JPH0627701B2 - Crystal observation device - Google Patents

Description

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

(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 a pressure crystallization method, which is attracting attention as a separation and purification technology for obtaining a high-purity product by causing crystals of a target component to be broken out from a mixture by high-pressure action, the pressure conditions for crystal precipitation / growth must be understood in advance. It is an indispensable requirement.

In order to understand the physical change of the crystal, the crystal is observed under pressure.

A typical example of a crystal observing apparatus conventionally used for observing the crystal is shown in FIG. 3, and will be described below based on this.

As shown in FIG. 3, the conventional crystal observing apparatus has a pressure-resistant container (1) having optical windows (5) made of a light-transmitting body on opposite upper and lower surfaces, and a pressure medium chamber (1) inside the container (1). It is composed of a pressurizing device (3) for increasing the pressure of 2), and is formed by a small container (6) having optical transparency and stretchability and the optical window (5) during crystal observation. The sample chamber (7) to be filled is filled with the sample (observed object) in advance, and the pressure medium (15) is pressure-fed into the pressure medium chamber (2) through the pressure resistant pipe (9). The light source (8) irradiates the optical window (5) with light.

By doing so, light is transmitted through the optical window (5), is irradiated to the sample, and simultaneously the sample is pressed, and the shape of the crystal, the growth process, etc. are observed from the outside of the optical window (5) by the naked eye or a microscope. It is observable, and the disappearance process of the crystal can be observed by reducing the pressure.

(Problems to be solved by the invention) By the way, a mounting bracket (4) having a sample chamber (7) and an optical window (5) integrally at the tip is inserted into the mounting portion (10) of the pressure vessel (1) from above. Then, when installing, the seal part (1
1), that is, when the O-ring (12) mounting portion is loaded by tightening from the loading start position (a) to the sealing position (b),
Since the pressure medium (15) in the pressure medium chamber (2) which is sealed is naturally compressed, it is necessary to extract the pressure medium in an amount commensurate with this.

Conventionally, as a means for removing the pressure medium (15), a pressure device (3)
Was operated on the decompression side,
It is necessary to carry out the depressurization operation while inserting (4), two kinds of work must be performed at the same time, and those operations must be synchronized to maintain a constant pressure. If this synchronization is not performed, it is necessary to put air, which is a compressible fluid, in the pressure medium chamber (2).

Therefore, there are problems that the tuning operation is not easy and that the observation cannot be performed accurately because the compressive fluid such as air is put in.

Therefore, as a result of repeated studies to solve the above problems, the present invention has been completed. The object of the present invention is to make it possible to omit the tuning operation, which is difficult to adjust, and to maintain the constant pressure accurately and easily. It is intended to ensure the crystal observation by eliminating the mixture of impure fluids such as air.

(Means for Solving the Problems) In order to achieve the above object, the crystal observation apparatus according to the present invention has the following configuration.

That is, the crystal observing apparatus according to claim 1 inserts a fitting having an optical window made of a light-transmitting body integrally at the tip into the fitting part of the pressure vessel from above and tightens from the charging start position to the sealing position. In the crystal observing device in which the pressure medium chamber connected to the pressurizing device is formed in the pressure vessel by inserting the high pressure pipe, the high pressure pipe is connected to the pressure medium chamber, and the charging medium is started higher than the charging start position. , The overflow liquid reservoir is connected to the upper end of the high-pressure pipe, and the valve is held at the same level as the charging start position in the middle of the high-pressure pipe to hold the valve closed after the fitting is tightened to the sealing position. It is a crystal observation device characterized in that a valve is interposed.

In the crystal observation apparatus according to claim 2, the overflow liquid reservoir is a container having a capacity sufficient to store the amount of pressure medium displacement generated when the fitting is tightened from the charging start position to the sealing position. The crystal observation apparatus according to claim 1.

(Operation) As described above, the crystal observation apparatus according to the present invention is provided with a high-pressure pipe connected to the pressure medium chamber, an overflow liquid reservoir connected to the upper end of the pipe, and a predetermined location in the middle of the high-pressure pipe. And a closed valve that has been closed.

Therefore, the following operations are performed prior to loading the mounting bracket into the mounting portion of the pressure resistant container. That is, the pressure medium is put into the pressure medium chamber up to the charging start position, the closing valve is left open, and the pressurizing device is stopped and inoperative. When the mounting metal fitting is inserted and tightened after this, the pressure medium rises in the high-pressure pipe accordingly and accumulates in the overflow liquid reservoir.

Then, the fitting is completely inserted into the sealing position, and when the tightening is completed, the closing valve is closed.

Thus, during the loading of the mounting bracket, the pressure in the pressure medium chamber does not rise and the atmospheric pressure is maintained, so that no special operation is required to maintain the pressure. Then, after closing the closing valve, the pressurizing device may be operated to pressurize.

The illustrated example is an apparatus in which the sample chamber and the pressure medium chamber are independent of each other, but as the crystal observation apparatus according to the present invention,
In addition to such an example, a device having a structure in which a sample is injected into the pressure medium chamber so as to serve also as the sample chamber is naturally included.

As described above, according to the present invention, it is not necessary to perform the depressurizing operation of the pressurizing device at the time of mounting the mounting bracket, and air is never mixed in the pressure medium chamber.

(Embodiment) An embodiment of the present invention is shown in FIG.
A pressure vessel (1), a pressure device (3) for increasing the pressure of the pressure medium chamber (2) in this vessel (1), and the pressure inside the pressure medium chamber (2) during assembly are adjusted. It consists of a pressure regulation part for.

Regarding the pressure-resistant container (1), (5) and (5) are optical windows made of sapphire provided on both upper and lower opposite surfaces of the container (1). Both optical windows (5) and (5) are hemispherical bodies, and a mounting member (a tapered tubular shape so that the circular surface of the bottom of the hemispherical bodies can be directed into the pressure vessel (1). It is integrally fixed to the tip of 4) by adhesion. In addition, the mounting bracket (4) has a male screw engraved on the outer peripheral surface of the maximum diameter part,
It is adapted to be inserted and fixed at a predetermined sealing position (B) by being screwed to a female screw engraved on the mounting portion (10) of (1).

(11) is a seal part having an O-ring (12), and in the state of the left half of the figure, the O-ring (12) comes into elastic contact with the inner wall of the pressure-resistant container (1), and the container ( 1) The inside and outside can be shut off airtightly.

The central portion of the spherical surface of the hemispherical body in the optical window (5) and its vicinity are flat, because the sample is more clearly observed.

(6) is a small container (silicon rubber small container) that is entirely light-transmissive and stretchable, and has a dish-like shape with its flange portion facing the optical window (5) peripheral portion and the peripheral portion. It is in close contact with the front end surface of the mounting metal fitting (4) surrounded by one, and this close contact state is firmly held by the small container pressing tool (13) screwed to the front end of the mounting metal fitting (4).

By doing so, an airtight sample chamber (7) is formed at the tip of the upper mounting bracket (4) by the small container (6) and the optical window (5), and in this sample chamber (7) The sample for crystal observation is sealed in a small amount.

Next, regarding the pressurizing device (3), the device (3) is installed in the pressure medium chamber.
A pressure resistant pipe (9) for connecting to (2) and a pipe (14) for injecting a pressure medium (15) are connected. Incidentally, (16)
Is a pressure gauge.

On the other hand, to explain the pressure regulating portion, the pressure-resistant container (1) is connected to the pressure medium chamber (2) in a liquid-tight manner and taken out, and is higher than the charging start position (A) of the mounting bracket (4). The elevated high-pressure pipe (17), the overflow reservoir (18) connected to the raised upper end, and the high-pressure pipe (17) were installed at the same level as the charging start position in the middle of the high-pressure pipe (17). The pressure regulating portion is composed of three members such as the shutoff valve (19).

The liquid reservoir (18) is a pressure medium chamber (2) generated when the mounting bracket (4) is tightened from the charging start position (A) to the seal position (B).
It is sufficient if the container has a capacity sufficient to store the displacement amount of the pressure medium inside, and strictly speaking, the volume in the high-pressure pipe (17) between the liquid reservoir (18) and the closing valve (19) is pushed to the above The condition is that the amount subtracted from the evasion amount can be stored as a minimum amount.

In addition, the closing valve (19) has the mounting bracket (4) at the sealing position (B).
Immediately after the charging is completed and tightened completely, the valve is closed during the pressurizing operation of the pressurizing device (3) and the crystal observation.The observation operation is terminated and the pressurizing operation is released to release the pressure medium. The valve is opened when the chamber (2) is returned to normal pressure.

The crystal observation by the apparatus of the example is performed as follows. That is, the pressure medium (15) is injected into the pressurizing device (3) after the mounting of the mounting bracket (4) and the closing valve (19) are closed, and the pressure medium chamber ( Fill 2) under initial pressure.
On the other hand, the light source (8) irradiates the optical window (5) (lower optical window) with light to start observation of the state of the sample in the sample chamber (7).
This observation is performed by an optical microscope (not shown) arranged above the upper optical window (5).

When the sample is pressurized by pressurizing the pressure medium (15) with the pressurizing device (3) in pairs, the small container (6) gradually contracts with the progress of the pressurization, and as a result, the liquid It shows changes such as crystal precipitation from the sample, and such changes in crystal state can be observed.

(Effects of the Invention) The present invention has the above-described structure and functions.
When charging the mounting bracket (4), it is sufficient to open and close the closing valve (19) and close it at the end of charging, and the operation is extremely simple. ) Does not require any troublesome means such as decompressing.

Furthermore, since it is possible to omit a conventional operation that requires skill such as synchronizing two operations, the work is extremely simple and there is no inconvenience that the O-ring is damaged by an erroneous operation.

Further, in the past, a compressive fluid such as air was partially used for the purpose of compensation when the tuning operation was not performed, but in the present invention, there is no need to put air or the like into the pressure medium chamber, and observation is accurate. In addition, there is an effect that problems such as equipment deterioration due to oxidation can be eliminated.

[Brief description of drawings]

1 is a partially cutaway side view according to an embodiment of the present invention, FIG.
The figure is a partially cutaway side view of the conventional apparatus. In both figures, the right half shows the charging start state of the mounting bracket, and the left half shows the charging completion state. (1) ...... Pressure-proof container, (2) ...... Pressure medium chamber (3) ...... Pressurizing device, (4) …… Mounting bracket (5) …… Optical window, (10) …… Mounting part (11) ...... Seal part, (12) …… O ring (15) …… Pressure medium, (17) …… High pressure piping (18) …… Overflow liquid reservoir, (19) …… Closed valve (A) …… Start position, (B) …… Seal position

Claims (2)

[Claims] 1. A pressurizing device by mounting a mounting bracket integrally having an optical window made of a light-transmitting body at its tip into a mounting portion of a pressure-resistant container and tightening it from a charging start position to a sealing position. In a crystal observation apparatus for forming a pressure medium chamber connected to the inside of the pressure resistant container, a high-pressure pipe is connected to the pressure medium chamber, and the liquid is used for overflow at the upper end of the charging medium starting up higher than the charging start position. In addition to connecting the reservoir, at the same level as the charging start position in the middle of this high-pressure pipe, a closing valve for holding the valve closed after the fitting was tightened to the sealing position was inserted. Characteristic crystal observation device. 2. The crystal according to claim 1, wherein the overflow liquid reservoir is a container having a capacity sufficient to store the amount of pressure medium displacement generated when the fitting is tightened from the charging start position to the sealing position. Observation device.