CN102248322A - High-temperature resistant Ag-Cu-O metal sealing material and use method thereof - Google Patents
High-temperature resistant Ag-Cu-O metal sealing material and use method thereof Download PDFInfo
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- CN102248322A CN102248322A CN2011101311536A CN201110131153A CN102248322A CN 102248322 A CN102248322 A CN 102248322A CN 2011101311536 A CN2011101311536 A CN 2011101311536A CN 201110131153 A CN201110131153 A CN 201110131153A CN 102248322 A CN102248322 A CN 102248322A
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Abstract
The invention relates to a preparation and use method of a high-temperature resistant Ag-Cu-O metal sealing material for solid mixing conductor oxygen permeation membrane ceramic and support body stainless steel thereof. The sealing material takes Ag as a matrix; the content of Ag is 90.5-98.3 percent by weight; the contents of Cu and O are respectively controlled within 1.5-8.5 percent by weight and 0.2-1.1 percent by weight; the sealing temperature is 970-990 DEG C; and brazing sealing is carried out in an inert atmosphere (pure Ar or pure N2). The high-temperature resistant Ag-Cu-O metal sealing material disclosed by the invention is prepared by feeding the Ag-Cu alloy prepared in advance into an oxygen atmosphere furnace, controlling the weight increment to be 0.2-1.1 percent by weight and maintaining the temperature of 850 DEG C for 30h. The high-temperature resistant Ag-Cu-O metal sealing material obtained in the invention has high sealing property for the solid mixing conductor oxygen permeation membrane ceramic and the support body stainless steel thereof, has favorable chemical stability and belongs to the technical field of special ceramic welding materials.
Description
Technical field
The present invention relates to a kind of special solid composite conductor oxygen-permeating film pottery and supporter stainless steel thereof with the preparation and the using method of high temperature resistant Ag-Cu-O metal sealing material, belong to the special cermacis technical field of welding materials.
Background technology
In high-temperature gas separation and membrane catalytic reaction, fine and close solid composite conductor oxygen-permeating film pottery is a kind of commonly used and important inoranic membrane, and it has broad application prospects in fields such as pure oxygen preparation, fuel cell and membrane reactors.At present, be the single-phase mixed oxygen ion/electron conductor material of cubic perovskite phase structure to the most active material of solid composite conductor oxygen-permeating film ceramic research both at home and abroad, wherein serial oxygen permeation membranes such as La-Sr-Co-Fe-O, Ba-Sr-Co-Fe-O, Ba-Co-Fe-Zr-O have obtained concern the most widely owing to have higher oxygen flow ability.The outstanding characteristics of such oxygen permeation membrane ceramic material are multicomponent (three above constituent elements), thermal coefficient of expansion big (20 * 10
-6K
-1About), structure and poor chemical stability (lattice variations and transformation mutually easily take place in the hot operation process), these material behaviors make the requirement harshness of oxygen permeable ceramic film spare to sealing-in.No matter so be breadboard basic research or large-scale later on the application, the high intermediate temperature sealing between solid composite conductor oxygen-permeating film pottery and the supporter stainless steel thereof all is the primary key issue that solves.
At present, the sealing-in mode between solid composite conductor oxygen-permeating film pottery and the supporter stainless steel thereof mainly contains following several: compression seal, glass capsulation and solder bonding metal sealing-in.Compare with glass capsulation, the solder bonding metal sealing-in is destructive less to ceramic oxygen-permeable membrane, and thermal coefficient of expansion mates easily; Simultaneously, solder bonding metal also complex structure, strict unlike compression seal in application process.Therefore, solder bonding metal sealing-in solid oxygen-ion membrane (som) pottery receives increasing concern.Wherein, Ag base solder prolongs plasticity and high-temperature oxidation resistance because of it is good, has caused both at home and abroad to the further research of Ag base solder as solid composite conductor oxygen-permeating film pottery and the stainless steel sealed material feasibility of supporter thereof.But pure Ag itself is nonwetting oxygen permeation membrane pottery and supporter stainless steel thereof, and just direct two kinds of materials of soldering must be realized solid composite conductor oxygen-permeating film pottery and the stainless reliable sealing-in of supporter thereof to wherein adding active element.The K.Scott Weil seminar of the U.S. has proposed to use Ag-Cu solder alloy soldering solid composite conductor oxygen-permeating film pottery under air atmosphere, make the Cu in the silver-base solder of high temperature melting under air atmosphere, be oxidized to CuO, utilize CuO to improve the wettability of solder, and utilize sessile drop method to study under the air atmosphere Ag-Cu solder alloy solid composite conductor oxygen-permeating film material (La to the oxygen permeation membrane pottery
0.6Sr
0.4) (Co
0.2Fe
0.8) O
3-δWettability, find that the Cu content in the solder is high more, the CuO that forms in the solder under the high-temperature liquid state is many more, ((1) the K. Scott Weil et al. Journal of the electrochemical society that improves that helps wettability more, 2004. (2) K. S. Weil et al. Journal of materials science, 2005), they call the air soldering to this method for sealing.But because the solubility of oxygen in liquid silver is nearly 100 times of solubility in solid-state silver, in the air brazing process, can dissolve a large amount of oxygen in the silver-base solder of fusion, and a large amount of oxygen that dissolves in the silver-base solder in the soldering temperature-fall period can be separated out, on the interface of solder and supporter stainless steel or solder and oxygen permeation membrane pipe, form a large amount of pores (seeing Fig. 1 a and Fig. 1 b), cause the gas leakage of sealing-in position, lost efficacy.Therefore this air method for welding can not satisfy the sealing-in requirement between solid composite conductor oxygen-permeating film pottery and its supporter stainless steel.
Summary of the invention
Seal interface produces the problem of a large amount of pores when the present invention seeks at the soldering of Ag-Cu solder alloy air, the money base high-temperature resistant metal sealing material and the method for sealing that provide a kind of effective control pore to form, make it sealing-in solid composite conductor oxygen-permeating film pottery and supporter stainless steel thereof simultaneously, on the soldering interface, can not produce pore, and solder has good wettability to oxygen permeation membrane pottery and supporter stainless steel thereof simultaneously, finally realizes the stainless reliable sealing-in of solid composite conductor oxygen-permeating film pottery and supporter thereof.
A kind of high temperature resistant Ag-Cu-O metal sealing material, it is characterized in that having following composition and weight percent: Ag is matrix, content is 90.5-98.3%; Cu content is 1.5-8.5%, and O content is 0.2-1.1%; Brazing temperature is between 970-990 ° of C, at inert atmosphere (pure Ar or pure N
2) in carry out the soldering sealing-in.
The preparation method of above-mentioned high temperature resistant Ag-Cu-O metal sealing material is characterized in that having following process and step:
(a) take by weighing raw material A g, Cu by formula rate and prepare burden, the gained batch is positioned in the graphite crucible;
(b) the above-mentioned batch of graphite crucible that places is put in the vaccum sensitive stove; Vacuum less than 2Pa, 1000-1150 ℃ temperature under melting 3-5 minute, make its fusion, induction stirs; Cool to room temperature then with the furnace, obtain the Ag-Cu alloy material;
(c) will go up the Ag-Cu alloy material that makes of step and place the oxygen atmosphere stove, the control weightening finish in 850 ° of C insulation 30h, cools to room temperature at 0.2-1.1wt% with the furnace then, finally obtains high temperature resistant Ag-Cu-O metal sealing material.
The using method of above-mentioned high temperature resistant Ag-Cu-O metal sealing material is characterized in that this using method is as follows: with above-mentioned prepared high temperature resistant Ag-Cu-O metal sealing material machining or pour into certain thickness and the sealing-in prefabricated component of shape in advance; The sealing-in prefabricated component is placed between solid mixed conductor oxygen permeable ceramic membrane spare and its supporter stainless steel, integral body is positioned over and is rapidly heated in the inert atmosphere to 970-990 ℃ then, heating rate 80-100 ℃/min, insulation is 2-3 minute under this temperature, speed with 30-40 ℃/min is cooled to room temperature at last, can realize the reliable sealing-in between solid mixed conductor oxygen permeable ceramic membrane spare and its supporter parts of stainless steel.
The present invention is high temperature resistant, and the Ag-Cu-O metal sealing material is with stable pure Ag is base-material, allocates that the O of The addition of C u and certain content makes into.Pass through the content of control Cu and the atmosphere of oxygen in the solder preparation process, make solder form proper C u oxide before soldering, these proper C u oxide has guaranteed that fusion Ag base solder has good wettability to solid composite conductor oxygen-permeating film pottery and supporter stainless steel simultaneously in the high temperature brazing process.Soldering is to finish under the inert atmosphere of anaerobic, can not dissolve in unnecessary oxygen in the Ag base of high-temperature fusion attitude, so having guaranteed does not have unnecessary oxygen to separate out from the solder melt in the soldering temperature-fall period, thereby can not form pore on seal interface, has realized the interfacial seal airtightness.Sealing strength has been improved at good wettability and imperforate interface greatly, has guaranteed the reliability of sealing structure.The solidus temperature of the present invention is high temperature resistant Ag-Cu-O metal sealing material is higher than 900 ℃ of the general maximum operating temperatures of solid composite conductor oxygen-permeating film, promptly under the oxygen permeation membrane condition of work, metal sealing material is in solid state, guaranteed the chemical inertness between seal, sealing materials and film spare itself, the general stability that can not influence membrane module has high bond strength simultaneously.So high temperature resistant Ag-Cu-O metal sealing material not only can be used in the sealing-in between small size oxygen permeation membrane sheet in the laboratory or film pipe and supporter stainless steel, also be fit to the sealing-in between large-sized tubulose and plate film spare and its supporter stainless steel, on large-scale application, have remarkable economy and practicality.
Description of drawings
Fig. 1 is Ag-Cu solder alloy air soldering solid composite conductor oxygen-permeating film ceramic material (BaCo
0.7Fe
0.2-
Nb
0.1O
3-δ) and supporter stainless steel (310S) after the reaction sectional drawing.
Fig. 2 is the high temperature resistant Ag-Cu-O metal sealing material of the present invention high intermediate temperature sealing solid composite conductor oxygen-permeating film pottery (BaCo under Ar gas atmosphere
0.7Fe
0.2Nb
0.1O
3-δ) and supporter stainless steel (310S) after the reaction sectional drawing.
Fig. 3 is the high temperature resistant Ag-Cu-O metal sealing material of the present invention high intermediate temperature sealing solid composite conductor oxygen-permeating film pottery (BaCo under Ar gas atmosphere
0.7Fe
0.2Nb
0.1O
3-δ) and supporter stainless steel (310S) after, with the section S EM at stainless steel reaction interface figure.
Fig. 4 (a) and (b) be respectively the high temperature resistant Ag-Cu-O metal sealing material of the present invention under Ar gas atmosphere with solid composite conductor oxygen-permeating film pottery (BaCo
0.7Fe
0.2Nb
0.1O
3-δ) and the wetting experiment picture of supporter stainless steel (310S).
Fig. 5 is under the Ar gas atmosphere, and the high temperature resistant Ag-Cu-O metal sealing material of the present invention is to solid composite conductor oxygen-permeating film pottery (BaCo during 1000 ° of C
0.7Fe
0.2Nb
0.1O
3-δ) and the angle of wetting of supporter stainless steel (310S) with the variation diagram of Cu content.
Fig. 6 is the operating position of the high temperature resistant Ag-Cu-O metal sealing material of the present invention annular seal sheet between solid mixed conductor oxygen permeable ceramic membrane sheet and its supporter stainless steel tube.
Fig. 7 fills in for the powder of the high temperature resistant Ag-Cu-O metal sealing material of the present invention or the operating position of prefabricated ring shaped slot form.
The specific embodiment
After now specific embodiments of the invention being described in.
Embodiment one:The preparation process of high temperature resistant Ag-Cu-O metal sealing material is as described below in the present embodiment:
Quality percentage composition according to five kinds of compositions of listed a.b.c.d.e in the table 1, take by weighing a certain amount of pure Ag and pure Cu respectively, compound is placed in the graphite crucible, place in the vaccum sensitive stove, vacuum less than 2Pa, 1000-1150 ℃ temperature under melting 3-5 minute, make its fusion, cool to room temperature with the furnace after induction stirs, obtain the Ag-Cu alloy material.Again the Ag-Cu alloy material that makes is placed the oxygen atmosphere stove, control weightening finish is at 0.2-1.1wt%, in 850 ° of C insulation 30h, cools to the high temperature resistant Ag-Cu-O metal sealing material (seeing Table 2) that obtains required composition after the room temperature then with the furnace.Become high temperature resistant Ag-Cu-O metal sealing material machining that makes or vacuum pouring the sealing-in prefabricated component of needs stand-by at last.
Table 1 Ag-Cu alloy material component table (quality percentage composition %)
| Kind is formed | Ag | Cu |
| a | 98.50 | 1.50 |
| b | 98.00 | 2.00 |
| c | 96.00 | 4.00 |
| d | 93.20 | 6.80 |
| e | 91.50 | 8.50 |
Table 2 is high temperature resistant Ag-Cu-O metal sealing material component table (quality percentage composition %)
| Kind is formed | Ag | Cu | O |
| a | 98.30 | 1.50 | 0.20 |
| b | 97.75 | 2.00 | 0.25 |
| c | 95.52 | 3.98 | 0.50 |
| d | 92.42 | 6.74 | 0.84 |
| e | 90.54 | 8.41 | 1.05 |
Comparative experimental example:
Ag-Cu solder alloy air soldering solid composite conductor oxygen-permeating film material (BaCo
0.7Fe
0.2Nb
0.1O
3-δ) and the result of the test of supporter stainless steel (310S) see shown in Figure 1.
Fig. 1 is the Ag-Cu solder alloy air soldering oxygen permeable film material (BaCo that is made by composition b in the table 1
0.7Fe
0.2Nb
0.1O
3-δ) and supporter stainless steel (310S) after the reaction sectional drawing.Wherein a is the W-response sectional drawing, and b is the exterior view with the Ag-Cu solder alloy of stainless steel side contacts.As can be seen from the figure, after the air soldering, a large amount of bubbles have appearred in Ag-Cu solder alloy and stainless reaction interface, and these bubbles have had a strong impact on the performance and the sealing-in sealing of sealing-in.
Test example: the present invention is high temperature resistant Ag-Cu-O metal sealing material high intermediate temperature sealing solid composite conductor oxygen-permeating film ceramic material (BaCo under inert atmosphere
0.7Fe
0.2Nb
0.1O
3-δ) and the result of the test of supporter stainless steel (310S) referring to Fig. 2,3.High temperature resistant Ag-Cu-O metal sealing material (see Table 2 in composition b, d) under Ar gas atmosphere the high intermediate temperature sealing solid composite conductor oxygen-permeating film ceramic material (BaCo of Fig. 2 for preparing among the embodiment
0.7Fe
0.2Nb
0.1O
3-δ) and supporter stainless steel (310S) after the reaction sectional drawing.As can be seen from the figure, the bubble at seal, sealing materials and stainless steel interface obviously reduces, and as seen from Figure 3, seal, sealing materials and stainless steel interface have formed continuous interfacial reaction layer, and boundary layer is not found pore, the sealing-in success.
The wettability test: good wettability is that the metal sealing solder carries out the assurance of soldering to solid composite conductor oxygen-permeating film pottery and supporter stainless steel thereof, so adopt sessile drop method to measure the high temperature resistant Ag-Cu-O metal sealing material of the present invention to solid composite conductor oxygen-permeating film pottery and the stainless wettability of supporter thereof.Result of the test is referring to Fig. 4,5.
Fig. 4 (a) and (b) are the high temperature resistant Ag-Cu-O metal sealing materials (seeing Table 2 composition c) that are prepared among the embodiment, under Ar gas atmosphere respectively to solid composite conductor oxygen-permeating film pottery (BaCo
0.7Fe
0.2Nb
0.1O
3-δ) and the wetting photo figure of supporter stainless steel (310S).As can be seen from the figure, this high temperature resistant Ag-Cu-O metal sealing material is all fine to solid oxygen-ion membrane (som) pottery and the stainless wetability of supporter thereof.
Fig. 5 is under the Ar gas atmosphere, during 1000 ° of C by the prepared high temperature resistant Ag-Cu-O metal sealing material a-e of embodiment to solid composite conductor oxygen-permeating film pottery and the stainless angle of wetting of supporter thereof variation diagram with Cu content.As can be seen from the figure, in the present invention got the Cu content range, angle of wetting was all less than 90 °, and angle of wetting reduces along with the increase of Cu content, and just wetability improves with the increase of Cu content.
Using method
The using method of the prepared high temperature resistant Ag-Cu-O metal sealing material of the embodiment of the invention is referring to Fig. 6 in the accompanying drawing, 7; Now be described below in conjunction with the accompanying drawings:
One of using method: referring to Fig. 6, Fig. 6 is that the high temperature resistant Ag-Cu-O metal sealing material of the present invention (sees Table a) operating position of annular seal sheet between solid mixed conductor oxygen permeable ceramic membrane sheet and its supporter stainless steel tube of 2 compositions.Wherein, a is the annular seal sheet, and b is a solid mixed conductor oxygen permeable ceramic membrane sheet, and c is the supporter stainless steel tube.
Two of using method: referring to Fig. 7, Fig. 7 fills in the operating position of form for the present invention's high temperature resistant Ag-Cu-O metal sealing material (seeing Table 2 ingredient e) slurries (or powder).Wherein a is the high temperature resistant Ag-Cu-O metal sealing material powder of filling in the annular groove, and b is relatively large solid mixed conductor oxygen permeable ceramic membrane pipe fitting, and c is the supporter stainless steel tube.
After sealing assembling by above-mentioned using method, its integral body is positioned over is rapidly heated in the inert atmosphere to 980 ℃ of (90 ℃ of heating rates/min), insulation is 3 minutes under this temperature, be cooled to room temperature with 35 ℃/min then, can realize the reliable sealing-in between solid mixed conductor oxygen permeable ceramic membrane spare and its supporter parts of stainless steel.
Detection to the solid mixed conductor oxygen permeable ceramic membrane spare sealing after the sealing-in assembling a: side of solid mixed conductor oxygen permeable ceramic membrane sheet is exposed to air, opposite side purges with pure He, purge gas detects wherein nitrogen with online gaseous mass spectrum, in mass spectral certainty of measurement scope, detect less than N
2, the sealing-in success.Since 950 ℃, be cooled to 900 ℃, 850 ℃, 800 ℃, 750 ℃, 700 ℃ and 650 ℃ then successively.Temperature rate in the experiment is 5 ℃/min.Each temperature spot insulation 1h, gas leakage is not found in the test of hunting leak.Illustrate that the high temperature resistant Ag-Cu-O metal sealing material of the present invention can use in very wide temperature range, in heating and cooling process, the thermal expansion matching of seal, sealing materials and oxygen flow diaphragm is better.End temperature is constant in 850 ℃, and purge gas becomes He+CH
4Gaseous mixture is tested more than the 500h continuously, and the sealing-in effect of system is still very good.After experiment finishes, the membrane reactor system is cooled off naturally with stove, behind the cool to room temperature, it is still intact to observe solid mixed conductor oxygen permeable ceramic membrane sheet surface, explanation is from the slow cool to room temperature of high temperature, the coefficient of expansion that this is high temperature resistant between Ag-Cu-O metal sealing material and solid mixed conductor oxygen permeable ceramic membrane sheet mates better always, and the strength test of reaction joint is found that joint still has very high intensity.High temperature resistant Ag-Cu-O metal sealing material does not have diffusion and the reaction with solid mixed conductor oxygen permeable ceramic membrane sheet generation deep layer substantially yet, therefore through after the long period, high temperature resistant Ag-Cu-O metal sealing material is very little to the stability influence of solid mixed conductor oxygen permeable ceramic membrane sheet.
Claims (3)
1. high temperature resistant Ag-Cu-O metal sealing material, it is characterized in that having following composition and percentage by weight thereof: Ag is matrix, content is 90.5-98.3%; Cu, O content are controlled at respectively in 1.5-8.5% and the 0.2-1.1% scope; Brazing temperature is between 970-990 ° of C, at inert atmosphere (pure Ar or pure N
2) in carry out sealing-in.
2. method for preparing high temperature resistant Ag-Cu-O metal sealing material according to claim 1 is characterized in that having following process and step:
(a) take by weighing raw material A g, Cu by certain prescription and prepare burden, the gained batch is positioned in the graphite crucible;
(b) the above-mentioned batch of graphite crucible that places is put in the vaccum sensitive stove; Vacuum less than 2Pa, 1000-1150 ℃ temperature under melting 3-5 minute, make its fusion, induction stirs; Cool to room temperature then with the furnace, obtain the Ag-Cu solder alloy;
(c) the above-mentioned Ag-Cu solder alloy that makes is placed the oxygen atmosphere stove, the control weightening finish in 850 ° of C insulation 30h, cools to room temperature with the furnace then in the 0.2-1.1wt% scope, finally make high temperature resistant Ag-Cu-O metal sealing material.
3. the using method of a high temperature resistant Ag-Cu-O metal sealing material according to claim 1 is characterized in that the concrete steps of this its using method are: with above-mentioned prepared seal, sealing materials machining or pour into certain thickness and the sealing-in prefabricated component of shape in advance; The sealing-in prefabricated component is placed between solid oxygen-ion membrane (som) ceramic member and its supporter stainless steel, integral body is positioned over and is rapidly heated in the inert atmosphere to 970-990 ℃ then, heating rate 80-100 ℃/min, insulation is 2-3 minute under this temperature, be cooled to room temperature with 30-40 ℃/min then, can realize the tight sealing-in between solid composite conductor oxygen-permeating film ceramic member and the supporter parts of stainless steel thereof.
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Cited By (4)
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| CN102773628A (en) * | 2012-06-26 | 2012-11-14 | 上海大学 | High-temperature resistant silver-copper-lithium-oxygen metal sealing material and application method thereof |
| CN103273212A (en) * | 2013-03-19 | 2013-09-04 | 上海大学 | High-temperature-resisting Ag-Cu-Mn metal sealing-in material, manufacturing method and purpose of high-temperature-resisting Ag-Cu-Mn metal sealing-in material |
| CN105960681A (en) * | 2014-03-12 | 2016-09-21 | 西屋电气有限责任公司 | Double-sealed fuel rod end plug for ceramic-containing cladding |
| CN113245653A (en) * | 2021-06-04 | 2021-08-13 | 哈尔滨工业大学 | Method for connecting ceramic and metal in air by using solid silver |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773628A (en) * | 2012-06-26 | 2012-11-14 | 上海大学 | High-temperature resistant silver-copper-lithium-oxygen metal sealing material and application method thereof |
| CN103273212A (en) * | 2013-03-19 | 2013-09-04 | 上海大学 | High-temperature-resisting Ag-Cu-Mn metal sealing-in material, manufacturing method and purpose of high-temperature-resisting Ag-Cu-Mn metal sealing-in material |
| CN103273212B (en) * | 2013-03-19 | 2015-10-07 | 上海大学 | High temperature resistant Ag-Cu-Mn metal sealing material, preparation method and its usage |
| CN105960681A (en) * | 2014-03-12 | 2016-09-21 | 西屋电气有限责任公司 | Double-sealed fuel rod end plug for ceramic-containing cladding |
| CN113245653A (en) * | 2021-06-04 | 2021-08-13 | 哈尔滨工业大学 | Method for connecting ceramic and metal in air by using solid silver |
| CN113245653B (en) * | 2021-06-04 | 2022-03-25 | 哈尔滨工业大学 | Method for connecting ceramic and metal in air by using solid silver |
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