CN111039579A - Low-temperature annealing process for reducing stress of glass-metal sealing structure - Google Patents
Low-temperature annealing process for reducing stress of glass-metal sealing structure Download PDFInfo
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- CN111039579A CN111039579A CN201911409097.0A CN201911409097A CN111039579A CN 111039579 A CN111039579 A CN 111039579A CN 201911409097 A CN201911409097 A CN 201911409097A CN 111039579 A CN111039579 A CN 111039579A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S10/00—Solar heat collectors using working fluids
- F24S10/70—Solar heat collectors using working fluids the working fluids being conveyed through tubular absorbing conduits
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/25—Coatings made of metallic material
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S80/00—Details, accessories or component parts of solar heat collectors not provided for in groups F24S10/00-F24S70/00
- F24S80/50—Elements for transmitting incoming solar rays and preventing outgoing heat radiation; Transparent coverings
- F24S80/58—Elements for transmitting incoming solar rays and preventing outgoing heat radiation; Transparent coverings characterised by their mountings or fixing means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
- Y02E10/44—Heat exchange systems
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- Mechanical Engineering (AREA)
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- Combustion & Propulsion (AREA)
- Sustainable Development (AREA)
- General Engineering & Computer Science (AREA)
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- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Abstract
The invention discloses a low-temperature annealing process for reducing stress of a glass-metal sealing structure, which comprises the following steps: the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace; step two: raising the temperature from room temperature to 200 ℃; step three: raising the temperature from 200 ℃ to 350 ℃; step four: raising the temperature from 350 ℃ to 450 ℃; step five: raising the temperature from 450 ℃ to 520 ℃; step six: reducing the temperature from 520 ℃ to 470 ℃; step seven: reducing the temperature from 470 ℃ to 370 ℃; step eight: reducing the temperature from 370 ℃ to 300 ℃; step nine: the temperature was reduced from 300 ℃ to room temperature. The invention uses the temperature below the glass strain point to carry out annealing treatment on the glass-metal sealing part, greatly reduces the stress value of the sealing part, improves the safety and reliability of the sealing part, and improves the qualification rate of products, thereby improving the effective life of the whole product.
Description
Technical Field
The invention relates to the technical field of a heat collecting tube glass-metal sealing structure annealing process, in particular to a low-temperature annealing process for reducing stress of a glass-metal sealing structure.
Background
The middle-high temperature solar heat collecting tube mainly comprises a glass outer tube with an antireflection coating and a metal inner tube with a solar selective absorption coating, is a key component for carrying out light-heat-electricity conversion of a solar photo-thermal power station, the reliability of the middle-high temperature solar heat collecting tube influences the normal operation of the power station to a great extent, the weakest part of the heat collecting tube is too much used at a glass-metal sealing part where the glass outer tube is connected with the metal inner tube, the glass and the metal cannot be completely consistent on line expansion due to the essential difference of the physical properties of the glass and the metal, so that the glass and the metal cannot avoid certain structural stress in the sealing process, the existence of the structural stress is a great hidden danger for the heat collecting tube, once the stress is released under a certain special condition, the sealing part generates cracks, the sealing part is directly damaged, and once the sealing part is damaged, the vacuum formed by the glass outer sleeve and the metal inner tube disappears, so that the solar selective absorption coating is directly exposed in the air, the aging attenuation of the film layer can be accelerated by the high-temperature oxidation environment, in addition, because the vacuum environment is not protected, the metal inner tube can absorb the light energy and simultaneously dissipate a large amount of heat energy to the outside, namely, the heat loss is increased, the light-heat conversion efficiency of the heat collecting tube is greatly reduced, the service life of the heat collecting tube is influenced, and the use cost is increased.
Because the linear expansion coefficient between the glass and the metal is only matched within a certain temperature range, corresponding structural stress is inevitably generated, if the generated structural stress is too large, temporary stress generated by cold and hot impact is superposed with the structural stress, the glass at the sealing part is likely to break, generally, the annealing temperature of the borosilicate glass is 550 +/-10 ℃, the glass tube and the sealing part are annealed at the temperature, the stress at the glass sealing part can be eliminated, but the stress value at the glass-metal sealing part after annealing shows larger stress value fluctuation compared with the condition before annealing, the stress value at the sealing part does not show a trend of descending all the time, but also shows descending all the time, the descending amplitude is not large, only 10 percent, so that the stress at the sealing part is still in a dangerous interval of 160 and 180nm/cm (note: the unit represents the birefringence optical path difference, it is generally believed that the resultant of temporary and structural stresses caused by external temperature differences above 120nm/cm may cause glass cracking
Disclosure of Invention
The invention aims to avoid the defects in the prior art and provides a low-temperature annealing process for reducing the stress of a glass-metal sealing structure, thereby effectively solving the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that: a low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature at 200 ℃ for 10-30 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 3-8 ℃/min, and the temperature is kept at 350 ℃ for 30-60 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 3-8 ℃/min, and the temperature is kept at 350 ℃ for 30-60 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 3-6 ℃/min, and the temperature is kept at 520 ℃ for 60-100 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 3-6 ℃/min, and keeping the temperature at 350 ℃ for 60-100 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 3-8 ℃/min, and keeping the temperature at 350 ℃ for 30-60 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 3-8 ℃/min, and keeping the temperature at 350 ℃ for 30-60 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
Further, in the second step, the heating rate is 8 ℃/min, and the heat preservation time is 20 min.
Further, in the third step, the heating rate is 7 ℃/min, and the heat preservation time is 40 min.
Further, in the fourth step, the temperature rising rate is 6 ℃/min, and the heat preservation time is 40 min.
Further, in the fifth step, the heating rate is 4 ℃/min, and the heat preservation time is 70 min.
Further, in the sixth step, the cooling rate is 4 ℃/min, and the heat preservation time is 70 min.
Further, in the seventh step, the cooling rate is 6 ℃/min, and the heat preservation time is 40 min.
Further, in the eighth step, the cooling rate is 8 ℃/min, and the heat preservation time is 40 min.
The technical scheme of the invention has the following beneficial effects: according to the comparison of the expansion curves of the glass and the metal, the contact ratio of the glass and the metal is higher within 520 ℃, and the difference gradually becomes larger after the temperature is exceeded; in addition, the reduction of the annealing temperature can reduce the consumption of electric energy, and the effects of energy conservation and consumption reduction are achieved.
Detailed Description
The following examples further describe embodiments of the present invention in detail. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
A low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace, wherein the inner diameter of the glass outer tube at the glass-metal sealing section is phi 125, and the wall thickness is 3mm (the same below);
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 5 ℃/min, and keeping the temperature at 200 ℃ for 30 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 3 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 3 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 3 ℃/min, and the temperature is kept at 520 ℃ for 70 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 3 ℃/min, and keeping the temperature at 350 ℃ for 70 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 3 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 3 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
Through detection, the structural stress of the glass-metal sealing part in the embodiment is 45 nm/cm.
Example 2
A low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 7.5 ℃/min, and keeping the temperature at 200 ℃ for 20 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 5 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 5 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 5 ℃/min, and the temperature is kept at 520 ℃ for 70 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 5 ℃/min, and keeping the temperature at 350 ℃ for 70 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 5 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 5 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
Through detection, the structural stress of the glass-metal sealing part in the embodiment is 75 nm/cm.
Example 3
A low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 10 ℃/min, and keeping the temperature at 200 ℃ for 20 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 8 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 8 ℃/min, and the temperature is kept at 350 ℃ for 40 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 6 ℃/min, and the temperature is kept at 520 ℃ for 70 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 6 ℃/min, and keeping the temperature at 350 ℃ for 70 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 8 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 8 ℃/min, and keeping the temperature at 350 ℃ for 40 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
The structural stress at the glass-metal seal in this example was examined to be 105 nm/cm.
Comparative example 1
A low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 15 ℃/min, and keeping the temperature at 200 ℃ for 15 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept for 15min at 350 ℃;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept for 15min at 350 ℃;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept for 15min at 520 ℃;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 15 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 15 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 15 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
Through detection, the structural stress of the glass-metal sealing part in the embodiment is 185 nm/cm.
Comparative example 2
A low-temperature annealing process for reducing stress of a glass-metal sealing structure comprises the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 20 ℃/min, and keeping the temperature at 200 ℃ for 30 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept at 350 ℃ for 30 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept at 350 ℃ for 30 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 10 ℃/min, and the temperature is kept at 520 ℃ for 30 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 30 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 30 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 10 ℃/min, and keeping the temperature at 350 ℃ for 30 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
Through detection, the structural stress of the glass-metal sealing part in the embodiment is 165 nm/cm.
Table 1: stress value comparison table
As can be seen from the comparison in Table 1, the annealing temperature interval, the temperature change rate and other parameters in the invention can greatly reduce the structural stress at the glass-metal sealing part.
The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Claims (8)
1. A low-temperature annealing process for reducing stress of a glass-metal sealing structure is characterized by comprising the following steps:
the method comprises the following steps: putting the sealed glass-metal sealing section into an annealing furnace;
step two: heating the temperature in the annealing furnace from room temperature to 200 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature at 200 ℃ for 10-30 min;
step three: raising the temperature in the annealing furnace from 200 ℃ to 350 ℃, wherein the raising rate is 3-8 ℃/min, and the temperature is kept at 350 ℃ for 30-60 min;
step four: raising the temperature in the annealing furnace from 350 ℃ to 450 ℃, wherein the raising rate is 3-8 ℃/min, and the temperature is kept at 350 ℃ for 30-60 min;
step five: raising the temperature in the annealing furnace from 450 ℃ to 520 ℃, wherein the raising rate is 3-6 ℃/min, and the temperature is kept at 520 ℃ for 60-100 min;
step six: reducing the temperature in the annealing furnace from 520 ℃ to 470 ℃, wherein the temperature reduction rate is 3-6 ℃/min, and keeping the temperature at 350 ℃ for 60-100 min;
step seven: reducing the temperature in the annealing furnace from 470 ℃ to 370 ℃, wherein the temperature reduction rate is 3-8 ℃/min, and keeping the temperature at 350 ℃ for 30-60 min;
step eight: reducing the temperature in the annealing furnace from 370 ℃ to 300 ℃, wherein the temperature reduction rate is 3-8 ℃/min, and keeping the temperature at 350 ℃ for 30-60 min;
step nine: and (3) reducing the temperature in the annealing furnace from 300 ℃ to room temperature, and adopting a natural cooling mode.
2. The process of claim 1, wherein in the second step, the temperature rise rate is 8 ℃/min and the holding time is 20 min.
3. The low-temperature annealing process for reducing the stress of a glass-metal sealing structure according to claim 1, wherein in the third step, the temperature rise rate is 7 ℃/min, and the holding time is 40 min.
4. The process of claim 1, wherein in step four, the temperature rise rate is 6 ℃/min and the holding time is 40 min.
5. The low-temperature annealing process for reducing the stress of a glass-metal sealing structure according to claim 1, wherein in the fifth step, the temperature rise rate is 4 ℃/min, and the holding time is 70 min.
6. The low-temperature annealing process for reducing the stress of a glass-metal sealing structure according to claim 1, wherein in the sixth step, the temperature reduction rate is 4 ℃/min, and the holding time is 70 min.
7. The low-temperature annealing process for reducing the stress of a glass-metal sealing structure according to claim 1, wherein in the seventh step, the temperature reduction rate is 6 ℃/min, and the holding time is 40 min.
8. The low-temperature annealing process for reducing the stress of a glass-metal sealing structure according to claim 1, wherein in step eight, the temperature reduction rate is 8 ℃/min, and the holding time is 40 min.
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| CN112573841A (en) * | 2020-12-28 | 2021-03-30 | 西安赛尔电子材料科技有限公司 | Multi-pin connector for glass-metal sealing and sealing process |
| CN113277748A (en) * | 2021-07-07 | 2021-08-20 | 泰极微(成都)技术发展有限公司 | Method for packaging metal needle by glass and glass packaging product |
| CN115180809A (en) * | 2022-07-01 | 2022-10-14 | 毛立国 | Low-stress glass production system and control method |
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