CN113461337A - Packaging glass for thermocouple and preparation and packaging methods thereof - Google Patents
Packaging glass for thermocouple and preparation and packaging methods thereof Download PDFInfo
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- CN113461337A CN113461337A CN202110748800.1A CN202110748800A CN113461337A CN 113461337 A CN113461337 A CN 113461337A CN 202110748800 A CN202110748800 A CN 202110748800A CN 113461337 A CN113461337 A CN 113461337A
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- 239000011521 glass Substances 0.000 title claims abstract description 66
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 11
- 238000002360 preparation method Methods 0.000 title description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 12
- 239000005394 sealing glass Substances 0.000 claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 29
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 21
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 21
- PEUPIGGLJVUNEU-UHFFFAOYSA-N nickel silicon Chemical compound [Si].[Ni] PEUPIGGLJVUNEU-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 16
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 11
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 abstract description 5
- 229910007676 ZnO—SiO2 Inorganic materials 0.000 abstract description 4
- 239000003566 sealing material Substances 0.000 abstract description 4
- DBUTVDSHVUGWOZ-UHFFFAOYSA-N [Si].[Ni].[Cr].[Ni] Chemical compound [Si].[Ni].[Cr].[Ni] DBUTVDSHVUGWOZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002241 glass-ceramic Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- 229910021484 silicon-nickel alloy Inorganic materials 0.000 abstract description 2
- 238000009736 wetting Methods 0.000 abstract description 2
- 239000011257 shell material Substances 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000011049 filling Methods 0.000 description 5
- 239000001993 wax Substances 0.000 description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
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Classifications
-
- 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
- C03C12/00—Powdered glass; Bead compositions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K1/00—Details of thermometers not specially adapted for particular types of thermometer
- G01K1/08—Protective devices, e.g. casings
- G01K1/10—Protective devices, e.g. casings for preventing chemical attack
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K1/00—Details of thermometers not specially adapted for particular types of thermometer
- G01K1/08—Protective devices, e.g. casings
- G01K1/12—Protective devices, e.g. casings for preventing damage due to heat overloading
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a packaging glass for a thermocouple, wherein P2O5 has a nucleation effect in the glass and is matched with K2O and MgO can increase Li2O‑ZnO‑SiO2The linear expansion coefficient of the glass ceramics is set to be 116-130 x 10‑7The temperature is approximate to the high-temperature alloy GH3039, the nickel-chromium alloy and the nickel-silicon alloy at room temperature of-300 ℃, and the sealing material can be used for sealing three metals; b is2O3MgO and Al2O3The combined use has the effects of reducing the wetting angle of glass and metal, improving the bonding force of the glass and the metal, and ensuring that the leakage rate of the sealing glass is lower than 1 multiplied by 10 after the sealing glass is used at the temperature of 350 ℃ at most‑10Pa.m 3/s, insulation resistance up toInfinity, and the sealed product has high mechanical strength and can pass the vibration test specified by GJB150.16A; BaO is added in the invention, and the component can adjust the softening temperature of glass, so that the disordered arrangement of internal atoms of the nickel-chromium-nickel-silicon material of the thermocouple can be avoided after the glass sealing, and the precision of the thermocouple after the glass sealing can meet the requirement of +/-0.004T DEG C specified in GB/T16839.2.
Description
Technical Field
The invention relates to the technical field of glass, in particular to packaging glass for a thermocouple and a preparation method and a packaging method thereof.
Background
The working environment of the high-temperature section of the modern aeroengine is severe, and the gas temperature of the modern aeroengine is mainly measured by an armored thermocouple. Insulation resistance is an important index of the armored thermocouple, and shunt errors can be introduced into temperature measurement due to the reduction of the insulation resistance, so that the test precision of the armored thermocouple is influenced, and therefore, the sealing of the output end of the armored thermocouple is particularly important.
The sealing material at the output end of the armored thermocouple depends on the temperature of the use environment, and can be sealed by silicon rubber and epoxy resin when the temperature is lower than 300 ℃, and sealed by glass when the temperature is higher than 300 ℃. The aviation armored thermocouple has high requirement on the corrosion resistance of a shell material, so that the traditional kovar alloy suitable for glass sealing cannot be used, the aviation armored thermocouple shell generally uses a high-temperature alloy GH3039 (the linear expansion coefficient is 132 multiplied by 10 < -7 >/DEG C, the room temperature is 300 ℃ below zero), the inner wire core is a nickel-chromium wire and a nickel-silicon wire (the linear expansion coefficient is 135 multiplied by 10 < -7 >/DEG C, the room temperature is 300 ℃ below zero), tests prove that the air tightness of the aviation armored thermocouple can meet the use requirement only when the air tightness reaches 1 multiplied by 10 < -10 > m < -3 >/s under the high-temperature and high-humidity environment of an aeroengine, and the insulation of the armored thermocouple can be reduced only when the traditional glass sealing is used, wherein the air tightness reaches 1 multiplied by 10 < -9 > m < -3 >/s, or even lower. In addition, if the glass sealing temperature can not reach the maximum service temperature of the thermocouple, the precision of the thermocouple is ultra-poor after sealing, and the requirement of +/-0.004T DEG C specified by GB/T16839.2 can not be met.
Li2O-ZnO-SiO2The glass is an important sealing material in glass packaging, and people are increasingly researching the glass, for example, Chinese patent document CN104529164A discloses devitrification type high-expansion glass powder, a preparation method and an application thereof, which comprises the following steps: 30-60 wt% SiO2、10-30wt％ZnO、5-15wt％Li2O、0-5wt％Al2O3、2-12wt％B2O3、0-8wt％K2O、0-10wt％Na2O、0-10wt％P2O5And 0-10 wt% NiO, Fe2O3And/or Cr2O3The sum of the weight fractions of the components is 100 percent. However, in the above-mentioned documents, Li is adjusted2O-ZnO-SiO2Is a glass composition formula, which has an expansion coefficient of 130--7In the range of/° c, enabling it to be sealed in high expansion metal devices. However, when it is applied to a sheathed thermocouple, its accuracy exceeds the national standard requirements and the leakage rate is relatively high.
Disclosure of Invention
In order to solve the technical problem, the invention provides packaging glass for a thermocouple, which comprises the following components in parts by weight: SiO 22：50-60wt％，ZnO：10-12wt％，Li2O：8-9wt％，Al2O3：5-7wt％，B2O3：5-7wt％，K2O：4-5wt％，MgO：4-5wt％，P2O5：1-3wt％，BaO：0.5-2wt％。
Further, the paint comprises the following components in parts by weight: SiO 22：55.3wt％，ZnO：10.3wt％，Li2O：8.6wt％，Al2O3：6.0wt％，B2O3：6.7wt％，K2O：4.8wt％，MgO：4.9wt％，P2O5：1.9wt％，BaO：1.5wt％。
The invention also provides a preparation method of the packaging glass for the thermocouple, which comprises the following steps: (1) mixing the components on a ball mill for 7-9h to form a mixture, heating the mixture at 1480-1520 ℃ for 5-7h, then quickly cooling, and grinding after quick cooling to ensure that the particle size is less than or equal to 75 micrometers to obtain glass powder; (2) mixing glass powder and high-purity paraffin according to the mass ratio of 25-35:1, stirring and mixing at 70-90 ℃, then performing dry pressing molding, and performing structural heat preservation and dewaxing to obtain a glass blank; as for the molding structure, without particular limitation, a cylindrical band having two or 4 holes is preferable; as for the rapid cooling, that is, the cooling process, there is no particular limitation, and natural cooling with air may be specifically employed.
The invention also provides a method for encapsulating the glass for the thermocouple, which comprises the steps of assembling the high-temperature alloy GH3039 shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then preserving the heat for 30-50min at the temperature of 1020-.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the P2O5 in the packaging glass for the thermocouple has the nucleation effect in the glass and is matched with K2O and MgO can increase Li2O-ZnO-SiO2The linear expansion coefficient of the glass ceramics is set to be 116-130 x 10-7The temperature is approximate to the high-temperature alloy GH3039, the nickel-chromium alloy and the nickel-silicon alloy at room temperature of-300 ℃, and the sealing material can be used for sealing three metals; b is2O3MgO and Al2O3The combined use has the effects of reducing the wetting angle of glass and metal, improving the bonding force of the glass and the metal, and ensuring that the leakage rate of the sealing glass is lower than 1 multiplied by 10 after the sealing glass is used at the temperature of 350 ℃ at most-10Pa.m 3/s, the insulation resistance can reach infinity, and simultaneously, the sealed product has very high mechanical strength and can pass a vibration test specified by GJB150.16A; BaO is added, the softening temperature of the glass is adjusted, the disordered arrangement of atoms in the nickel-chromium-nickel-silicon material of the thermocouple can be guaranteed after the glass sealing, the precision of the thermocouple after the glass sealing can meet the requirement of +/-0.004T DEG C specified by GB/T16839.2, and the precision error is plus or minus 4 degrees taking 1000 ℃ as an example.
(2) According to the preparation method and the packaging method of the packaging glass for the thermocouple, disclosed by the invention, when the glass blank prepared from the glass raw materials is used for preparing the thermocouple, the mechanical strength is high, the leakage rate is low, and the precision meets the national standard requirement.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to derive other drawings without creative efforts.
FIG. 1 is a diagram of the packaging effect of the present invention;
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. The embodiments in the present invention, other embodiments obtained by persons skilled in the art without any inventive work, belong to the protection scope of the present invention.
Example 1
1) Weighing the following components in parts by weight: SiO 22：55.3wt％，ZnO：10.3wt％，Li2O：8.6wt％，Al2O3：6.0wt％，B2O3：6.7wt％，K2O：4.8wt％，MgO：4.9wt％，P2O5：1.9wt％，BaO：1.5wt％；
2) Mixing the components on a ball mill for 8 hours, heating the mixture in a crucible at 1495 ℃ for 6 hours, then cooling the mixture by air, naturally cooling the mixture, and then grinding the mixture to obtain glass powder with the particle size of 75 microns at most;
3) mixing the glass powder with the high-purity paraffin wax slices (mass ratio is 30:1), stirring and mixing at 80 ℃, then performing dry pressing and molding, and then performing heat preservation at 610 ℃ for 4 hours to remove wax to prepare a glass blank;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
d) Assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then filling nitrogen into a vacuum furnace, maintaining the temperature of 1055 ℃ for 40min, cooling along with the furnace, and taking out to obtain the thermocouple.
Example 2
1) Weighing the following components in parts by weight: SiO 22：50wt％，ZnO：12wt％，Li2O：9wt％，Al2O3：7wt％，B2O3：7wt％，K2O：5wt％，MgO：5wt％，P2O5：3wt％，BaO：2wt％；
2) Mixing the components on a ball mill for 7 hours, heating the mixture in a crucible at the temperature of 1480 ℃ for 5 hours, then cooling the mixture with air, and grinding the mixture after natural cooling to obtain glass powder with the particle size of 75 microns at most;
3) mixing glass powder and high-purity paraffin wax slices (mass ratio is 25:1), stirring and mixing at 70 ℃, then performing dry pressing and molding, and then performing heat preservation at 610 ℃ for 4 hours to remove wax to prepare a glass blank;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
d) And assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then filling nitrogen into a vacuum furnace, maintaining the temperature at 1020 ℃ for 30min, cooling along with the furnace, and taking out to obtain the thermocouple.
Example 3
1) Weighing the following components in parts by weight: SiO 22：60wt％，ZnO：10wt％，Li2O：8.5wt％，Al2O3：5wt％，B2O3：5.5wt％，K2O：4wt％，MgO：5wt％，P2O5：1.5wt％，BaO：0.5wt％；
2) Mixing the components on a ball mill for 9h, heating the mixture in a crucible at 1520 ℃ for 6h, then cooling the mixture by air, and grinding the mixture after natural cooling to obtain glass powder with the particle size of 75 microns at most;
3) mixing glass powder and high-purity paraffin wax slices (mass ratio is 35:1), stirring and mixing at 90 ℃, then performing dry pressing and molding, and then performing heat preservation at 610 ℃ for 4 hours to remove wax to prepare a glass blank;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
d) And assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then filling nitrogen into a vacuum furnace, maintaining the temperature at 1070 ℃ for 50min, cooling along with the furnace, and taking out to obtain the thermocouple.
Example 4
1) Weighing the following components in parts by weight: SiO 22：59wt％，ZnO：11wt％，Li2O：8wt％，Al2O3：6wt％，B2O3：5wt％，K2O：4.5wt％，MgO：4.5wt％，P2O5：1wt％，BaO：1wt％；
2) Mixing the components on a ball mill for 8 hours, heating the mixture in a crucible at 1495 ℃ for 5 hours, then cooling the mixture with air, and grinding the mixture after natural cooling to obtain glass powder with the particle size of 75 microns at most;
3) mixing the glass powder with the high-purity paraffin wax slices (mass ratio is 30:1), stirring and mixing at 80 ℃, then performing dry pressing and molding, and then performing heat preservation at 610 ℃ for 4 hours to remove wax to prepare a glass blank;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
d) Assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then filling nitrogen into a vacuum furnace, maintaining the temperature of 1055 ℃ for 40min, cooling along with the furnace, and taking out to obtain the thermocouple.
Comparative example 1
1) Weighing the following components in parts by weight: SiO 22：56.8wt％，ZnO：10.3wt％，Li2O：8.6wt％，Al2O3：6.0wt％，B2O3：6.7wt％，K2O：4.8wt％，MgO：4.9wt％，P2O5：1.9wt％；
2) Mixing the components on a ball mill for 8 hours, heating the mixture in a crucible at 1495 ℃ for 6 hours, then cooling the mixture with air, and grinding the mixture after natural cooling to obtain glass powder with the particle size of 75 microns at most;
3) mixing the glass powder with the high-purity paraffin wax slices (mass ratio is 30:1), stirring and mixing at 80 ℃, then performing dry pressing and molding, and then performing heat preservation at 610 ℃ for 4 hours to remove wax to prepare a glass blank;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
d) Assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then filling nitrogen into a vacuum furnace, maintaining the temperature of 1055 ℃ for 40min, cooling along with the furnace, and taking out to obtain the thermocouple.
Comparative example 2
1) Weighing the following components in parts by weight: SiO 22：55wt％，ZnO：13wt％，Li2O：11wt％，Al2O3：2wt％，B2O3：4wt％，Na2O：6wt％，P2O5：4wt％，Fe2O3：5wt％；
2) The components are fully and uniformly mixed and then are put into a crucible, a crucible cover is added, and the temperature is kept for 2 hours in a 1480-DEG silicon-molybdenum rod electric furnace;
3) then, rolling, crushing, drying and ball-milling the melted glass liquid to form particles with the particle size of 50 particles at most;
4) and (3) deoiling and cleaning the shell, the nickel-chromium wire core and the nickel-silicon wire core, then placing the shell, the nickel-chromium wire core and the nickel-silicon wire core in a common box furnace at 700 ℃, preserving heat for 10min, and then taking out for air cooling.
5) Assembling the shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass particle powder, preserving heat for 40min at 1055 ℃ in a vacuum nitrogen protection furnace, and cooling along with the furnace; and finally, carrying out heat treatment at 671 ℃ for 3.5 h.
Test example 1
The surface effect observation of the thermocouple obtained in example 1 shows that the glass is tightly combined with the wire core and the shell, the unshelling phenomenon does not occur, and the formed glass has no air holes and a smooth surface.
Test example 2
The thermocouples obtained in examples 1 to 4 and comparative examples 1 to 2 were subjected to a test of thermal expansion coefficient, leak rate, and thermocouple accuracy. The specific method comprises the following steps: the thermal expansion coefficient is tested according to the method specified in GB/T1697-2015; the leak rate was tested according to the method specified in section 1008 of GJB 1217; thermocouple accuracy was tested according to the method specified in section 6.3 of JB/T8205-1999.
Wherein the thermal expansion coefficient results, leakage rate results and accuracy results are shown in Table 1
In conclusion, through the tests, compared with the comparative example 1, the results of the 3 tests are that the effect of the thermocouple obtained by the invention is far better than that of the comparative example 1; in comparative example 2, although the thermal expansion coefficient was substantially the same as the result of the present invention, the effect was far less excellent in terms of leakage rate and accuracy than that of the thermocouple obtained by the present invention.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (4)
1. The packaging glass for the thermocouple is characterized by comprising the following components in parts by weight: SiO 22：50-60wt％，ZnO：10-12wt％，Li2O：8-9wt％，Al2O3：5-7wt％，B2O3：5-7wt％，K2O：4-5wt％，MgO：4-5wt％，P2O5：1-3wt％，BaO：0.5-2wt％。
2. The sealing glass for a thermocouple according to claim 1, characterized in that it comprises the following components in parts by weight: SiO 22：55.3wt％，ZnO：10.3wt％，Li2O：8.6wt％，Al2O3：6.0wt％，B2O3：6.7wt％，K2O：4.8wt％，MgO：4.9wt％，P2O5：1.9wt％，BaO：1.5wt％。
3. A method for producing the sealing glass for a thermocouple according to claim 1 or 2, characterized in that: (1) mixing all the components on a ball mill for 7-9h to form a mixture, heating the mixture at 1480-1520 ℃ for 5-7h, then quickly cooling, and grinding after quick cooling to ensure that the particle size is less than or equal to 75 micrometers to obtain glass powder; (2) mixing the glass powder and the high-purity paraffin according to the mass ratio of 25-35:1, stirring and mixing at 70-90 ℃, then performing dry pressing molding, and performing structural heat preservation and dewaxing to obtain a glass blank.
4. A method for sealing a sealing glass for a thermocouple according to claim 1 or 2, comprising: assembling the high-temperature alloy GH3039 shell, the nickel-chromium wire core, the nickel-silicon wire core and the glass blank, then preserving the heat for 30-50min at the temperature of 1020-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110748800.1A CN113461337A (en) | 2021-07-02 | 2021-07-02 | Packaging glass for thermocouple and preparation and packaging methods thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110748800.1A CN113461337A (en) | 2021-07-02 | 2021-07-02 | Packaging glass for thermocouple and preparation and packaging methods thereof |
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| CN113461337A true CN113461337A (en) | 2021-10-01 |
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| CN202110748800.1A Pending CN113461337A (en) | 2021-07-02 | 2021-07-02 | Packaging glass for thermocouple and preparation and packaging methods thereof |
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| CN (1) | CN113461337A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2035289A (en) * | 1978-11-28 | 1980-06-18 | Standard Telephones Cables Ltd | Glass for encapsulation of semiconductor devices |
| CN104529164A (en) * | 2014-12-17 | 2015-04-22 | 中国科学院上海硅酸盐研究所 | Devitrification type high-expansion sealing glass powder as well as preparation method and application thereof |
| CN106882922A (en) * | 2015-12-16 | 2017-06-23 | 辽宁省轻工科学研究院 | A kind of seal glass of resistance to 550 DEG C of high temperature and preparation method thereof |
| CN108423998A (en) * | 2018-05-31 | 2018-08-21 | 北京北旭电子材料有限公司 | Glass powder composition, glass sealing material and preparation method thereof and battery |
| CN111170639A (en) * | 2019-12-30 | 2020-05-19 | 西安赛尔电子材料科技有限公司 | Glass material for sensor sealing and preparation method thereof |
-
2021
- 2021-07-02 CN CN202110748800.1A patent/CN113461337A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2035289A (en) * | 1978-11-28 | 1980-06-18 | Standard Telephones Cables Ltd | Glass for encapsulation of semiconductor devices |
| CN104529164A (en) * | 2014-12-17 | 2015-04-22 | 中国科学院上海硅酸盐研究所 | Devitrification type high-expansion sealing glass powder as well as preparation method and application thereof |
| CN106882922A (en) * | 2015-12-16 | 2017-06-23 | 辽宁省轻工科学研究院 | A kind of seal glass of resistance to 550 DEG C of high temperature and preparation method thereof |
| CN108423998A (en) * | 2018-05-31 | 2018-08-21 | 北京北旭电子材料有限公司 | Glass powder composition, glass sealing material and preparation method thereof and battery |
| CN111170639A (en) * | 2019-12-30 | 2020-05-19 | 西安赛尔电子材料科技有限公司 | Glass material for sensor sealing and preparation method thereof |
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