CN111056744B - Method for preparing low-temperature glass solder sheet by sintering and application thereof - Google Patents

Method for preparing low-temperature glass solder sheet by sintering and application thereof Download PDF

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Publication number
CN111056744B
CN111056744B CN201911400560.5A CN201911400560A CN111056744B CN 111056744 B CN111056744 B CN 111056744B CN 201911400560 A CN201911400560 A CN 201911400560A CN 111056744 B CN111056744 B CN 111056744B
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temperature
low
glass solder
sintering
solder sheet
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CN111056744A (en
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王振江
牛济泰
楚军龙
高增
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Henan Jingtai Aerospace High Novel Materials Technology Co ltd
Henan University of Technology
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Henan Jingtai Aerospace High Novel Materials Technology Co ltd
Henan University of Technology
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Priority to JP2020080326A priority patent/JP7076739B2/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a method for preparing a low-temperature glass solder sheet by sintering and application thereof, and relates to a method for preparing a low-temperature glass solder sheet by sintering and application thereof. The invention aims to solve the problems that the existing paste glass material is connected with an aluminum-based composite material, so that many air holes are generated, impurities are introduced, the strength is difficult to ensure, and the glass powder granulation process is complicated. The sintering method comprises the following steps: and designing a mold according to the shape of a test piece to be welded, filling low-temperature glass powder into a mold cavity, and sintering under the action of a constant-pressure block at the temperature 20-40 ℃ higher than the softening point of the low-temperature glass powder to obtain the glass solder sheet. The application method comprises the following steps: and assembling a glass solder sheet in the middle of the test piece to be welded, placing the glass solder sheet in a special welding tool, then transferring the glass solder sheet into an atmosphere sintering furnace for sintering, and forming a low-temperature glass solder layer in the middle after sintering is finished to obtain the welded test piece. The invention is used for the connection between the high volume fraction aluminum-based composite materials or the connection between the high volume fraction aluminum-based composite materials and glass.

Description

Method for preparing low-temperature glass solder sheet by sintering and application thereof
Technical Field
The invention relates to a method for preparing a low-temperature glass solder sheet by sintering and application thereof.
Background
The aluminum-based composite material is one of the hottest composite materials researched in recent years, in particular to a particle reinforced aluminum-based composite material (comprising high-silicon aluminum and silicon aluminum carbon), the preparation process of the material is relatively mature at present, the aluminum-based composite material has the advantages of low expansion coefficient, high thermal conductivity, light weight and the like, and is widely applied to the fields of electronic packaging, aerospace, military equipment, automobiles, sports goods and the like, but the reinforced phase silicon carbide or silicon particles belong to a non-metal phase, so that great difficulty is brought to welding of the reinforced phase silicon carbide or silicon particles. The scholars at home and abroad carry out series of researches on the fusion welding, the brazing and the like, the problem of interface reaction exists at all times after the fusion welding, the brazing is generally carried out in a vacuum furnace, even the surface of the aluminum matrix composite material needs to be alloyed for welding, and the welding process is complex. Some adopt paste low temperature glass brazing filler metal to weld it, but the defect of gas pocket, the introduction and intensity of impurity are difficult to guarantee, if adopt the granulation process of glass powder, make the welding process complicated, introduce impurity too inevitable. The use of low temperature glass solder sheets solves the above problems.
Disclosure of Invention
The invention provides a method for preparing a low-temperature glass solder sheet by sintering and application thereof, aiming at solving the problems that the existing paste glass material is connected with an aluminum-based composite material, the air holes are more, the impurities are introduced, the strength is difficult to ensure, and the glass powder granulation process is complicated.
The method for preparing the low-temperature glass solder sheet by sintering specifically comprises the following steps:
and designing a mold according to the shape of a test piece to be welded, wherein the mold is made of stainless steel, filling low-temperature glass powder into a mold cavity, and sintering the glass powder at a temperature 20-40 ℃ higher than the softening point of the low-temperature glass powder under the action of a constant-pressure block to obtain the glass solder sheet.
The glass solder sheet is used for connecting high volume fraction aluminum matrix composite materials or connecting the high volume fraction aluminum matrix composite materials with glass; the method comprises the following steps:
assembling a glass solder sheet in the middle of a test piece to be welded, placing the glass solder sheet in a special welding tool, transferring the glass solder sheet to an atmosphere sintering furnace for sintering, wherein in the sintering process, the pressure is kept at 5-10 KPa, and after sintering is finished, a low-temperature glass solder layer is formed in the middle to obtain a welded test piece; the thickness of the low-temperature glass solder layer is less than 100 mu m;
the volume fraction of the reinforcing phase in the high volume fraction aluminum-based composite material is 55-70%.
The invention has the beneficial effects that:
the invention adopts the original low-temperature glass solder sheet sintering technology to weld the aluminum-based composite material, and adopts the low-temperature glass powder with corresponding softening temperature and linear expansion coefficient and process parameters according to different connected materials (high-silicon aluminum and aluminum-based composite materials) and utilizes a special die and a tool to realize the connection of the aluminum-based composite material or the aluminum-based composite material and the glass. The process has the advantages that the defects of uneven coating, impurity introduction, more air holes, poor strength guarantee and the like of the conventional paste brazing filler metal can be avoided, the glass powder does not need to be granulated, simplicity and high efficiency can be realized, the low-temperature glass solder brazing seam which is compact, has no air holes and high strength can be obtained, and the air tightness of a sealing part can meet the requirements of relevant standards.
Drawings
FIG. 1 is a schematic view of a mold;
FIG. 2 is a schematic representation of a glass solder sheet obtained in accordance with example one;
FIG. 3 is an assembly view of the welding tool;
FIG. 4 is a metallographic photograph of a high-silicon aluminum joint welded using low-temperature glass according to example one;
FIG. 5 is a scanning electron microscope image of a low temperature glass welded high silicon aluminum interconnect in accordance with one embodiment; wherein, the area A is low-temperature glass, and the area B is high-silicon aluminum alloy;
FIG. 6 is a shear fracture diagram of a high silicon aluminum joint welded using low temperature glass in accordance with an example.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the method for preparing the low-temperature glass solder sheet by sintering is specifically carried out according to the following steps:
and designing a mold according to the shape of a test piece to be welded, wherein the mold is made of stainless steel, filling low-temperature glass powder into a mold cavity, and sintering the glass powder at a temperature 20-40 ℃ higher than the softening point of the low-temperature glass powder under the action of a constant-pressure block to obtain the glass solder sheet.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the die consists of a constant pressure block 1, a fixed plate 2, a positioning pin 3, a male die 4 and a female die component 5; the molded surface of the male die 4 corresponds to the molded surface of the female die component 5 and forms a die cavity; the fixing plate 2 is transversely arranged on the upper end face of the male die 4, the male die 4 and the female die assembly 5 are fixed through the positioning pin 3, and the constant pressure block 1 is arranged on the upper end face of the fixing plate 2. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the material of the die is 0Cr18Ni9 or other austenitic stainless steel. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the low-temperature glass powder is lead-containing low-temperature glass, bismuth-system lead-free low-temperature glass, phosphorus-system lead-free low-temperature glass or composite glass powder containing an expansion coefficient regulating phase. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the softening point of the low-temperature glass powder is 400-450 ℃, the welding temperature is higher than the softening point by 50-100 ℃, and the thermal expansion coefficient is (65-110) multiplied by 10-7V. C. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the thickness of the glass solder sheet is 0.5-1.5 mm. The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the sintering adopts step temperature, the temperature is firstly increased to 250-350 ℃ from room temperature, the heat preservation is carried out for 10-60 min under the condition that the temperature is 250-350 ℃, then the temperature is increased to 20-40 ℃ higher than the softening point of the low-temperature glass powder from 250-350 ℃, and the heat preservation is carried out for 10-60 min at the temperature; wherein the heating rate is lower than 5 ℃/min. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the glass solder sheet of the embodiment is used for connecting the high volume fraction aluminum-based composite materials or connecting the high volume fraction aluminum-based composite materials with glass; the method comprises the following steps:
assembling a glass solder sheet in the middle of a test piece to be welded, placing the glass solder sheet in a special welding tool, transferring the glass solder sheet to an atmosphere sintering furnace for sintering, wherein in the sintering process, the pressure is kept at 5-10 KPa, and after sintering is finished, a low-temperature glass solder layer is formed in the middle to obtain a welded test piece; the thickness of the low-temperature glass solder layer is less than 100 mu m;
the volume fraction of the reinforcing phase in the high volume fraction aluminum-based composite material is 55-70%.
The glass solder sheet of the embodiment melts and wets the base material and spreads all around, and in the spreading process, the surrounding air is discharged, so that a compact, high-strength and pore-free low-temperature glass solder layer can be obtained.
The thickness of the low-temperature glass solder layer is less than 100 mu m, so that the low-temperature glass solder layer can be prevented from cracking.
The present embodiment can be adapted to the bonding of other volume fractions of aluminum-based composites (as well as aluminum alloys) to glass by adjusting the glass composition.
The specific implementation method nine: the eighth embodiment is different from the eighth embodiment in that: the glass solder sheet is used for packaging an aluminum-based composite material for a T/R tube shell of a phased array radar in aviation, aerospace, ships or ground. The rest is the same as the embodiment eight.
The specific implementation mode is ten: the present embodiment differs from the embodiment eight or nine in that: the sintering adopts step temperature, the temperature is firstly increased from room temperature to 250-350 ℃, the temperature is kept for 10-60 min at the temperature of 250-350 ℃, then the temperature is increased from 250-350 ℃ to 50-100 ℃ higher than the softening point of the glass solder sheet, and the temperature is kept for 10-60 min at the temperature; then cooling the glass solder sheet to 250-350 ℃ from the temperature 50-100 ℃ higher than the softening point of the glass solder sheet, and taking out the glass solder sheet after furnace cooling to 100 ℃; wherein the heating rate is lower than 5 ℃/min, and the cooling rate is lower than 5 ℃/min. The others are the same as the embodiments eight or nine.
The concrete implementation mode eleven: this embodiment differs from one of the eighth to tenth embodiments in that: the special welding tool consists of a constant-force pressing block 6 and a graphite backing plate 7; the test piece to be welded is arranged between the two layers of graphite backing plates 7, and the constant-force pressing block 6 is arranged on the upper end face of the upper layer of graphite backing plate 7. The others are the same as the eighth to the tenth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: the method for welding high-silicon aluminum by using the bismuth-based low-temperature glass comprises the following steps:
firstly, taking 0.5g of low-temperature glass powder, filling the low-temperature glass powder into a mold cavity, applying pressure of 0.5KPa under the action of a constant pressure block, then placing the mold cavity into an atmospheric sintering furnace, heating the temperature of the sintering furnace from room temperature to 300 ℃ within 40min, preserving heat for 30min under the condition that the temperature is 300 ℃, then heating the temperature from 300 ℃ to 460 ℃ within 40min, preserving heat for 30min, cooling the mold cavity to below 100 ℃ along with the furnace, and taking out the mold cavity to obtain a low-temperature glass solder sheet, wherein the low-temperature glass solder sheet is shown in figure 2; the size of the obtained low-temperature glass solder sheet is 10 multiplied by 7 multiplied by 1.4 mm; macroscopic and microscopic observation shows that the surface is smooth, the glossiness is good, and the combination is compact. The low-temperature glass powder is bismuth-system low-temperature glass.
Secondly, cutting the massive high-silicon aluminum alloy into welding test pieces with the size of 10mm multiplied by 15mm multiplied by 2mm by a spark wire cutting machine, and grinding one side of the high-silicon aluminum alloy with No. 400 metallographic abrasive paper to remove surface impurities and oxide films; the method comprises the steps of firstly, ultrasonically cleaning acetone for 15 minutes to remove oil, ultrasonically cleaning alcohol for 2-3 times, drying the cleaned glass solder piece by cold air, assembling the glass solder piece in the middle of a test piece to be welded, placing the test piece in a special welding tool, applying pressure of 5KPa under the action of a constant-force pressing block, and then transferring the test piece to an atmosphere sintering furnace for welding. The process comprises the following steps: and (3) heating the temperature of the sintering furnace from room temperature to 300 ℃ within 40min, preserving the heat for 30min under the condition that the temperature is 300 ℃, then heating from 300 ℃ to 490 ℃ within 40min, preserving the heat for 30min, reducing the temperature from 490 ℃ to 300 ℃ within 40min, finally cooling to below 100 ℃ along with the furnace, and taking out, namely completing the welding. The device to be packaged is made of high-silicon aluminum alloy with the trade name of 2AS50CE11, and the Si content is 50.3%; the softening point of the low-melting-point glass powder is 429 ℃.
The appearance, the strength and the air tightness after welding are detected to reach the standard, and the parameters are as follows: the appearance is well formed, the texture is uniform, and no air holes are formed; shear strength: 33.7 MPa; airtightness: 1.0X 10-10Pa·m3/s。
The metallographic phase, SEM image and cut material picture of an optical microscope for welding the high-silicon aluminum connecting joint by using bismuth-based low-temperature glass are respectively shown in figures 4-6.
Example two: the embodiment of welding the high volume fraction aluminum-based composite material by using the bismuth-based low-temperature glass specifically comprises the following steps:
firstly, taking out 0.5g of low-temperature glass powder, filling the low-temperature glass powder into a mold cavity, applying pressure of 0.5KPa under the action of a constant pressure block, then placing the mold cavity into an atmospheric sintering furnace, heating the temperature of the sintering furnace from room temperature to 300 ℃ within 40min, preserving heat for 30min under the condition that the temperature is 300 ℃, then heating the temperature from 300 ℃ to 460 ℃ within 40min, preserving heat for 30min, cooling the mold cavity to below 100 ℃ along with the furnace, and taking out the mold cavity to obtain a low-temperature glass solder sheet, wherein the low-temperature glass solder sheet is shown in figure 2; the size of the obtained low-temperature glass solder sheet is 10 multiplied by 7 multiplied by 1.4 mm; macroscopic and microscopic observation shows that the surface is smooth, the glossiness is good, and the combination is compact.
Secondly, cutting the plate-shaped high-volume-fraction aluminum-based composite material into welding test pieces with the dimensions of 10mm multiplied by 20mm multiplied by 2mm by using a spark wire cutting machine, and grinding one surface of each composite material piece by using No. 400 metallographic abrasive paper to remove surface impurities and an oxide film; the method comprises the steps of firstly, ultrasonically cleaning acetone for 15 minutes to remove oil, ultrasonically cleaning alcohol for 2-3 times, drying the cleaned glass solder piece by cold air, assembling the glass solder piece in the middle of a test piece to be welded, placing the test piece in a special welding tool, applying pressure of 5KPa under the action of a constant-force pressing block, and then transferring the test piece to an atmosphere sintering furnace for welding. The process comprises the following steps: and (3) heating the temperature of the sintering furnace from room temperature to 300 ℃ within 40min, preserving the heat for 30min under the condition that the temperature is 300 ℃, then heating the temperature from room temperature to 490 ℃ within 40min, preserving the heat for 40min, setting the temperature from 490 ℃ to 300 ℃ within 40min, and finally cooling the sintering furnace to below 100 ℃ along with the furnace, and taking out the sintering furnace, namely completing the welding. The material of the device to be packaged is 55 vol.% SiCp/ZL102 high-volume-fraction aluminum-based composite material; the softening point of the low-melting-point glass powder is 429 ℃.
The appearance, the strength and the air tightness of the welded steel plate are detected to reach the standard, and the parameters are as follows: the appearance is well formed, the texture is uniform, and no air holes are seen; shear strength: 31.5 MPa; airtightness: 4.0X 10-10Pa·m3/s。

Claims (1)

1. The application of the low-temperature glass solder sheet prepared by sintering is characterized in that the preparation of the low-temperature glass solder sheet is specifically carried out according to the following steps: designing a mold according to the shape of a test piece to be welded, wherein the mold is made of stainless steel, filling low-temperature glass powder into a mold cavity, and sintering the glass powder at a temperature 20-40 ℃ higher than the softening point of the low-temperature glass powder under the action of a constant-pressure block to obtain a glass solder sheet; the die consists of a constant pressure block (1), a fixing plate (2), a positioning pin (3), a male die (4) and a female die component (5); the molded surface of the male die (4) corresponds to the molded surface of the female die component (5) and forms a die cavity; the fixed plate (2) is transversely arranged on the upper end face of the male die (4), the male die (4) and the female die component (5) are fixed through the positioning pin (3), and the upper end face of the fixed plate (2) is provided with a constant pressure block (1); the low-temperature glass powder is bismuth-based lead-free low-temperature glass, phosphorus-based lead-free low-temperature glass or composite glass powder containing an expansion coefficient regulating phase; the softening point of the low-temperature glass powder is 400-450 ℃, the welding temperature is higher than the softening point by 50-100 ℃, and the thermal expansion coefficient is (65-110) multiplied by 10-7/° c; the thickness of the glass solder sheet is 0.5-1.5 mm; the glass solder sheet is used for packaging an aluminum-based composite material for a T/R tube shell of a phased array radar in aviation, aerospace, ships or ground; the method comprises the following steps:
assembling a glass solder sheet in the middle of a test piece to be welded, placing the test piece in a special welding tool, transferring the test piece to an atmosphere sintering furnace for sintering, wherein the sintering adopts a step temperature, firstly heating the temperature from room temperature to 250-350 ℃, preserving the heat for 10-60 min at the temperature of 250-350 ℃, then heating the temperature from 250-350 ℃ to 50-100 ℃ higher than the softening point of the glass solder sheet, and preserving the heat for 10-60 min at the temperature; then, cooling the temperature from 50-100 ℃ higher than the softening point of the glass solder sheet to 250-350 ℃, cooling the glass solder sheet to 100 ℃ along with the furnace, and taking out the glass solder sheet; wherein the heating rate is lower than 5 ℃/min, and the cooling rate is lower than 5 ℃/min; in the sintering process, the pressure is kept at 5-10 KPa, and a low-temperature glass solder layer is formed in the middle after sintering is completed, so that a welded test piece is obtained; the thickness of the low-temperature glass solder layer is less than 100 mu m;
the volume fraction of the reinforcing phase in the high volume fraction aluminum-based composite material is 55-70%.
CN201911400560.5A 2019-12-30 2019-12-30 Method for preparing low-temperature glass solder sheet by sintering and application thereof Active CN111056744B (en)

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JP2020080326A JP7076739B2 (en) 2019-12-30 2020-04-30 Sintering and manufacturing method of low temperature glass solder preform and how to use the glass solder preform

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JPH10152705A (en) * 1996-11-26 1998-06-09 Kubota Corp Production of bulk compacted body of amorphous alloy powder
JP5311274B2 (en) * 2008-07-14 2013-10-09 日本電気硝子株式会社 Bismuth glass composition and sealing material
CN101531474B (en) * 2009-04-17 2011-05-11 西安华泰有色金属实业有限责任公司 Process for sealing multipin connector for glass and metal
CN107021635B (en) * 2017-04-26 2020-02-04 南京广兆测控技术有限公司 Glass solder and preparation method thereof

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