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CN103240540B - A kind of for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof - Google Patents

A kind of for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof Download PDF

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Publication number
CN103240540B
CN103240540B CN201310192224.2A CN201310192224A CN103240540B CN 103240540 B CN103240540 B CN 103240540B CN 201310192224 A CN201310192224 A CN 201310192224A CN 103240540 B CN103240540 B CN 103240540B
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sio
solder
pottery
matric composite
ceramic matric
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CN103240540A (en
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张丽霞
张大磊
亓钧雷
石俊秒
冯吉才
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

A kind of for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof, the present invention relates to solder and preparation method thereof.The present invention will solve current SiO 2pottery and SiO 2ceramic matric composite is difficult to by solder wetting, and the problem that strength of joint is not high.A kind of for SiO 2pottery and SiO 2the solder that ceramic matric composite connects is made up of Cu, Sn and Ti; Method: one, take; Two, ball milling; Three, compressing tablet.Solder prepared by the present invention can realize SiO 2pottery and SiO 2ceramic matric composite self and the direct soldering with metal, do not need before weldering to carry out any modification to material surface, and in solder, active element Ti can realize the wetting of ceramic matrix thus realize solder and SiO 2pottery and SiO 2the metallurgical binding of ceramic matric composite.Solder prepared by the present invention is for SiO 2pottery and SiO 2the connection of ceramic matric composite.

Description

A kind of for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof
Technical field
The present invention relates to solder and preparation method thereof.
Background technology
SiO 2pottery and SiO 2ceramic matric composite has excellent heat shock resistance, high-mechanic, and dielectric loss is little, and chemical stability is high, is therefore with a wide range of applications in the field such as Aero-Space, weaponry.Due to the restriction of such material in preparation and manufacturing process, successfully realize it self or be ensure SiO with the soldering of other material 2pottery and SiO 2the key that ceramic matric composite is applied in above-mentioned field.But, in actual soldering, due to SiO 2pottery and SiO 2the inertia on ceramic matric composite surface, is difficult to by general solder wetting.
Publication number is that two patents of CN10314192B and CN101333116B all propose SiO 2pottery and SiO 2the method of attachment of ceramic matric composite and metal, but intermediate layer used in the above-mentioned methods be containing Ag atomic percentage conc be 72 AgCu eutectic solder, therefore welding cost is higher.And the patent that publication number is CN101381207B proposes the method for attachment of a kind of silica fibrage compound material and metal material, the method needs before not only welding to carry out pretreatment, complicated operation to composite material surface, and SiO 2ceramic matric composite be connected with Invari alloy after strength of joint also only have 10MPa, strength of joint is not high.
Summary of the invention
The present invention will solve current SiO 2pottery and SiO 2ceramic matric composite is difficult to by solder wetting, and the problem that strength of joint is not high, and the one provided is for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof.
A kind of for SiO 2pottery and SiO 2the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is according to mass percent by Cu:50 ~ 72%, and Sn:13 ~ 28%, Ti:5 ~ 22% forms.
Prepare above-mentioned for SiO 2pottery and SiO 2the method of the solder that ceramic matric composite connects, specifically prepare according to following steps:
One, according to mass percent Cu:50 ~ 72%, Sn:13 ~ 28%, Ti:5 ~ 22%, takes Cu, Sn and Ti;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4 ~ 5h, obtain mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 0.01 ~ 2mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects.
The invention has the beneficial effects as follows: solder prepared by the present invention can realize SiO 2pottery and SiO 2ceramic matric composite self and the direct soldering with metal, do not need before weldering to carry out any modification to material surface, and in solder, active element Ti can realize the wetting of ceramic matrix thus realize solder and SiO 2pottery and SiO 2the metallurgical binding of ceramic matric composite.Postwelding mother metal performance is hardly by the impact of Thermal Cycle.The SiO obtained 2pottery and TC4 joint room temperature shearing strength can reach 19 ~ 37MPa, reach SiO 238% ~ 74% of pottery strength of parent.The SiO obtained 2ceramic matric composite and Invar alloy-junction room temperature shearing strength can reach 11 ~ 28MPa, reach SiO 2110% ~ 280% of composite strength of parent (parallel direction).The SiO obtained 2ceramic matric composite and TC4 joint room temperature shearing strength can reach 14 ~ 31MPa, reach SiO 2140% ~ 310% of composite strength of parent (parallel direction).
Solder prepared by the present invention is for SiO 2pottery and SiO 2the connection of ceramic matric composite.
Accompanying drawing explanation
Fig. 1 is the solder brazing SiO utilizing embodiment two to prepare 2the scanning electron microscope (SEM) photograph of the soldered fitting of ceramic matric composite and Invar alloy.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: present embodiment one is used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is according to mass percent by Cu:50 ~ 72%, and Sn:13 ~ 28%, Ti:5 ~ 22% forms.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the purity of described raw material is: Cu: >=99.0%, Sn: >=99.0%, Ti: >=99.0%.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one unlike: the particle diameter of Cu, Sn and Ti is 300 orders.Other is identical with detailed description of the invention one.
Detailed description of the invention four: present embodiment and detailed description of the invention one unlike: be a kind ofly used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:68%, Sn:25%, Ti:7% according to mass percent.Other is identical with detailed description of the invention one.
Detailed description of the invention five: present embodiment and detailed description of the invention one unlike: be a kind ofly used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:65%, Sn:25%, Ti:10% according to mass percent.Other is identical with detailed description of the invention one.
Detailed description of the invention six: present embodiment and detailed description of the invention one unlike: be a kind ofly used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:70%, Sn:17%, Ti:13% according to mass percent.Other is identical with detailed description of the invention one.
Detailed description of the invention seven: the one of preparation described in detailed description of the invention one is used for SiO 2pottery and SiO 2the method of the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the preparation method of the solder that ceramic matric composite connects, specifically prepares according to following steps:
One, according to mass percent Cu:50 ~ 72%, Sn:13 ~ 28%, Ti:5 ~ 22%, takes Cu, Sn and Ti, and wherein the particle diameter of Cu, Sn and Ti is 300 orders;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4 ~ 5h, obtain mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 0.01 ~ 2mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects.
Detailed description of the invention eight: present embodiment and detailed description of the invention seven unlike: control in step 2 that rotational speed of ball-mill is 280 ~ 320r/min, ball material mass ratio is 12 ~ 16: 1.Other is identical with detailed description of the invention seven.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The present embodiment one is used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:68%, Sn:25%, Ti:7% according to mass percent.
The purity of described raw material is: Cu: >=99.0%, Sn: >=99.0%, Ti: >=99.0%.
One described in the present embodiment is used for SiO 2pottery and SiO 2the preparation method of the solder that ceramic matric composite connects, carries out according to following steps:
One, according to mass percent Cu:68%, Sn:25%, Ti:7%, take Cu, Sn and Ti, and wherein the particle diameter of Cu, Sn and Ti is 300 orders;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4h, and control rotational speed of ball-mill is 300r/min, ball material mass ratio is 15: 1, obtains mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 1mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects.
The solder brazing SiO utilizing the present embodiment to prepare 2pottery and TC4: by SiO 2pottery is clean with the welded removing surface of TC4; Again by SiO 2pottery and TC4 put into acetone, carry out Ultrasonic Cleaning 30min; By the SiO after cleaning 2pottery and TC4 natural air drying after, be SiO in accordance with the order from top to bottom 2pottery/solder/TC4 assembles, and at SiO 2the pressure that ceramic surface applies 0.1MPa is fixed; Put into vacuum furnace again, controlling vacuum is 1 × 10 -3pa, programming rate are 15 DEG C/min, are warming up to 860 DEG C, and insulation 15min, then controlling cooling rate is 25 DEG C/min, is cooled to 400 DEG C, then cools to room temperature with the furnace, complete SiO 2the soldering of pottery and TC4.
After tested, SiO 2pottery reaches 37MPa with the soldered fitting room temperature shearing strength of TC4.
Embodiment two:
The present embodiment one is used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:65%, Sn:25%, Ti:10% according to mass percent.
The purity of described raw material is: Cu: >=99.0%, Sn: >=99.0%, Ti: >=99.0%.
One described in the present embodiment is used for SiO 2pottery and SiO 2the preparation method of the solder that ceramic matric composite connects, carries out according to following steps:
One, according to mass percent Cu:65%, Sn:25%, Ti:10%, take Cu, Sn and Ti, and wherein the particle diameter of Cu, Sn and Ti is 300 orders;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4h, and control rotational speed of ball-mill is 300r/min, ball material mass ratio is 15: 1, obtains mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 1mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects.
The solder brazing SiO utilizing the present embodiment to prepare 2ceramic matric composite and Invar alloy: by SiO 2the welded removing surface of ceramic matric composite and Invar alloy is clean; Again by SiO 2acetone put into by ceramic matric composite and Invar alloy, carries out Ultrasonic Cleaning 30min; By the SiO after cleaning 2after ceramic matric composite and Invar alloy natural air drying, be SiO in accordance with the order from top to bottom 2ceramic matric composite/solder/Invar alloy assembles, and at SiO 2the pressure that ceramic matric composite surface applies 0.1MPa is fixed; Put into vacuum furnace again, controlling vacuum is 1 × 10 -3pa, programming rate are 15 DEG C/min, are warming up to 880 DEG C, and insulation 15min, then controlling cooling rate is 25 DEG C/min, is cooled to 400 DEG C, then cools to room temperature with the furnace, complete SiO 2the soldering of ceramic matric composite and Invar alloy.
The solder brazing SiO utilizing the present embodiment to prepare 2as shown in Figure 1, as can be seen from the figure, soldering interface is complete for the scanning electron microscope (SEM) photograph of the soldered fitting of ceramic matric composite and Invar alloy, generates without defects such as cavity, crackles.In brazing process, solder and both sides mother metal all react, multiple phase is defined in interface, be distributed in joint regional, according to the tissue characteristic in each region, four representative regions are divided into, i.e. nearly irregular particle Dispersed precipitate district, composite side and narrow strip interfacial reaction district, composite side in nearly solid solution tagma, alloy side, brazed seam in Invar alloy side Dark grey chain form interfacial reaction district, brazed seam by left-to-right.
After tested, SiO 2the soldered fitting room temperature shearing strength of ceramic matric composite and Invar alloy reaches 28MPa.
Embodiment three:
The present embodiment one is used for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:70%, Sn:17%, Ti:13% according to mass percent.
The purity of described raw material is: Cu: >=99.0%, Sn: >=99.0%, Ti: >=99.0%.
One described in the present embodiment is used for SiO 2pottery and SiO 2the preparation method of the solder that ceramic matric composite connects, carries out according to following steps:
One, according to mass percent Cu:70%, Sn:17%, Ti:13%, take Cu, Sn and Ti, and wherein the particle diameter of Cu, Sn and Ti is 300 orders;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4h, and control rotational speed of ball-mill is 300r/min, ball material mass ratio is 15: 1, obtains mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 0.01 ~ 2mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects.
The solder brazing SiO utilizing the present embodiment to prepare 2ceramic matric composite and TC4: by SiO 2the welded removing surface of ceramic matric composite and TC4 is clean; Again by SiO 2ceramic matric composite and TC4 put into acetone, carry out Ultrasonic Cleaning 30min; By the SiO after cleaning 2after ceramic matric composite and TC4 natural air drying, be SiO in accordance with the order from top to bottom 2ceramic matric composite/solder/TC4 assembles, and at SiO 2the pressure that ceramic matric composite surface applies 0.1MPa is fixed; Put into vacuum furnace again, controlling vacuum is 1 × 10 -3pa, programming rate are 15 DEG C/min, are warming up to 880 DEG C, and insulation 15min, then controlling cooling rate is 25 DEG C/min, is cooled to 400 DEG C, then cools to room temperature with the furnace, complete SiO 2the soldering of ceramic matric composite and TC4.
After tested, SiO 2the soldered fitting room temperature shearing strength of ceramic matric composite and TC4 reaches 31MPa.
Solder prepared by the present invention can realize SiO 2pottery and SiO 2ceramic matric composite self and the direct soldering with metal, do not need before weldering to carry out any modification to material surface, and in solder, active element Ti can realize the wetting of ceramic matrix thus realize solder and SiO 2pottery and SiO 2the metallurgical binding of ceramic matric composite.Postwelding mother metal performance is hardly by the impact of Thermal Cycle.The SiO obtained 2pottery and TC4 joint room temperature shearing strength can reach 19 ~ 37MPa, reach SiO 238% ~ 74% of pottery strength of parent.The SiO obtained 2ceramic matric composite and Invar alloy-junction room temperature shearing strength can reach 11 ~ 28MPa, reach SiO 2110% ~ 280% of composite strength of parent (parallel direction).The SiO obtained 2ceramic matric composite and TC4 joint room temperature shearing strength can reach 14 ~ 31MPa, reach SiO 2140% ~ 310% of composite strength of parent (parallel direction).

Claims (5)

1. one kind for SiO 2pottery and SiO 2the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the raw material of solder that ceramic matric composite connects according to mass percent by Cu:50 ~ 72%, Sn:13 ~ 28%, Ti:5 ~ 22% forms; The purity of raw material is: Cu:>=99.0%, Sn:>=99.0%, Ti:>=99.0%; The particle diameter of Cu, Sn and Ti is 300 orders.
2. one according to claim 1 is used for SiO 2pottery and SiO 2the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:68%, Sn:25%, Ti:7% according to mass percent.
3. one according to claim 1 is used for SiO 2pottery and SiO 2the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:65%, Sn:25%, Ti:10% according to mass percent.
4. one according to claim 1 is used for SiO 2pottery and SiO 2the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the raw material of the solder that ceramic matric composite connects is made up of Cu:70%, Sn:17%, Ti:13% according to mass percent.
5. prepare one according to claim 1 and be used for SiO 2pottery and SiO 2the method of the solder that ceramic matric composite connects, is characterized in that a kind of for SiO 2pottery and SiO 2the preparation method of the solder that ceramic matric composite connects, specifically prepares according to following steps:
One, according to mass percent Cu:50 ~ 72%, Sn:13 ~ 28%, Ti:5 ~ 22%, takes Cu, Sn and Ti, and wherein the particle diameter of Cu, Sn and Ti is 300 orders;
Two, under argon shield, room temperature condition, Cu, Sn and Ti of step one being taken put into ball grinder ball milling 4 ~ 5h, obtain mixed-powder;
Three, the mixed-powder adopting tablet press machine step 2 to be obtained is pressed into the paillon foil that thickness is 0.01 ~ 2mm, then cleans paillon foil with acetone, then air-dry, obtains for SiO 2pottery and SiO 2the solder that ceramic matric composite connects;
Control in step 2 that rotational speed of ball-mill is 280 ~ 320r/min, ball material mass ratio is 12 ~ 16: 1.
CN201310192224.2A 2013-05-22 2013-05-22 A kind of for SiO 2pottery and SiO 2solder that ceramic matric composite connects and preparation method thereof Active CN103240540B (en)

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CN106007773B (en) * 2016-05-24 2019-06-07 哈尔滨工业大学（威海） A kind of vacuum brazing method of porous silicon nitride ceramic and TiAl-base alloy
CN106001980A (en) * 2016-06-15 2016-10-12 中国科学院电工研究所 High-temperature lead-free soldering lug for encapsulating power electronic module and preparation method thereof
CN111299905B (en) * 2020-03-20 2022-04-15 安徽工业大学 Composite brazing filler metal containing WC and ZrC simultaneously, preparation method thereof and brazing method

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JPS5471748A (en) * 1977-11-21 1979-06-08 Seiko Epson Corp Brazing filler metal
JPS6120696A (en) * 1984-07-06 1986-01-29 Tanaka Kikinzoku Kogyo Kk Palladium brazing filler metal
CN101987402A (en) * 2010-11-30 2011-03-23 哈尔滨工业大学 Cu-Sn-Ti solder and method for brazing Ti2AlC ceramics and Cu with same
CN102689109A (en) * 2012-06-21 2012-09-26 哈尔滨工业大学 High-entropy brazing filler metal for brazing non-oxide ceramics and non-oxide ceramic composite material and preparation method of brazing filler metal
CN102699571A (en) * 2012-06-21 2012-10-03 哈尔滨工业大学 Moderate-temperature brazing filler metal for graphite-base composite material connection and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5471748A (en) * 1977-11-21 1979-06-08 Seiko Epson Corp Brazing filler metal
JPS6120696A (en) * 1984-07-06 1986-01-29 Tanaka Kikinzoku Kogyo Kk Palladium brazing filler metal
CN101987402A (en) * 2010-11-30 2011-03-23 哈尔滨工业大学 Cu-Sn-Ti solder and method for brazing Ti2AlC ceramics and Cu with same
CN102689109A (en) * 2012-06-21 2012-09-26 哈尔滨工业大学 High-entropy brazing filler metal for brazing non-oxide ceramics and non-oxide ceramic composite material and preparation method of brazing filler metal
CN102699571A (en) * 2012-06-21 2012-10-03 哈尔滨工业大学 Moderate-temperature brazing filler metal for graphite-base composite material connection and preparation method thereof

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