JP2005329330A - Structure of window for high temperature and high pressure vessel - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide the structure of a window for a high pressure and high temperature vessel which is free from crack even in a relatively thick sapphire window. <P>SOLUTION: In the structure of the window for observing the inside apace of the high temperature and high pressure vessel, the window is formed of a transparent member which has specific thickness and where a taper is formed at a circumferential part. In fixing the window to the vessel, a large diameter part is arranged inside the vessel and a small diameter part is arranged outside the vessel. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to the structure of a window of a high-temperature / high-pressure container, and for example, relates to the structure of a window of a high-temperature / high-pressure container used for analyzing a component of a substance such as a plastic resin.

  When analyzing a component of a substance such as plastic resin, the component of the substance is analyzed using a spectroscope and a detector connected to the container with an optical fiber.

  As a container used for such an analysis, for example, an analysis object is fed into a through hole provided in the container, a reaction gas is allowed to flow into the through hole, and the analysis object is heated and pressurized to be put into the container. There is one in which a near infrared ray is emitted from a mounted probe to a substance in a through hole and a predetermined wavelength contained in the near infrared ray is absorbed (see Patent Document 1).

  Light that introduces and condenses light energy into an object to be processed in a high-pressure gas atmosphere contained in a high-pressure vessel. Light that introduces light from the outside of the high-pressure vessel into components of the high-pressure vessel. An introduction member is attached in an airtight state, and an internal optical system is provided that emits light rays emitted from the light introduction member in the normal direction of the emission surface and then collects the light without any refraction at the interface with the high-pressure medium. There is a thing (refer patent document 2).

JP 2002-310907 A Japanese Examined Patent Publication No. 7-87894

  In performing component analysis of an analysis object, it is desired to continuously measure the analysis object and visually recognize the change in real time. However, in the conventional analysis system, the analysis of the component of the analysis object is performed by analyzing the predetermined wavelength absorbed by the near-infrared light with a spectroscope, so that the near-infrared light is absorbed by the container at the predetermined wavelength. The component change of the analysis object cannot be visually recognized in real time.

  FIGS. 5A and 5B are configuration diagrams showing a conventional example of such an analyzer, FIG. 5A is an overall configuration diagram of the analyzer, and FIG. 5B is an AA cross-sectional configuration diagram of the container. is there. In these drawings, reference numeral 20 denotes a cylindrical container, and a through hole 21 (see FIG. B) is formed in the axial center. An upper lid 22 is disposed on one end surface of the container 20, and a lower lid 45 is disposed on the other end, and are fixed by screws 27.

A temperature sensor (not shown) is inserted in the center of the upper lid 22. Reference numeral 41 denotes a T joint that can introduce gas into the through hole 21 from the outside.
A pair of probes 54 and 55 are connected from both sides of the container. The window lid 58 is airtightly fixed with screws, and is removed during maintenance so that dirt on the probe tip can be cleaned.

In the above-described configuration, for example, when measuring physical properties of a plastic resin, a predetermined amount of resin formed in powder or granular form is put into the through-hole 21 and heated to a predetermined temperature via a T joint. For example, N ₂ or CO ₂ gas is allowed to flow to react with the gas generated from the resin.
In such an apparatus, when the reaction state in the container is visually confirmed as described above, a transparent member such as sapphire or quartz is used as the window lid 58.

As the window lid of the container having such a configuration, an iron / nickel alloy constant elastic member such as Kovar is generally used. Kovar has a thermal expansion coefficient almost equal to that of hard glass.
6A, 6B and 6C, a circular hole 2a is formed in a kovar (sealing metal) 2, and sapphire 1 as a window formed in a diameter larger than the hole is brazed with a row 3. FIG. The case of fixing is shown. Fig. (A) is a cross-sectional perspective view showing a state in which sapphire 1 is attached to a hole 2a formed in Kovar (sealing metal) 2, and Fig. (B) is only one surface from the direction of arrow A to window 1 by brazing (C) shows a state in which an upward force is generated at the edge of the window 1 when the pressure B is applied to the brazed window 1. ing.

In such a state, when the sapphire is thin at the portion of arrows A and C where pressure is applied, sealing is possible, but when sapphire is strong against compressive force but weak against tensile force, There was a problem that cracking occurred.
Therefore, the problem to be solved by the present invention is to provide a structure of a high temperature and high pressure resistant window which does not crack even in a relatively thick sapphire window.

In order to achieve such a problem, the invention according to claim 1 of the present invention is:
A window structure for observing the internal space of a high-temperature / high-pressure vessel, the window comprising a transparent member having a predetermined thickness and having a taper at the periphery, and fixing the window to the vessel In this case, the large diameter portion of the window is arranged inside the container, and the small diameter portion is arranged outside the container.

In claim 2, in the structure of the window of the container for high temperature and high pressure according to claim 1,
The container is metal, the transparent member is sapphire, and the tapered portion of the window is fixed by brazing.
In claim 3, in the structure of the window of the container for high temperature / high pressure according to claim 1 or 2,
A groove having a predetermined depth is provided around the window from the small diameter side toward the large diameter side.

The present invention has the following effects. According to the high-temperature / high-pressure container according to claim 1,
When the window is fixed to the container by brazing, the large diameter part of the window is inside the container and the small diameter part is outside the container. Therefore, the stress is evenly applied to the edge of the window and cracking can be prevented.
According to the high temperature / high pressure container according to claim 3,
Since a groove having a predetermined depth is provided around the window from the small diameter side to the large diameter side, the stress applied to the edge of the window can be absorbed and the occurrence of cracks can be prevented.

Hereinafter, the present invention will be described in detail with reference to the drawings. FIG. 1 is a block diagram showing a main part of a high-temperature / high-pressure container window according to the present invention.
1A and 1B, FIG. 1A is a plan view, and FIG. 1B is a cross-sectional view taken along line AA in FIG. In these drawings, 1 is sapphire made of a transparent member to be a window, and 2 is kovar made of a sealing metal.
In this example, the plate pressure c of Kovar is about 10.5 mm, for example, and the vertical and horizontal (a, b) dimensions are about A = 60 and B = 50 mm.

  A taper hole having a large diameter portion e = 30 mm and a small diameter portion f = 25 mm is formed in the central portion of the sealing metal 2. Reference numeral 6 denotes a groove having a diameter g = 40 mm, a width 1 mm, and a depth d = 6 mm formed from the small diameter hole side toward the large meridian side.

The sapphire 1 made of a transparent member is inserted into a tapered hole 4 formed in the sealing metal 2 and has a large diameter portion e of 30 mm, a small diameter portion f of about 25 mm, and a thickness of about 10 mm. Reference numeral 5 denotes an attachment hole for attaching the sealing metal to a high pressure / high temperature container as shown in FIG. 7 is a low reservoir formed around the window 1. A powder or ribbon-like brazing material is placed in the low reservoir and heated to about 700 to 900 ° C. to raise the temperature to soak the low in the circumference. Let them join together.
Note that when the sealing metal returns to room temperature, compressive stress acts on the edge of sapphire, but this force is evenly applied to the edge so that cracking can be prevented.

The sealing metal to which this sapphire is bonded is formed, for example, by placing the large diameter portion of the window inside the container and the small diameter portion outside the container through the attachment hole 5 in the portion of the window lid 58 of the container 20 shown in FIG. Secure with screws.
The container is heated to a high temperature of several hundred degrees and has an internal pressure of about several tens of MPa, but the strength is sufficiently maintained because the large diameter portion of the window is located inside the container and the small diameter portion is located outside the container. When the sealing metal is distorted due to internal pressure, the strain is absorbed by the groove 6 and the stress generated in the sapphire 1 can be reduced.

  2A and 2B show another application example. FIG. 2A is a cross-sectional view of a reaction cell (such as a high-pressure vessel), and FIG. 2B is a cross-sectional view of a sealing metal (lid). A transparent member 1 made of sapphire is formed in the center of the sealing metal (Kovar) 2a in the same manner as in FIG. 1, and its edge is brazed. The sealing metal is fixed with screws as a lid of the reaction cell.

  FIG. (B) shows the pressure distribution when a reaction occurs inside such a reaction cell and a high pressure is applied. When pressure is applied to the sealing metal 2 from the direction of the arrow A (inside), The pressure can be applied evenly in the edge (B) direction of the sapphire 1 to prevent cracking.

  3 and 4 show still another application example, and FIG. 3 shows a case where it is used as a component of a probe (or a flow cell) 10. In such a case, the wall 11 that separates the observation object is used. Internal observation can be performed relatively easily by screwing the tip of the probe 10 into the provided screw hole.

  FIG. 4 shows an application to a probe of a near-infrared spectrometer, and shows a case where windows of sapphire 1 are provided at both ends of the flow path 12 and the tip of the optical fiber 13 is connected to each window. According to such a configuration, the component of the fluid flowing in the flow path can be analyzed.

The above description merely shows a specific preferred embodiment for the purpose of explanation and illustration of the present invention. For example, sapphire as the transparent member may be quartz or the like, and is not limited to the illustrated application example, and can be applied to windows of various high temperature / high pressure containers. Furthermore, it is not restricted to the dimension of each part shown in FIG.
Therefore, the present invention is not limited to the above-described embodiments, and includes many changes and modifications without departing from the essence thereof.

It is a principal part block diagram which shows one Example of the window for high temperature / high pressure containers of this invention. It is sectional drawing which shows another application example. It is sectional drawing which shows another application example. It is sectional drawing which shows another application example. It is explanatory drawing which shows the structure of the conventional high temperature and high voltage | pressure window. It is explanatory drawing which shows the structure of the conventional high temperature and high voltage | pressure window.

Explanation of symbols

1 Window (Sapphire)
2 Sealing metal (Kovar)
3 Low 4 Tapered hole 5 Mounting hole 6 Groove 7 Low pool 10 Probe 11 Channel 12 Optical fiber 20 Container 21 Through hole 22 Upper lid 45 Lower lid 54 First probe 55 Second probe 58 Window lid

Claims (3)

  A window structure for observing the internal space of a high-temperature / high-pressure vessel, the window comprising a transparent member having a predetermined thickness and having a tapered periphery, and fixing the window to the vessel In this case, the structure of the window of the high-temperature / high-pressure container is characterized in that the large-diameter portion of the window is disposed inside the container and the small-diameter portion is disposed outside the container.   2. The structure of a high-temperature / high-pressure container window according to claim 1, wherein the container is made of metal, the transparent member is sapphire, and the tapered portion of the window is fixed by brazing. The high-temperature / high-pressure container window structure according to claim 1 or 2, wherein a groove having a predetermined depth is provided around the window from the small diameter side toward the large diameter side.

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