CN101709000A - Method for connecting SiC ceramic by high-temperature liquid phase - Google Patents
Method for connecting SiC ceramic by high-temperature liquid phase Download PDFInfo
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- CN101709000A CN101709000A CN200910219183A CN200910219183A CN101709000A CN 101709000 A CN101709000 A CN 101709000A CN 200910219183 A CN200910219183 A CN 200910219183A CN 200910219183 A CN200910219183 A CN 200910219183A CN 101709000 A CN101709000 A CN 101709000A
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Abstract
The invention relates to a method for connecting SiC ceramic by high-temperature liquid phase. The method mainly comprises the following steps: (1) preparing Ni-Si paste; (2) preprocessing the SiC ceramic and producing an Mo sheet; (3) coating the Ni-Si paste; and (4) assembling the Mo sheet to connect the SiC ceramic by the high-temperature liquid phase. The method can connect the SiC ceramic by the low-reaction high-temperature liquid phase, has simple and economical process and can realize the scale production and ensure that the produced connecting piece has reliable structure. The method is suitable for load bearing and high-temperature applying occasions.
Description
Technical field
The present invention relates to the method that pottery is connected with ceramic high temperature, the high-temperature liquid-phase method of attachment between particularly a kind of SiC pottery and the SiC pottery.
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 the high temperature of SiC pottery Deng alloy or compound as solder.But since its 1 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.
High-temperature liquid-phase method of attachment between a kind of SiC pottery and the SiC pottery is characterized in that, comprises 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 and make the Mo sheet: the joint face of the SiC pottery of two butt joints polished successively, polishes, cleans and dry, cutting processing Mo sheet adapts with SiC pottery joint face size again, and cleans and drying;
(3) coating Ni-Si paste: the joint face at the SiC of two butt joints pottery applies the Ni-Si layer of paste respectively, or applies the Ni-Si layer of paste respectively on two surfaces of Mo sheet, dries then;
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery of two butt joints, it is fixing to exert pressure, and in vacuum oven, is heated to 1330～1400 ℃ then, and 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; In vacuum oven, vacuum tightness is better than 1 * 10
-1Get final product under the Pa condition.
The present invention compared with prior art, its advantage is: 1) ceramic interface has low reactivity and strong binding characteristic: (〉=40at.%) Ni-Si alloy has good non-reaction high-temperature moisture to the SiC pottery and the fabulous characteristic of sprawling on the Mo surface because si content is higher, by alloy composition be connected regulation and control such as technology, in the high temperature connection procedure, middle layer Mo and Ni-Si coating are by interacting, can promote the Ni-Si alloy at SiC wettability of the surface and spreading rate, eliminate most of crackle in the Ni-Si layer, keep the low reactivity between middle layer and the SiC parts, increase the bonding strength at Ni-Si coating and SiC pottery interface; 2) connect process economics, but high temperature is used: this technology is that high-temperature liquid-phase connects technology, and is low 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.Therefore, side preparation technology of the present invention is simple, and economy can be used for the connection and the large-scale production of large-scale SiC pottery; 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 in the embodiment of the invention 1 three kinds and connect under the temperature condition SiC/Ni-Si/Mo interface junction composition in the SiC/SiC joint; Wherein, the connection temperature of Fig. 1 is 1350 ℃; The connection temperature of Fig. 1 is 1375 ℃; 1400 ℃ of the connection temperature of Fig. 3; Among the figure: 1, SiC pottery; 2, Ni-Si middle layer; 3, Mo.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
High-temperature liquid-phase method of attachment between flaky SiC pottery of circle and the SiC pottery specifically may further comprise the steps:
(1) preparation Ni-Si paste: Ni-56Si powdered alloy (the atomicity percentage composition of Si is 56at.%) is added dehydrated alcohol, roll bastard mill 72h, oven dry is crossed 200 mesh sieves, in the vial of packing into, add oxalic acid second diester again, ultrasonic homogenizing is handled 20min, and then adds collodion solution (pyroxylin (e) cement) in bottle, stirs 30min at least with glass stick, make the Ni-Si paste, stand-by; Wherein: the Ni-56Si powder: oxalic acid second diester: collodion solution=4g: 6ml: 8ml.
(2) pre-treatment of SiC pottery and 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.With thick be the big Mo sheet of 100 μ m, cutting is processed as the thin discs of Φ 15, and passes through two-sided slight polishing, cleaning and drying successively.
(2) pre-treatment SiC pottery 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 the SiC pottery of Φ 15 * 3mm, with the joint face of the SiC pottery of two butt joints on diamond disk, polish successively, polishing, dehydrated alcohol clean and the baking oven inner drying, again with thick be that the Mo sheet cutting of 100 μ m is processed as the thin discs of Φ 15, and pass through two-sided slight polishing, cleaning and drying successively.
(3) coating Ni-Si paste: two surfaces at the Mo sheet apply the Ni-Si layer of paste respectively, dry then (dry or air-dry).
(4) assembling: the Mo sheet is placed between the joint face of SiC pottery of two butt joints, the about 1KPa of additional pressure carries out mount.
(5) high temperature connects: prepare 3 groups of samples by above-mentioned steps (1)～(4), the every group of sample that assembles placed respectively in the vacuum oven, be better than 1 * 10 in vacuum tightness
-1Under the Pa condition, the temperature rise rate with 10 ℃ of min is heated to 1330 ℃, 1350 ℃ and 1350 ℃ respectively, is incubated 10min, 5min and 30min respectively, and the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, takes out.
(6) make the strength trial sample, with the joint of 3 groups of SiC potteries making and SiC pottery cut growth 10mm * wide 6mm * thick 6mm sample respectively, the method that adopts shear-type load is the strength of joint of test sample respectively.The result shows that strength of joint is all greater than 40MPa, and each joint all ruptures in ceramic body.
In addition, with reference to Fig. 1, Fig. 2, Fig. 3, from the joint interface microstructure as can be seen, the interface is clear between the SiC/ middle layer, does not have tangible reaction product, shows that this high temperature method of attachment is that low reaction connects.
High-temperature liquid-phase method of attachment between flaky Si/SiC pottery of circle and the Si/SiC pottery specifically may further comprise the steps:
(1) preparation Ni-Si paste: Ni-40Si powdered alloy (the atomicity percentage composition of Si is 40at.%) is added dehydrated alcohol, roll bastard mill 72h, oven dry is crossed 200 mesh sieves, in the vial of packing into, add oxalic acid second diester again, ultrasonic homogenizing is handled 20min, and then adds collodion solution (pyroxylin (e) cement) in bottle, stirs 30min at least with glass stick, make the Ni-Si paste, stand-by; Wherein: the Ni-40Si powdered alloy: oxalic acid second diester: collodion solution=3g: 4ml: 8ml.
(2) pre-treatment SiC pottery and making Mo sheet: with two Si/SiC ceramic plates of reaction sintering, processing is into about Φ 15 * 5mm SiC pottery, with the joint face of the SiC pottery of two butt joints on diamond disk, polish successively, polishing, dehydrated alcohol clean and the baking oven inner drying, again with thick be that the Mo sheet cutting of 100 μ m is processed as the thin discs of Φ 15, and pass through two-sided slight polishing, cleaning and drying successively.
(3) coating Ni-Si paste: two surfaces at the Mo sheet apply the Ni-Si layer of paste respectively, dry then (dry or air-dry).
(4) assembling: the Mo sheet is placed between the joint face of SiC pottery of two butt joints, the about 10KPa of additional pressure carries out mount.
(5) high temperature connects: prepare 3 groups of samples by above-mentioned steps (1)～(4), the every group of sample that assembles placed respectively in the vacuum oven, be better than 1 * 10 in vacuum tightness
-1Under the Pa condition, the temperature rise rate with 5 ℃/min is heated to 1330 ℃, 1350 ℃ and 1350 ℃ respectively, is incubated 10min, 5min and 30min respectively, and the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, takes out.
(6) make the strength trial sample, with the joint of 3 groups of SiC potteries making and SiC pottery cut growth 10mm * wide 10mm * thick 6mm sample respectively, the method that adopts shear-type load is the strength of joint of test sample respectively.The result shows that strength of joint is 50MPa-100MPa, and the interface is clear between the SiC/ middle layer, does not have tangible reaction product.
High-temperature liquid-phase method of attachment between flaky SiC pottery of circle and the SiC pottery specifically may further comprise the steps:
(1) preparation Ni-Si paste: Ni-56Si powdered alloy (the atomicity percentage composition of Si is 56at.%) is added dehydrated alcohol, roll bastard mill 72h, oven dry is crossed 200 mesh sieves, in the vial of packing into, add oxalic acid second diester again, ultrasonic homogenizing is handled 20min, and then adds collodion solution (pyroxylin (e) cement) in bottle, stirs 30min at least with glass stick, make the Ni-Si paste, stand-by; Wherein: the Ni-56Si powdered alloy: oxalic acid second diester: collodion solution=3g: 5ml: 7ml.
(2) pre-treatment SiC pottery 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, the cutting back is into about Φ 15 * 2.5mm SiC pottery, with the joint face of the SiC pottery of two butt joints on diamond disk, polish successively, polishing, dehydrated alcohol clean and the baking oven inner drying, again with thick be that the Mo sheet cutting of 100 μ m is processed as the thin discs of Φ 15, and pass through two-sided slight polishing, cleaning and drying successively.
(3) coating Ni-Si paste: the joint face at the SiC of two butt joints pottery applies the Ni-Si layer of paste respectively, dries then or air-dry.
4) assembling: the Mo sheet is placed between the joint face of SiC pottery of two butt joints, the about 1KPa of additional pressure carries out mount.
(5) high temperature connects: the sample that assembles is placed in the vacuum oven, be better than 1 * 10 in vacuum tightness
-1Under the Pa condition, be heated to 1350 ℃ with the temperature rise rate of 20 ℃/min, insulation 10min, the rate of temperature fall with≤5 ℃/min slowly cools to room temperature again, takes out.
(6) make the strength trial sample, with the SiC pottery of making and the joint cutting growth 10mm * wide 6mm * thick 5mm sample of SiC pottery, the method for employing shear-type load is the strength of joint of test sample respectively.The result shows that strength of joint is about 30MPa, and the interface is clear between the SiC/ middle layer, does not have tangible reaction product.
Claims (3)
1. the high-temperature liquid-phase method of attachment between SiC pottery and the SiC pottery is characterized in that, comprises 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 and make the Mo sheet: the joint face of the SiC pottery of two butt joints polished successively, polishes, cleans and dry, cutting processing Mo sheet adapts with SiC pottery joint face size again, and cleans and drying;
(3) coating Ni-Si paste: the joint face at the SiC of two butt joints pottery applies the Ni-Si layer of paste respectively, or applies the Ni-Si layer of paste respectively on two surfaces of Mo sheet, dries then;
(4) assembling and high temperature connect: the Mo sheet is placed between the joint face of SiC pottery of two butt joints, it is fixing to exert pressure, and in vacuum oven, is heated to 1330～1400 ℃ then, and insulation 5～30min is cooled to room temperature, gets final product.
2. the high-temperature liquid-phase method of attachment between a kind of SiC pottery according to claim 1 and the SiC pottery, 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 high-temperature liquid-phase method of attachment between a kind of SiC pottery according to claim 1 and the SiC pottery is characterized in that the atomicity percentage composition of Si is 40at.%～60at.% in the described Ni-Si powdered alloy.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102191835A CN101709000B (en) | 2009-11-27 | 2009-11-27 | Method for connecting SiC ceramic by high-temperature liquid phase |
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| CN101709000B CN101709000B (en) | 2012-01-04 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885618A (en) * | 2010-08-19 | 2010-11-17 | 哈尔滨工业大学 | Connection method of reactive sintered silicon carbide ceramics |
| CN103193499A (en) * | 2013-04-02 | 2013-07-10 | 江苏大学 | Connection method of carbon/carbon composite material |
| CN103232257A (en) * | 2013-04-02 | 2013-08-07 | 西安交通大学 | Fast connection method of carbon/carbon composite material |
| CN105060914A (en) * | 2015-07-21 | 2015-11-18 | 中国科学院上海应用物理研究所 | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion |
| CN108329047A (en) * | 2017-12-21 | 2018-07-27 | 中核北方核燃料元件有限公司 | A kind of SiCf/SiC composite pipes connection structure and method |
| CN109369209A (en) * | 2018-12-06 | 2019-02-22 | 哈尔滨工业大学 | A kind of method of porous negative expansion ceramic inter-layer assistant brazing |
| CN111185686A (en) * | 2020-01-10 | 2020-05-22 | 西北工业大学 | Method for in-situ connection of SiC/SiC core cladding tube by adopting Zr alloy end plug |
| CN112299869A (en) * | 2020-10-28 | 2021-02-02 | 中国科学院上海硅酸盐研究所 | Laser welding method for silicon carbide and composite material thereof |
-
2009
- 2009-11-27 CN CN2009102191835A patent/CN101709000B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885618A (en) * | 2010-08-19 | 2010-11-17 | 哈尔滨工业大学 | Connection method of reactive sintered silicon carbide ceramics |
| CN101885618B (en) * | 2010-08-19 | 2013-03-06 | 哈尔滨工业大学 | Connection method of reactive sintered silicon carbide ceramics |
| CN103193499A (en) * | 2013-04-02 | 2013-07-10 | 江苏大学 | Connection method of carbon/carbon composite material |
| CN103232257A (en) * | 2013-04-02 | 2013-08-07 | 西安交通大学 | Fast connection method of carbon/carbon composite material |
| CN103232257B (en) * | 2013-04-02 | 2014-12-10 | 西安交通大学 | Fast connection method of carbon/carbon composite material |
| CN103193499B (en) * | 2013-04-02 | 2016-03-02 | 江苏大学 | A kind of method of attachment of carbon-carbon composites |
| CN105060914A (en) * | 2015-07-21 | 2015-11-18 | 中国科学院上海应用物理研究所 | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion |
| CN108329047A (en) * | 2017-12-21 | 2018-07-27 | 中核北方核燃料元件有限公司 | A kind of SiCf/SiC composite pipes connection structure and method |
| CN109369209A (en) * | 2018-12-06 | 2019-02-22 | 哈尔滨工业大学 | A kind of method of porous negative expansion ceramic inter-layer assistant brazing |
| CN109369209B (en) * | 2018-12-06 | 2021-03-30 | 哈尔滨工业大学 | Method for auxiliary brazing of porous negative expansion ceramic interlayer |
| CN111185686A (en) * | 2020-01-10 | 2020-05-22 | 西北工业大学 | Method for in-situ connection of SiC/SiC core cladding tube by adopting Zr alloy end plug |
| CN112299869A (en) * | 2020-10-28 | 2021-02-02 | 中国科学院上海硅酸盐研究所 | Laser welding method for silicon carbide and composite material thereof |
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| CN101709000B (en) | 2012-01-04 |
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