CN106007773B - A kind of vacuum brazing method of porous silicon nitride ceramic and TiAl-base alloy - Google Patents
A kind of vacuum brazing method of porous silicon nitride ceramic and TiAl-base alloy Download PDFInfo
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- CN106007773B CN106007773B CN201610347362.7A CN201610347362A CN106007773B CN 106007773 B CN106007773 B CN 106007773B CN 201610347362 A CN201610347362 A CN 201610347362A CN 106007773 B CN106007773 B CN 106007773B
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Abstract
The invention discloses the vacuum brazing methods of a kind of porous silicon nitride ceramic and TiAl-base alloy, Step 1: the nano silicon nitride silicon particle, the Ti powder that mass fraction is 2 ~ 4wt.% and AgCu powder that mass fraction is 1.5 ~ 3wt.% are carried out 4 ~ 6h of mechanical ball mill, composite soldering is mentioned；Step 2: the composite soldering after ball milling is assembled with pretreated TiAl-base alloy and porous silicon nitride base material, keep solder powder thickness between 50 ~ 200 μm；Step 3: the soldered fitting assembled is put into vacuum drying oven, it is heated to 840 DEG C ~ 900 DEG C under vacuum conditions, keep the temperature 5min ~ 30min, realize effective connection high-intensitive between porous ceramics and alloy substrate, technical solution of the present invention can effectively solve the problem that the connectivity problem of porous ceramics and TiAl-base alloy, obtain the soldered fitting of good mechanical performance.
Description
Technical field
The present invention relates to radome manufacturing technology fields, and in particular to a kind of porous silicon nitride ceramic and TiAl base close
The vacuum brazing method of gold.
Background technique
It is known that porous silicon nitride ceramic because of its good wave, all has outstanding in room temperature and hot environment
Mechanical performance and lower dielectric constant and the cover material for being applied to manufacture radome, and radar antenna cover
It needs in application process and there is high specific strength, specific stiffness, good inoxidizability and excellent mechanical behavior under high temperature
TiAl-base alloy bracket is effectively connected.However thermal expansion coefficient and Young's modulus etc. between ceramics and metal exist compared with
Big difference is also easy to produce biggish residual stress during the connection process and influences the performance of jointing between base material.To understand
Certainly this problem, researcher introduces the concept of composite soldering in the connection of ceramics and metal, i.e., in common metal base pricker
Second Phase Particle or fiber etc. are introduced in material, it is made to produce the similar interface group with metal-based compound solder during the connection process
It knits to alleviate the difference of the thermal expansion coefficient between dissimilar material base material, Young's modulus.The thinking of this composite soldering is introduced into
And be applied among the present invention, to obtain effective soldering connection of porous silicon nitride ceramic and TiAl-base alloy.
Summary of the invention
It can be realized effective connection high-intensitive between porous ceramics and alloy substrate the object of the present invention is to provide a kind of,
The porous silicon nitride ceramic of soldered fitting good mechanical performance and the vacuum brazing method of TiAl-base alloy.
In order to achieve the above objectives, the technical scheme adopted by the invention is that:
A kind of vacuum brazing method of porous silicon nitride ceramic and TiAl-base alloy, includes the following steps:
Step 1: nano silicon nitride silicon particle, Ti powder and AgCu powder 4 ~ 6h of mechanical ball mill are obtained into composite soldering, it is described
Composite soldering in containing weight fraction be 1.5 ~ 3wt.% nano silicon nitride silicon particle, weight fraction be 2 ~ 4wt.% Ti powder,
Surplus is AgCu powder；
Step 2: the composite soldering after ball milling is filled with pretreated TiAl-base alloy and porous silicon nitride base material
Match, keep solder powder thickness between 50 ~ 200 μm,
Step 3: the soldered fitting assembled is put into vacuum drying oven, it is heated to 840 DEG C ~ 900 DEG C under vacuum conditions,
Keep the temperature 5min ~ 30min.
The size of nano silicon nitride silicon particle described in step 1 is 20nm ~ 50nm, Ti powder and AgCu eutectic in the present invention
The size of powder is 10 μm ~ 50 μm.
The porosity of porous silicon nitride base material is 45% ~ 60% in step 2 of the present invention.
Pretreated TiAl-base alloy refers to that chemical constituent is the TiAl of Ti-46Al-2Nb-2Cr in step 2 of the present invention
Alloy.
Pretreated porous silicon nitride base material refers to that group is divided into 92%Si in step 2 of the present invention3N4 +6% Y2 O3 +2%
Al2 O3Porous ceramics.
The surface to be welded of TiAl-base alloy and porous silicon nitride base material 200#, 400#, 800#SiC sand in step 2 of the present invention
Paper is polished, and is cleaned by ultrasonic 15min ~ 20min in acetone soln.
In step 3 of the present invention, to guarantee coming into full contact between solder and base material, on the fitting side apply 0.5MPa ~
The axial compressive force of 2MPa, the more preferably axial compressive force of 1.5MPa, to improve joint quality.
Further, method for welding of the invention guarantees that vacuum degree is 10 in furnace in brazing process-2~10-4Pa, soldering rise
Warm rate is 5 DEG C/min ~ 10 DEG C/min, and cooling rate is 1 DEG C/min ~ 5 DEG C/min.
In step 3 of the present invention, to guarantee coming into full contact between solder and base material, side applies 1.5MPa on the fitting
Axial compressive force, guarantee that vacuum degree is 10 in furnace in brazing process-4Pa, soldering heating rate are 10 DEG C/min, cooling rate 1
℃/min。
The present invention realizes effective connection high-intensitive between porous ceramics and alloy substrate, and the mechanical property of soldered fitting is excellent
Good, the expansion for improving porous ceramics and solder bonding metal connector is extensively applied.
Detailed description of the invention
Fig. 1 is a kind of back scattering photo of jointing of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
A kind of vacuum brazing method of porous silicon nitride ceramic and TiAl-base alloy, includes the following steps:
Step 1: nano silicon nitride silicon particle, Ti powder and AgCu powder 4 ~ 6h of mechanical ball mill are obtained into composite soldering, it is described
Composite soldering in containing weight fraction be 1.5 ~ 3wt.% nano silicon nitride silicon particle, weight fraction be 2 ~ 4wt.% Ti powder,
Surplus is AgCu powder；
Step 2: the composite soldering after ball milling is filled with pretreated TiAl-base alloy and porous silicon nitride base material
Match, keep solder powder thickness between 50 ~ 200 μm,
Step 3: the soldered fitting assembled is put into vacuum drying oven, it is heated to 840 DEG C ~ 900 DEG C under vacuum conditions,
Keep the temperature 5min ~ 30min；The size of the nano silicon nitride silicon particle is 20nm ~ 50nm, the size of Ti powder and AgCu eutectic powder
It is 10 μm ~ 50 μm；The porosity of porous silicon nitride base material is 45% ~ 60% in rapid two；Pretreated TiAl base closes in step 2
Gold refers to that chemical constituent is the TiAl alloy of Ti-46Al-2Nb-2Cr；Pretreated porous silicon nitride base material is in step 2
Finger group is divided into 92%Si3N4 +6% Y2 O3 +2%Al2 O3Porous ceramics；TiAl-base alloy and porous silicon nitride are female in step 2
The surface to be welded of material is polished with 200#, 400#, 800#SiC sand paper, and is cleaned by ultrasonic 15min ~ 20min in acetone soln；
In step 3, to guarantee coming into full contact between solder and base material, side applies the axial pressure of 0.5MPa ~ 2MPa on the fitting
Power, to improve joint quality；Guarantee that vacuum degree is 10 in furnace in brazing process-2~10-4Pa, soldering heating rate be 5 DEG C/min ~
10 DEG C/min, cooling rate is 1 DEG C/min ~ 5 DEG C/min, in addition, in step 3 of the present invention, to guarantee between solder and base material
It comes into full contact with, side applies the axial compressive force of 1.5MPa on the fitting, guarantees that vacuum degree is 10 in furnace in brazing process-4Pa, pricker
Weldering heating rate is 10 DEG C/min, and cooling rate is 1 DEG C/min.
Embodiment 1:
Step 1: the porosity of porous silicon nitride be 45% ~ 60%, by mass fraction be 1.5 ~ 3wt.% having a size of 20nm ~
Nano silicon nitride silicon particle, the mass fraction of 50nm is 2 ~ 4wt.% mechanical having a size of 10 μm ~ 50 μm of Ti powder and AgCu powder progress
4 ~ 6h of ball milling.
Step 2: the surface to be welded of TiAl-base alloy and porous silicon nitride base material is carried out with 200#, 400#, 800#SiC sand paper
Polishing, and it is cleaned by ultrasonic 15min ~ 20min in acetone soln.Composite soldering after ball milling is closed with pretreated TiAl base
Gold and porous silicon nitride base material are assembled, and keep solder powder thickness between 50 ~ 200 μm.
Step 3: side applies the axis of 0.5MPa ~ 2MPa on the fitting to guarantee coming into full contact between solder and base material
To pressure, the soldered fitting assembled is put into vacuum drying oven, in vacuum degree 10-2~10-4With heating rate for 5 under Pa environment
DEG C/min ~ 10 DEG C/min is heated to 840 DEG C ~ 900 DEG C, 5min ~ 30min is kept the temperature, then with 1 DEG C/min ~ 5 DEG C/min cooling rate
It is cooled to room temperature.
Embodiment 2:
The difference of the present embodiment and embodiment 1 is that the porosity of porous silicon nitride in step 1 is 50%.Other steps
It is identical as specific embodiment 1.
Embodiment 3:
Difference of the present embodiment from embodiment 2 is that the mass percent of nano silicon nitride silicon particle in step 1 is
The mass percent of 2wt.%, Ti powder is 2wt.%.Other steps are identical as specific embodiment 2.
Embodiment 4:
The difference of the present embodiment and embodiment 3 is in step 3 that brazing process parameter is 10 DEG C/min of heating rate,
Brazing temperature be 860 DEG C, soaking time 10min, after be cooled to room temperature with 1 DEG C/min.Other steps and 3 phase of specific embodiment
Together.
Embodiment 5:
The difference of the present embodiment and embodiment 3 is in step 3 that brazing process parameter is 10 DEG C/min of heating rate,
Brazing temperature be 880 DEG C, soaking time 20min, after be cooled to room temperature with 3 DEG C/min.Other steps and 3 phase of specific embodiment
Together.
Embodiment 6:
The difference of the present embodiment and embodiment 3 is in step 3 that brazing process parameter is 5 DEG C/min of heating rate, pricker
Weld temperature be 900 DEG C, soaking time 10min, after be cooled to room temperature with 5 DEG C/min.Other steps and 3 phase of specific embodiment
Together.
Embodiment 7:
The difference of the present embodiment and embodiment 2 be solder powder in step 2 with a thickness of 100 μm.Other steps and tool
Body embodiment 2 is identical.
Embodiment 8:
The difference of the present embodiment and embodiment 2 is in step 3, to guarantee coming into full contact between solder and base material,
Side applies the axial compressive force of 1.5MPa on the fitting, guarantees that vacuum degree is 10 in furnace in brazing process-4Pa is brazed heating rate
For 10 DEG C/min, cooling rate is 1 DEG C/min.
It is provided for the embodiments of the invention the vacuum brazing side of a kind of porous silicon nitride ceramic and TiAl-base alloy above
Method is described in detail, and used herein a specific example illustrates the principle and implementation of the invention, above
The explanation of embodiment is merely used to help understand method and its core concept of the invention；Meanwhile for the general skill of this field
Art personnel, according to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion this
Description should not be construed as limiting the invention.
Claims (1)
1. the vacuum brazing method of a kind of porous silicon nitride ceramic and TiAl-base alloy, it is characterised in that the following steps are included:
Step 1: nano silicon nitride silicon particle, Ti powder and AgCu powder 4 ~ 6h of mechanical ball mill are obtained into composite soldering, it is described
The nano silicon nitride silicon particle for being 1.5 ~ 3wt.% containing weight fraction in composite soldering, weight fraction are the Ti of 2 ~ 4wt.%
Powder, surplus are AgCu powder, and the partial size of the nano silicon nitride silicon particle is 20nm ~ 50nm, Ti powder and AgCu eutectic powder
Partial size be 10 μm ~ 50 μm；
Step 2: the composite soldering after ball milling is assembled with pretreated TiAl-base alloy and porous silicon nitride base material,
Guarantee that solder powder thickness carries out polishing surface to be welded with 200#, 400#, 800#SiC sand paper between 50 ~ 200 μm, and in acetone
It is cleaned by ultrasonic 15min ~ 20min in solution, the pretreated TiAl-base alloy refers to that chemical constituent is Ti-46Al-
The TiAl alloy of 2Nb-2Cr, the porous silicon nitride base material refer to that group is divided into 92%Si3N4+6% Y2O3+2%Al2O3Porous pottery
Porcelain, the porosity of porous silicon nitride base material are 45% ~ 60%；
Step 3: the soldered fitting assembled is put into vacuum drying oven, it is heated to 840 DEG C ~ 900 DEG C under vacuum conditions, protects
Warm 5min ~ 30min guarantees that vacuum degree is 1 × 10 in furnace in brazing process-2~ 1×10-4Pa, soldering heating rate are 5
DEG C/min ~ 10 DEG C/min, cooling rate is 1 DEG C/min ~ 5 DEG C/min, wherein applies the axial pressure of 1.5MPa above assembly parts
Power guarantees coming into full contact between solder and base material.
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| CN108516871B (en) * | 2018-04-23 | 2020-12-22 | 哈尔滨工业大学（威海） | Surface metallization method of porous silicon nitride ceramic |
| CN108555476B (en) * | 2018-04-25 | 2020-02-07 | 哈尔滨工业大学 | Composite brazing filler metal for brazing quartz fiber reinforced composite ceramic and Invar alloy and preparation method and brazing method thereof |
| CN108856943B (en) * | 2018-06-27 | 2021-01-01 | 衢州学院 | Brazing method of TiAl and silicon nitride |
| CN111747769B (en) * | 2020-06-30 | 2022-12-09 | 哈尔滨工业大学（威海） | AlMgB 14 -TiB 2 Vacuum brazing method for composite ceramic and TiAl-based alloy |
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| CN102699572A (en) * | 2012-06-21 | 2012-10-03 | 哈尔滨工业大学 | Nano particle reinforced Ag-base composite brazing filler metal and preparation method thereof |
| CN103204694A (en) * | 2013-04-03 | 2013-07-17 | 哈尔滨工业大学 | Method for diffusely connecting TiAl-based alloy and Ti3AlC2 ceramic by adopting Zr/Ni composite intermediate layer |
| CN103240540A (en) * | 2013-05-22 | 2013-08-14 | 哈尔滨工业大学 | Brazing filler metal for connecting SiO2 ceramic and SiO2 ceramic matrix composite materials and preparing method thereof |
| CN104690386A (en) * | 2015-03-25 | 2015-06-10 | 哈尔滨工业大学（威海） | Method for connecting Cf/LAS composite material via AgCuTi brazing filler metal |
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| CN102699572A (en) * | 2012-06-21 | 2012-10-03 | 哈尔滨工业大学 | Nano particle reinforced Ag-base composite brazing filler metal and preparation method thereof |
| CN103204694A (en) * | 2013-04-03 | 2013-07-17 | 哈尔滨工业大学 | Method for diffusely connecting TiAl-based alloy and Ti3AlC2 ceramic by adopting Zr/Ni composite intermediate layer |
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