CN102390132A - Composite middle layer component connecting Si3N4 ceramic samples and connecting method thereof - Google Patents
Composite middle layer component connecting Si3N4 ceramic samples and connecting method thereof Download PDFInfo
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- CN102390132A CN102390132A CN2011101918996A CN201110191899A CN102390132A CN 102390132 A CN102390132 A CN 102390132A CN 2011101918996 A CN2011101918996 A CN 2011101918996A CN 201110191899 A CN201110191899 A CN 201110191899A CN 102390132 A CN102390132 A CN 102390132A
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- paper tinsel
- filler metal
- brazing filler
- pottery
- amorphous brazing
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Abstract
The invention discloses a composite middle layer component connecting Si3N4 ceramic samples and a connecting method thereof. The composite middle layer component consists of amorphous brazing filler metal foils, Cu foils and Ni foils, wherein the amorphous brazing filler metal foils, the Cu foils and the Ni foils are closely connected in an order of amorphous brazing filler metal foil, Cu foil, Ni foil, Cu foil and amorphous brazing filler metal foil. The connecting method disclosed by the invention comprises the following steps of: firstly, grinding, polishing and washing Si3N4 ceramic samples to be connected and the composite middle layer component; then, closely assembling the Si3N4 ceramic, amorphous brazing filler metal foil, Cu foil, Ni foil, Cu foil, amorphous brazing filler metal foil and Si3N4 ceramic in turn, and placing the same in a vacuum furnace; and performing two steps of heating brazing and dispersing to connect the Si3N4 ceramic samples. In the invention, the room-temperature bending strength at four points of a joint of the connected Si3N4 ceramic samples is greater than 170MPa, and the high-temperature performance of the joint is much greater than that of the Ag-Cu-Ti brazing filler metal and Ti-Zr-Ni-Cu brazing filler metal; and when the test temperature is increased from 293K to 1,073K, the high-temperature bending strength at three points of the joint is greater than 120MPa.
Description
Technical field
The present invention relates to a kind of connection Si
3N
4The composite interlayer assembly and the method for pottery more specifically relate to a kind of TiZrCuB amorphous/Cu/Ni/Cu/TiZrCuB amorphous and reach two step heating solderings in vacuum drying oven-diffusions connection Si as the composite interlayer assembly
3N
4The method of pottery belongs to the ceramic welding technical field.
Background technology:
Si
3N
4Pottery is a kind of up-and-coming engineering structure ceramic material, and its main application fields is hot machine, wear parts and heat exchanger etc., is the important materials of making the new ceramics engine.Along with Si
3N
4The extensive use of ceramic material, people's pay attention to day by day is to Si
3N
4Pottery/Si
3N
4Pottery, Si
3N
4The research that ceramic/metal connects.It is to connect Si at present that active soldering is connected with solid-state diffusion
3N
4Two main method of pottery.Series of advantages such as the active soldering technology is simple with its technology, bonding strength is high, wide adaptability, the relative cost of good reproducibility, joint dimension and shape be low as a result and the one preferred technique that metal/ceramic connects that becomes.And a lot of achievements have been obtained.The disadvantage of active soldering is that high-temperature behavior is poor; The solid-state diffusion weldering can be satisfied the requirement that high temperature is used, but complex technical process is high to the requirement that connects surperficial processing and connection device.
Abroad be connected in the new type high temperature solder of usefulness with metal at the research pottery, design morely and contain precious metal or be the solder composition of base with precious metal Au, Pd, Pt, Ag-Pd, goal in research is that joint after the soldering can be worked under 923K or higher temperature.It is higher that but this type connects material cost.What up to the present obtain better result has 41Ni-34Cr-25Pd, an Au-Ni-Cr-Fe-Mo etc.The Sialon jointing bending strength that the 41Ni-34Cr-25Pd solder obtains can be stabilized in more than the 250MPa from room temperature to 973K always.The problem that this solder exists is direct ceramic soldering, and it sprays layer of even carbon film at the Sialon ceramic surface to the wetting and join dependency of Sialon pottery before welding; Au-Ni-Cr-Fe-Mo solder brazing Si
3N
4Joint intensity level under 923K that pottery obtains is higher and compared with just slightly decline of room temperature, this solder brazing is preceding to be needed at Si but use
3N
4Surface metalation is handled; Also there is design Ni-20.35Cr-10.04Si solder to carry out Si abroad
3N
4The report that connects; Wherein element Cr plays the effect of active element; Between solder and pottery, formed the CrN interfacial reaction layer, reached 200MPa though joint four-point bending intensity under 973～1173K high temperature can be stablized, its room temperature strength is the 118MPa that is merely on the low side obviously.Connect Si
3N
4The preparation moulding of the high temperature active solder of pottery also is the problem that urgent need will solve.
Adopt the new method of two step of amorphous composite interlayer heating soldering-diffusion connection to connect Si
3N
4Pottery, the advantage that the comprehensive active soldering of ability is connected with diffusion adopts amorphous brazing filler metal can solve the moulding problem in the above-mentioned active solder preparation, and employing composite interlayer assembly can improve the gentle elevated temperature strength in junction chamber simultaneously.
Summary of the invention:
The objective of the invention is in order to solve present Si
3N
4Problems such as pottery jointing room temperature, high-temperature behavior is poor, Ti-Zr-Ni-Cu brazing filler metal fragility is big provide a kind of connection Si
3N
4The composite interlayer assembly and the method for attachment of pottery.
To achieve these goals, technical scheme of the present invention is:
A kind of connection Si
3N
4The composite interlayer assembly of pottery; Be made up of Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel, described Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel are close to by the order of Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Cu paper tinsel, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel and are connected.Wherein said Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel is by mass percentage by component: Ti is: 40.0～45.0%; Zr is: 20～30%; B is: 0.1～0.3%; All the other are formed for Cu, and gross mass percentage is 100%, and thickness is the technical grade of 35～45 μ m; Described Cu paper tinsel purity is more than 99.9%, and thickness is the technical grade of 180～250 μ m; Described Ni paper tinsel purity is more than 99.9%, the technical grade of thickness 600-800 μ m.
To achieve these goals, the present invention's another technical scheme of being taked of dealing with problems is:
A kind of connection Si
3N
4The method of the composite interlayer assembly of pottery comprises the steps:
(1) preparatory stage: earlier with Si to be connected
3N
4The ceramic sample end face polishes with diamond paste, and amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel are polished with No. 5 abrasive paper for metallograph, places acetone to carry out ultrasonic waves for cleaning 10 minutes then together;
(2) installation step: after will cleaning with amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Si
3N
4Pottery is pressed Si
3N
4Pottery, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Cu paper tinsel, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Si
3N
4The order of pottery is close to and is assemblied in the soldering special fixture, on weldment, places a miniweights simultaneously to produce the pressure of 0.029-0.056MPa;
(3) first step connects: anchor clamps integral body is placed vacuum drying oven, and at first the speed with 10-15K/min is warming up to 1073K, insulation 30min, and the speed with 10-15K/min continues to be warming up to first step heating-up temperature T again
1=1283～1333K, temperature retention time t
1=20～60min;
(4) second steps connected: when temperature retention time is t
1After, be cooled to 1173K with the speed of 10K/min, insulation 30min; Speed with 10-15K/min continues to be warmed up to the second step heating-up temperature T again
2=1363～1433K, insulation a period of time t
2=60～180min; Speed with 4-6K/min is chilled to 873K then; Vacuum is less than 1.2 * 10
-2Pa; Naturally cool to the sampling of room temperature blow-on door.
The present invention has following advantage and effect compared with prior art:
1, the present invention adopts Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Cu paper tinsel, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel composite interlayer to connect Si
3N
4Pottery can not only be avoided forming more Ni-Ti frangible compounds and because the not existence of molten Ni paper tinsel improves the joint room temperature strength, can also improve the elevated temperature strength of joint through the high-temperature behavior of intermetallic compound.Its room temperature four-point bending intensity is not less than 170MPa; High-temperature behavior is much higher than the Ag-Cu-Ti solder of individual layer and the Ti-Zr-Ni-Cu solder of individual layer, and when probe temperature rose to 1073K from 293K, joint high temperature three-point bending strength was not less than 120MPa.
2, the present invention adopts the soldering-diffusion method of attachment of two steps heating not only to simplify technology, can also improve Si to greatest extent
3N
4The room temperature and the elevated temperature strength of pottery.
3, the Si of the present invention's acquisition
3N
4But ceramic joint stable performance repetition, this method can significantly improve Si
3N
4The room temperature strength of ceramic joint and elevated temperature strength have especially enlarged Si
3N
4The scope of application under the ceramic high temperature.
Description of drawings
Fig. 1 is the organigram of composite interlayer assembly of the present invention.
Fig. 2 is method of attachment process curve figure of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing 1 and accompanying drawing 2, through the specific embodiment to a kind of connection Si of the present invention
3N
4The pottery composite interlayer assembly and method do further explain.
Embodiment 1:
One, choose the composite interlayer assembly:
1, the component of amorphous brazing filler metal paper tinsel and content are by mass percentage: Ti:40.0%; Zr:25%; B:0.2%; All the other are Cu; The gross mass degree is 100%, and thickness is the technical grade of 40 μ m.
2, copper thickness is the technical grade of 180 μ m.
3, Ni paper tinsel thickness is the technical grade of 600 μ m.
Two, method of attachment and step:
1, with Si to be connected
3N
4Pottery 1 end face polishes with the 3.5um diamond paste, and amorphous brazing filler metal paper tinsel 2, No. 5 abrasive paper for metallograph of Copper Foil 3 and Ni paper tinsel 4 usefulness polish before being connected; Place acetone to carry out ultrasonic waves for cleaning 10 minutes then together;
2, as shown in Figure 1, with amorphous brazing filler metal paper tinsel 2, Copper Foil 3, Ni paper tinsel 4, the Si after cleaning
3N
4Pottery 1 is pressed Si
3N
4Pottery 1/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Cu paper tinsel 3/Ni paper tinsel 4/Cu paper tinsel 3/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Si
3N
4Pottery 1 order is close to and is assemblied in the soldering special fixture; On weldment, place a miniweights simultaneously to produce 0.040MPa pressure;
3, the first step connects: as shown in Figure 2, soldering is connected in the vacuum drying oven to be carried out, and at first the speed with 10-15K/min is warming up to 1073K, insulation 30min, and the speed with 10-15K/min continues to be warming up to first step heating-up temperature T again
1=1293K, insulation a period of time t
1=30min;
4, second step connected: as shown in Figure 2, and as temperature retention time t
1Behind=the 30min, be cooled to 1173K, insulation 30min with the speed of 10K/min; Speed with 10-15K/min continues to be warmed up to the second step heating-up temperature T again
2=1373K is incubated a period of time t again
2=90min; Speed with 4-6K/min is chilled to 873K then; Vacuum is less than 1.2 * 10
-2Pa; Naturally cool to the sampling of room temperature blow-on door.
Adopting its room temperature four-point bending intensity of joint of the soldering-method of diffusion welding of present embodiment is 187MPa, and when probe temperature was 1073K, when probe temperature rose to 1073K from 293K, strength of joint was not less than 138MPa.
Embodiment 2:
One, choose the composite interlayer assembly:
1, the component of amorphous brazing filler metal paper tinsel and content are by mass percentage: Ti:45.0%; Zr:20%; B:0.3%; All the other are Cu; The gross mass degree is 100%, and thickness is the technical grade of 45 μ m.
2, copper thickness is the technical grade of 250 μ m.
3, Ni paper tinsel thickness is the technical grade of 800 μ m.
Two, method of attachment and step:
1, with Si to be connected
3N
4Pottery 1 end face polishes with the 3.5um diamond paste, and amorphous brazing filler metal paper tinsel 2, No. 5 abrasive paper for metallograph of Copper Foil 3 and Ni paper tinsel 4 usefulness polish before being connected; Place acetone to carry out ultrasonic waves for cleaning 10 minutes then together;
2, as shown in Figure 1, with amorphous brazing filler metal paper tinsel 2, Copper Foil 3, Ni paper tinsel 4, the Si after cleaning
3N
4Pottery 1 is pressed Si
3N
4Pottery 1/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Cu paper tinsel 3/Ni paper tinsel 4/Cu paper tinsel 3/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Si
3N
4Pottery 1 order is close to and is assemblied in the soldering special fixture; On weldment, place a miniweights simultaneously to produce 0.056MPa pressure;
3, the first step connects: as shown in Figure 2, soldering is connected in the vacuum drying oven to be carried out, and at first the speed with 10-15K/min is warming up to 1073K, insulation 30min, and the speed with 10-15K/min continues to be warming up to first step heating-up temperature T again
1=1283K, insulation a period of time t
1=60min;
4, second step connected: as shown in Figure 2, and as temperature retention time t
1Behind=the 60min, be cooled to 1173K, insulation 30min with the speed of 10K/min; Speed with 10-15K/min continues to be warmed up to the second step heating-up temperature T again
2=1413K is incubated a period of time t again
2=60min; Speed with 4-6K/min is chilled to 873K then; Vacuum is less than 1.2 * 10
-2Pa; Naturally cool to the sampling of room temperature blow-on door.
Adopt present embodiment, its room temperature strength of the joint of acquisition is 185MPa; When probe temperature rose to 1073K from 293K, strength of joint was not less than 127MPa.
Embodiment 3:
One, choose the composite interlayer assembly:
1, the component of amorphous brazing filler metal paper tinsel and content are by mass percentage: Ti:42.0%; Zr:30%; B:0.1%; All the other are Cu; The gross mass degree is 100%, and thickness is the technical grade of 35 μ m.
2, copper thickness is the technical grade of 200 μ m.
3, Ni paper tinsel thickness is the technical grade of 600 μ m.
Two, method of attachment and step:
1, with Si to be connected
3N
4Pottery 1 end face polishes with the 3.5um diamond paste, and amorphous brazing filler metal paper tinsel 2, No. 5 abrasive paper for metallograph of Copper Foil 3 and Ni paper tinsel 4 usefulness polish before being connected; Place acetone to carry out ultrasonic waves for cleaning 10 minutes then together;
2, as shown in Figure 1, with amorphous brazing filler metal paper tinsel 2, Copper Foil 3, Ni paper tinsel 4, the Si after cleaning
3N
4Pottery 1 is pressed Si
3N
4Pottery 1/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Cu paper tinsel 3/Ni paper tinsel 4/Cu paper tinsel 3/Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel 2/Si
3N
4Pottery 1 order is close to and is assemblied in the soldering special fixture; On weldment, place a miniweights simultaneously to produce 0.029MPa pressure;
3, the first step connects: as shown in Figure 2, soldering is connected in the vacuum drying oven to be carried out, and at first the speed with 10-15K/min is warming up to 1073K, insulation 30min, and the speed with 10-15K/min continues to be warming up to first step heating-up temperature T again
1=1333K, insulation a period of time t
1=20min;
4, second step connected: as shown in Figure 2, and as temperature retention time t
1Behind=the 20min, be cooled to 1173K, insulation 30min with the speed of 10K/min; Speed with 10-15K/min continues to be warmed up to the second step heating-up temperature T again
2=1363K is incubated a period of time t again
2=180min; Speed with 4-6K/min is chilled to 873K then; Vacuum is less than 1.2 * 10
-2Pa; Naturally cool to the sampling of room temperature blow-on door.
Its room temperature strength of joint that adopts present embodiment to obtain is 170MPa; When probe temperature rose to 1073K from 293K, strength of joint was not less than 122MPa.
Claims (5)
1. one kind connects Si
3N
4The composite interlayer assembly of pottery is characterized in that being made up of amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel, and described amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel are close to by the order of amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Cu paper tinsel, amorphous brazing filler metal paper tinsel and are connected.
2. connection Si according to claim 1
3N
4The pottery the composite interlayer assembly, it is characterized in that described amorphous brazing filler metal paper tinsel by mass percentage content be 40.0～45.0% by component: Ti; Zr is 20～30%; B is 0.1～0.3%; All the other are formed for Cu, and the gross mass degree is 100%, and thickness is the technical grade of 35～45 μ m.
3. connection Si according to claim 1
3N
4The composite interlayer assembly of pottery is characterized in that described Cu paper tinsel purity is more than 99.9%, and thickness is the technical grade of 180～250 μ m.
4. connection Si according to claim 1
3N
4The composite interlayer assembly of pottery is characterized in that described Ni paper tinsel purity is more than 99.9%, the technical grade of thickness 600-800 μ m.
5. connection Si as claimed in claim 1
3N
4The method of attachment of the composite interlayer assembly of pottery is characterized in that comprising the steps:
(1) preparatory stage: earlier with Si to be connected
3N
4The ceramic sample end face polishes with diamond paste, and amorphous brazing filler metal paper tinsel, Cu paper tinsel and Ni paper tinsel are polished with No. 5 abrasive paper for metallograph, places acetone to carry out ultrasonic waves for cleaning 10 minutes then together;
(2) installation step: after will cleaning with amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Si
3N
4Pottery is pressed Si
3N
4Pottery, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Cu paper tinsel, Ni paper tinsel, Cu paper tinsel, Ti-Zr-Cu-B amorphous brazing filler metal paper tinsel, Si
3N
4The order of pottery is close to and is assemblied in the soldering special fixture, on weldment, places a miniweights simultaneously to produce the pressure of 0.029-0.056MPa;
(3) first step connects: anchor clamps integral body is placed vacuum drying oven, and at first the speed with 10-15K/min is warming up to 1073K, insulation 30min, and the speed with 10-15K/min continues to be warming up to first step heating-up temperature T again
1=1283～1333K, temperature retention time t
1=20～60min;
(4) second steps connected: when temperature retention time is t
1After, be cooled to 1173K with the speed of 10K/min, insulation 30min; Speed with 10-15K/min continues to be warmed up to the second step heating-up temperature T again
2=1363～1433K, insulation a period of time t
2=60～180min; Speed with 4-6K/min is chilled to 873K then; Vacuum is less than 1.2 * 10
-2Pa; Naturally cool to the sampling of room temperature blow-on door.
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|---|---|---|---|
| CN2011101918996A CN102390132A (en) | 2011-07-11 | 2011-07-11 | Composite middle layer component connecting Si3N4 ceramic samples and connecting method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102699558A (en) * | 2012-06-29 | 2012-10-03 | 哈尔滨工业大学 | Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal |
| CN105174990A (en) * | 2015-10-20 | 2015-12-23 | 哈尔滨工业大学 | High-temperature-application-based composite active middle layer diffusion bonding method for implementing interstitial carbide or nitride ceramic seamless connection |
| CN107043269A (en) * | 2017-04-12 | 2017-08-15 | 武汉理工大学 | A kind of method that ceramic low-temp rapid welding is modified |
| CN107914424A (en) * | 2016-10-11 | 2018-04-17 | 张跃 | A kind of multi-layer board and its manufacture method |
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| CN101172880A (en) * | 2007-09-21 | 2008-05-07 | 江苏科技大学 | Titanium group high temperature amorphous solder of hard solder Si*N* ceramic and method for producing the same |
| CN101823188A (en) * | 2010-05-10 | 2010-09-08 | 江苏科技大学 | High-temperature amorphous solder for soldering Si3N4 ceramics |
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2011
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| CN101172880A (en) * | 2007-09-21 | 2008-05-07 | 江苏科技大学 | Titanium group high temperature amorphous solder of hard solder Si*N* ceramic and method for producing the same |
| CN101823188A (en) * | 2010-05-10 | 2010-09-08 | 江苏科技大学 | High-temperature amorphous solder for soldering Si3N4 ceramics |
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|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102699558A (en) * | 2012-06-29 | 2012-10-03 | 哈尔滨工业大学 | Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal |
| CN105174990A (en) * | 2015-10-20 | 2015-12-23 | 哈尔滨工业大学 | High-temperature-application-based composite active middle layer diffusion bonding method for implementing interstitial carbide or nitride ceramic seamless connection |
| CN105174990B (en) * | 2015-10-20 | 2018-03-30 | 哈尔滨工业大学 | A kind of composite reactive intermediate layer diffusion connection method realized gap carbide or nitride ceramics and be seamlessly connected based on high temperature application |
| CN107914424A (en) * | 2016-10-11 | 2018-04-17 | 张跃 | A kind of multi-layer board and its manufacture method |
| CN107043269A (en) * | 2017-04-12 | 2017-08-15 | 武汉理工大学 | A kind of method that ceramic low-temp rapid welding is modified |
| CN107043269B (en) * | 2017-04-12 | 2020-08-18 | 武汉理工大学 | Method for modifying ceramic by low-temperature rapid welding |
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Application publication date: 20120328 |