CN106065950A - The encapsulating method of a kind of perovskite oxygen permeation membrane assembly and device - Google Patents
The encapsulating method of a kind of perovskite oxygen permeation membrane assembly and device Download PDFInfo
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- CN106065950A CN106065950A CN201610635214.5A CN201610635214A CN106065950A CN 106065950 A CN106065950 A CN 106065950A CN 201610635214 A CN201610635214 A CN 201610635214A CN 106065950 A CN106065950 A CN 106065950A
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- perovskite oxygen
- perovskite
- oxygen permeation
- permeation membrane
- membrane assembly
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/14—Sealings between relatively-stationary surfaces by means of granular or plastic material, or fluid
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- General Engineering & Computer Science (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses encapsulating method and the device of a kind of perovskite oxygen permeation membrane assembly；It is respectively coated with gold sealing coat in the periphery of two end tube walls of perovskite oxygen flow membrane tube, and is arranged with ceramic seal cap and ceramic support pipe respectively in the outside of each end gold sealing coat；It is respectively coated with glass cement in the junction of ceramic seal cap and ceramic support Guan Yujin sealing coat；Encapsulating method is before perovskite oxygen permeation membrane comes into operation, and after titanium ore oxygen flow membrane tube two ends are uniformly coated with one layer of gold paste, heat up, are cooled to room temperature, then seals binding site with glass cement, shapes；Obtained perovskite oxygen permeation membrane assembly, solves prior art and occurs owing to revealing, and makes the oxygen spilt gas reaction directly and near leak source, easily produces hot localised points, thus affect the technical problem of whole film using effect.There is technique be simple and convenient to operate；Obtained by perovskite oxygen flow membrane module with good performance, the advantage such as good seal performance.
Description
Technical field
The present invention relates to encapsulation method, particularly relate to encapsulating method and the device of a kind of perovskite oxygen permeation membrane assembly.
Background technology
Perovskite oxygen permeation membrane is most-often used a kind of composite conductor oxygen-permeating film, under the high temperature conditions (especially more than 800
DEG C), when film both sides exist difference in oxygen concentration, oxygen can transit to low concentration from high concentration end by oxygen vacancies with the form of oxonium ion
End.Selective penetrated property to oxygen is 100% in theory.Perovskite oxygen permeation membrane is widely used in ambient oxygen partial from, methane moiety
In the industrial process such as oxidation, favorable operating conditions for production of hydrogen by methane autothermal and selectively oxidizing ethane ethylene, it can not only provide oxygen for reaction
Gas, also has catalytic action to some reaction.
Although a lot of scholars have carried out substantial amounts of research and experiment to perovskite oxygen permeation membrane, but the elevated-temperature seal of film is still
One of key technical problem needing solution badly.The material of reactor is generally rustless steel, and intensity is higher, and the mechanicalness of film itself
Can be poor, directly film is linked together with reactor, under the conditions of high-temperature operation, film is easily rupturable, it is therefore desirable to a supporter will
Film couples together with reactor rustless steel base.And perovskite oxygen permeation membrane is different from the thermal coefficient of expansion of supporter, for a long time at height
The lower running of temperature easily produces leak source, makes membrane efficiency be greatly reduced；And the oxygen spilt can gas directly and near leak source anti-
Should, it is possible to create hot localised points, thus affect the use of whole film.
Summary of the invention
It is an object of the invention to overcome the shortcoming and defect of above-mentioned prior art, it is provided that a kind of perovskite oxygen permeation membrane assembly
Encapsulating method and device.This encapsulating method flow process is simple, easy to operate, good seal performance.
The present invention is achieved through the following technical solutions:
The sealing device of a kind of perovskite oxygen permeation membrane assembly, including perovskite oxygen flow membrane tube 4；Described perovskite oxygen flow membrane tube
The periphery of two end tube walls of 4 has been respectively coated with gold sealing coat 3, and is arranged with respectively in the outside of each end gold sealing coat 3
Ceramic seal cap 1 and ceramic support pipe 5；
In ceramic seal cap 1 and ceramic support pipe 5 and the junction of gold sealing coat 3, it is respectively coated with for sealing this
The glass cement 2 of interface gap.
The longitudinal section of ceramic support pipe 5 orifice region being connected this end with perovskite oxygen flow membrane tube 4 is trapezoidal faces；This glass
Glue 2 is coated in the calmodulin binding domain CaM of this trapezoidal faces and gold sealing coat 3.
The coated length of each gold sealing coat 3 is respectively 1cm～2cm.
The degree of depth of ceramic seal cap 1 is 4mm～5mm, the top of perovskite oxygen flow membrane tube 4 and the inner bottom of ceramic seal cap 1
Portion offsets.
Contact length between perovskite oxygen flow membrane tube 4 outer surface and ceramic support pipe 5 inner surface is 0.5cm～1cm.
The tube length of perovskite oxygen flow membrane tube 4 is 140mm, external diameter 3.7mm, thickness of pipe wall 0.47mm.
The encapsulating method of a kind of perovskite oxygen permeation membrane assembly is as follows:
Step (201): gold paste coats
Starch with tweezers depletion, and two end peripheries in perovskite oxygen flow membrane tube 4 smear one layer equably, Mei Geduan
A length of 1.5cm, at room temperature air drying 2h smear in portion, form gold sealing coat 3；Gold paste coating step completes；
Step (202): heating cooling
After completing gold paste coating step, perovskite oxygen flow membrane tube 4 is put into Muffle furnace is slowly heated to 1000 DEG C, heating
Speed is 2 DEG C of min-1, and it is incubated 1h at this temperature, naturally cool to room temperature subsequently；Heating cooling step completes；
Step (203): glass cement seals
Taking glass dust and put in alcohol solvent, being sufficiently stirred for Glass rod until in thick, obtaining glass dust viscous solution；
After completing to heat cooling step, one end of perovskite oxygen flow membrane tube 4 is inserted in ceramic seal cap 1, insertion depth
For 5mm, then perovskite oxygen flow membrane tube 4 horizontal positioned, and the glass dust viscous solution prepared is spread upon perovskite oxygen flow
Membrane tube 4 and the junction of ceramic seal cap 1, for making the distribution of glass dust viscous solution more uniform, use rotation to smear；Then by calcium
The other end of titanium ore oxygen flow membrane tube 4 inserts in ceramic support pipe 5, and insertion depth is about 1cm, at perovskite oxygen flow membrane tube 4 and pottery
Porcelain props up the junction of stay tube 5 and smears glass dust viscous solution；Complete the preliminary fixing of perovskite oxygen permeation membrane assembly；
Step (204): glass cement is shaped
Tentatively fixing perovskite oxygen permeation membrane assembly is put in vertical electric furnace and is slowly heated, until 1020
DEG C, the rate of heat addition is 2 DEG C of min-1, it is incubated 1h at this temperature, now through the molten one-tenth of glass dust viscous solution being slowly heated
Smooth glass cement 2, subsequently with 2 DEG C of min-1Cooldown rate be cooled to room temperature；Complete the sealing of perovskite oxygen permeation membrane assembly.
Before above-mentioned glass cement sealing step starts, first the orifice region of ceramic support pipe 5 is polished into trapezoidal faces；Then
Calmodulin binding domain CaM in this trapezoidal faces with gold sealing coat 3 smears glass dust viscous solution.Trapezoidal faces is conducive to the stream of glass dust viscous solution
Dynamic, the colloid surface after sealing can be made the most smooth.
Above-mentioned smear glass dust viscous solution during, for improving the sealing property of junction and intensity, repeatable step
Suddenly (203) and step (204) are repeatedly, until sealing property and intensity reach necessary requirement.
Described in described step (201), the tube length of perovskite oxygen flow membrane tube 4 is 140mm, external diameter 3.7mm, thickness of pipe wall
0.47mm。
Use the perovskite oxygen permeation membrane assembly obtained by encapsulating method of the present invention, operate under long term high temperature and be not likely to produce leakage
Point, makes to be greatly improved membrane efficiency.
Use the perovskite oxygen permeation membrane assembly obtained by encapsulating method of the present invention, solve prior art and send out owing to revealing
Raw, make the oxygen spilt gas reaction directly and near leak source, easily produce hot localised points, thus affect whole film and use effect
The technical problem of fruit.
Sealing technology of the present invention is simple and convenient to operate；Obtained by perovskite oxygen flow membrane module with good performance, sealing property
Good.
Accompanying drawing explanation
Fig. 1 is perovskite oxygen permeation membrane modular construction schematic diagram of the present invention.
Fig. 2 is perovskite oxygen permeation membrane assembly preparation technology block diagram of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is more specifically described in detail.
Embodiment
As illustrated in fig. 1 and 2.The invention discloses the sealing device of a kind of perovskite oxygen permeation membrane assembly, saturating including perovskite
Oxygen membrane tube 4；The periphery of two end tube walls of described perovskite oxygen flow membrane tube 4 has been respectively coated with gold sealing coat 3, and in each end
The outside of gold sealing coat 3 is arranged with ceramic seal cap 1 and ceramic support pipe 5 respectively；
In ceramic seal cap 1 and ceramic support pipe 5 and the junction of gold sealing coat 3, it is respectively coated with for sealing this
The glass cement 2 of interface gap.
The longitudinal section of ceramic support pipe 5 orifice region being connected this end with perovskite oxygen flow membrane tube 4 is trapezoidal faces；This glass
Glue 2 is coated in the calmodulin binding domain CaM of this trapezoidal faces and gold sealing coat 3.
The coated length of each gold sealing coat 3 is respectively 1cm～2cm.
The degree of depth of ceramic seal cap 1 is 4mm～5mm, the top of perovskite oxygen flow membrane tube 4 and the inner bottom of ceramic seal cap 1
Portion offsets.
Contact length between perovskite oxygen flow membrane tube 4 outer surface and ceramic support pipe 5 inner surface is 0.5cm～1cm.
The tube length of perovskite oxygen flow membrane tube 4 is 140mm, external diameter 3.7mm, thickness of pipe wall 0.47mm.
The encapsulating method of perovskite oxygen permeation membrane assembly of the present invention, can be realized by following processing step:
Step (201): gold paste coats
Appropriate gold paste (gold content 85～90%) is taken with tweezers, and equably in two ends of perovskite oxygen flow membrane tube 4
Periphery smears very thin one layer, each end smear a length of 1.5cm, at room temperature air drying 1.5h～2.5h
(preferably 2h), forms gold sealing coat 3；Gold paste coating step completes；
Step (202): heating cooling
After completing gold paste coating step, perovskite oxygen flow membrane tube 4 is put into Muffle furnace is slowly heated to 950 DEG C～1200
DEG C (preferably 1000 DEG C), the rate of heat addition is 2 DEG C of min-1, and insulation 1.5h～2.5h (preferably 1h) at this temperature, natural subsequently
It is cooled to room temperature；Heating cooling step completes；
Step (203): glass cement seals
Take appropriate glass dust and put in alcohol solvent, be sufficiently stirred for Glass rod until in thick, obtaining glass dust and glue
Magma；
After completing to heat cooling step, one end of perovskite oxygen flow membrane tube 4 is inserted in ceramic seal cap 1, insertion depth
For 5mm, then perovskite oxygen flow membrane tube 4 horizontal positioned, and the glass dust viscous solution prepared is spread upon perovskite oxygen flow
Membrane tube 4 and the junction of ceramic seal cap 1, for making the distribution of glass dust viscous solution more uniform, use rotation to smear；Then by calcium
The other end of titanium ore oxygen flow membrane tube 4 inserts in ceramic support pipe 5, and insertion depth is about 1cm, at perovskite oxygen flow membrane tube 4 and pottery
Porcelain props up the junction of stay tube 5 and smears glass dust viscous solution；Complete the preliminary fixing of perovskite oxygen permeation membrane assembly；Use ceramic seal
Cap 1 is to fix to realize one end of membrane module, if two ends are fixed, when expanding with heat and contract with cold, internal stress can make membrane module rupture.By
In ethanol highly volatile, glass dust viscous solution can quickly be dried.
Step (204): glass cement is shaped
Tentatively fixing perovskite oxygen permeation membrane assembly is put in vertical electric furnace and is slowly heated, until 1000
DEG C～1050 DEG C (preferably 1020 DEG C), the rate of heat addition is 2 DEG C of min-1, it is incubated 1h at this temperature, now process is slowly heated
The glass cement 2 that the molten one-tenth of glass dust viscous solution is smooth, subsequently with 2 DEG C of min-1Cooldown rate be cooled to room temperature；Complete calcium titanium
The sealing of ore deposit oxygen permeation membrane assembly.
Before above-mentioned glass cement sealing step starts, first the orifice region of ceramic support pipe 5 is polished into trapezoidal faces；Then
Calmodulin binding domain CaM in this trapezoidal faces with gold sealing coat 3 smears glass dust viscous solution.Trapezoidal faces is conducive to the stream of glass dust viscous solution
Dynamic, the colloid surface after sealing can be made the most smooth.
Above-mentioned smear glass dust viscous solution during, for improving the sealing property of junction and intensity, repeatable step
Suddenly (203) and step (204) repeatedly (general 2～3 times, the most specifically can as the case may be depending on), until sealing
Energy and intensity reach necessary requirement.
Described in described step (201), the tube length of perovskite oxygen flow membrane tube 4 is 140mm, external diameter 3.7mm, thickness of pipe wall
0.47mm.Depending on the most concrete size can be applied according to reality.
As it has been described above, just can preferably realize the present invention.
Embodiments of the present invention are also not restricted to the described embodiments, other any spirit without departing from the present invention
With the change made under principle, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, be included in the present invention's
Within protection domain.
Claims (10)
1. the sealing device of a perovskite oxygen permeation membrane assembly, it is characterised in that: include perovskite oxygen flow membrane tube (4)；Described calcium
The periphery of two end tube walls of titanium ore oxygen flow membrane tube (4) has been respectively coated with gold sealing coat (3), and at each end gold sealing coat
(3) outside is arranged with ceramic seal cap (1) and ceramic support pipe (5) respectively；
In the junction of ceramic seal cap (1) and ceramic support pipe (5) with gold sealing coat (3), it is respectively coated with for sealing
The glass cement (2) of this interface gap.
The sealing device of perovskite oxygen permeation membrane assembly the most according to claim 1, it is characterised in that: with perovskite oxygen flow membrane tube
(4) longitudinal section of ceramic support pipe (5) orifice region connecting this end is trapezoidal faces；This glass cement (2) is coated in this trapezoidal faces
Calmodulin binding domain CaM with gold sealing coat (3).
The sealing device of perovskite oxygen permeation membrane assembly the most according to claim 1 or claim 2, it is characterised in that: each gold sealing coat (3)
Coated length be respectively 1cm～2cm.
The sealing device of perovskite oxygen permeation membrane assembly the most according to claim 1 or claim 2, it is characterised in that: ceramic seal cap (1)
The degree of depth be 4mm～5mm, the top of perovskite oxygen flow membrane tube (4) offsets with the inner bottom part of ceramic seal cap (1).
The sealing device of perovskite oxygen permeation membrane assembly the most according to claim 1 or claim 2, it is characterised in that: perovskite oxygen permeation membrane
Contact length between pipe (4) outer surface and ceramic support pipe (5) inner surface is 0.5cm～1cm.
The sealing device of perovskite oxygen permeation membrane assembly the most according to claim 1 or claim 2, it is characterised in that: perovskite oxygen permeation membrane
The tube length of pipe (4) is 140mm, external diameter 3.7mm, thickness of pipe wall 0.47mm.
7. the encapsulating method of a perovskite oxygen permeation membrane assembly, it is characterised in that comprise the steps:
Step (201): gold paste coats
Starch with tweezers depletion, and two end peripheries at perovskite oxygen flow membrane tube (4) smear one layer equably, each end
Smear a length of 1.5cm, at room temperature air drying 2h, form gold sealing coat (3)；Gold paste coating step completes；
Step (202): heating cooling
After completing gold paste coating step, perovskite oxygen flow membrane tube (4) is put into Muffle furnace is slowly heated to 1000 DEG C, heating speed
Rate is 2 DEG C of min-1, and it is incubated 1h at this temperature, naturally cool to room temperature subsequently；Heating cooling step completes；
Step (203): glass cement seals
Taking glass dust and put in alcohol solvent, being sufficiently stirred for Glass rod until in thick, obtaining glass dust viscous solution；
After completing to heat cooling step, one end of perovskite oxygen flow membrane tube (4) is inserted in ceramic seal cap (1), insertion depth
For 5mm, then perovskite oxygen flow membrane tube (4) horizontal positioned, and it is saturating that the glass dust viscous solution prepared is spread upon perovskite
Oxygen membrane tube (4) and the junction of ceramic seal cap (1), for making the distribution of glass dust viscous solution more uniform, use rotation to smear；Connect
And inserted in ceramic support pipe (5) by the other end of perovskite oxygen flow membrane tube (4), insertion depth is about 1cm, at perovskite oxygen flow
Glass dust viscous solution is smeared in the junction of membrane tube (4) and ceramic support pipe (5)；Complete the preliminary solid of perovskite oxygen permeation membrane assembly
Fixed；
Step (204): glass cement is shaped
Tentatively fixing perovskite oxygen permeation membrane assembly is put in vertical electric furnace and is slowly heated, until 1020 DEG C,
The rate of heat addition is 2 DEG C of min-1, it is incubated 1h at this temperature, now the molten one-tenth of glass dust viscous solution through being slowly heated is smooth
Glass cement (2), subsequently with 2 DEG C of min-1Cooldown rate be cooled to room temperature；Complete the sealing of perovskite oxygen permeation membrane assembly.
The encapsulating method of perovskite oxygen permeation membrane assembly the most according to claim 7, it is characterised in that: seal step at glass cement
Before beginning, first the orifice region of ceramic support pipe (5) is polished into trapezoidal faces；Then at this trapezoidal faces and gold sealing coat (3)
Calmodulin binding domain CaM smears glass dust viscous solution.Trapezoidal faces is conducive to the flowing of glass dust viscous solution, can make the colloid surface after sealing
The most smooth.
The encapsulating method of perovskite oxygen permeation membrane assembly the most according to claim 7, it is characterised in that: smearing glass dust thickness
During liquid, for improving the sealing property of junction and intensity, repeatable step (203) and step (204) repeatedly, until close
Sealing property and intensity reach necessary requirement.
The encapsulating method of perovskite oxygen permeation membrane assembly the most according to claim 7, it is characterised in that: in described step (201)
The tube length of described perovskite oxygen flow membrane tube (4) is 140mm, external diameter 3.7mm, thickness of pipe wall 0.47mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110660919A (en) * | 2018-06-29 | 2020-01-07 | 湖北万度光能有限责任公司 | Packaging method of perovskite solar cell |
| CN111396556A (en) * | 2020-02-26 | 2020-07-10 | 上海亿鼎电子系统集成有限公司 | Method for generating sealing film sleeve |
| CN111874999A (en) * | 2020-08-03 | 2020-11-03 | 深圳市怡盛源净水产业有限公司 | Water purification membrane pipe assembly |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20161102 |