CN101096316A - Instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technique - Google Patents
Instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technique Download PDFInfo
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- CN101096316A CN101096316A CNA2006100470892A CN200610047089A CN101096316A CN 101096316 A CN101096316 A CN 101096316A CN A2006100470892 A CNA2006100470892 A CN A2006100470892A CN 200610047089 A CN200610047089 A CN 200610047089A CN 101096316 A CN101096316 A CN 101096316A
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- sic
- jointing
- phase
- pervasion
- silicification
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- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 239000007791 liquid phase Substances 0.000 title claims description 16
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 title claims description 9
- 238000000034 method Methods 0.000 title abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract 2
- 239000010936 titanium Substances 0.000 claims description 52
- 239000005030 aluminium foil Substances 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 11
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 3
- 238000003466 welding Methods 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005452 bending Methods 0.000 abstract description 3
- 229910009817 Ti3SiC2 Inorganic materials 0.000 abstract 3
- 239000011888 foil Substances 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000001052 transient effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000013001 point bending Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention discloses a new instant liquid-phased dispersing connecting technique of ternary layered ceramic Ti3SiC2, which comprises the following steps: adding aluminum foil with thickness between 50 um and 100um among the welded ternary layered ceramic Ti3SiC2; placing the test sample in the hot-pressed furnace; aerating argon gas to protect; insulating under 600-650 deg. c at 10-20Mpa for 10-30 min; heating at 10-15deg. c/min; setting the welding temperature at 1400-1500 deg. c under 2-5Mpa for 90-180 min. The invention avoids the influence of relative joint strength due to brittle to improve the joint bending strength by 65%, which expands the using scale of Ti3SiC2 ceramic under 1000 deg. c.
Description
Technical field
The present invention relates to ceramic interconnection technique, be specially one and get ternary layered ceramic titanium carbon silicide (Ti
3SiC
2) transient liquid phase diffusion connection novel process.
Background technology
Ti
3SiC
2It is a kind of novel ternary layered ceramic material.U.S. pottery (the Joumal of theAmerican Ceramic Society 79 of association journal, 1953 (1996)) studies show that in that it combines the plurality of advantages of pottery and metal, have low density, high-modulus, high strength, high specific conductivity and thermal conductivity and easy characteristics such as processing, thereby Ti
3SiC
2Pottery is a kind of novel texture/function integration material that gets a good chance of being applied in high-tech sectors such as Aeronautics and Astronautics, nuclear industry and electronic information, especially is suitable as high-temperature structural material.Though to Ti
3SiC
2Synthetic and the performance of pottery carries out studying extensively and profoundly, but owing to can not synthesize large-sized block materials or member, it is restricted in practical application.And welding technique can connect into sample little, simple shape large-sized, complex-shaped member, thereby significantly enlarges the range of application of pottery.Relevant connection Ti
3SiC
2The research of pottery seldom.In investigation of materials journal (Joumal of Materials Research 17,52 (2002)), studied Ti
3SiC
2Pottery is connected with the diffusion of Ti6Al4V.But they connect the joint flexural strength that obtains and have only 100MPa, only are Ti
3SiC
2/ 4th of a pottery flexural strength.And because the high temperature active of Ti has reduced Ti
3SiC
2The ceramic high temperature antioxidant property has also limited Ti
3SiC
2The application of pottery.
Summary of the invention
The object of the invention is to provide a kind of transient liquid phase diffusion to connect ternary layered ceramic Ti
3SiC
2Technology is not reducing ternary layered ceramic Ti
3SiC
2The high-temperature oxidation resistant implementations is foretold, jointing that again can the obtained performance excellence.
Technical scheme of the present invention is:
A kind of ternary layered ceramic Ti
3SiC
2The transient liquid phase diffusion connects novel method.At first, weldment is carried out surface treatment, aluminium foil will be removed surface film oxide, Ti
3SiC
2Pottery is through grinding, polishing.After the sample ultrasonic cleaning, in hot pressing furnace, under the argon shield, be constant voltage insulation 10-30min under the 10-20MPa, guarantee aluminium foil and Ti at 600-650 ℃, pressure
3SiC
2Closely contact reduces the influence of oxygen partial pressure as far as possible.With the temperature rise rate heating of 10-15 ℃/min, the loading rate with 0.2-0.5kN/min is forced into 2-5MPa (as hydraulic loaded) simultaneously then.At target temperature (1400-1500 ℃) insulation 90-180min, the transient liquid phase diffusion connects Ti
3SiC
2Pottery.Unloading after cooling to 1200-1300 ℃ at last with the furnace.Connecting rear interface is Ti mutually
3Si (Al) C
2Sosoloid is avoided the generation of intermetallic compound, obtains high-intensity jointing.
The used aluminium foil purity of the present invention 〉=99% (weight), thickness are 50-100 μ m.All connection procedures all carry out under argon shield.
The transient liquid phase diffusion connection of mentioning among the present invention is meant liquid aluminium in the constant voltage insulating process, diffusion Ti
3SiC
2In the pottery, thereby reach isothermal solidification, diffusion purpose of connecting.So-called " moment liquid state " is meant that when welding temperature began to lower the temperature, liquid aluminium had spread disappearance, rather than solidifies below aluminium fusing point (667 ℃).
The pressure of mentioning among the present invention is meant uniaxial pressure, and loading direction is perpendicular to connecting the surface.
Advantage of the present invention is:
1, the joint mechanical property (comprising high-temperature behavior) that adopts the present invention to obtain is good, and welding residual stress is little.Connect rear interface and generate Ti
3Si (Al) C
2Sosoloid is avoided the formation of intermetallic compound, reduces welding residual stress, avoids intermetallic compound self fragility butt junction Effect on Performance, thereby obtains to have the welding joint of premium properties, and the joint flexural strength can reach Ti
3SiC
265% of ceramics strength, and this intensity can remain to 1000 ℃, can satisfy the needs of practical application, enlarged Ti
3SiC
2The range of application of pottery.
2, the joint of adopting firm the present invention's acquisition does not reduce Ti
3SiC
2High-temperature oxidation resistance, can satisfy its requirement as high-temperature structural material.Generate Ti at the interface owing to connect the back
3Si (Al) C
2Sosoloid generates Al in oxidising process
2O
3, have good anti-oxidation protection performance.
3, adopt technology of the present invention simple, cost is low.Because the appearance of liquid phase is arranged in connection procedure, utilize the quick mass transfer process of liquid phase, the reaction times is shortened greatly.Connect with respect to solid phase diffusion, the tie-time is short, and low to the specimen surface processing requirements, has saved expense again.
Description of drawings
Fig. 1 is Ti
3SiC
2/ Al/Ti
3SiC
2Sample is at 1500 ℃, 120min, 5MPa connection rear interface backscattered electron image photo.
Fig. 2 is for connecting rear interface phase (A) and mother metal Ti
3SiC
2(B) X-ray diffraction spectrum.
Fig. 3 is jointing and Ti
3SiC
2The room temperature of pottery and the contrast of high-temperature bending strength.
Embodiment
Embodiment 1
With Ti
3SiC
2Ceramic grinding, polishing; With aluminium foil with 1000
#SiC sand paper grinds removes surface film oxide, and grinding the back aluminium foil is that 50 μ m are thick; After the sample ultrasonic cleaning, be middle bath layer with aluminium foil, two-layer up and down is Ti
3SiC
2Pottery connects in argon shield in the high temperature hot pressing furnace of packing into.At first constant voltage 20MPa insulation 30min in the time of 600 ℃ guarantees Ti
3SiC
2Pottery closely contacts with Al.With the temperature rise rate heating of 10 ℃/min, the loading rate with 0.2kN/min is forced into 5MPa simultaneously then.At 1500 ℃, insulation 120min cools to 1300 ℃ of unloadings then with the furnace.Connect the rear interface microscopic appearance with scanning electron microscopic observation, found simple substance Al completely dissolve, the interface connects good, does not have pore or remaining welding line to exist.With the phase composite of X-ray diffraction analysis joint interface, the interface forms Ti
3Si (Al) C
2Sosoloid.Joint room temperature three-point bending strength is Ti
3SiC
2The joint three-point bending strength is Ti during pottery 65%, 1000 ℃ of three-point bending strength
3SiC
274% of pottery three-point bending strength.
Embodiment 2
With Ti
3SiC
2Ceramic grinding, polishing; With aluminium foil with 1000
#SiC sand paper grinds removes surface film oxide, and grinding the back aluminium foil is that 70 μ m are thick; After the sample ultrasonic cleaning, be the middle layer with the aluminium foil, two-layer up and down is Ti
3SiC
2Pottery connects in argon shield in the high temperature hot pressing furnace of packing into.At first constant voltage 20MPa insulation 30min in the time of 600 ℃ guarantees Ti
3SiC
2Pottery closely contacts with Al.With the temperature rise rate heating of 15 ℃/min, the speed with 0.5kN/min is forced into 5MPa simultaneously then.After being heated to 1400 ℃, insulation 150min cools to 1200 ℃ of unloadings then with the furnace.Connect the rear interface microscopic appearance with scanning electron microscopic observation, do not observe the existence of simple substance Al, the interface connects good, does not have pore or remaining welding line to exist.With the phase composite of X-ray diffraction analysis joint interface, the interface forms Ti
3Si (Al) C
2Sosoloid.
Embodiment 3
With Ti
3SiC
2Ceramic grinding, polishing; With aluminium foil firm 1000
#SiC sand paper grinds removes surface film oxide, and grinding the back aluminium foil is that 100 μ m are thick; After the sample ultrasonic cleaning, be the middle layer with the aluminium foil, two-layer up and down is Ti
3SiC
2Pottery connects in argon shield in the high temperature hot pressing furnace of packing into.At first constant voltage 10MPa insulation 10min in the time of 650 ℃ guarantees Ti
3SiC
2Pottery closely contacts with Al.With the temperature rise rate heating of 15 ℃/min, the speed with 0.2kN/min is forced into 2MPa simultaneously then.After being heated to 1500 ℃, insulation 180min cools to 1300 ℃ of unloadings then with the furnace.Connect the rear interface microscopic appearance with scanning electron microscopic observation, do not observe the existence of simple substance Al, the interface connects good, does not have pore or remaining welding line to exist.With the phase composite of X-ray diffraction analysis joint interface, the interface forms Ti
3Si (Al) C
2Solid solution is stopped.
Fig. 1 is Ti
3SiC
2/ Al/Ti
3SiC
2Sample is at 1500 ℃, 120min, 5MPa connection rear interface backscattered electron image photo.Simple substance Al has disappeared as seen from the figure, and the interface moulding is good, does not have the existence of pore and remaining welding line.Fig. 2 is for connecting rear interface phase and Ti
3SiC
2X-ray diffraction spectrum.As seen connect rear interface and only generate Ti
3Si (Al) C
2Sosoloid.Do not find any other reacting phase in the drawings, the method for attachment of mentioning in this point and the background technology is significantly different, and the former generates binary or ternary compound.Fig. 3 is jointing and Ti
3SiC
2The room temperature of pottery and the contrast of high-temperature bending strength.As seen utilize the inventive method to connect Ti
3SiC
2Can the good joint of obtained performance, and strength of joint can remain to 1000 ℃.
By embodiment 1, embodiment 2 and embodiment 3 as seen, utilize transient liquid phase diffusion interconnection technique can the obtained performance excellence, be applicable to the welded construction of thermal structure.
Claims (6)
1, a kind of instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology is characterized in that comprising following processing step:
(1) with the aluminium foil be the middle layer, two-layer up and down is Ti
3SiC
2Pottery in hot pressing furnace, under the argon shield, is constant voltage insulation 10-30min under the 10-20MPa at 600-650 ℃, pressure, guarantees aluminium foil and Ti
3SiC
2Closely contact;
(2) be that 1400-1500 ℃, pressure are constant voltage insulation 90-180min under the 2-5MPa in temperature, connect Ti
3SiC
2Pottery;
(3) cool to 1200-1300 ℃ with the furnace after the unloading.
2, according to the described instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology of claim 1, it is characterized in that: in the described step (2), be heated to 1400-1500 ℃, insulation 90-180min with the temperature rise rate of 10-15 ℃/min.
3, according to the described instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology of claim 1, it is characterized in that: in the described step (2), be forced into 2-5MPa with the loading rate of 0.2-0.5kN/min.
4, according to the described instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology of claim 1, it is characterized in that: be the middle layer with the aluminium foil, aluminium foil purity 〉=99%, thickness are 50-100 μ m.
5, according to the described instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology of claim 1, it is characterized in that: in described step (1) before, weldment is shown and handled, aluminium foil will be removed surface film oxide, Ti
3SiC
2Pottery is through grinding, polishing; Then, to aluminium foil and Ti
3SiC
2Pottery carries out ultrasonic cleaning.
6, according to the described instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technology of claim 1, it is characterized in that: described connection atmosphere is argon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100470892A CN100460362C (en) | 2006-06-30 | 2006-06-30 | Instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technique |
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|---|---|---|---|
| CNB2006100470892A CN100460362C (en) | 2006-06-30 | 2006-06-30 | Instant liquid-phase pervasion jointing ternary layered ceramic titanium carbon silicification technique |
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| Publication Number | Publication Date |
|---|---|
| CN101096316A true CN101096316A (en) | 2008-01-02 |
| CN100460362C CN100460362C (en) | 2009-02-11 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584311A (en) * | 2012-02-21 | 2012-07-18 | 内蒙古工业大学 | Ceramic connection method by using high-temperature interlayer material |
| CN104874909A (en) * | 2015-06-10 | 2015-09-02 | 湖北三江航天江北机械工程有限公司 | Liquid-phase diffusion bonding method for quartz composite ceramic and iron-nickel alloy |
| CN105016763A (en) * | 2015-07-27 | 2015-11-04 | 大连理工大学 | Method for connecting TiAl-base alloy and Ti3SiC2 ceramic |
| CN106699214A (en) * | 2016-12-26 | 2017-05-24 | 安徽工业大学 | Ternary lamellar ceramic titanium silicon carbide and metallic nickel diffusion bonding method |
| CN106868331A (en) * | 2017-01-20 | 2017-06-20 | 华南理工大学 | A kind of preparation method of three-dimensional netted Metal Substrate titanium Si-C composite material |
| 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 |
| CN108947558A (en) * | 2017-05-27 | 2018-12-07 | 天津大学 | A kind of metal and Ti3SiC2The connection method of ceramics |
| CN114029601A (en) * | 2021-12-09 | 2022-02-11 | 哈尔滨工业大学 | Method for diffusion bonding of Ti3SiC2 ceramic by adopting gold foil intermediate layer at low temperature |
| CN114180983A (en) * | 2020-09-15 | 2022-03-15 | 中国科学院金属研究所 | Ternary layered ceramic titanium silicon carbon based on Zn foil interlayer and diffusion connection method of solid solution of ternary layered ceramic titanium silicon carbon and ferritic stainless steel |
| CN114180982A (en) * | 2020-09-15 | 2022-03-15 | 青岛大学 | Diffusion connection method of ternary layered ceramic titanium silicon carbon based on Al foil interlayer and solid solution thereof and ferritic stainless steel |
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| CN1179918C (en) * | 2003-06-20 | 2004-12-15 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block body material by using si as adjurant through hot pressing process |
| CN1179917C (en) * | 2003-06-20 | 2004-12-15 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block material by using Al as adjuvant through discharge plasma agglomeration process |
-
2006
- 2006-06-30 CN CNB2006100470892A patent/CN100460362C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584311A (en) * | 2012-02-21 | 2012-07-18 | 内蒙古工业大学 | Ceramic connection method by using high-temperature interlayer material |
| CN104874909A (en) * | 2015-06-10 | 2015-09-02 | 湖北三江航天江北机械工程有限公司 | Liquid-phase diffusion bonding method for quartz composite ceramic and iron-nickel alloy |
| CN104874909B (en) * | 2015-06-10 | 2017-01-25 | 湖北三江航天江北机械工程有限公司 | Liquid-phase diffusion bonding method for quartz composite ceramic and iron-nickel alloy |
| CN105016763A (en) * | 2015-07-27 | 2015-11-04 | 大连理工大学 | Method for connecting TiAl-base alloy and Ti3SiC2 ceramic |
| 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 |
| CN106699214A (en) * | 2016-12-26 | 2017-05-24 | 安徽工业大学 | Ternary lamellar ceramic titanium silicon carbide and metallic nickel diffusion bonding method |
| CN106868331A (en) * | 2017-01-20 | 2017-06-20 | 华南理工大学 | A kind of preparation method of three-dimensional netted Metal Substrate titanium Si-C composite material |
| CN108947558A (en) * | 2017-05-27 | 2018-12-07 | 天津大学 | A kind of metal and Ti3SiC2The connection method of ceramics |
| CN114180983A (en) * | 2020-09-15 | 2022-03-15 | 中国科学院金属研究所 | Ternary layered ceramic titanium silicon carbon based on Zn foil interlayer and diffusion connection method of solid solution of ternary layered ceramic titanium silicon carbon and ferritic stainless steel |
| CN114180982A (en) * | 2020-09-15 | 2022-03-15 | 青岛大学 | Diffusion connection method of ternary layered ceramic titanium silicon carbon based on Al foil interlayer and solid solution thereof and ferritic stainless steel |
| CN114180983B (en) * | 2020-09-15 | 2022-09-06 | 中国科学院金属研究所 | Ternary layered ceramic titanium silicon carbon based on Zn foil interlayer and diffusion connection method of solid solution of ternary layered ceramic titanium silicon carbon and ferritic stainless steel |
| CN114180982B (en) * | 2020-09-15 | 2022-12-20 | 青岛大学 | Diffusion connection method of ternary layered ceramic titanium silicon carbon and solid solution thereof and ferritic stainless steel based on Al foil interlayer |
| CN114029601A (en) * | 2021-12-09 | 2022-02-11 | 哈尔滨工业大学 | Method for diffusion bonding of Ti3SiC2 ceramic by adopting gold foil intermediate layer at low temperature |
| CN114029601B (en) * | 2021-12-09 | 2023-02-28 | 哈尔滨工业大学 | Method for low-temperature diffusion connection of Ti3SiC2 ceramic by adopting gold foil intermediate layer |
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| Publication number | Publication date |
|---|---|
| CN100460362C (en) | 2009-02-11 |
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Granted publication date: 20090211 Termination date: 20110630 |