CN108422126B - Microcrystalline glass brazing filler metal, preparation method thereof and method for connecting ferrite - Google Patents
Microcrystalline glass brazing filler metal, preparation method thereof and method for connecting ferrite Download PDFInfo
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- CN108422126B CN108422126B CN201810230594.3A CN201810230594A CN108422126B CN 108422126 B CN108422126 B CN 108422126B CN 201810230594 A CN201810230594 A CN 201810230594A CN 108422126 B CN108422126 B CN 108422126B
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- ferrite
- microcrystalline glass
- glass solder
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- filler metal
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- 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
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- 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
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- 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)
- Food Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
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Abstract
A microcrystalline glass brazing filler metal, a preparation method thereof and a method for connecting ferrite belong to the technical field of ferrite brazing connection. The invention aims to solve the problem that the long-term use affects the performance stability of a microwave ferrite device. Solder (20-x) Li2O‑xY2O3‑35Fe2O3‑(20‑y)BaO‑25SiO2‑yCr2O3The alloy is prepared by a melting-cold quenching method. The method for connecting the ferrite comprises the following steps: pretreating yttrium ferrite, mixing microcrystalline glass solder with terpineol to obtain uniform paste, uniformly coating the paste between surfaces to be connected of pretreated yttrium ferrite by a screen printing method to form a part to be welded, and drying; and then applying pressure to the parts to be welded, carrying out brazing treatment, and cooling along with a furnace to complete the connection of the ferrite. The strength of the connection joint obtained by the method is high (90-100 MPa), and the thermal stability and corrosion resistance of the joint are improved, so that the service life of the ferrite device is prolonged, and the stability of the whole service cycle is improved.
Description
Technical Field
The invention belongs to the technical field of ferrite soldering connection; relates to a ferrite microcrystalline glass brazing connection technology; in particular to a microcrystalline glass solder, a preparation method thereof and a method for connecting ferrite.
Background
Ferrite as a microwave material has wide application in national defense, satellite communication and the like, and the narrow ferromagnetic resonance line width, low saturation magnetization and low dielectric loss of the ferrite cause the ferrite to be widely applied to circulators, isolators, modulators, oscillators, phase shifters and the like.
Because the difference of the electromagnetic property of the metal-based brazing filler metal and the ferrite base metal is large, and the chemical compatibility is also large, the formed joint has a certain influence on the dielectric property and the magnetic property of the ferrite functional part, so that the metal-based brazing filler metal is not suitable for connecting the ferrite. In addition, the shearing strength of the ferrite joint connected by the adhesive is 15-30 MPa, the joint strength is low, and the failure problem of the adhesive in an extreme environment cannot be avoided, so that the use stability of the ferrite functional part is influenced.
Disclosure of Invention
The invention aims to solve the defects of large difference, cracks and the like of the electromagnetic performance of the soldering of the ferrite metal-based solder, and the problems of poor corrosion resistance, thermal stability, permeability resistance and the like of an adhesive method, and the performance stability of a microwave ferrite device is influenced after long-term use; and provides a microcrystalline glass solder, a preparation method thereof and a method for connecting ferrite.
In order to solve the technical problem, the microcrystalline glass solder is (20-x) Li in percentage by mass2O-xY2O3-35Fe2O3-(20-y)BaO-25SiO2-yCr2O3Wherein x is 0 or 20, and y is 0-5; the microcrystalline glass solder is prepared by the following steps:
step one, weighing raw material Li according to given mass percentage2O、Y2O3、Fe2O3、BaO、SiO2、Cr2O3Then mixing, grinding by a wet grinding method and drying;
and step two, melting, pouring into water, performing cold quenching to obtain particles, grinding by a wet grinding method, and drying to obtain the microcrystalline glass solder.
Further limiting, in the first step, the ball milling rotation speed n is 200-400 r/min, the ball milling time is 1-3 h, all raw materials are grinding balls, dispersing agents are 1, (1.5-2) and (1-1.5), and the dispersing agents are absolute ethyl alcohol; the drying temperature is 50-65 ℃, and the drying time is 10-12 h.
Further limiting, the melting temperature in the second step is 1100-1380 ℃, and the time is 1-3 h.
Further, in the second step, the rotation speed n of the ball mill is 500r/min to 600r/min, the grinding time is 10h to 24h, and the particle: grinding balls: the dispersant is 1 (2-2.5) and 1-1.5, and the dispersant is absolute ethyl alcohol; the drying temperature is 50-65 ℃, and the drying time is 10-12 h.
DSC test is carried out on the microcrystalline glass solder powder, and the glass transition temperature (T) of the microcrystalline glass solder isg) A softening point (T) of 400 to 530 DEG Cf) 550-600 ℃ and 800-1000 ℃ of crystallization temperature.
The method for connecting the microcrystalline glass brazing filler metal with the ferrite is completed by the following steps:
and 3, applying pressure to the workpiece to be welded, performing brazing treatment, and cooling along with a furnace to complete the connection of the ferrite.
Further limiting, the pretreatment in the step 1 is ultrasonic cleaning by acetone, then mechanical polishing is carried out step by using 400#, 800#, 1000#, and 1200# water-mill sandpaper, and then absolute ethyl alcohol and acetone are adopted for ultrasonic cleaning in sequence, wherein the cleaning time is 5-10 min.
Further limiting, the mass ratio of the microcrystalline glass solder to the terpineol in the step 2 is 1 (4-6).
Further limiting, the thickness of the brazing filler metal coating in the step 2 is 20-200 mu m.
Further limiting, applying pressure of 0-10 KPa to the welding piece in the step 3; the brazing treatment process comprises the following steps: heating to 300-400 ℃ at a heating speed of 5-20 ℃/min in an air atmosphere, preserving heat for 20-40 min, then continuously heating to 1100-1200 ℃ at a heating speed of 5-10 ℃/min, preserving heat for 30-60 min, ensuring that the glass brazing filler metal and a base metal interface fully react, then cooling to 800-1000 ℃ at 5-10 ℃/min, preserving heat for 1-3 h, ensuring that the glass is fully crystallized, and forming a microcrystalline glass tissue joint.
The microcrystalline glass solder connection technology for ferrite connection has good corrosion resistance, thermal stability and permeability resistance;
the invention adopts the microcrystalline glass solder connection technology, and the microcrystalline glass has excellent dielectric property and insulating property, can be applied in the microwave field and conforms to the application field of ferrite;
the microcrystalline glass brazing filler metal joint is obtained through a heat treatment connection process, the mechanical strength of the microcrystalline glass is higher than that of glass, and the joint strength can be improved;
the expansion coefficient of the microcrystalline glass can be adjusted in a large range, and the ferrite can be well connected together, so that the problem of joint stress caused by mismatching of the thermal expansion coefficients of the ferrite structural member obtained by the brazing method is effectively alleviated.
The microcrystalline glass brazing filler metal has similar chemical bonds with ferrite, and the thermal expansion coefficient and the electromagnetic property are more matched with those of a base material, so that the joint structure strength is higher, and the joint structure and the function of the ferrite are integrally and jointly improved.
According to the invention, the microcrystalline glass brazing filler metal is used for connecting the ferrite, the strength of the obtained connecting joint is higher (90-100 MPa), and the thermal stability and the corrosion resistance of the joint are improved, so that the service life of a ferrite device is prolonged and the stability of the whole service cycle is improved. In addition, the formed microcrystalline glass welding seam has electromagnetic performance similar to that of the base material, so that the magnetic performance of the formed ferrite connecting joint can reach more than 80% of that of the base material.
Drawings
FIG. 1 is a schematic view of the brazing process of the present invention, in which 1-ferrite, 2-solder layer, and 3-pressed sheet.
Detailed Description
The first embodiment is as follows: the microcrystalline glass solder is 20Y in percentage by mass2O3-35Fe2O3-18BaO-25SiO2-2Cr2O3(ii) a The microcrystalline glass solder is prepared by the following steps:
step one, weighing raw material Y according to set mass percentage2O3、Fe2O3、BaO、SiO2、Cr2O3Post-mixing, extractingGrinding by wet grinding method, and oven drying at 65 deg.C for 10 h;
wherein, in the step one, the ball milling rotation speed n is 300r/min, the ball milling time is 2h, all raw materials comprise grinding balls and a dispersing agent which is 1:2:1, and the dispersing agent is absolute ethyl alcohol;
step two, melting for 2h at 1200 ℃, pouring into water for cold quenching to form particles, grinding by a wet grinding method, and drying for 10h at 65 ℃ to obtain the microcrystalline glass solder;
wherein, the rotation speed n of the ball mill in the second step is 500r/min, the grinding time is 12h, and the particle: grinding balls: the dispersant is 1:2:1, and the dispersant is absolute ethyl alcohol.
The microcrystalline glass solder powder obtained in this embodiment was subjected to DSC measurement, and the glass transition temperature (Tg) was 480 ℃, the softening point (Tf) was 550 ℃, and the crystallization temperature was 900 ℃.
The method for connecting the microcrystalline glass solder with the ferrite, which is prepared by the method of the embodiment, comprises the following steps:
wherein, the brazing treatment process in the step 3: heating to 300 ℃ at a heating speed of 10 ℃/min in air atmosphere, preserving heat for 40min, then continuing heating to 1100 ℃ at a heating speed of 5 ℃/min, preserving heat for 60min, ensuring that the glass solder and the base material interface fully react, then cooling to 900 ℃ at 5 ℃/min, preserving heat for 2h, ensuring that the glass is fully crystallized, and forming a microcrystalline glass tissue joint.
The shear strength of the yttrium ferrite joint connected with the microcrystalline glass prepared by the embodiment reaches 90-100 MPa, is improved by about 20% compared with that of a common glass joint, is 4-6 times of that of an adhesive joint (15-30 MPa), and the obtained yttrium ferrite joint has no defects such as pore cracks and the like due to good matching of thermal expansion coefficients and is high in use stability. In addition, the formed microcrystalline glass joint has a composition close to that of the base material, so that the electromagnetic performance of the formed microcrystalline glass joint is 80% or more of that of the base material.
The second embodiment is as follows: the microcrystalline glass solder is 20Li in percentage by mass2O-35Fe2O3-15BaO-25SiO2-5Cr2O3(ii) a The microcrystalline glass solder is prepared by the following steps:
step one, weighing raw material Li according to given mass percentage2O、Fe2O3、BaO、SiO2、Cr2O3Then mixing, grinding by a wet grinding method, and drying for 10 hours at the temperature of 65 ℃;
wherein, in the step one, the ball milling rotation speed n is 300r/min, the ball milling time is 2h, all raw materials comprise grinding balls and a dispersing agent which is 1:2:1, and the dispersing agent is absolute ethyl alcohol;
step two, melting for 2h at 1200 ℃, pouring into water for cold quenching to form particles, grinding by a wet grinding method, and drying for 10h at 65 ℃ to obtain the microcrystalline glass solder;
wherein, the rotation speed n of the ball mill in the second step is 500r/min, the grinding time is 12h, and the particle: grinding balls: the dispersant is 1:2:1, and the dispersant is absolute ethyl alcohol.
DSC measurement was performed on the microcrystalline glass solder powder obtained in this embodiment, and the glass transition temperature (Tg) was 460 ℃, the softening point (Tf) was 520 ℃, and the crystallization temperature was 800 ℃.
The method for connecting the microcrystalline glass solder with the ferrite, which is prepared by the method of the embodiment, comprises the following steps:
wherein, the brazing treatment process in the step 3: heating to 400 ℃ at a heating speed of 5 ℃/min in air atmosphere, preserving heat for 30min, then continuing heating to 1100 ℃ at a heating speed of 10 ℃/min, preserving heat for 30min, ensuring that the glass solder and the base material interface fully react, then cooling to 800 ℃ at 5 ℃/min, preserving heat for 1h, ensuring that the glass is fully crystallized, and forming a microcrystalline glass tissue joint.
The shear strength of the yttrium ferrite joint connected with the microcrystalline glass prepared by the embodiment reaches 90-100 MPa, is improved by about 20% compared with that of a common glass joint, is 4-6 times of that of an adhesive joint (15-30 MPa), and the obtained yttrium ferrite joint has no defects such as pore cracks and the like due to good matching of thermal expansion coefficients and is high in use stability. In addition, the formed microcrystalline glass joint has a composition close to that of the base material, so that the electromagnetic performance of the formed microcrystalline glass joint is 80% or more of that of the base material.
Claims (10)
1. The microcrystalline glass brazing filler metal is characterized by comprising (20-x) Li in percentage by mass2O-xY2O3-35Fe2O3-(20-y)BaO-25SiO2-yCr2O3Wherein x is 0 or 20, and y is 0-5.
2. The preparation method of the microcrystalline glass solder as claimed in claim 1, wherein the microcrystalline glass solder is prepared by the following steps:
step one, weighing raw material Li according to given mass percentage2O、Y2O3、Fe2O3、BaO、SiO2、Cr2O3Then mixing, grinding by a wet grinding method and drying;
and step two, melting, pouring into water, performing cold quenching to obtain particles, grinding by a wet grinding method, and drying to obtain the microcrystalline glass solder.
3. The preparation method of the microcrystalline glass solder according to claim 2, wherein the wet grinding in the first step is grinding by a ball mill, wherein the rotation speed n of the ball mill is 200-400 r/min, the ball milling time is 1-3 h, and all raw materials comprise grinding balls and a dispersing agent, wherein the dispersing agent comprises (1.5-2) - (1-1.5), and the dispersing agent is absolute ethyl alcohol; the drying temperature is 50-65 ℃.
4. The method for preparing the microcrystalline glass solder according to claim 2, wherein the melting temperature in the second step is 1100-1380 ℃ and the time is 1-3 h.
5. A method for preparing a microcrystalline glass solder according to claim 2, wherein the wet milling in step two is performed by using a ball mill, the rotation speed n of the ball mill is 500r/min to 600r/min, the milling time is 10h to 24h, the particle: grinding balls: the dispersant is 1 (2-2.5) and 1-1.5, and the dispersant is absolute ethyl alcohol; the drying temperature is 50-65 ℃.
6. The method for connecting the microcrystalline glass solder with the ferrite as claimed in claim 1, wherein the method for connecting the microcrystalline glass solder with the ferrite is completed by the following steps:
step 1, pretreating the surface of yttrium ferrite of a to-be-connected piece;
step 2, the microcrystalline glass solder is mixed to be uniform paste by terpineol, then is uniformly coated among the surfaces to be connected of the pretreated yttrium ferrite by a screen printing method to form a part to be welded, and is dried;
and 3, applying pressure to the workpiece to be welded, performing brazing treatment, and cooling along with a furnace to complete the connection of the ferrite.
7. The method for connecting the microcrystalline glass solder with the ferrite as claimed in claim 6, wherein the pretreatment in step 2 is ultrasonic cleaning with acetone, then mechanical polishing with 400#, 800#, 1000#, 1200# water-milled sand paper step by step, and then ultrasonic cleaning with absolute ethyl alcohol and acetone sequentially, wherein the cleaning time is 5-10 min.
8. The method for connecting the ferrite through the microcrystalline glass solder as claimed in claim 6, wherein the mass ratio of the microcrystalline glass solder to the terpineol in the second step is 1 (4-6).
9. A method for connecting ferrite by using microcrystalline glass and brazing filler metal as claimed in claim 6, wherein the thickness of the brazing filler metal coating in the step 2 is 20-200 μm.
10. The method for connecting the ferrite through the microcrystalline glass brazing filler metal as claimed in claim 6, wherein 0-10 KPa pressure is applied to the welded part in the step 3; the brazing treatment process comprises the following steps: heating to 300-400 ℃ at a heating speed of 5-20 ℃/min in an air atmosphere, preserving heat for 20-40 min, then continuously heating to 1100-1200 ℃ at a heating speed of 5-10 ℃/min, preserving heat for 30-60 min, then cooling to 800-1000 ℃ at 5-10 ℃/min, and preserving heat for 1-3 h.
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CN110330356B (en) * | 2019-07-16 | 2022-03-01 | 哈尔滨工业大学 | Silicon carbide ceramic brazing connection method |
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 |
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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CN103922597B (en) * | 2014-04-17 | 2016-01-20 | 哈尔滨工业大学 | The preparation method of compound green low-melting-point glass solder soldering paste |
CN105149890A (en) * | 2015-10-19 | 2015-12-16 | 哈尔滨工业大学 | Method for Li-series ferrite connection through compound glass solder |
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