CN1387815A - Metal vacuum double-layer container and its producing method, composition for sealing - Google Patents
Metal vacuum double-layer container and its producing method, composition for sealing Download PDFInfo
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- CN1387815A CN1387815A CN 02122048 CN02122048A CN1387815A CN 1387815 A CN1387815 A CN 1387815A CN 02122048 CN02122048 CN 02122048 CN 02122048 A CN02122048 A CN 02122048A CN 1387815 A CN1387815 A CN 1387815A
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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Abstract
The invention provide a metallic vacuum double container includes inner and outer containers 1 and 2, form a vacuum heat insulation space by sealing with inner and outer containers 1, 2. The purpose is attained by carrying out the sealing using a low melting point glass sealing material 43 having a softening temperature higher than fluorocarbon coating sintering temperature and degassing temperature at the time of evacuation, and which does not contain ingredients having food hygienical problem.
Description
Technical field
The invention relates to a kind of metal vacuum double-layer container and manufacture method thereof, used sealing compositions.As: the present invention relates to diet such as insulating pot, portable thermos, incubation canteen, warm enamelware pot, magnetic cup metal vacuum double-layer container and manufacture method and composition for sealing.
Background technology
Between metal vacuum double-layer container inner pressurd vessel and outer container vacuum heat-insulating layer is arranged, heat insulating ability is very high, so consider from aspects such as low heat conductivity, corrosion resistance, high strength faces, mainly uses stainless steel material.For between inner pressurd vessel and outer container, forming vacuum heat-insulating layer, at first, become vacuum by the steam vent discharged air, then, under the maintenance vacuum state, seal steam vent with encapsulant and sealed.
Be to improve exhaust efficiency, vacuum exhaust will be carried out in the heat air in heating furnace, seals to be treated to, and under the vacuum exhaust state, encapsulant is softening and even dissolve, and seal vents makes sealing material curing then.
During vacuum exhaust, the high more exhaust efficiency of temperature is high more, but, if temperature is very high, make encapsulant soften, dissolve, then be not about to earlier encapsulant be installed on the outer container.But will be difficult however, keeping the vacuum exhaust following later stage of state to place encapsulant.Therefore, in the past, the vacuum exhaust temperature was set at fusing point less than encapsulant, and temperature was increased to the temperature that encapsulant softens, dissolves, and then seals processing under the vacuum state keeping.
The disclosed technology of Te Kaiping 06-169850 communique is: the use softening temperature dissolves glass as encapsulant at 200 ℃～600 ℃ low temperature, and the vacuum exhaust temperature is controlled at 200 ℃～600 ℃ from original about 950 ℃ high-temperature exhaust air.
In above-mentioned communique, dissolve glass as low temperature, use B
2O
3-PbO series, B
2O
3-ZnO series, PbO-B
2O
3-ZnO-SiO
2Series, PbO-B
2O
3-Al
2O
3-SiO
2Series, PbO-B
2O
3-SiO
2Series, PbO-B
2O
3-BaO-SiO
2The solder glass of series.
Like this, can realize that cryopumping, low temperature seal, and reduce the cost of special vacuum furnace.And, under the unoxidized situation of metal system double container, need not remove the operation of oxide.The soakage of encapsulant and double container is good, the yield rate height.Because double container is that process annealing forms, so, compare the hardness height with high annealing.These are its strong point.
In interior outer container, added on the surface of at least one in the metal vacuum double-layer container of fluorine coating, as shown in Figure 4, fluorine coating bake temperature up to 380 ℃, reach 400 ℃ sometimes.Therefore,, use metal encapsulant such as Ni scolder to seal processing, the high temperature in the time of then can baking and destroy and seal because of fluorine coating thereafter if to the additional metal vacuum double-layer container that fluorine coating is arranged.
But, if use the metal encapsulant, then since seal treatment temperature can be up to 1010 ℃ about, so cryopumping, low temperature can't obtain using the low-melting glass encapsulant time seal the benefit of being brought.
Again, even use the hot mastication point metal encapsulant identical with glass sealing material, but because described material is main component with lead, so can exert an influence to human body, environment, device.Be not suitable for the diet cool-bag especially.At present, seal handling part and be, prevent plumbous immersion stripping because of water by pasting immersion such as the anti-sealing of diaphragm seal, but during its operation cost.In the vacuum furnace of vacuum, heating, the metal oxide composition in the softening and even encapsulant that dissolves also can evaporate in the air that is spread in vacuum exhaust, thereby is difficult to the operating personnel is isolated fully.Therefore, the operating personnel must take to wear protection countermeasure such as mask and protective garment, and like this, health moves and just is restricted, and operational difficulty influences operating efficiency.In a word, can cause increases too much expense, causes manufacturing cost to rise.And in vacuum furnace, the lead that disperses can adhere to, be piled up in the stove inner face.The lead of piling up is owing to be to be in so-called evaporation state, thus be difficult to remove, and, can become the secondary lead source of loosing, so can shorten device lifetime,, thereby make the product cost increase because the maintenance and the replacing of device cause circulation capital to increase.
Even dissolve again and utilize to using leaded encapsulant to seal inside and outside the stainless steel of processing container, owing to residual in the stainless steel of dissolving a large amount of lead is arranged, so can't utilize again.
In addition, there are very big gap in existing low-melting glass encapsulant and stainless thermal coefficient of expansion, aspect connecting airtight property, sealing, hinder the raising of yield rate.
Main purpose of the present invention is, provides a kind of and do not have environmental issue, is beneficial to stainless cycling and reutilization, has the excellent low-melting glass encapsulant of handling yield rate that seals, seal with it, and the additional metal vacuum double-layer container that fluorine coating is arranged.And provide a kind of solve existing influence human body, environment, device, hinder in the outer container dissolving utilize again, with stainless connecting airtight property and manufacture method problem, better metal vacuum double-layer container such as sealing is low, the finished product rate can't improve, and glass for sealing composition.
Summary of the invention
For achieving the above object, a kind of like this metal vacuum double-layer container of metal vacuum double-layer container system of the present invention: described metal vacuum double-layer container is handled by the vacuum exhaust of steam vent, in stainless steel (layer) container and outside form vacuum heat-insulating layer between (layer) container, the additional container that fluorine coating is arranged is gone up at least one surface in the interior outer container, it is characterized in that: the low-melting glass encapsulant of the degassing temperature when being higher than fluorine coating and being baked temperature and vacuum exhaust by softening point seals steam vent, to seal is a basic structure, and above-mentioned low-melting glass encapsulant can not influence at interior outer container, utilization again after outer container dissolves simultaneously in making.
Another feature is, though lead is the same with other heavy metals, and existing problems aspect food hygiene, and the low-melting glass encapsulant that steam vent is sealed of the present invention does not contain the composition that influences food hygiene.
Feature of the present invention also is: can utilize that to require corresponding low-melting glass encapsulant be that a thermal coefficient of expansion is 25 * 10 less than stainless thermal coefficient of expansion, coefficient of thermal expansion differences with aforesaid coating fluorine and food hygiene, stainless dissolving again
-7The encapsulant that/K is following.
If stainless steel is a martensitic stain less steel, then its advantage is: seal even surpass cryopumping and the low temperature that fluorine coating bakes temperature, described material can sensitization yet.
The low-melting glass encapsulant is actually unleaded bismuth glass, and for satisfying above-mentioned characteristic, each content of material is preferably as follows, that is: Bi
2O
3Be that 70～90wt%, ZnO are 0-2wt%, B
2O
3Be 5～29wt%, SiO
2Be 1～15wt%, Al
2O
3Be that 0～10wt%, CuO are 0～10wt%.At this moment, also can use the encapsulant and the glass for sealing composition of other materials such as metal such as Al beyond the salable stainless steel and pottery.
In addition, as mentioned above, be not to use CuO, but, as containing Bi
2O
370～90wt%, ZnO0-2wt%, B
2O
35～28wt%, SiO
21～15wt%, Al
2O
30～10wt%, CuO are the material of 0.5～6wt%, be with B
2O
3Be controlled at 5～28wt%,, then can improve connecting airtight property with metal if must use CuO.
In the above-mentioned characteristic of performance, when making metal vacuum double-layer container, use above-mentioned material, steam vent is passed through between stainless steel inner pressurd vessel and outer container, carry out vacuum exhaust with the temperature that is lower than the encapsulant softening point, after the evacuate air, under vacuum state, the low melting point encapsulant is softened and even melt with the temperature that is higher than the encapsulant softening point, steam vent is sealed processing.
Description of drawings
The metal vacuum double-layer container of Fig. 1 for obtaining in the embodiment of the invention---the cutaway view of electric hot water bottle bottom; Fig. 2 is the whole cutaway view of Fig. 1 electricity water bottle; Temperature when Fig. 3 carries out vacuum exhaust and seals processing for the metal vacuum double-layer container to Fig. 1 and processing time and routine in the past comparative graph; Fig. 4 is for sealing the additional fluorine coating of double container, the temperature changing curve diagram during sintering processes through the metal that seals processing.
Among the figure, 1 is inner pressurd vessel; 2 is outer container; 3 is the vacuum heat-insulation space; 41 is steam vent; 43 is the low-melting glass encapsulant.
The specific embodiment
Embodiment
Specify embodiments of the invention below with reference to figure, so that better the present invention is understood.
As shown in Figure 2, present embodiment is the metal system double container A of a kind of formation electric hot water bottle B that makes with stainless steel.But, also inner pressurd vessel 1 and outer container 2 combinations can be formed vacuum heat-insulating layer at the two, can form any form and purposes.Metal vacuum double-layer container itself can be the combination of inner pressurd vessel 1 and outer container 2, also can form as one.
The electric hot water bottle B of present embodiment is, the metal vacuum double-layer container A synthetic resin system of packing into is adorned outward and formed bodies 23 in the shell 21, by being located at the synthetic resin system shoulder member 22 between outer dress shell 21 and metal vacuum double-layer container A upper end, form the body opening 25 of the oral area 24 of the metal vacuum double-layer container A that passes through body 23, simultaneously, by joint pin the lid 26 of body 23 is fixed on the rear portion, but and switch.Ground floor bottom 28 at metal vacuum double-layer container A places on the heater, and its internal liquid is heated.By electrodynamic pump 31, internal liquid is drained into outside discharge road 31 be connected on the ground floor bottom 28.Be provided with in the lid 26 internal liquid is pressurizeed, be depressed into outside manual pump 33 by discharging road 32.Lid 26 is provided with the metal system inner cap 34 of the oral area 24 that closes the border metal vacuum double-layer container A and steam is drained into outside steam passage 35.On the protuberance 22a of the front portion that projects to shoulder member 22, be provided with guidance panel 36, below protuberance 22a, be provided with the delivery port 32a that downward-sloping opening is discharged road 22.
Heat metal vacuum double-layer container A on the limit, will carry out vacuum exhaust from 41 pairs of inner pressurd vessels 1 of steam vent shown in Figure 1,2 of outer containers.Under vacuum state, steam vent 41 is carried out encapsulation process then.After the encapsulation process, the inner peripheral surface of the inner pressurd vessel 1 of metal vacuum double-layer container A is provided with fluorine coating 37 shown in Figure 2.Metal vacuum double-layer container A also can be used for electric hot water bottle and the vacuum flask that body exposes.At this moment, the outer surface of outer container 2 also can have fluorine coating.A kind of situation is that steam vent 41 is located at the most inboard of outer container 2 depressed parts 40.At depressed part 40 up under the state, to carrying out vacuum exhaust between inner pressurd vessel 1, the outer container 2, in this process, encapsulant will be stablized and is positioned at depressed part 40, and after vacuum exhaust, the softening and even encapsulant spontaneous current that dissolves is to steam vent 41, after the hardening by cooling, seal exhaust outlet 41.In the vacuum heat-insulation space 3 of Xing Chenging, getter 42 is housed like this, in vacuum heat-insulation space 3, absorbs the gas that after this constantly produces, keep required vacuum as degasser.
Fluorine coating is after the formation of filming, and is transported in the stove of temperature about 385 ℃ by conveyer belt and carries out sintering processes.In the processing procedure, follow the tracks of variations in temperature shown in Figure 4, keep about 385 ℃ high temperature.
For carrying out the above-mentioned processing of sealing, the metal vacuum double-layer container A of present embodiment uses low melting point encapsulant 43, like this, and can be not destroyed at fluorine coating sintering temperature lower sealing yet.And, compare with existing metal encapsulant, can under enough low temperature, soften and even melt, realize that cryopumping, low temperature seal.That is to say, after stainless steel inner pressurd vessel 1,2 of outer containers carried out vacuum exhaust and handle, form vacuum heat-insulation space 3, at least scribble in the metal vacuum double-layer container of fluorine coating 37 at inner pressurd vessel 1 or outer container 2 surfaces, 43 pairs of steam vents 41 of low-melting glass encapsulant of degassing temperature seal when being higher than fluorine coating sintering temperature and vacuum exhaust by softening point.Low melting point encapsulant 43 can not take place in the temperature range of sensitization at inner pressurd vessel 1, outer container 2, softening in work hardening can be controlled the temperature range of inner pressurd vessel 1, outer container 2 thickness, fusing, and degassing temperature is lower.As stainless steel, if use martensitic stain less steel such as JIS SUS436, can sensitization under 600 ℃ yet, and can equally with common stainless steel carry out work hardening and handle.
The softening point of low-melting glass encapsulant 43 must be about 380 ℃～600 ℃, in order to avoid be subjected to the influence of fluorine coating sintering temperature.From the angle of effective vacuum exhaust, 600 ℃ of the softening point upper limits of the relative low-melting glass encapsulant 43 of degassing temperature, it preferably is set between 450 ℃～600 ℃.Therefore, the actual softening point range of low-melting glass encapsulant 43 is at 450 ℃～600 ℃.
Like this, present embodiment metal vacuum double-layer container A can carry out vacuum exhaust and seal processing in suitable low-melting glass encapsulant 43, the humidity province lower than metal encapsulant temperature, reduce the wall thickness of the work hardening part that sintering not causes, and, because the softening point of low-melting glass sealing 43 is higher than degassing temperature, so in when operation degassing, softening, fusing is sealed processing conscientiously under indeformable, situation about running off.Because softening point is higher than fluorine coating sintering temperature, so can not destroy the vacuum double-layer container that obtains fluorine coating under the situation of sealing.Owing to use fluorine coating, compare with the container of present use metal encapsulant, in light weight, cost is low simultaneously.
Metal vacuum double-layer container can be used because distortion, damage, stained, variable color, insufficiency, style are aging etc. when former thereby discarded again.When the stainless steel material of discarded metal vacuum double-layer container fuses, owing to use leaded glass sealing material at present, much can remain in the stainless steel composition of fusion, can exert an influence, can't utilize again in food hygiene, environment and to device.
But, in the present embodiment,, can dissolve again stainless steel material and utilize, thereby help energy savings, reduce cost owing to used lead-free low-melting glass encapsulant 43.
Plumbous and other heavy metals etc. are the same, have edible toxicity, and the low-melting glass encapsulant 43 in the present embodiment do not contain the composition of the problem with food hygiene aspect.Therefore, metal vacuum double-layer container A can be used for food service items such as portable thermos, lunch box, warm enamelware pot, magnetic cup.In the in-problem existing low-melting glass encapsulant, seal location only limits to the part of outer container 2, and seals aspect food hygiene, prevent that seal location from touching water and hot water, lead composition can stripping, and the people touches and damage, and is very time-consuming during fabrication.At this problem, by using the lead-free low-melting glass encapsulant 43 of present embodiment, can address this problem, safe in utilization and can reduce cost.In vacuum furnace, seal simultaneously when handling, can not diffuse to the periphery to the harmful lead of people, environment, device etc., therefore needn't take plumbous diffusion countermeasure, and, because device lifetime is long, so metal vacuum double container A makes simply and be with low cost.
Low-melting glass encapsulant 43 thermal coefficient of expansions of present embodiment are less than stainless thermal coefficient of expansion, and coefficient of thermal expansion differences is 25 * 10
-7Below/the K.Low-melting glass encapsulant 43 thermal coefficient of expansions are less than stainless thermal coefficient of expansion, because the contraction during cooling is poor, steam vent is compressing little mutual the connecting airtight property that improved, simultaneously, because both coefficient of thermal expansion differences are little, so, even under above-mentioned compression, can not produce problem such as peel off yet, improve sealing and fixing, and sealed the finished product rate in the processing procedure.
It is the martensitic stain less steel of representative that stainless steel adopts with SUS436, so above cryopumping and the low temperature of fluorine coating sintering temperature seals relatively, its advantage is, can sensitization.
Be bismuth class glass as the low-melting glass encapsulant 43 that satisfies above-mentioned characteristic, contain Bi
2O
3, ZnO, B
2O
3, SiO
2, Al
2O
3, the CuO composition is then better.
Bi
2O
3Be the formation oxide of glass, content is preferably in 70～90wt%.Less than 70wt%, then the softening point of glass is too high, when heat-treating below the temperature about 600 ℃, possibly can't seal.If surpass 90wt%, then glass meeting opaque (crystallization), simultaneously, the glass branchpoint is low excessively.Consider soft spots, melting of glass etc., Bi
2O
3Content is preferably in 75～86wt%.
ZnO is the composition that can improve glass eutectic effect, but also is a kind of vapour pressure height, volatile composition simultaneously.Therefore, under vacuum, can evapotranspire during heat treatment, think and prevent the variation of forming and pollute heat-treatment furnace etc. that its content preferably is controlled at below the 2wt%.Consider the factors such as low fusing of glass, the content of ZnO preferably is controlled at more than the 0.5wt%.
B
2O
3Also be the formation oxide of glass, be the necessary composition of the low fusing of glass.B
2O
3Content is preferably in 5～29wt%.If less than 5wt%, then its low fusing effect is low, and on the contrary, if its content is crossed 29wt%, then its resistance to water can worsen.The low fusing of consideration glass, resistance to water etc., B
2O
3Content preferably be controlled at 6～21wt%.
SiO
2Also being the formation oxide of glass, is the necessary composition of stabilizationization.SiO
2Content be preferably in 1～15wt%.Less than 1wt%, can't reach the effect of stabilized glass.On the contrary, if surpass 15wt%, then softening point can be too high, when heat-treating under the temperature of regulation, possibly can't seal.And when matrix material was metal such as stainless steel, it is too small that thermal coefficient of expansion is compared with matrix material, produces stress, under the connecting airtight property.The stabilisation of consideration glass, softening point, thermal coefficient of expansion etc., SiO
2Content is then better at 2～10wt%.
Al
2O
3For preventing the composition of glass devitrification, stabilized glass, if surpass 10wt%, softening point can be too high, when heat-treating under the temperature of regulation, is difficult to sealing, seals.Consider stabilisation, softening point of glass etc., Al
2O
3Content is then better at 1～6wt%.
CuO can be under metal, the particularly stainless situation at matrix material, can improve the composition of glass and connecting airtight property of stainless steel, and content will be below 10wt%.If surpass 10wt%, then softening point may be low excessively.The connecting airtight property of consideration glass and matrix material, softening point etc., CuO content is then better at 0.5～6wt%.
From above-mentioned situation, bismuth class low-melting glass encapsulant 43 is for satisfying above-mentioned characteristic, and each component content is preferably as follows, Bi
2O
3Content 70～90wt%, ZnO content 0～2wt%, B
2O
3Content 5～29wt%, SiO
2Content 1～15wt%, Al
2O
3Content 0～10wt%, CuO content 0-10wt%.At this moment, also can be used as the glass composition of metal such as Al beyond the relative stainless steel and ceramic material encapsulant.
As mentioned above, CuO is not essential composition, but at Bi
2O
3Content 70～90wt%, ZnO content 0～2wt%, B
2O
3Content 5～28wt%, SiO
2Content 1～15wt%, Al
2O
3In the composition of content 0～10wt%, CuO content 0.5～6wt%, if Bi
2O
3Content is controlled at 5～28wt%, in the time of must using CuO, can improve especially its with the connecting airtight property of metal.
If Bi
2O
3Content 70～90wt%, ZnO content 0～2wt%, B
2O
3Content 5～23wt%, SiO
2Content 1～10wt%, Al
2O
3Content 0～6wt%, CuO content 0.5～6wt% are more suitable for stainless steel is sealed, seals.
Again, if Bi
2O
3Content 70～86wt%, ZnO content 0～2wt%, B
2O
3Content 5～21wt%, SiO
2Content 2～10wt%, Al
2O
3Content 0～6wt%, CuO content 0.5～6wt% are suitable for stainless steel, particularly are suitable for martensitic stain less steel.
As will make low-melting glass encapsulant 43 in the present embodiment be applicable to the matrix material that various materials constitute sealing, seal, then must make thermal coefficient of expansion very approaching mutually.But then, at matrix material desired treatment temp lower seal, sealing can be not destroyed, and, the function that low-melting glass encapsulant 43 soft spots points must can not influence the material of matrix material side and carry the various elements such as semiconductor on it under sealing, sealing temperature.Usually, softening point improves, and coefficient of thermal expansion differences increases.
With martensitic stain less steel and the material that has an equal thermal coefficient of expansion is under the situation of matrix material, and the thermal coefficient of expansion of bismuth class low-melting glass is preferably 82～105 * 10
-7/ K, softening point are preferably 450～550 ℃.The glass branchpoint is preferably 370～450 ℃.
About above-mentioned composition, embodiment 1～6 and 1 comparative example are as shown in table 1 below.
Table 1
*Judge during 1:600 ℃ heat treated soldering,
*Implement 400 ℃ fluorine coating after the 2:600 ℃ of following soldering, judge.
The evaluation of the measurement of the branchpoint of glass, softening point, thermal coefficient of expansion and connecting airtight property, outward appearance, sealing is as follows.
The measurement of glass branchpoint and softening point is as follows: the about 80mg of each powdered sample of about 45～75 μ m of particle diameter is packed in the platinum system micro cell of differential thermal analysis device (DTA), the programming rate that divides with 20K/ makes temperature rise to 800 ℃ from room temperature, measures.The temperature of the initial heat absorption beginning portion shoulder that embodies is the glass branchpoint, is softening point through minimal point to the temperature that heat absorption finishes.
Thermal coefficient of expansion is measured as: use thermo-mechanical analysis device (TMA), sample is the glass bar of the about 5mm of diameter, long 15～20mm, is standard specimen with the quartz glass, and the speed of dividing with 10K/ begins to heat up from room temperature, according to the TMA curve that obtains, try to achieve 30～350 ℃ mean value.
Being evaluated as of connecting airtight property and outward appearance: the about 2mm of diameter, the glass bar that is about 6.5mm are tiled on the exhaust outlet of stainless steel double container, heat-treat with under the downforce, make the state of sealing, estimate at 600 ℃, 15 minutes 1.33Pa.Whether connecting airtight property is connected airtight on exhaust outlet and is estimated with glass flow, and its outward appearance is passed through visual assessment.Outward appearance is the devitrification and have or not bubble and the one-tenth degree is judged by whether mainly.Leak check is by behind 400 ℃ of following fluorine coating sintering, and glass sealing material has or not to be peeled off and come off and enter exhaust outlet and introduce vacuum leak and degree thereof.Be well zero, relatively poor is △, differ to be *.
Here, glass branchpoint, glass softening point, the thermal coefficient of expansion of existing leadization glass low-melting glass encapsulant are as shown in table 2 below.
Table 2
| Current material | |
| The glass branchpoint | ??290℃ |
| Glass softening point | ??355℃ |
| Thermal coefficient of expansion | ??123×10 -7/K |
Again, the thermal coefficient of expansion of used SUS436 is compared as follows shown in the table 3 in present stainless steel cylinder used JIS specification SUS304 and the present embodiment.
Table 3
| Bottle SUS304 | Electric hot water bottle SUS436 | |
| Thermal coefficient of expansion | ??170×10 -7/K | ??104×10 -7/K |
The metal vacuum double-layer container A that has the above-mentioned characteristic of performance for manufacturing, use the material of the foregoing description, as shown in Figure 3, utilize steam vent 41, under the temperature (450 ℃) of the softening point that is lower than low-melting glass encapsulant 43, stainless steel inner pressurd vessel 1 and 2 of outer containers are carried out vacuum exhaust, the degassing, then under the vacuum exhaust state, make low-melting glass encapsulant 43 softening under the temperature of softening point (600 ℃) being higher than, fusing, exhaust outlet 41 is sealed processing, then, temperature about 380 ℃ is carried out fluorine coating sintering, forms fluorine coating 37.
Specifically, as shown in Figure 1, low-melting glass encapsulant 43 is loaded on the depressed part 40 of inner pressurd vessel 1, outer container 2, successively at the uniform velocity by preparation room, the 1st degas chamber～the 3rd degas chamber (each is 30 minutes), at the uniform velocity by braze chamber (about 15 minutes), at the uniform velocity, last by heaterless slow cooling chamber (about 1 hour), pass through N with same constant speed
2The cooling chamber of gas (about 40 minutes).At this moment, in preparation room, be heated to 430 ℃ from the room temperature intensification, and keep this temperature.Then be rapidly heated to 450 ℃, and keep this temperature at the 1st degas chamber.Keep these 450 ℃ at the 2nd degas chamber, the 3rd degas chamber.During this period, the 1st～the 3rd degas chamber is made as the specified vacuum degree, below 1.33Pa, the space pressure between inner pressurd vessel 1 and the outer container 2 is dropped to 1.33Pa.At braze chamber, under the vacuum exhaust state of maintenance and cup uniform pressure state, low-melting glass encapsulant 43 is softened, melts with the sealing temperature about 600 ℃, exhaust outlet 41 is sealed processing, form vacuum heat-insulation space 3.After sealing processing, below the temperature when naturally cooling to vacuum exhaust, at N by heaterless slow cool down chamber
2Gas compartment is forced to be cooled to about normal temperature.Temperature in () among Fig. 3 is a series of treatment temperatures of existing low-melting glass encapsulant.Like this, carry out fluorine coating through the metal vacuum double-layer container A that seals processing after, as shown in Figure 4, be transported to by conveyer belt and carry out sintering processes in the heating furnace that remains on about 385 ℃, form fluorine coating 37.Sintering time is about 30 minutes, and metal vacuum double-layer container A remained on about 380 ℃ at back about 17 minutes.
Utilize the present invention, can carry out vacuum exhaust and seal processing, can reduce because the work hardening wall thickness partly that causes of sintering not in the humidity province that is lower than the metal encapsulant that is fit to the low-melting glass encapsulant.Simultaneously, because the softening point of low-melting glass encapsulant is higher than degassing temperature,, can when the degassing, not introduce softening, fusing, distortion, loss etc. so can seal processing conscientiously.And, because temperature is higher than fluorine coating sintering temperature,, compare with the container of present use metal encapsulant so can owing to add fluorine coating be arranged not destroying additional fluorine coating under the situation of sealing, in light weight, and cost is low.
Claims (10)
1. metal vacuum double-layer container, described metal vacuum double-layer container is to pass through steam vent, the vacuum exhaust processing is carried out in the space of being located between stainless steel inner pressurd vessel and outer container, form the vacuum heat-insulation space, at inner pressurd vessel, at least one surface in the outer container scribbles fluorine coating, it is characterized in that, the low-melting glass encapsulant of the degassing temperature when utilizing its softening point to be higher than fluorine coating sintering temperature and vacuum exhaust, exhaust outlet is sealed processing, even like this inner pressurd vessel and outer container are fused simultaneously, described glass sealing material can not hinder inner pressurd vessel yet, the utilization again of outer container.
2. metal vacuum double-layer container, described metal vacuum double-layer container is to pass through steam vent, the vacuum exhaust processing is carried out in the space of being located between stainless steel inner pressurd vessel and outer container, form the vacuum heat-insulation space, at least one surface in inner pressurd vessel, outer container scribbles fluorine coating, it is characterized in that, the low-melting glass encapsulant of the degassing temperature when utilizing softening point to be higher than fluorine coating sintering temperature and vacuum exhaust seals processing to exhaust outlet, and described low-melting glass encapsulant does not contain the in-problem composition in food hygiene aspect.
3. metal vacuum double-layer container, described metal vacuum double-layer container is to pass through steam vent, the vacuum exhaust processing is carried out in the space of being located between stainless steel inner pressurd vessel and outer container, form the vacuum heat-insulation space, at least one surface in inner pressurd vessel, outer container scribbles fluorine coating, it is characterized in that, the low-melting glass encapsulant of the degassing temperature when utilizing softening point to be higher than fluorine coating sintering temperature and vacuum exhaust seals processing to exhaust outlet, and described low-melting glass encapsulant is not leaded.
4. metal vacuum double-layer container, described metal vacuum double-layer container is to pass through steam vent, the vacuum exhaust processing is carried out in the space of being located between stainless steel inner pressurd vessel and outer container, form the vacuum heat-insulation space, at least one surface in inner pressurd vessel, outer container scribbles fluorine coating, it is characterized in that, the low-melting glass encapsulant of the degassing temperature when utilizing softening point to be higher than fluorine coating sintering temperature and vacuum exhaust seals processing to exhaust outlet, the thermal coefficient of expansion of described low-melting glass encapsulant is less than stainless steel, and its thermal expansion system difference is 25 * 10
-7Below/the K.
5. as each described metal vacuum double-layer container of claim 1 to 4, it is characterized in that described low-melting glass encapsulant is a bismuth class glass.
6. as each described metal vacuum double-layer container of claim 1 to 5, it is characterized in that described stainless steel is a martensitic stain less steel.
7. a glass for sealing composition is characterized in that, each component content of described glass for sealing composition is as follows: Bi
2O
3Be that 70～90wt%, ZnO are 0-2wt%, B
2O
3Be 5～29wt%, SiO
2Be 1～15wt%, Al
2O
3Be that 0～10wt%, CuO are 0～10wt%.
8. a glass for sealing composition is characterized in that, each component content of described glass for sealing composition is as follows: Bi
2O
3Be that 70～90wt%, ZnO are 0-2wt%, B
2O
3Be 5～28wt%, SiO
2Be 1～15wt%, Al
2O
3Be that 0～10wt%, CuO are 0.5～6wt%.
9. the manufacture method of a metal vacuum double-layer container, it is characterized in that, in each described metal vacuum double-layer container of claim 1 to 6, by steam vent the temperature that is lower than low-melting glass encapsulant softening point the space between stainless steel inner pressurd vessel, outer container is carried out vacuum exhaust, the degassing after, under the vacuum exhaust state, the low-melting glass encapsulant is softening with the temperature that is higher than softening point, fusing are sealed processing to exhaust outlet.
10. the manufacture method of metal vacuum double-layer container as claimed in claim 9 is characterized in that, as the low-melting glass encapsulant, uses claim 7, each described moral glass for sealing composition of 8.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001161169A JP2002348152A (en) | 2001-05-29 | 2001-05-29 | Metallic vacuum double container and method for making the same, sealing composition |
| JP2001161169 | 2001-05-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1387815A true CN1387815A (en) | 2003-01-01 |
| CN1247143C CN1247143C (en) | 2006-03-29 |
Family
ID=19004488
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02122048 Expired - Fee Related CN1247143C (en) | 2001-05-29 | 2002-05-29 | Metal vacuum double-layer container and its producing method, composition for sealing |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2002348152A (en) |
| KR (1) | KR20020090921A (en) |
| CN (1) | CN1247143C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161393A (en) * | 2011-01-25 | 2011-08-24 | 胡广 | Method for manufacturing metal vacuum double-layer container for spraying coating |
| CN105266654A (en) * | 2015-09-10 | 2016-01-27 | 膳魔师（中国）家庭制品有限公司 | Vacuum heat preservation container bottom sealing structure and sealing method thereof |
| CN104936491B (en) * | 2013-12-09 | 2018-01-26 | 布巴品牌股份有限公司 | With internally coated double-walled, the vacuum insulation vessels solidified at high temperature |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4626173B2 (en) * | 2004-04-06 | 2011-02-02 | タイガー魔法瓶株式会社 | Vacuum double structure heating vessel |
| JP5150058B2 (en) * | 2006-03-17 | 2013-02-20 | 日本山村硝子株式会社 | Lead-free glass composition for sealing stainless steel vacuum double containers |
| JP2008024558A (en) * | 2006-07-24 | 2008-02-07 | Nihon Yamamura Glass Co Ltd | Lead-free glass composition for sealing metal-made vacuum double container |
| JP5413562B2 (en) * | 2007-12-06 | 2014-02-12 | 日本電気硝子株式会社 | Sealing material |
| WO2010016318A1 (en) * | 2008-08-06 | 2010-02-11 | 日本電気硝子株式会社 | Sealing glass |
| JP5314969B2 (en) * | 2008-09-03 | 2013-10-16 | 富士フイルム株式会社 | Optical glass |
| CN205568688U (en) * | 2015-10-01 | 2016-09-14 | 史利利 | Vacuum electric heating container |
| JP7132735B2 (en) * | 2018-03-30 | 2022-09-07 | 日本山村硝子株式会社 | Metal Vacuum Double Container Sealing Glass Composition and Metal Vacuum Double Container |
| CN112216313B (en) * | 2020-09-16 | 2022-04-19 | 上海三利数字技术有限公司 | Data disaster recovery storage device and carrier |
-
2001
- 2001-05-29 JP JP2001161169A patent/JP2002348152A/en active Pending
-
2002
- 2002-05-29 CN CN 02122048 patent/CN1247143C/en not_active Expired - Fee Related
- 2002-05-29 KR KR1020020029774A patent/KR20020090921A/en not_active Application Discontinuation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161393A (en) * | 2011-01-25 | 2011-08-24 | 胡广 | Method for manufacturing metal vacuum double-layer container for spraying coating |
| CN104936491B (en) * | 2013-12-09 | 2018-01-26 | 布巴品牌股份有限公司 | With internally coated double-walled, the vacuum insulation vessels solidified at high temperature |
| CN105266654A (en) * | 2015-09-10 | 2016-01-27 | 膳魔师（中国）家庭制品有限公司 | Vacuum heat preservation container bottom sealing structure and sealing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2002348152A (en) | 2002-12-04 |
| CN1247143C (en) | 2006-03-29 |
| KR20020090921A (en) | 2002-12-05 |
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