light-transmitting sample chamber in a pressure-resistant container, FIG. 3 is a side view showing a typical example of a conventional crystal observation apparatus. (1) optical window, (2) optical window (3) pressure-resistant container, (4) pressure-increasing means (5) (6) piping, (7) pressure-resistant container Inside (8) Light source (9) Sample (10) Sample chamber (11) Holder (12) Optical window holder (13) Seal member (14) ... side wall of pressure vessel, (15) ... pressure medium (16) ... through-hole, (17) ... piston (18) ... male screw of piston large diameter part (19) ... pressure gauge, (20) … Piston drive mechanism (21)… Feed screw, (22)… Worm reducer (23)… Rotating means (24)… Packing for pressure medium (25)… Female screw part of feed screw

Claims (1)

(57) [Claims] 1. A pressure-resistant container having an optical window made of a light transmitting body on a side surface, a stretchable sample chamber disposed in the pressure-resistant container, and a pressure medium for increasing the pressure in the pressure-resistant container. And a pressurizing means, wherein the pressurizing means is provided with a through-hole provided in a side wall of the pressure-resistant container, and a piston which fits into an inner peripheral portion of the through-hole and moves forward and backward. And a drive mechanism for moving the piston forward and backward.