CN112014028A - Quartz tube assembly and vacuum inspection method thereof - Google Patents
Quartz tube assembly and vacuum inspection method thereof Download PDFInfo
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- CN112014028A CN112014028A CN202010878577.8A CN202010878577A CN112014028A CN 112014028 A CN112014028 A CN 112014028A CN 202010878577 A CN202010878577 A CN 202010878577A CN 112014028 A CN112014028 A CN 112014028A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L21/00—Vacuum gauges
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
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Abstract
The application discloses a quartz tube component and a vacuum inspection method thereof, wherein the method comprises the steps of obtaining a quartz tube component to be inspected after primary vacuum sealing, wherein the quartz tube component has a first vacuum degree, and comprises a quartz tube, mercury positioned at the bottom of the quartz tube, a wafer positioned in the middle of the quartz tube and a quartz sleeve positioned in the top of the quartz tube; vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again; comparing the second vacuum degree with the first vacuum degree; and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified. In this application after obtaining the quartz capsule subassembly of examining, carry out evacuation processing to the quartz capsule subassembly, obtain the second vacuum, utilize mercury to volatilize and judge whether sealed with the quartz capsule is tight with the quartz capsule, when the second vacuum is not more than first vacuum, show that there is not the gap between quartz capsule and the quartz capsule, be in high vacuum state, it is qualified to examine.
Description
Technical Field
The application relates to the technical field of quartz tube sealing, in particular to a quartz tube assembly and a vacuum inspection method thereof.
Background
The tellurium-cadmium-mercury material is a semiconductor material, has the advantages of adjustable forbidden band width, high photoelectric detection efficiency and the like, and has the detection spectral range extending from a short wave band to a very long wave band, and is an important material for preparing and producing the high-performance infrared focal plane detector. In order to meet the performance of the infrared focal plane detector, the chemical stoichiometric ratio and the components of the mercury cadmium telluride wafer are generally adjusted by adopting a heat treatment method.
The heat treatment requires a vacuum environment in the quartz tube, otherwise an oxide layer is formed on the surface of the wafer, the oxide layer not only has a very obvious barrier effect on the communication of internal and external atoms of the surface layer, but also affects the adhesion of the surface film layer of the subsequent passivation process of the wafer, so that the wafer needs to be sealed in the high-vacuum quartz tube. At present, when sealing is carried out, mercury is firstly placed in a bubble-shaped tail end at one end of a quartz tube, a wafer sample is placed in a sample chamber in the middle of the quartz tube, then the quartz tube is placed in a quartz sleeve, the quartz tube is pumped to high vacuum through an exhaust table of a high vacuum pump set, and then the quartz tube and the quartz sleeve are sealed by oxyhydrogen flame, wherein the quartz sleeve is positioned in the quartz tube. Because the quartz sleeve is positioned in the quartz tube, the outer diameter of the quartz sleeve is smaller than the inner diameter of the quartz tube, the sintering effect of the quartz sleeve and the quartz tube can only be observed by naked eyes during high-temperature sintering, and in the cooling process, a gap may be generated between the quartz sleeve and the quartz tube due to the stress difference between the quartz tube and the quartz sleeve, so that the vacuum in the quartz tube cannot meet the requirement.
Therefore, how to solve the above technical problems should be a great concern to those skilled in the art.
Disclosure of Invention
The invention aims to provide a quartz tube component and a vacuum inspection method thereof, so as to realize the inspection of the high vacuum state of the quartz tube component.
In order to solve the above technical problem, the present application provides a method for vacuum inspection of a quartz tube assembly, including:
obtaining a quartz tube assembly to be inspected after primary vacuum sealing, wherein the quartz tube assembly has a first vacuum degree, and comprises a quartz tube, mercury positioned at the bottom of the quartz tube, a wafer positioned in the middle of the quartz tube, and a quartz sleeve positioned in the top of the quartz tube;
vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again;
comparing the second vacuum degree with the first vacuum degree;
and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified.
Optionally, before the step of evacuating the quartz tube assembly, the method further includes:
and heating the bottom of the quartz tube by using a heat source.
Optionally, the step of evacuating the quartz tube assembly includes:
and installing the quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the quartz tube assembly.
Optionally, the quartz tube assembly to be tested after obtaining the first vacuum sealing comprises:
obtaining the quartz tube;
placing mercury at the bottom of the quartz tube, placing a wafer in the middle of the quartz tube, and placing the quartz sleeve into the top of the quartz tube to obtain a quartz tube assembly to be treated;
vacuumizing the quartz tube assembly to be processed to enable the vacuum degree of the quartz tube assembly to be processed to be the first vacuum degree;
and sintering the quartz tube and the quartz sleeve by using oxyhydrogen flame, and cooling to obtain the quartz tube assembly.
Optionally, the step of vacuumizing the to-be-processed quartz tube assembly includes:
and installing the to-be-treated quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the to-be-treated quartz tube assembly.
Optionally, the temperature of the heat source is 50 ℃ ± 5 ℃.
The present application further provides a quartz tube assembly sealed by the vacuum inspection method of the quartz tube assembly as described in any one of the above.
The application provides a quartz tube assembly vacuum inspection method, which comprises the following steps: obtaining a quartz tube assembly to be inspected after primary vacuum sealing, wherein the quartz tube assembly has a first vacuum degree, and comprises a quartz tube, mercury positioned at the bottom of the quartz tube, a wafer positioned in the middle of the quartz tube, and a quartz sleeve positioned in the top of the quartz tube; vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again; comparing the second vacuum degree with the first vacuum degree; and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified.
Therefore, according to the vacuum inspection method for the quartz tube assembly, after the quartz tube assembly to be inspected after primary vacuum sealing is obtained, the quartz tube assembly is vacuumized again to obtain the second vacuum degree of the quartz tube assembly, whether the quartz tube and the quartz sleeve are tightly sealed is judged by utilizing the influence of mercury volatilization on the vacuum degree, when the second vacuum degree is not greater than the first vacuum degree of the quartz tube assembly after primary vacuum sealing, it is shown that no gap exists between the quartz sleeve and the quartz tube, the quartz tube assembly is in a high vacuum state, and the quartz tube assembly is inspected to be qualified at this moment.
In addition, the application also provides a quartz tube component with a high vacuum state.
Drawings
For a clearer explanation of the embodiments or technical solutions of the prior art of the present application, the drawings needed for the description of the embodiments or prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart illustrating a method for vacuum testing a quartz tube assembly according to an embodiment of the present disclosure;
FIG. 2 is a flow chart of another method for vacuum testing a quartz tube assembly according to an embodiment of the present application;
fig. 3 is a schematic structural diagram of re-evacuating a quartz tube assembly according to an embodiment of the present application.
Detailed Description
In order that those skilled in the art will better understand the disclosure, the following detailed description will be given with reference to the accompanying drawings. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
As described in the background section, in the sealing process, mercury and a wafer are put into a quartz tube, then the quartz tube is put into a quartz sleeve, the quartz tube is pumped to high vacuum through an exhaust table of a high vacuum pump set, then the quartz tube and the quartz sleeve are sealed by oxyhydrogen flame, and the sealing process is completed after cooling. Because the quartz sleeve is positioned in the quartz tube, the outer diameter of the quartz sleeve is smaller than the inner diameter of the quartz tube, the sintering effect of the quartz sleeve and the quartz tube can only be observed by naked eyes during high-temperature sintering, and in the cooling process, a gap may be generated between the quartz sleeve and the quartz tube due to the stress difference between the quartz tube and the quartz sleeve, so that the vacuum in the quartz tube cannot meet the requirement.
In view of the above, the present application provides a method for vacuum testing a quartz tube assembly, please refer to fig. 1, where fig. 1 is a flowchart of a method for vacuum testing a quartz tube assembly according to an embodiment of the present application, the method including:
step S101: obtain the quartz capsule subassembly of waiting to inspect behind the first vacuum seal, the quartz capsule subassembly has first vacuum, wherein, the quartz capsule subassembly includes the quartz capsule, is located mercury of quartz capsule bottom, be located the wafer at quartz capsule middle part, be located quartz capsule in the quartz capsule top.
As a specific embodiment, the quartz tube component to be inspected after primary vacuum sealing is obtained comprises the following components:
step S1011: obtaining the quartz tube.
Step S1012: and placing mercury at the bottom of the quartz tube, placing a wafer in the middle of the quartz tube, and placing the quartz sleeve into the top of the quartz tube to obtain the quartz tube assembly to be treated.
The wafer is a mercury cadmium telluride wafer.
It will be appreciated that the outer diameter of the quartz sleeve is smaller than the inner diameter of the quartz tube.
Step S1013: and vacuumizing the to-be-treated quartz tube assembly to enable the vacuum degree of the to-be-treated quartz tube assembly to be the first vacuum degree.
Specifically, the step of vacuumizing the to-be-treated quartz tube assembly comprises the following steps:
and installing the to-be-treated quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the to-be-treated quartz tube assembly.
It should be noted that the ultimate vacuum degree of the exhaust platform of the high vacuum pump set is 5X 10-6Pa, the first vacuum degree in this application needs to be less than 5X 10 to meet the process requirements-5Pa, but the specific value of the first degree of vacuum is not limited.
Step S1014: and sintering the quartz tube and the quartz sleeve by using oxyhydrogen flame, and cooling to obtain the quartz tube assembly.
Specifically, the oxyhydrogen flame is adjusted, the quartz tube and the quartz sleeve are sintered together, and then natural cooling is carried out.
Step S102: and vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again.
Specifically, the step of vacuumizing the quartz tube assembly comprises:
and installing the quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the quartz tube assembly.
Step S103: and comparing the second vacuum degree with the first vacuum degree.
Step S104: and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified.
The bottom of the quartz tube is prevented from containing mercury, mercury vapor can be volatilized from mercury at normal temperature, a second vacuum degree is obtained when vacuumizing is carried out again, if the second vacuum degree is not larger than the first vacuum degree, namely the second vacuum degree is superior to the first vacuum degree, no gap exists between the quartz tube and the quartz sleeve, the quartz tube is in a high vacuum state, and subsequent heat treatment processes can be carried out.
Further, if the second vacuum degree is larger than the first vacuum degree, mercury atoms in the quartz tube are escaped, so that the vacuum degree is further reduced, and the quartz tube assembly is not qualified.
According to the quartz tube component vacuum inspection method, after the quartz tube component to be inspected after primary vacuum sealing is obtained, the quartz tube component is vacuumized again to obtain the second vacuum degree of the quartz tube component, whether the quartz tube and the quartz sleeve are tightly sealed is judged by utilizing the influence of mercury volatilization on vacuum, when the second vacuum degree is not more than the first vacuum degree of the quartz tube component to be inspected after primary vacuum sealing, it is shown that no gap exists between the quartz sleeve and the quartz tube, the quartz tube component is in a high vacuum state, and the quartz tube component is qualified in inspection.
Referring to fig. 2, fig. 2 is a flowchart illustrating another method for vacuum testing a quartz tube assembly according to an embodiment of the present application, the method including:
step S201: obtain the quartz capsule subassembly of waiting to inspect behind the first vacuum seal, the quartz capsule subassembly has first vacuum, wherein, the quartz capsule subassembly includes the quartz capsule, is located mercury of quartz capsule bottom, be located the wafer at quartz capsule middle part, be located quartz capsule in the quartz capsule top.
Step S202: and heating the bottom of the quartz tube by using a heat source.
Specifically, the bottom of the quartz tube may be heated in warm water.
Preferably, the temperature of the heat source is 50 ℃ ± 5 ℃.
The bottom of the quartz tube is heated, so that the volatilization of mercury can be accelerated, and the influence of mercury on high vacuum is increased, thereby improving the accuracy of judging whether the quartz tube assembly is in a high vacuum state.
Step S203: and vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again.
The schematic structural diagram of re-vacuumizing the quartz tube assembly is shown in fig. 3, wherein mercury 2 is located at the bottom of the quartz tube 1, the wafer 3 is located in the middle of the quartz tube 1, the quartz sleeve 4 is located in the top of the quartz tube 1, the heat source 5 heats the bottom of the quartz tube 1, the high vacuum pump unit 6 performs vacuum pumping, and the vacuum gauge 7 measures a second vacuum degree.
Step S204: and comparing the second vacuum degree with the first vacuum degree.
Step S205: and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified.
Please refer to the above embodiments for steps S201, S203, S204, and S205, which are not described in detail herein.
The application also provides a quartz tube component which is obtained by the quartz tube component vacuum inspection method in the embodiment after the quartz tube component is qualified.
The quartz tube subassembly in this application is when sealing-in, carry out first vacuum sealing-in back to the quartz tube subassembly, carry out evacuation processing to the quartz tube subassembly again, obtain the second vacuum degree of quartz tube subassembly, utilize mercury to volatilize and judge whether it is tight with quartz sleeve sealing-in to the influence of vacuum, when the second vacuum degree is not more than the first vacuum degree of waiting to inspect after the first vacuum sealing-in quartz tube subassembly, show that there is not the gap between quartz sleeve and the quartz tube, the quartz tube subassembly is in high vacuum state, obtains the quartz tube subassembly.
The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same or similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The quartz tube assembly and the vacuum inspection method thereof provided by the present application are described in detail above. The principles and embodiments of the present application are explained herein using specific examples, which are provided only to help understand the method and the core idea of the present application. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present application without departing from the principle of the present application, and such improvements and modifications also fall within the scope of the claims of the present application.
Claims (7)
1. A vacuum inspection method for a quartz tube assembly is characterized by comprising the following steps:
obtaining a quartz tube assembly to be inspected after primary vacuum sealing, wherein the quartz tube assembly has a first vacuum degree, and comprises a quartz tube, mercury positioned at the bottom of the quartz tube, a wafer positioned in the middle of the quartz tube, and a quartz sleeve positioned in the top of the quartz tube;
vacuumizing the quartz tube assembly to obtain a second vacuum degree of the quartz tube assembly after vacuumizing again;
comparing the second vacuum degree with the first vacuum degree;
and if the second vacuum degree is not greater than the first vacuum degree, the quartz tube assembly is qualified.
2. The method for vacuum testing a quartz tube assembly of claim 1, wherein before evacuating the quartz tube assembly, further comprising:
and heating the bottom of the quartz tube by using a heat source.
3. The quartz tube assembly vacuum inspection method of claim 1, wherein the evacuating the quartz tube assembly comprises:
and installing the quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the quartz tube assembly.
4. The method for vacuum testing a quartz tube assembly as claimed in claim 1, wherein the obtaining of the quartz tube assembly to be tested after the initial vacuum sealing comprises:
obtaining the quartz tube;
placing mercury at the bottom of the quartz tube, placing a wafer in the middle of the quartz tube, and placing the quartz sleeve into the top of the quartz tube to obtain a quartz tube assembly to be treated;
vacuumizing the quartz tube assembly to be processed to enable the vacuum degree of the quartz tube assembly to be processed to be the first vacuum degree;
and sintering the quartz tube and the quartz sleeve by using oxyhydrogen flame, and cooling to obtain the quartz tube assembly.
5. The method for vacuum inspection of a quartz tube assembly as set forth in claim 4, wherein the evacuating the quartz tube assembly to be processed comprises:
and installing the to-be-treated quartz tube assembly on an exhaust table of a high vacuum pump set, and opening a high vacuum pump set to vacuumize the to-be-treated quartz tube assembly.
6. The vacuum inspection method of a quartz tube assembly as set forth in claim 2, wherein the temperature of the heat source is 50 ℃ ± 5 ℃.
7. A quartz tube assembly characterized in that it is obtained by the quartz tube assembly vacuum test method as claimed in any one of claims 1 to 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115771996A (en) * | 2022-11-18 | 2023-03-10 | 云南中科鑫圆晶体材料有限公司 | Vacuum sealing and welding method of oversized-diameter quartz tube for VGF crystal growth |
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| CN112014028B (en) | 2021-04-13 |
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