CN108422126A - A kind of devitrified glass solder and preparation method thereof and connect ferritic method - Google Patents
A kind of devitrified glass solder and preparation method thereof and connect ferritic method Download PDFInfo
- Publication number
- CN108422126A CN108422126A CN201810230594.3A CN201810230594A CN108422126A CN 108422126 A CN108422126 A CN 108422126A CN 201810230594 A CN201810230594 A CN 201810230594A CN 108422126 A CN108422126 A CN 108422126A
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- Prior art keywords
- devitrified glass
- glass solder
- ferritic
- solder
- ferrite
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
- B23K35/3602—Carbonates, basic oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/06—Selection or use of additives to aid disintegrating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C25/00—Control arrangements specially adapted for crushing or disintegrating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Food Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Glass Compositions (AREA)
- Magnetic Heads (AREA)
Abstract
A kind of devitrified glass solder and preparation method thereof and ferritic method is connected, belongs to the technical field of ferrite soldering connection.The invention solves the stability for influencing Microwave Iron Oxide Elements is used for a long time.Solder (20 x) Li2O‑xY2O3‑35Fe2O3‑(20‑y)BaO‑25SiO2‑yCr2O3It is prepared using melting cold quenching method.Connect ferritic method:Yttrium ferrite is pre-processed, devitrified glass solder is adjusted to homogeneous paste with terpinol, then be evenly applied to pretreated yttrium ferrite with silk screen print method and wait for forming part to be welded between joint face, is dried;Then pressure, soldering processing are applied to part to be welded, ferritic connection is completed in furnace cooling.The intensity of the obtained jointing of the present invention is higher (90~100MPa), improves thermal stability, the corrosion resistance of connector, to improve the service life of ferrite device and use complete period stability.
Description
Technical field
The invention belongs to the technical fields of ferrite soldering connection;It is related to a kind of ferrite devitrified glass soldering connection skill
Art;More particularly to a kind of devitrified glass solder and preparation method thereof and connect ferritic method.
Background technology
Ferrite has extensive use, narrow ferromagnetic resonance line as a kind of microwave material in national defence, satellite communication etc.
Wide, low saturation magnetization and low-dielectric loss, make its be widely used in circulator, isolator, modulator, oscillator,
Phase shifter etc..
Since Metal Substrate solder and the electromagnetic performance difference of ferrite base material are big, and chemical compatibility also differs greatly,
The connector of formation certainly will influence the dielectric properties and magnetic property of ferrite functor, therefore Metal Substrate solder is not suitable for carrying out iron
The connection of oxysome.In addition the ferrite joint bending stiffness of adhesive connection is in 15~30MPa, and strength of joint is low, and gluing
The Problem of Failure of agent in extreme circumstances can not also avoid, to affect the stability in use of ferrite functor.
Invention content
The defects of the invention solves ferrite material base solder brazing electromagnetic performance differences greatly, crackle and gluing
The performance for influencing Microwave Iron Oxide Elements is used for a long time in the problems such as existing corrosion resistance, thermal stability, poor permeability resistance
Stability;And it provides a kind of devitrified glass solder and preparation method thereof and connects ferritic method.
In order to solve the above-mentioned technical problem, by percentage to the quality, devitrified glass solder of the present invention is (20-x)
Li2O-xY2O3-35Fe2O3-(20-y)BaO-25SiO2-yCr2O3, wherein x=0 or 20, y=0~5;Above-mentioned devitrified glass pricker
Material carries out in the steps below:
Step 1: weighing raw material Li according to set mass percent2O、Y2O3、Fe2O3、BaO、SiO2、Cr2O3After mix, adopt
It is ground, is dried with wet grinding;
Step 2: then melting, it is poured into water cold quenching and is in granular form, ground using wet grinding, drying is to get to crystallite glass
Glass solder.
It further limits, rotational speed of ball-mill n=200~400r/min described in step 1, Ball-milling Time is 1~3h, Suo Youyuan
Material:Mill ball:Dispersant=1:(1.5~2):(1~1.5), dispersant are absolute ethyl alcohol;The drying temperature is 50 DEG C~65
DEG C, it dries and takes 10~12h.
It further limits, melting temperature described in step 2 is 1100 DEG C~1380 DEG C, and the time is 1h~3h.
Further limit, drum's speed of rotation n=500r/min~600r/min described in step 2, milling time be 10h~
For 24 hours, the particle:Mill ball:Dispersant=1:(2~2.5):(1~1.5), dispersant are absolute ethyl alcohol;The drying temperature
It is 50 DEG C~65 DEG C, dries and take 10~12h.
DSC tests, the glass transition temperature of devitrified glass solder of the invention are carried out to devitrified glass solder powder
(Tg) it is 400~530 DEG C, softening point (Tf) be 550~600 DEG C and recrystallization temperature it is 800~1000 DEG C.
Above-mentioned devitrified glass solder, which connects ferritic method, to be completed by following step:
Step 1 is treated connector yttrium ferrite surface and is pre-processed;
Above-mentioned devitrified glass solder is adjusted to homogeneous paste with terpinol, then is evenly applied to silk screen print method by step 2
Pretreated yttrium ferrite is waited for forming part to be welded between joint face, be dried;
Step 3 and then pressure is applied to part to be welded, soldering processing, furnace cooling completes ferritic connection.
Further limit, the pretreatment described in step 1 is cleaned by ultrasonic with acetone, then use 400#, 800#, 1000#,
1200# silicon carbide papers carry out mechanical grinding step by step, then absolute ethyl alcohol, acetone ultrasound are used to clean successively, scavenging period is 5
~10min.
It further limits, the mass ratio 1 of devitrified glass solder and terpinol in step 2:(4~6).
It further limits, the thickness that solder described in step 2 coats is 20~200 μm.
It further limits, butt-welding fitting applies 0~10KPa pressure in step 3;Brazing process:In air atmosphere, with
5~20 DEG C/min heating speeds are heated to 300~400 DEG C, keep the temperature 20~40min, then proceed to heat speed with 5~10 DEG C/min
Degree is heated to 1100~1200 DEG C, keeps the temperature 30~60min, ensures that glass solder is fully reacted with parent material interface, then with 5~10
DEG C/min is cooled to 800~1000 DEG C, 1~3h is kept the temperature, ensures the abundant crystallization of glass, forms the connector of devitrified glass tissue.
The present invention is used for the devitrified glass solder interconnection technique of ferrite connection, corrosion resistance, thermal stability and impervious
Permeability is preferable;
The present invention uses devitrified glass solder interconnection technique, devitrified glass to have excellent dielectric properties, insulation performance, can
It is applied in microwave regime, is consistent with ferritic application field;
The present invention obtains devitrified glass solder connector, the high mechanical strength of devitrified glass itself by being heat-treated connection procedure
In glass, strength of joint can be improved;
The coefficient of expansion of devitrified glass of the present invention can be adjustable in very large range, can ferrite be connected to one well
It rises, has effectively mitigated method for welding and obtained ferrite structure part because coefficient of thermal expansion mismatch has connector stress.
The devitrified glass solder of the present invention has similar chemical bond, coefficient of thermal expansion and electromagnetic performance and mother with ferrite
Material electromagnetic performance more matches, therefore joint microstructure intensity higher, to realize the integration of ferrite jointing structure, function
Joint improves.
The present invention connects ferrite using devitrified glass solder, and the intensity of obtained jointing is higher (90~100MPa),
Thermal stability, the corrosion resistance for improving connector, to improve the service life of ferrite device and be stablized using the complete period
Property.In addition, the devitrified glass weld seam formed has electromagnetic performance similar with base material so that be formed by ferrite jointing
Magnetic property can reach 80% of base material or more.
Description of the drawings
Fig. 1 is present invention soldering schematic diagram, 1 in figure --- ferrite, 2 --- and solder layer, 3 --- tabletting.
Specific implementation mode
Specific implementation mode one:By percentage to the quality, devitrified glass solder of the present invention is
20Y2O3-35Fe2O3-18BaO-25SiO2-2Cr2O3;Above-mentioned devitrified glass solder carries out in the steps below:
Step 1: weighing raw material Y according to set mass percent2O3、Fe2O3、BaO、SiO2、Cr2O3After mix, use is wet
Mill method is ground, and 10h is dried under the conditions of 65 DEG C;
Wherein, rotational speed of ball-mill n=300r/min described in step 1, Ball-milling Time 2h, all raw materials:Mill ball:Dispersion
Agent=1:2:1, dispersant is absolute ethyl alcohol;
Step 2: then melting 2h at 1200 DEG C, it is poured into water cold quenching and is in granular form, ground using wet grinding, at 65 DEG C
Under the conditions of drying 10h to get to devitrified glass solder;
Wherein, drum's speed of rotation n=500r/min described in step 2, milling time 12h, particle:Mill ball:Dispersant
=1:2:1, dispersant is absolute ethyl alcohol.
DSC tests are carried out to the devitrified glass solder powder that present embodiment obtains, glass transition temperature (Tg) is
480 DEG C, softening point (Tf) be that 550 DEG C and recrystallization temperature are 900 DEG C.
The devitrified glass solder prepared using present embodiment method, which connects ferritic method, to be completed by following step
's:
Step 1 is treated connector yttrium ferrite surface and is pre-processed:Using inner circle cutting machine by the yttrium of a diameter of 6mm
Ferrite Material is cut into the cylinder that thickness is in 2mm, and oil removing is gone in the yttrium ferrite material acetone ultrasonic cleaning after cutting
Dirt then carries out mechanical grinding step by step with 400#, 800#, 1000#, 1200# silicon carbide paper, then uses absolute ethyl alcohol, third successively
Ketone is cleaned by ultrasonic, and 10min is respectively washed, and it is for use that 10h is dried under the conditions of 65 DEG C (please supplement);
Above-mentioned devitrified glass solder terpinol by devitrified glass solder and terpinol mass ratio is 1 by step 2:5 proportionings
It is adjusted to homogeneous paste, then is evenly applied to 3 layers of pretreated yttrium ferrite with silk screen print method and waits for forming between joint face waiting for
Weldment, solder coating layer thickness are controlled at 100 μm or so, and 30min is dried under the conditions of 150 DEG C;
Step 3 and then 10KPa pressure is applied to part to be welded, is handled in resistance furnace brazing, furnace cooling completes iron
The connection of oxysome;
Wherein, step 3 brazing process:In air atmosphere, 300 DEG C are heated to 10 DEG C/min heating speeds, is protected
Warm 40min then proceedes to be heated to 1100 DEG C with 5 DEG C/min heating speeds, keeps the temperature 60min, ensures glass solder and base material circle
Face is fully reacted, and is then cooled to 900 DEG C with 5 DEG C/min, keeps the temperature 2h, ensures the abundant crystallization of glass, forms devitrified glass tissue
Connector.
The shearing strength for the yttrium ferrite connector that devitrified glass made from the present embodiment connects reaches 90~100MPa, than general
Logical adapter glass improves 20% or so, is 4~6 times of cemented joint shearing strength (15~30MPa), and obtained yttrium iron oxygen
The defects of body connector preferable due to matched coefficients of thermal expansion pore-free crackle, connector stability in use is very high.Further, since being formed
Devitrified glass linker components and base material it is close, therefore its electromagnetic performance also reaches 80% or more of base material.
Specific implementation mode two:By percentage to the quality, devitrified glass solder of the present invention is
20Li2O-35Fe2O3-15BaO-25SiO2-5Cr2O3;Above-mentioned devitrified glass solder carries out in the steps below:
Step 1: weighing raw material Li according to set mass percent2O、Fe2O3、BaO、SiO2、Cr2O3(analysis is pure) mixes afterwards
It closes, is ground using wet grinding, 10h is dried under the conditions of 65 DEG C;
Wherein, rotational speed of ball-mill n=300r/min described in step 1, Ball-milling Time 2h, all raw materials:Mill ball:Dispersion
Agent=1:2:1, dispersant is absolute ethyl alcohol;
Step 2: then melting 2h at 1200 DEG C, it is poured into water cold quenching and is in granular form, ground using wet grinding, at 65 DEG C
Under the conditions of drying 10h to get to devitrified glass solder;
Wherein, drum's speed of rotation n=500r/min described in step 2, milling time 12h, particle:Mill ball:Dispersant
=1:2:1, dispersant is absolute ethyl alcohol.
DSC tests are carried out to the devitrified glass solder powder that present embodiment obtains, glass transition temperature (Tg) is
460 DEG C, softening point (Tf) be that 520 DEG C and recrystallization temperature are 800 DEG C.
The devitrified glass solder prepared using present embodiment method, which connects ferritic method, to be completed by following step
's:
Step 1 is treated connector yttrium ferrite surface and is pre-processed:Using inner circle cutting machine by the yttrium of a diameter of 6mm
Ferrite Material is cut into the cylinder that thickness is in 2mm, and oil removing is gone in the yttrium ferrite material acetone ultrasonic cleaning after cutting
Dirt then carries out mechanical grinding step by step with 400#, 800#, 1000#, 1200# silicon carbide paper, then uses absolute ethyl alcohol, third successively
Ketone is cleaned by ultrasonic, and it is 10min to be cleaned by ultrasonic the time, and it is for use that 10min is dried under the conditions of 65 DEG C;
Above-mentioned devitrified glass solder terpinol by devitrified glass solder and terpinol mass ratio is 1 by step 2:5 proportionings
It is adjusted to homogeneous paste, then is evenly applied to 4 layers of pretreated yttrium ferrite with silk screen print method and waits for forming between joint face waiting for
Weldment, solder coating layer thickness are controlled at 120 μm or so, and 30min is dried under the conditions of 150 DEG C;
Step 3 then to part to be welded apply 5KPa pressure, resistance furnace brazing handle, furnace cooling, that is, complete iron oxygen
The connection of body;
Wherein, step 3 brazing process:In air atmosphere, 400 DEG C are heated to 5 DEG C/min heating speeds, heat preservation
30min then proceedes to be heated to 1100 DEG C with 10 DEG C/min heating speeds, keeps the temperature 30min, ensures glass solder and parent material interface
Then fully reaction is cooled to 800 DEG C with 5 DEG C/min, keep the temperature 1h, ensures the abundant crystallization of glass, forms devitrified glass tissue
Connector.
The shearing strength for the yttrium ferrite connector that devitrified glass made from the present embodiment connects reaches 90~100MPa, than general
Logical adapter glass improves 20% or so, is 4~6 times of cemented joint shearing strength (15~30MPa), and obtained yttrium iron oxygen
The defects of body connector preferable due to matched coefficients of thermal expansion pore-free crackle, connector stability in use is very high.Further, since being formed
Devitrified glass linker components and base material it is close, therefore its electromagnetic performance also reaches 80% or more of base material.
Claims (10)
1. a kind of devitrified glass solder, it is characterised in that by percentage to the quality, the devitrified glass solder is (20-x) Li2O-
xY2O3-35Fe2O3-(20-y)BaO-25SiO2-yCr2O3, wherein x=0 or 20, y=0~5.
2. a kind of preparation method of devitrified glass solder as described in claim 1, it is characterised in that the devitrified glass solder is
It carries out in the steps below:
Step 1: weighing raw material Li according to set mass percent2O、Y2O3、Fe2O3、BaO、SiO2、Cr2O3After mix, use is wet
Mill method is ground, drying;
Step 2: then melting, it is poured into water cold quenching and is in granular form, ground using wet grinding, drying is to get to devitrified glass pricker
Material.
3. a kind of preparation method of devitrified glass solder according to claim 2, it is characterised in that ball milling described in step 1
Rotating speed n=200~400r/min, Ball-milling Time are 1~3h, all raw materials:Mill ball:Dispersant=1:(1.5~2):(1~
1.5), dispersant is absolute ethyl alcohol;The drying temperature is 50 DEG C~65 DEG C.
4. a kind of preparation method of devitrified glass solder according to claim 2, it is characterised in that melted described in step 2
Temperature is 1100 DEG C~1380 DEG C, and the time is 1h~3h.
5. a kind of preparation method of devitrified glass solder according to claim 2, it is characterised in that ball milling described in step 2
Machine rotating speed n=500r/min~600r/min, milling time are 10h~for 24 hours, the particle:Mill ball:Dispersant=1:(2~
2.5):(1~1.5), dispersant are absolute ethyl alcohol;The drying temperature is 50 DEG C~65 DEG C.
6. a kind of devitrified glass solder as described in claim 1 connects ferritic method, it is characterised in that the crystallite glass
Glass solder, which connects ferritic method, to be completed by following step:
Step 1 is treated connector yttrium ferrite surface and is pre-processed;
Devitrified glass solder is adjusted to homogeneous paste with terpinol, then is evenly applied to pre-process with silk screen print method by step 2
Yttrium ferrite wait for forming part to be welded between joint face, dry;
Step 3 and then pressure is applied to part to be welded, soldering processing, furnace cooling completes ferritic connection.
7. a kind of devitrified glass solder described in claim 6 connects ferritic method, it is characterised in that pre- described in step 2
Processing is cleaned by ultrasonic with acetone, then carries out mechanical grinding step by step with 400#, 800#, 1000#, 1200# silicon carbide paper, then
It is cleaned successively using absolute ethyl alcohol, acetone ultrasound, scavenging period is 5~10min.
8. a kind of devitrified glass solder described in claim 6 connects ferritic method, it is characterised in that crystallite in step 2
The mass ratio 1 of glass solder and terpinol:(4~6).
9. a kind of devitrified glass solder described in claim 6 connects ferritic method, it is characterised in that solder described in step 2
The thickness of coating is 20~200 μm.
10. a kind of devitrified glass solder described in claim 6 connects ferritic method, it is characterised in that butt welding in step 3
Part applies 0~10KPa pressure;Brazing process:In air atmosphere, 300 are heated to 5~20 DEG C/min heating speeds~
400 DEG C, 20~40min is kept the temperature, then proceedes to be heated to 1100~1200 DEG C with 5~10 DEG C/min heating speeds, heat preservation 30~
Then 60min is cooled to 800~1000 DEG C with 5~10 DEG C/min, keep the temperature 1~3h.
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CN201810230594.3A CN108422126B (en) | 2018-03-20 | 2018-03-20 | Microcrystalline glass brazing filler metal, preparation method thereof and method for connecting ferrite |
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CN201810230594.3A CN108422126B (en) | 2018-03-20 | 2018-03-20 | Microcrystalline glass brazing filler metal, preparation method thereof and method for connecting ferrite |
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CN108422126B CN108422126B (en) | 2020-03-06 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110330356A (en) * | 2019-07-16 | 2019-10-15 | 哈尔滨工业大学 | A kind of silicon carbide ceramics soldering connecting method |
CN110526298A (en) * | 2019-09-30 | 2019-12-03 | 北京无线电测量研究所 | A kind of ferritic method of magnetic field auxiliary glass crystallization method low temperature preparation |
CN112456804A (en) * | 2020-12-11 | 2021-03-09 | 哈尔滨工业大学 | Magnetic nanocrystalline glass solder, preparation method thereof and method for connecting ferrite by applying magnetic nanocrystalline glass solder |
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CN103922597A (en) * | 2014-04-17 | 2014-07-16 | 哈尔滨工业大学 | Preparation method of composite environment-friendly glass brazing filer metal |
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CN110330356A (en) * | 2019-07-16 | 2019-10-15 | 哈尔滨工业大学 | A kind of silicon carbide ceramics soldering connecting method |
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CN110526298A (en) * | 2019-09-30 | 2019-12-03 | 北京无线电测量研究所 | A kind of ferritic method of magnetic field auxiliary glass crystallization method low temperature preparation |
CN110526298B (en) * | 2019-09-30 | 2022-07-15 | 北京无线电测量研究所 | Method for preparing ferrite at low temperature by magnetic field assisted glass crystallization method |
CN112456804A (en) * | 2020-12-11 | 2021-03-09 | 哈尔滨工业大学 | Magnetic nanocrystalline glass solder, preparation method thereof and method for connecting ferrite by applying magnetic nanocrystalline glass solder |
CN112456804B (en) * | 2020-12-11 | 2022-04-05 | 哈尔滨工业大学 | Magnetic nanocrystalline glass solder, preparation method thereof and method for connecting ferrite by applying magnetic nanocrystalline glass solder |
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