CN216273715U

CN216273715U - Glass container for removing raw material oxides and oxygen removing device

Info

Publication number: CN216273715U
Application number: CN202122397270.9U
Authority: CN
Inventors: 王培新; 原保平; 胡斌
Original assignee: Cdgm LLC
Current assignee: Cdgm LLC
Priority date: 2021-09-30
Filing date: 2021-09-30
Publication date: 2022-04-12
Anticipated expiration: 2031-09-30

Abstract

The utility model provides a glass container for removing oxide of raw material and an oxygen removing device, which can prevent the separated raw material from mixing with oxide again. A glass container for getting rid of raw materials oxide, including raw materials box, lid, take the quartz capsule of glass flange, take first ring flange, second ring flange and the fastening bolt of KF clamp interface, the glass flange of quartz capsule is cliied through fastening bolt to first ring flange and second ring flange. The raw material area and the condensation area of the glass container adopt a separation type structure, and the separated raw materials are prevented from being mixed with oxides again by utilizing the characteristic that the steam pressure of the raw materials and the steam pressure of the oxides of the raw materials are different at the same temperature, so that the aim of separating the oxides in the simple substance raw materials is fulfilled.

Description

Glass container for removing raw material oxides and oxygen removing device

Technical Field

The utility model relates to a glass container used for pretreatment of high-purity raw materials before infrared glass melting, in particular to a device for removing surface oxides from the high-purity raw materials.

Background

The chalcogenide infrared glass is made of high-purity glassMixing elementary raw materials (such As germanium (Ge), arsenic (As), antimony (Sb), selenium (Se) and the like with the purity of more than or equal to 5N) according to a certain proportion, and vacuumizing (the vacuum degree is more than 10)^-3Pa) and cooling the quartz ampoule bottle according to a process schedule to obtain the infrared-transmitting glass material, but the transmittance of the infrared glass is reduced due to Ge-O bonds, As-O bonds and the like formed in the melting process of oxides remaining in raw materials. The oxidation phenomenon is inevitable under the influence of the factors of packaging, storage conditions and storage time, and the quality index of the molten chalcogenide glass fluctuates due to the residual quantity of the oxides, so that unpredictable loss is brought to downstream customers. In order to avoid the problems, the raw materials need to be deoxidized and pretreated before being mixed to achieve the purpose of removing oxides, and the pretreated raw materials are put into the processes of mixing, sealing by melting and the like in a very short time, so that the time for generating oxidation is reduced as much as possible, and the consistency of quality is ensured. The principle of the existing deoxidation is mainly to evaporate the oxide at a proper temperature by utilizing the characteristic that the steam pressure of the simple substance and the oxide thereof is different at the same temperature, thereby achieving the purpose of separating the simple substance from the oxide. However, since the oxide vapor condenses on the inner wall of the container near the opening of the heating furnace due to temperature reduction, when the elemental raw material is poured out from the end of the integral evaporation container, the raw material will scratch from the surface of the oxide crystal, and inevitably a part of the separated oxide will be carried back into the elemental raw material.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a glass container and a deaerating device for removing raw material oxides, which can prevent separated raw materials from being mixed with oxides again.

The technical scheme adopted by the utility model for solving the technical problem is as follows: a glass container for getting rid of raw materials oxide, including raw materials box, lid, take the quartz capsule of glass flange, take KF (vacuum quick-release flange, the same below) the first ring flange of clamp interface, second ring flange and fastening bolt, the glass flange of quartz capsule is cliied through fastening bolt to first ring flange and second ring flange.

Furthermore, the quartz tube sealing device further comprises an O-shaped sealing ring, wherein the O-shaped sealing ring is arranged on the working surface of the first flange plate and is in contact with the glass flange on the quartz tube. The O-shaped sealing ring is made of rubber.

Furthermore, the shape of the box cover is matched with that of the raw material box.

Furthermore, the first flange plate and the second flange plate are made of stainless steel.

Deoxidization device, including foretell glass container to and heating furnace, heating furnace temperature control system, vacuum pipeline, vacuum unit and cooling air pipe, the cooling air pipe sets up the condensation zone at the quartz capsule, the glass container sets up in the insulating sleeve of heating furnace, first ring flange passes through the KF clamp and is connected with the vacuum pipeline one end that has the KF interface, the vacuum pipeline other end with the vacuum unit adopts the KF clamp to connect, the temperature of heating furnace temperature control system control heating furnace.

Furthermore, the heating furnace is composed of a furnace shell, a heat insulation material, an insulation sleeve, a heating element and a thermocouple.

The utility model has the beneficial effects that: the raw material area and the condensation area of the glass container adopt a separation type structure, and the separated raw materials are prevented from being mixed with the oxide again by utilizing the characteristic that the steam pressure of the raw materials and the steam pressure of the oxide of the raw materials are different at the same temperature, so that the purpose of separating the oxide in the simple substance raw materials is achieved.

Drawings

FIG. 1a is a sectional view of a front view of a raw material box for a glass container of the present invention.

Fig. 1b is a cross-sectional view of a front view of the cover of the glass container of the present invention.

Fig. 2 is a sectional view of a front view of the glass container of the present invention except for the material case and the case cover.

FIG. 3 is a cross-sectional view of a front view of the oxygen scavenging device of the present invention.

FIG. 4 is a graph showing the transmittance of molten glass before and after deoxidation of raw materials in example 1 of the present invention.

FIG. 5 is a graph showing the transmittance of molten glass before and after deoxidation of raw materials in example 2 of the present invention.

Detailed Description

As shown in fig. 1a, 1b and 2, the glass container of the present invention comprises a raw material box 1, a box cover 2, a quartz tube 3 with a glass flange 31, a first flange 4 with a KF clamp interface 41, a second flange 5, a fastening bolt 6 and an O-ring 7, wherein the O-ring 7 is disposed on a working surface of the first flange 4 and contacts with the glass flange 31 on the quartz tube 3; the first flange plate 4 and the second flange plate 5 form a group of flange plates which are arranged on the bottle mouth of the quartz tube 3, clamp the glass flange 31 of the quartz tube 3 and are connected and fixed through the fastening bolt 6; lid 2 matches with raw materials box 1 shape, sets up on raw materials box 1 after raw materials deoxidation handles, and the deoxidation in-process does not lid 2, and the evaporation of the oxide of being convenient for because the raw materials after the deoxidation need shift to the anaerobic glove box in the shortest time, can not clear up the crystallization earlier and take out raw materials box 1 again, consequently for avoiding the crystallization of condensation zone to fall into in raw materials box 1 again, it is the fastest quick effectual method to cover lid 2. In operation, the raw material box 1 is arranged in the quartz tube 3.

The first flange plate 4 and the second flange plate 5 are made of stainless steel, and the O-shaped sealing ring 7 is made of rubber.

The utility model also provides a deaerating device, as shown in fig. 3, the deaerating device comprises the glass container, a heating furnace 8, a heating furnace temperature control system, a vacuum pipeline, a vacuum unit and a cooling air pipe (not shown in the figure), wherein the heating furnace 8 is composed of a furnace shell 81, a heat insulation material 82, an insulating sleeve 83, a heating element 84 and a thermocouple 85, the cooling air pipe is arranged in a condensation area of the quartz tube 3, the glass container is arranged in the insulating sleeve 83 of a hearth of the heating furnace 8, the first flange plate 4 is connected with one end of the vacuum pipeline with a KF interface through a KF clamp, the other end of the vacuum pipeline is connected with the vacuum unit through the KF clamp, and the heating furnace temperature control system controls the temperature of the heating furnace 8.

When the vacuum pumping device works, a raw material 9 with an oxidized surface is put into a raw material box 1, then a quartz tube 3 with one closed end and the other end provided with a glass flange 31 is horizontally put into the raw material box, a group of flanges consisting of a first flange 4 and a second flange 5 clamp the glass flange 31 through a fastening bolt 6, and an O-shaped sealing ring 7 embedded on the first flange 4 close to the outside ensures the air tightness in the vacuum pumping process; the first flange plate 4 is connected with one end of a stainless steel vacuum pipeline with a KF interface through a KF clamp, and the other end of the stainless steel vacuum pipeline is connected with a vacuum unit through the KF clamp; according to the process specification, the process stages of vacuum pumping, heating of a heating furnace, cooling of a condensation area by a cooling air pipe, heat preservation of the heating furnace, cooling of the heating furnace and the like are carried out, the quartz pipe 3 is provided with a condensation area at the outer part of the furnace, and the evaporated oxide steam is condensed on the pipe wall of the condensation area; after the temperature of the hearth is reduced to room temperature, closing a vacuum unit, opening a KF clamp for breaking vacuum, opening a fastening bolt 6, taking down a first flange plate 4, extending a box cover 2 into a quartz tube 3 to cover the raw material box 1, hooking out the raw material box 1, wherein when the raw material box 1 passes through a condensation zone, falling oxides cannot enter the raw material box 1 due to the blocking of the box cover 2; then carefully erasing the oxide crystals falling from the box cover 2 and opening the box cover 2 to obtain the deoxidized raw materials, so that the two materials of the raw materials and the crystals are not contacted with each other, the deoxidized raw materials are prevented from being contacted with the crystals when being taken out, and the deoxidized raw materials are prevented from being polluted by the oxide crystals again.

Example 1

The infrared glass (brand: HWS6) melted after the As raw material is deoxidized by adopting the glass container and the raw material deoxidizing device has the lowest transmittance improved from 28 percent to 50 percent in the working wavelength range of 8-14 microns. FIG. 4 is a graph showing a comparison of the transmittances of molten glass before and after deoxidation of As raw materials.

Example 2

The infrared glass (brand: HWS5) melted after the Ge and Te raw materials are deoxidized by adopting the glass container and the raw material deoxidizing device provided by the utility model has the lowest transmittance improved from 27% to 61% in the working wavelength band of 8-14 microns. Ge. FIG. 5 shows a comparison of the transmittances of molten glasses before and after deoxidation of Te base materials.

Claims

1. A glass container for removing raw material oxides, characterized by: the quartz tube clamping device comprises a raw material box (1), a box cover (2), a quartz tube (3) with a glass flange (31), a first flange plate (4) with a KF clamp interface (41), a second flange plate (5) and fastening bolts (6), wherein the first flange plate (4) and the second flange plate (5) are arranged on a bottle opening of the quartz tube (3) and used for clamping the glass flange (31) of the quartz tube (3) through the fastening bolts (6).

2. The glass vessel for removing a raw oxide as claimed in claim 1, wherein: the quartz tube sealing device is characterized by further comprising an O-shaped sealing ring (7), wherein the O-shaped sealing ring (7) is arranged on the working surface of the first flange plate (4) and is in contact with a glass flange (31) on the quartz tube (3).

3. The glass vessel for removing a raw oxide as claimed in claim 2, wherein: the O-shaped sealing ring (7) is made of rubber.

4. The glass vessel for removing a raw oxide as claimed in claim 1, wherein: the shape of the box cover (2) is matched with that of the raw material box (1).

5. The glass vessel for removing a raw oxide as claimed in claim 1, wherein: the first flange plate (4) and the second flange plate (5) are made of stainless steel.

6. Deoxidization device, its characterized in that: the glass container comprises the glass container as claimed in any one of claims 1 to 5, and a heating furnace (8), a heating furnace temperature control system, a vacuum pipeline, a vacuum unit and a cooling air pipe, wherein the cooling air pipe is arranged in a condensation area of the quartz tube (3), the glass container is arranged in an insulating sleeve (83) of the heating furnace (8), the first flange (4) is connected with one end of the vacuum pipeline with a KF interface through a KF clamp, the other end of the vacuum pipeline is connected with the vacuum unit through the KF clamp, and the heating furnace temperature control system controls the temperature of the heating furnace (8).

7. The oxygen-scavenging device of claim 6 wherein: the heating furnace (8) is composed of a furnace shell (81), a heat insulation material (82), an insulating sleeve (83), a heating element (84) and a thermocouple (85).