CN101717270A - Method for connecting SiC ceramic and high-temperature alloy - Google Patents
Method for connecting SiC ceramic and high-temperature alloy Download PDFInfo
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- CN101717270A CN101717270A CN200910219188A CN200910219188A CN101717270A CN 101717270 A CN101717270 A CN 101717270A CN 200910219188 A CN200910219188 A CN 200910219188A CN 200910219188 A CN200910219188 A CN 200910219188A CN 101717270 A CN101717270 A CN 101717270A
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Abstract
The invention relates to a method for connecting a ceramic and a high-temperature alloy, and discloses the method for connecting SiC ceramic and the high-temperature alloy, which comprises the following steps: (1) preparing a Ni-Si paste; (2) preprocessing the SiC ceramic and the high-temperature alloy and manufacturing a Mo sheet; (3) coating the Ni-Si paste on the SiC ceramic, the high-temperature alloy and the Mo sheet; and (4) assembling and connecting the SiC ceramic and the high-temperature alloy at a high temperature. The method for connecting the SiC ceramic and the high-temperature alloy can realize the low-reaction high-temperature connection between the SiC ceramic and the high-temperature alloy, has simple and economic process, and can produce on large scale; and the prepared connecting piece has a reliable structure and can be used for bearing and in high-temperature places.
Description
Technical field
The present invention relates to the method for attachment of pottery and superalloy, the method for attachment of particularly a kind of SiC pottery and superalloy.
Background technology
At present, about being connected between pottery and ceramic, pottery and the metal, mainly consider the factors such as intensity, heat-resisting ability, reliability, manufacturing cost of web member structure.Connect for the high temperature of SiC pottery and mainly to comprise technological methods such as soldering, diffusion welding, self propagating high temperature be synthetic.About the active soldering of SiC pottery, the general solder that adopts mainly comprises Ag base, Cu base, Ni base, Pd base etc.Yet, since the SiC pottery under hot conditions can with most metallic element generation intensive chemical reactions, form the ternary compound of brittle silicide, carbide, siliceous and carbon in joint interface, form crackle easily, thereby cause joint fails.Diffusion welding about the SiC pottery, be easy to prepare the heat-proof corrosion-resistant joint although diffusion welding has, joint tighness better reaches advantages such as joint quality is stable, and it is very high to the requirement of the processing that connects the surface and linking device, be not suitable for connecting big parts, need big connection pressure.And, face high surface reaction, bigger connection pressure equally and shelve problems such as complexity for the self propagating high temperature synthetic technology of SiC pottery.
In recent years, some foreign study persons were engaged in the non-reaction or the low reaction high temperature brazing research of relevant SiC pottery, as only adopting Si-17Pr, Si-22Ti, Si-16Ti, Si-18Cr, Si-44Cr and SiCr
2Directly the SiC pottery is connected with superalloy Deng alloy or compound as solder.But since its to contain Si too high, alloy fragility is bigger, has more crackle in brazing process more or less in solder layer, also has the problem of the easy oxidation of high temperature simultaneously, the possibility of practical application is less.
Summary of the invention
The object of the present invention is to provide the high-temperature liquid-phase method of attachment between a kind of SiC pottery and the SiC pottery, its syndeton is firm, reliable, and technology is simple, low cost of manufacture.
For reaching above purpose, the present invention takes following technical scheme to be achieved.
The method of attachment of a kind of SiC pottery and superalloy is characterized in that, may further comprise the steps:
(1) preparation Ni-Si paste: the Ni-Si powdered alloy is rolled the bastard mill, sieves, in the vial of packing into, add oxalic acid second diester and collodion solution again, stir 30min at least, make the Ni-Si paste, stand-by;
(2) pre-treatment SiC pottery, superalloy and making Mo sheet: the joint face of SiC pottery is polished successively, polishes, cleans and drying; The joint face of superalloy is polished successively, cleans and drying; The joint face size of cutting processing Mo sheet and SiC pottery adapts again, and cleans and drying;
(3) coating Ni-Si paste:, or, dry then in a surface applied Ni-Si layer of paste of Mo sheet in the joint face coating Ni-Si of SiC pottery layer of paste;
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery and superalloy, the Ni-Si layer of paste is between Mo sheet and SiC pottery, and it is fixing to exert pressure, in vacuum oven, be heated to 1330～1400 ℃ then, insulation 5～30min is cooled to room temperature, gets final product.
In the such scheme, in the described preparation Ni-Si alloy paste, Ni-Si powdered alloy: oxalic acid second diester: the proportioning of collodion solution is (3～4) g: (4～6) ml: (6～8) ml; Si content is 40at.%～60at.% (an atomicity per-cent) in the described Ni-Si powdered alloy; Described superalloy comprises kovar alloy, Ni based high-temperature alloy; Mo sheet thickness is 300～400 μ m; In vacuum oven, vacuum tightness is better than 1 * 10
-1Get final product under the Pa condition.
The present invention compared with prior art has the following advantages: 1) SiC pottery bonding interface has a low reactivity.2) has the strong interfacial bond characteristic.At the interface of SiC pottery with middle layer Mo sheet, because in the high temperature connection procedure, Mo enters the Ni-Si coating, can promote the Ni-Si alloy at SiC wettability of the surface and spreading rate, eliminate the crackle in the Ni-Si layer, increase the bonding strength at Ni-Si coating and SiC pottery interface; At middle layer Mo sheet and superalloy interface, because what adopt is High temperature diffusion welding technology between the metal, the bonding strength height.3) the Mo sheet helps alleviating residual thermal stress as the middle layer.4) technology simple relatively, be widely used.In ceramic side, the SiC pottery is connected technology with the high-temperature liquid-phase that is connected to of middle layer Mo; In metal side, be mainly the diffusion welding between the metal between middle layer Mo sheet and the superalloy, even comprise that also transient liquid phase connects, therefore lower to linking device and processing requirement, and to form be the high temperature phase mutually in the middle layer, can be applied to the high temperature occasion.
In sum, technology of the present invention is simple relatively, economical, can be used for being connected and large-scale production of large size ceramic and metal parts; And the web member reliable in structure of preparation, have good resistance to elevated temperatures, applicable to carrying and pyritous application scenario.
Description of drawings
Fig. 1, Fig. 2, Fig. 3 are respectively the SiC pottery of the embodiment of the invention 1 preparation and the section or the interface junction composition of the joint of kovar alloy; Wherein, Fig. 1 is the SiC/Kovar sectional structure chart of joint; Fig. 2 is a joint Kovar/Mo interface junction composition; Fig. 3 is a joint Mo/Ni-Si/SiC interface junction composition.Among the figure: 1, kovar alloy (Fe-32Ni-15Co); 2, Mo sheet; 3, Ni-Si coating; 4, SiC ceramic member; 5, the interfacial layer of Kovar/Mo interface formation; 6, the interfacial layer of Mo/Ni-Si interface formation.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
The method of attachment of a kind of SiC pottery and kovar alloy specifically may further comprise the steps:
(1) preparation Ni-Si paste: earlier with Ni-56Si powdered alloy (atom percentage content of Si is 56at.%), add dehydrated alcohol, roll bastard mill 72h, 200 mesh sieves are crossed in oven dry, again the Ni-56Si powder is placed vial, add oxalic acid second diester, ultrasonic homogenizing is handled 20min, adds collodion solution (pyroxylin (e) cement) then in vial, stir 30min at least with glass stick, can be stand-by; Wherein: the Ni-56Si powder: oxalic acid second diester: collodion solution=4g: 6ml: 8ml.
(2) pre-treatment SiC pottery, kovar alloy and making Mo sheet: with the SiC ceramic plate of plasma activated sintering (PAS), wherein pottery is with 6%Al
2O
3And 4%Y
2O
3Be sintering aid, be of a size of Φ 15 * 3mm, connect successively face through on diamond disk, polish, polishing, dehydrated alcohol clean and the baking oven inner drying; (Fe-32Ni-15Co) is machined into Φ 15 * 3mm with kovar alloy, and the face that connects successively then is through polishing on diamond disk, polish, clean and drying; The Mo sheet is processed as the disk of Φ 15mm * 400 μ m, and passes through twin polishing, cleaning and drying successively.
(3) coating Ni-Si paste: with the Ni-Si paste application that mixes up in processing, clean and a surface of dry good Mo sheet, treat to dry fully or air-dry.
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery and kovar alloy, the Ni-Si layer of paste is between Mo sheet and SiC pottery, and it is fixing under the condition of additional pressure 1Kpa, place in the vacuum oven then, be heated to 1350 ℃ with 10 ℃/min temperature rise rate, insulation 10min, the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, gets final product.
With reference to Fig. 1,2,3, adopt the microscopic analysis of the joint of present embodiment making to show: form certain thickness interfacial layer respectively at Kovar/Mo and Mo/Ni-Si interface, and the Ni-Si/SiC interface to be clear, smooth, does not have tangible reaction product or responding layer.
The method of attachment of another kind of Si/SiC pottery and kovar alloy specifically may further comprise the steps:
(1) preparation Ni-Si paste: earlier Ni-40Si powdered alloy (atom percentage content of Si is 40at.%) is added dehydrated alcohol, roll bastard mill 72h, oven dry, cross 200 mesh sieves, again the Ni-40Si powder is placed vial, add oxalic acid second diester, ultrasonic homogenizing is handled 20min, in vial, add collodion solution (pyroxylin (e) cement) then, stir 30min at least with glass stick, can be stand-by; Wherein: the Ni-40Si powder: oxalic acid second diester: collodion solution=3g: 4ml: 8ml.
(2) pre-treatment SiC pottery, kovar alloy and making Mo sheet: with reaction sintering Si/SiC ceramic plate, processing is into about Φ 15 * 5mm ceramic plate, connect successively face through on diamond disk, polish, polishing, dehydrated alcohol clean and the baking oven inner drying; (Fe-32Ni-15Co) is machined into Φ 15 * 3mm with kovar alloy, and the face that connects successively is through polishing on diamond disk, polish, clean and drying; The Mo sheet is processed as the disk of Φ 15mm * 350 μ m, and passes through twin polishing, cleaning and drying successively.
(3) coating Ni-Si paste: in the joint face coating Ni-Si of SiC pottery layer of paste, dry then (dry or air-dry).
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery and kovar alloy, the Ni-Si layer of paste is between Mo sheet and SiC pottery, and is and fixing under the condition of additional pressure 10Kpa, places then in the vacuum oven, and vacuum tightness is better than 1 * 10
-1Under the Pa condition, be heated to 1330 ℃ with 10 ℃/min temperature rise rate, insulation 10min, the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, gets final product.
Adopt the microscopic analysis of the joint of present embodiment making to show: form certain thickness interfacial layer respectively at Kovar/Mo and Mo/Ni-Si interface, and the Ni-Si/SiC interface to be clear, smooth, does not have tangible reaction product or responding layer.
A kind of SiC pottery and the method for attachment of Ni based high-temperature alloy, specifically may further comprise the steps:
(1) preparation Ni-Si paste: earlier Ni-56Si powdered alloy (atom percentage content of Si is 56at.%) is added dehydrated alcohol, roll bastard mill 72h, oven dry, cross 200 mesh sieves, again the Ni-40Si powder is placed vial, add oxalic acid second diester, ultrasonic homogenizing is handled 20min, in vial, add collodion solution (pyroxylin (e) cement) then, stir 30min at least with glass stick, can be stand-by; Wherein: the Ni-56Si powder: oxalic acid second diester: collodion solution=3g: 4ml: 6ml.
(2) pre-treatment SiC pottery, Ni based high-temperature alloy and making Mo sheet: the SiC ceramic rod that will wait hot isostatic pressing (HIP) sintering to form, with 1%Al
2O
3Be sintering aid, cutting back is into about Φ 15 * 3mm ceramic plate, connect successively face through on diamond disk, polish, polishing, dehydrated alcohol clean and the baking oven inner drying; (IN738LC) is machined into Φ 15 * 3mm with the Ni based high-temperature alloy, connects the surface then successively through polishing on diamond disk, polish, clean and drying; The Mo sheet is processed as the disk of Φ 15mm * 300 μ m, and passes through twin polishing, cleaning and drying successively.
(3) coating Ni-Si paste:, air-dry then in the joint face coating Ni-Si of SiC pottery layer of paste.
(4) assembling: the Mo sheet is placed between the joint face of SiC pottery and Ni based high-temperature alloy, the Ni-Si layer of paste is between Mo sheet and SiC pottery, and is and fixing under the condition of additional pressure 1Kpa.
(5) high temperature connects: prepare 2 samples according to above-mentioned steps (1)～(4); Then, place respectively in the vacuum oven, vacuum tightness is better than 1 * 10
-1Under the Pa condition, be heated to 1330 ℃ and 1400 ℃ respectively with 10 ℃/min temperature rise rate, and be incubated 30min and 5min respectively, the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, gets final product.
Adopt the microscopic analysis of the joint of present embodiment making to show: form certain thickness interfacial layer respectively at IN738LC/Mo and Mo/Ni-Si interface, and the Ni-Si/SiC interface to be clear, smooth, does not have tangible reaction product or responding layer.
Although above embodiment is described embodiment of the present invention, the present invention is not limited to above-mentioned specific embodiments, and above-mentioned specific embodiments only is schematic, guiding, rather than restrictive.Those of ordinary skill in the art under the enlightenment of this specification sheets, described hot metal also comprise can with Mo
-Alloys such as other Ni bases that the sheet High temperature diffusion connects, Co base, Nb base, Fe base, these all belong to the row of the present invention's protection.
Claims (4)
1. the method for attachment of SiC pottery and superalloy is characterized in that, may further comprise the steps:
(1) preparation Ni-Si paste: the Ni-Si powdered alloy is rolled the bastard mill, sieves, in the vial of packing into, add oxalic acid second diester and collodion solution again, stir 30min at least, make the Ni-Si paste, stand-by;
(2) pre-treatment SiC pottery, superalloy and making Mo sheet: the joint face of SiC pottery is polished successively, polishes, cleans and drying; The joint face of superalloy is polished successively, cleans and drying; The joint face size of cutting processing Mo sheet and SiC pottery adapts again, and cleans and drying;
(3) coating Ni-Si paste:, or, dry then in a surface applied Ni-Si layer of paste of Mo sheet in the joint face coating Ni-Si of SiC pottery layer of paste;
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery and superalloy, the Ni-Si layer of paste is between Mo sheet and SiC pottery, and it is fixing to exert pressure, in vacuum oven, be heated to 1330～1400 ℃ then, insulation 5～30min is cooled to room temperature, gets final product.
2. the method for attachment of a kind of SiC pottery according to claim 1 and superalloy, it is characterized in that, in the described preparation Ni-Si alloy paste, Ni-Si powdered alloy: oxalic acid second diester: the proportioning of collodion solution is (3～4) g: (4～6) ml: (6～8) ml.
3. the method for attachment of a kind of SiC pottery according to claim 1 and superalloy is characterized in that the atom percentage content of Si is 40at.%～60at.% in the described Ni-Si powdered alloy.
4. the method for attachment of a kind of SiC pottery according to claim 1 and superalloy is characterized in that described superalloy comprises kovar alloy, Ni based high-temperature alloy.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920366A (en) * | 2010-08-31 | 2010-12-22 | 中国航空工业集团公司北京航空材料研究院 | Method for brazing Cf/SiC composite material and wrought superalloy |
| CN103467140A (en) * | 2013-09-03 | 2013-12-25 | 江苏大学 | Surface metalized layer of silicon carbide ceramic and metalizing method of silicon carbide ceramic |
| CN113182514A (en) * | 2021-03-31 | 2021-07-30 | 北京科技大学 | TiAl alloy ceramic welding part and integral forming preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193507B (en) * | 2013-04-22 | 2014-10-29 | 江苏大学 | Method for improving wettability of metal to SiC ceramic |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100361935C (en) * | 2006-05-15 | 2008-01-16 | 西北工业大学 | Connection method for carbon/carbon, carbon/silicon carbonate composite material and thermal-resisting alloy |
| CN100584801C (en) * | 2008-03-19 | 2010-01-27 | 哈尔滨工业大学 | Braze welding method of composite powder used for carbon/silicon carbide and niobium or niobium alloy |
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2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920366A (en) * | 2010-08-31 | 2010-12-22 | 中国航空工业集团公司北京航空材料研究院 | Method for brazing Cf/SiC composite material and wrought superalloy |
| CN103467140A (en) * | 2013-09-03 | 2013-12-25 | 江苏大学 | Surface metalized layer of silicon carbide ceramic and metalizing method of silicon carbide ceramic |
| CN103467140B (en) * | 2013-09-03 | 2015-10-28 | 江苏大学 | A kind of side metallization of silicon carbide ceramics and method for metallising |
| CN113182514A (en) * | 2021-03-31 | 2021-07-30 | 北京科技大学 | TiAl alloy ceramic welding part and integral forming preparation method thereof |
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