CN102584311A - Ceramic connection method by using high-temperature interlayer material - Google Patents
Ceramic connection method by using high-temperature interlayer material Download PDFInfo
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- CN102584311A CN102584311A CN2012100384676A CN201210038467A CN102584311A CN 102584311 A CN102584311 A CN 102584311A CN 2012100384676 A CN2012100384676 A CN 2012100384676A CN 201210038467 A CN201210038467 A CN 201210038467A CN 102584311 A CN102584311 A CN 102584311A
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Abstract
The invention belongs to the field of ceramic material preparation and provides a ceramic connection method by using a high-temperature interlayer material. Ti3SiC2 is used as a high-temperature interlayer material, the high-temperature interlayer material and a ceramic material are loaded in a graphite die in a sequence of the ceramic material, the high-temperature interlayer material and the ceramic material, the connection of the ceramic material is realized through a spark plasma sintering technology, and excellent connection effect is achieved during the connection of carborundum ceramic. The high-temperature interlayer material can be directly used for connecting the ceramic material and a ceramic-based composite material without conducting surface pre-coating or other modification treatments to the surface of the ceramic material before connection. The ceramic material connected by the high-temperature interlayer material has high connection strength and stable high-temperature property.
Description
Technical field
The invention belongs to field of ceramic material preparation, relate in particular to a kind of high temperature intermediate layer material that adopts and carry out the method that pottery connects.
Background technology
Advanced structural ceramic is like silicon nitride, silit, zirconium white, aluminum oxide, hexagonal boron nitride; Because of its excellent high-temperature mechanical property, low thermal coefficient of expansion, high thermal conductivity, good thermal-shock resistance and light specific gravity; Have only 1/3rd of common metal, be widely used in the hot environment of various harshnesses.But because the structural characteristics of stupalith, lower like fracture toughness property, intensity is dispersed big, and work reliability is poor, poor in processability, these drawbacks limit their development and application.Concrete manifestation is both ways: at first, the vice proper of bulk stupalith is difficult to eliminate and skewness like pore, tiny crack etc., causes intensity to be disperseed; Comparatively speaking, the fritter pottery is easy to manufacture, obtains the good mechanical performance more easily.Secondly,, and can not shift and relax, cause fracture through viscous deformation because the intrinsic fragility and the non-deformable property of stupalith be prone to produce stress concentration at its sharp corner when making complex-shaped ceramic component.Make the practical applications of advanced ceramics material be restricted to a great extent thus.When practical application,, usually need connect the back and use in order to overcome problems such as its fragility and difficult processing.Simultaneously, utilize interconnection technique can the widget of simple shape be connected to complex-shaped big parts, thereby overcome the unmanageable shortcoming of stupalith.In addition, thus utilize interconnection technique can be at an easy rate repair the safety and the work-ing life of improving ceramic structure to component.Owing to the reason of these several respects makes pottery be connected to become advanced structural ceramic material practicability, through engineering approaches, thereby promote one of advanced ceramics material broader applications very necessary technology.
Though what better used at present is in stressed less electron tube and the stressed big but not high occasion of use temperature.With the most sophisticated solder Ag-Cu-Ti (3-7wtTi) the soldering Si that generally acknowledges
3N
4-Si
3N
4Pottery, room temperature joint four-point bending intensity can reach 789MPa.But Ag-Cu-Ti solder oxidation-resistance is poor, uses the joint of its soldering can not be used for the environment more than 450 ℃, has therefore restricted the performance of advanced structural ceramic high-temperature behavior.
Connected in the new type high temperature solder of usefulness at the research pottery since more than ten years recently both at home and abroad, the mode of employing has: (1) adopts dystectic precious metal as solder.People such as J.H.Selrverian are using Au-Pd-Ni soldering Si
3N
4When pottery and Ni, on ceramic surface, plate Ti, Zr or Hf respectively, the wettability of solder is best when finding plating Ti; Shear strength is the highest, is 75-100MPa under the room temperature, and shear strength is 85-105MPa in the time of 500 ℃; And the price comparison of precious metal solder is expensive, is difficult in the actual production promote.
(2) adopt CuNiTiB chilling solder to connect Si
3N
4Pottery discovers that the tissue of Cu-(5-25) Ni-(16-28) the TiB solder of handling through chilling is more even than the solder of handling without chilling, helps improving Si
3N
4/ Si
3N
4The intensity of joint.
(3) adopt amorphous intermediate layer.Amorphous filler metal also is that present pottery/pottery, ceramic/metal belong to the important research direction in soldering field.The Cu-Ti amorphous filler metal that Naka has studied 3 kinds of compositions connects Si
3N
4Pottery, joint room temperature shearing resistance is up to 313MPa.
Yet adopt metallic substance still to have a lot of shortcomings as the middle layer: (1) pottery and metal be not easy to produce good engaging at the interface.Be because the lattice types of these two kinds of materials is different, and metallic substance is a metallic bond on the one hand, and mostly stupalith is covalent linkage; On the other hand, the stupalith chemicalstability is good, and the wettability of metal pair stupalith is relatively poor usually, and promptly the consistency of two kinds of materials is relatively poor.(2) thermal expansivity of pottery and metal differs greatly, and has caused the unrelieved stress that connects in the joint of back too high.(3) metal intermediate layer oxidation-resistance, erosion resistance are relatively poor, and the joint that connects with their is not suitable for complicated hot environment.In the surface reaction process, form frangible compounds when (4) metal intermediate layer connects stupalith easily, influence the web member performance.
In sum, also lack at present both at home and abroad and can be used for directly that advanced structural ceramic connects and joint at high temperature has the practical high temperature intermediate layer material and the interconnection technique of stable high-temperature behavior.
Summary of the invention
The invention provides a kind of high temperature intermediate layer material that adopts and carry out the ceramic method that connects, be intended to solve domestic and international at present also shortage and can directly be used for the stupalith connection and at high temperature have the high temperature intermediate layer material of stable high-temperature behavior and the problem of stupalith interconnection technique.
The object of the present invention is to provide a kind of preparation method who is used for the high temperature intermediate layer material of pottery connection, this preparation method may further comprise the steps:
The raw material composition of selecting for use is allocated according to certainweight per-cent;
The raw material that proportioning is good adds absolute ethyl alcohol, and carries out ball-milling processing;
Dry with loft drier, adopt discharge plasma sintering technique to handle.
Further, said high temperature intermediate layer material is Ti
3SiC
2System, material composition and the weight percent selected for use consist of: Ti:68-78%, Si:14-70%, C:12-13%, TiC:30-90%, SiC:22-40%.
Further, said material composition of selecting for use and the available combination of weight percent have:
First kind of combination: Ti:68-78%, Si:14-20%, C:12-13%;
Second kind of combination: TiC:30-90%, Si:14-70%;
The third combination: Ti:68-78%, SiC:22-40%.
Further, to add the time of carrying out ball-milling processing behind the absolute ethyl alcohol be 1-4h to said raw material that proportioning is good.
Temperature when further, said drying baker is dried is 50-70 ℃.
Further, when adopting discharge plasma sintering technique among the said preparation method, need rise to 1100-1400 ℃ with 50-100 ℃/min temperature rise rate, sintering time is 5-15min, applies the pressure of 20-40MPa, and in sintering process, feeds argon gas.
Another object of the present invention is to provide a kind of high temperature intermediate layer material that adopts to carry out the method that pottery connects, this method may further comprise the steps:
High temperature intermediate layer material and stupalith are fitted into graphite jig in a certain order;
Adopt discharge plasma sintering technique that stupalith is connected;
Stupalith is cooled to room temperature.
Further, the order that said high temperature intermediate layer material and stupalith are fitted into graphite jig is: at first put into stupalith, put into the high temperature intermediate layer material then, put into stupalith at last.
Further, said employing discharge plasma sintering technique to the implementation method that stupalith connects is: the graphite jig that will be equipped with high temperature intermediate layer material and stupalith is put into the discharge plasma sintering stove and is heated, is incubated.
Further, the discharge plasma sintering technique in the said method can be substituted by high temperature sintering.
Employing high temperature intermediate layer material provided by the invention carries out the method that pottery connects, and adopts Ti
3SiC
2As the high temperature intermediate layer material; High temperature intermediate layer material and stupalith are fitted into graphite jig according to stupalith, high temperature intermediate layer material, stupalith mode; Adopt discharge plasma sintering technique to realize that the high temperature of stupalith connects; When connecting silicon carbide ceramics, obtained good connection effect.The high temperature intermediate layer material can be used for directly connecting stupalith and ceramic matric composite; Need before connection, not carry out surperficial preplating film or other modification processing to ceramic material surfaces; The stupalith that adopts this high temperature intermediate layer material to connect, strength of joint is high and have stable high-temperature performance.
Description of drawings
Fig. 1 is the preparing method's who is used for the high temperature intermediate layer material that pottery connects that provides of the embodiment of the invention realization flow figure;
Fig. 2 is the realization flow figure that employing high temperature intermediate layer material that the embodiment of the invention provides carries out the method that pottery connects.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further specified below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in the qualification invention.
Fig. 1 shows that the embodiment of the invention provides is used for the preparing method's of the high temperature intermediate layer material that pottery connects realization flow.
This preparation method may further comprise the steps:
In step S101, the raw material composition of selecting for use is allocated according to certainweight per-cent;
In step S102, the raw material that proportioning is good adds absolute ethyl alcohol, and carries out ball-milling processing;
In step S103, dry with loft drier, adopt discharge plasma sintering technique to handle.
In embodiments of the present invention, the high temperature intermediate layer material is Ti
3SiC
2System, material composition and the weight percent selected for use consist of: Ti:68-78%, Si:14-70%, C:12-13%, TiC:30-90%, SiC:22-40%.
In embodiments of the present invention, the available combination of material composition of selecting for use and weight percent has:
1、Ti：68-78％，Si：14-20％，C：12-13％；
2、TiC：30-90％，Si：14-70％；
3、Ti：68-78％，SiC：22-40％。
In embodiments of the present invention, to add the time of carrying out ball-milling processing behind the absolute ethyl alcohol be 1-4h for raw material that proportioning is good.
Temperature when in embodiments of the present invention, drying baker is dried is 50-70 ℃.
In embodiments of the present invention, when adopting discharge plasma sintering technique among the preparation method, need rise to 1100-1400 ℃ with 50-100 ℃/min temperature rise rate, sintering time is 5-15min, applies the pressure of 20-40MPa, and in sintering process, feeds argon gas.
The employing high temperature intermediate layer material that Fig. 2 shows the embodiment of the invention to be provided carries out the realization flow of the method for pottery connection.
In step S201, high temperature intermediate layer material and stupalith are fitted into graphite jig in a certain order;
In step S202, adopt discharge plasma sintering technique that stupalith is connected;
In step S203, stupalith is cooled to room temperature.
In embodiments of the present invention, the order that high temperature intermediate layer material and stupalith are fitted into graphite jig is: at first put into stupalith, put into the high temperature intermediate layer material then, put into stupalith at last.
In embodiments of the present invention, adopt discharge plasma sintering technique to the implementation method that stupalith connects to be: the graphite jig that will be equipped with high temperature intermediate layer material and stupalith is put into the discharge plasma sintering stove and is heated, is incubated.
In embodiments of the present invention, the discharge plasma sintering technique in the method can be substituted by high temperature sintering.
Below in conjunction with accompanying drawing and specific embodiment application principle of the present invention is further described.
The high temperature intermediate layer material that is used for advanced structural ceramic and ceramic matric composite connection that the embodiment of the invention provides; Available composition and weight percent consist of: Ti:68-78%; Si:14-70%, C:12-13%, TiC:30-90%; SiC:22-40%, wherein the high temperature intermediate layer material is Ti
3SiC
2System; According to the requirement of above-mentioned total technical scheme, multiple weight percent below can further proposing is formed:
1、Ti：68-78％，Si：14-20％，C：12-13％；
2、TiC：30-90％，Si：14-70％；
3、Ti：68-78％，SiC：22-40％。
The method for preparing the high temperature intermediate layer material is: after the raw material that proportioning is good adds absolute ethyl alcohol ball-milling processing 1-4h; Dry down at 50-70 ℃ with loft drier; Adopt discharge plasma sintering technique, rise to 1100-1400 ℃ with 50-100 ℃/min temperature rise rate, sintering time 5-15min; Apply 20-40MPa pressure, and in sintering process, lead to argon gas atmosphere.
The method of using above-mentioned high temperature intermediate layer material to carry out the pottery connection is:
High temperature intermediate layer material and stupalith are gone into graphite jig according to the assembled in sequence of stupalith, intermediate layer material, stupalith, put into discharge plasma sintering stove heat tracing together with graphite jig, and then cool to room temperature with the furnace.
The employing high temperature intermediate layer material that the embodiment of the invention provides carries out the method that pottery connects, and adopts Ti
3SiC
2As the high temperature intermediate layer material; High temperature intermediate layer material and stupalith are fitted into graphite jig according to stupalith, high temperature intermediate layer material, stupalith mode; Adopt discharge plasma sintering technique to realize that the high temperature of stupalith connects; When connecting silicon carbide ceramics, obtained good connection effect.The high temperature intermediate layer material can be used for directly connecting stupalith and ceramic matric composite; Need before connection, not carry out surperficial preplating film or other modification processing to ceramic material surfaces; The stupalith that adopts this high temperature intermediate layer material to connect, strength of joint is high and have stable high-temperature performance.
More than be merely preferred embodiment of the present invention,, all any modifications of within spirit of the present invention and principle, being done, be equal to and replace and improvement etc., all should be included within protection scope of the present invention not in order to restriction the present invention.
Claims (10)
1. preparation method who is used for the high temperature intermediate layer material that pottery connects is characterized in that this preparation method may further comprise the steps:
The raw material composition of selecting for use is allocated according to certainweight per-cent;
The raw material that proportioning is good adds absolute ethyl alcohol, and carries out ball-milling processing;
Dry with loft drier, adopt discharge plasma sintering technique to handle.
2. preparation method as claimed in claim 1 is characterized in that, said high temperature intermediate layer material is the Ti3SiC2 system; Material composition and the weight percent selected for use consist of: Ti:68-78%, Si:14-70%, C:12-13%; TiC:30-90%, SiC:22-40%.
3. according to claim 1 or claim 2 preparation method is characterized in that said material composition of selecting for use and the available combination of weight percent have:
First kind of combination: Ti:68-78%, Si:14-20%, C:12-13%;
Second kind of combination: TiC:30-90%, Si:14-70%;
The third combination: Ti:68-78%, SiC:22-40%.
4. preparation method as claimed in claim 1 is characterized in that, it is 1-4h that said raw material that proportioning is good adds the time of carrying out ball-milling processing behind the absolute ethyl alcohol.
5. preparation method as claimed in claim 1 is characterized in that, the temperature when said drying baker is dried is 50-70 ℃.
6. preparation method as claimed in claim 1; It is characterized in that; When adopting discharge plasma sintering technique among the said preparation method, need rise to 1100-1400 ℃ with 50-100 ℃/min temperature rise rate, sintering time is 5-15min; Apply the pressure of 20-40MPa, and in sintering process, feed argon gas.
7. one kind is adopted the high temperature intermediate layer material to carry out the method that pottery connects, and it is characterized in that this method may further comprise the steps:
High temperature intermediate layer material and stupalith are fitted into graphite jig in a certain order;
Adopt discharge plasma sintering technique that stupalith is connected;
Stupalith is cooled to room temperature.
8. preparation method as claimed in claim 7 is characterized in that, the order that said high temperature intermediate layer material and stupalith are fitted into graphite jig is: at first put into stupalith, put into the high temperature intermediate layer material then, put into stupalith at last.
9. preparation method as claimed in claim 7; It is characterized in that said employing discharge plasma sintering technique to the implementation method that stupalith connects is: the graphite jig that will be equipped with high temperature intermediate layer material and stupalith is put into the discharge plasma sintering stove and is heated, is incubated.
10. preparation method as claimed in claim 7 is characterized in that, the discharge plasma sintering technique in the said method can be substituted by high temperature sintering.
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Cited By (8)
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| CN104725066A (en) * | 2013-12-24 | 2015-06-24 | 中国科学院兰州化学物理研究所 | Hot pressing reaction sintering connection method for ceramic material titanium silicon carbide |
| CN107487055A (en) * | 2016-06-12 | 2017-12-19 | 中国科学院宁波材料技术与工程研究所 | The application of multilayer complex films, its preparation method and the connecting material as carbon fibre-reinforced carbon composite material |
| CN107827477A (en) * | 2017-10-27 | 2018-03-23 | 兰州理工大学 | Based on Ti3SiC2Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer |
| 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 |
| CN108838504A (en) * | 2018-07-17 | 2018-11-20 | 合肥工业大学 | It is a kind of for spread connection silicon carbide ceramics composite interlayer and its Joining Technology |
| CN109899602A (en) * | 2019-04-10 | 2019-06-18 | 上海伟星新型建材有限公司 | Flame retardant type fiber reinforcement polypropylene random copolymer composite tube and preparation method thereof |
| CN110041090A (en) * | 2019-05-23 | 2019-07-23 | 合肥工业大学 | A kind of plasma discharging diffusion connection method of silicon carbide ceramics |
| CN115073152A (en) * | 2022-07-22 | 2022-09-20 | 内蒙古工业大学 | Laminated ceramic composite material and preparation method thereof, lanthanum chromate ceramic and manufacturing process thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725066A (en) * | 2013-12-24 | 2015-06-24 | 中国科学院兰州化学物理研究所 | Hot pressing reaction sintering connection method for ceramic material titanium silicon carbide |
| CN107487055A (en) * | 2016-06-12 | 2017-12-19 | 中国科学院宁波材料技术与工程研究所 | The application of multilayer complex films, its preparation method and the connecting material as carbon fibre-reinforced carbon composite material |
| CN107487055B (en) * | 2016-06-12 | 2019-08-20 | 中国科学院宁波材料技术与工程研究所 | The application of multilayer complex films, preparation method and the connecting material as carbon fibre-reinforced carbon composite material |
| CN107827477A (en) * | 2017-10-27 | 2018-03-23 | 兰州理工大学 | Based on Ti3SiC2Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer |
| CN107827477B (en) * | 2017-10-27 | 2020-09-08 | 兰州理工大学 | Based on Ti3SiC2Reaction diffusion bonding method for carbon-carbon composite material with-Al mixed powder as intermediate layer |
| 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 |
| CN108838504A (en) * | 2018-07-17 | 2018-11-20 | 合肥工业大学 | It is a kind of for spread connection silicon carbide ceramics composite interlayer and its Joining Technology |
| CN109899602A (en) * | 2019-04-10 | 2019-06-18 | 上海伟星新型建材有限公司 | Flame retardant type fiber reinforcement polypropylene random copolymer composite tube and preparation method thereof |
| CN110041090A (en) * | 2019-05-23 | 2019-07-23 | 合肥工业大学 | A kind of plasma discharging diffusion connection method of silicon carbide ceramics |
| CN115073152A (en) * | 2022-07-22 | 2022-09-20 | 内蒙古工业大学 | Laminated ceramic composite material and preparation method thereof, lanthanum chromate ceramic and manufacturing process thereof |
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Application publication date: 20120718 |