CN112194499A - Solder for low-temperature rapid welding of heterogeneous ceramics - Google Patents
Solder for low-temperature rapid welding of heterogeneous ceramics Download PDFInfo
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention relates to a solder for rapidly welding heterogeneous ceramics at low temperature under the assistance of an electric field, belonging to the field of welding. The invention provides a solder for rapidly welding heterogeneous ceramics at low temperature under the assistance of an electric field, which is obtained by uniformly mixing, press-forming and sintering rare earth stabilized zirconia and magnesia-doped alumina powder; the mass ratio of zirconia to alumina in the solder is as follows: 2:8 to 8: 2; the sintering temperature is 1450-. The welding flux for rapidly welding the heterogeneous ceramics at low temperature under the assistance of the electric field not only realizes the high-efficiency welding between the zirconia and the alumina heterogeneous ceramics; and the welding rate can be controlled by adjusting the concentration of the dopant in the welding flux; meanwhile, the strength of the welding interface can be regulated and controlled by regulating the composition of the welding flux. In addition, as the solder is used, the welding temperature is low, and the welding time is short, the thermal stress of the welding sample is eliminated, which is beneficial to improving the welding strength.
Description
Technical Field
The invention relates to a solder for quickly welding heterogeneous ceramics at low temperature, belonging to the field of welding.
Background
Welding between dissimilar ceramics to an enlarged extent for widening the range of applicationsMeeting the actual needs is of great significance. Such as zirconium oxide (ZrO)2) And alumina (Al)2O3) Ceramics have been regarded as typical oxide ceramics in the field of engineering technology, and the welding between them has been widely used in the fields of aviation, transportation and energy ("t.nano, h.kato, Diffusion Bonding of Zirconia/Alumina composites. journal of the American Ceramic Society,73[11 ] and](1990)3476–3480”“M.Boniecki,D.Kaliński,Z.Librant,W.
Superplastic joining of alumina and zirconia ceramics.Journal of the European Ceramic Society.27(2007)1351–1355”)。ZrO2ceramics have excellent mechanical properties and corrosion resistance, and good chemical stability and oxygen ion conductivity, and thus are widely used in the fields of industry, aerospace, and biomedical science. At the same time, Al2O3Ceramics are widely used as structural ceramics and electronic ceramics due to their high strength, high hardness, and good chemical stability and electrical insulation. Although both of these typical oxide ceramics have their own advantages, they sometimes need to be combined because they have different mechanical and electrical properties. The method of material connection for preparing the composite member of zirconia and alumina is an effective method for solving the problem.
Traditionally, the two materials are welded at a certain high temperature, the welding temperature is usually high (not less than 1200 ℃), and the welding time is long (not less than 2 hours). The use of active metals as solder can reduce the soldering temperature, however, the soldering components are used at a lower temperature and the introduction of foreign elements may contaminate the soldered material. ("proofing, distributing and joining in the alumina-zirconia-Inconel 738system [ J ]. Scripta materials 50(2004) 325-330"). The patent "a method for the rapid welding at low temperature of zirconia or zirconia-based composites" describes a method for the rapid welding at low temperature between zirconia or zirconia-based composites using an electric field assisted method above a critical value. Due to the different microstructures between the two materials, direct welding cannot be performed by the electric field assisted method.
Based on the reasons, the invention adopts the rare earth doped zirconia and the magnesia doped alumina as the solder, and applies a certain electric field to the sample at a certain temperature to carry out the low-temperature rapid welding between the zirconia and the alumina ceramics. Because the solder contains zirconium oxide and aluminum oxide, the zirconium oxide and the aluminum oxide ceramic can be respectively subjected to diffusion mass transfer with the same components in the solder, and further the welding between the zirconium oxide and the aluminum oxide ceramic is realized. And the higher the content of which phase in the solder, the higher the interface bonding strength between the ceramic and the solder.
Disclosure of Invention
The invention aims to provide a solder for rapidly welding heterogeneous ceramics at low temperature under the assistance of an electric field, which consists of rare earth doped zirconia and magnesia doped alumina, wherein the welding rate is controlled by controlling the concentration of dopants in the zirconia and the alumina, and the strength of a welding surface is controlled by adjusting the proportion of the zirconia and the alumina in the solder.
The purpose of the invention is realized by the following technical scheme.
A solder for low-temperature rapid soldering of heterogeneous ceramics, which consists of rare earth stabilized zirconia and magnesia doped alumina; uniformly mixing zirconia and alumina ceramic powder, pressing and molding, and sintering at a certain temperature to obtain the zirconia-alumina ceramic powder; the mass ratio of the zirconia to the alumina is as follows: 2:8 to 8: 2; the sintering temperature is 1450-1550 ℃;
the rare earth stabilized zirconia includes: stabilized zirconia such as yttria, ceria, calcia, or scandia.
The method for rapidly welding the zirconia and alumina heterogeneous ceramics by adopting the welding flux under the electric field comprises the following steps:
polishing the surfaces of zirconia, alumina ceramics and solder to be less than 10 mu m, placing the solder between the zirconia and the alumina, and enabling the polished surfaces of the zirconia and the alumina to be attached to each other tightly to obtain a sample;
step two, applying pressure to the sample obtained in the step one; the pressure is more than or equal to 1MPa and is less than the compressive strength of the material; then heating the sample to a certain temperature; the temperature is 800-1300 ℃; and finally, applying a certain electric field to the sample and keeping for a certain time to finish the welding of the sample. The electric field intensity is more than or equal to 30V/cm, and the current density is more than or equal to 5mA/mm2(ii) a The time is 1-300 s;
the theory of the invention is that the solder contains the components of zirconium oxide and aluminum oxide at the same time, so that the welded material can respectively carry out mass transfer with the same components in the solder, and further realize the welding between the two. The higher the content of a certain phase in the solder, the higher the interface bonding strength between the solder and such ceramics. The interface strength between a certain phase and the solder is controlled by adjusting the content of the phase in the solder. The method can also be applied to welding between heterogeneous ceramics such as titanium oxide and barium oxide.
Advantageous effects
The welding flux for rapidly welding the heterogeneous ceramics at low temperature under the assistance of the electric field not only realizes the efficient welding between the zirconia and the alumina heterogeneous ceramics; and the welding rate can be controlled by adjusting the concentration of the dopant in the welding flux; meanwhile, the strength of the welding interface can be regulated and controlled by regulating the composition of the welding flux. In addition, due to the use of the solder and the lower soldering temperature and shorter soldering time, the thermal stress of the soldering sample is eliminated, which is beneficial to the improvement of the soldering strength.
Drawings
FIG. 1 is a schematic view of a material combination for welding zirconia and alumina according to the present invention, wherein ZA is solder;
FIG. 2 shows ZrO in a mass ratio of 50% for zirconia and alumina ceramics2-50％Al2O3Scanning electron microscope pictures of solder (ZA) soldered samples; wherein, the picture a is a low-power scanning electron microscope picture of a sample; FIG. b is ZrO2High power scanning electron microscope pictures of the interface with solder (ZA); FIG. c is Al2O3High power scanning of the interface with solder (ZA)And (5) taking an electron microscope picture.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1:
a) mixing 3 mass percent of yttria-stabilized zirconia powder and 1 mass percent of magnesia-doped alumina powder according to the mass ratio of 50 percent to 50 percent, then pressing and molding the obtained mixed powder, and sintering at 1500 ℃ to obtain the required solder.
b) Polishing the surfaces of the solder, the zirconia and the alumina ceramics obtained in the step a) to 10 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying a pressure of 2 MPa;
d) heating the sample obtained in the step c) to 1200 ℃;
e) applying the sample obtained in the step d) with the electric field intensity of 800V/cm and the current density of 5mAmm–2And holding for 30s to complete the welding between the samples.
And (4) conclusion: by using the solder with the mass ratio of 50% to 50% of zirconia and alumina, the efficient welding of the zirconia and the alumina is realized, and the welding effect is good.
Example 2:
a) uniformly mixing 3 mass percent of yttria-stabilized zirconia powder and 1 mass percent of magnesia-doped alumina powder according to a mass ratio of 20 to 80 percent, then pressing and molding the obtained mixed powder, and sintering at 1450 ℃ to obtain the solder.
b) Polishing the surfaces of the solder, the zirconia and the alumina ceramics obtained in the step a) to 5 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying a pressure of 2 MPa;
d) heating the sample obtained in the step c) to 1200 ℃;
e) applying the sample obtained in the step d) with the electric field intensity of 800V/cm and the current density of 5mAmm-2And holding for 30s to complete the welding between the samples.
And (4) conclusion: by using the solder with the mass ratio of 20% to 80% of zirconia to alumina, the high-efficiency welding of the zirconia and the alumina is realized, a welding sample with high welding flux-alumina interface strength is obtained, and the welding effect is good.
Example 3:
a) uniformly mixing 2 mass percent of calcium oxide stabilized zirconia powder and 1 mass percent of magnesium oxide doped alumina powder according to the mass ratio of 40 to 60 percent, then pressing and molding the obtained mixed powder, and sintering at 1550 ℃ to obtain the solder.
b) Polishing the surfaces of the solder, the stabilized zirconia and the alumina ceramics obtained in the step a) to 1 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying a pressure of 1 MPa;
d) heating the sample obtained in the step c) to 1300 ℃;
e) applying an electric field strength of 750V/cm and a current density of 10mAmm to the sample obtained in the step d)-2And the samples were welded together while being held for 10 seconds.
And (4) conclusion: by using the solder with the mass ratio of 40% to 60% of zirconia and alumina, the efficient welding of the zirconia and the alumina is realized, and the welding effect is good.
Example 4:
a) uniformly mixing 5 mass percent of cerium oxide stabilized zirconia powder and 1 mass percent of magnesium oxide doped alumina powder according to the mass ratio of 35 percent to 65 percent, then pressing and molding the obtained mixed powder, and sintering at 1480 ℃ to obtain the required solder.
b) Polishing the surfaces of the solder, the zirconia and the alumina ceramics obtained in the step a) to 1 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying a pressure of 1 MPa;
d) heating the sample obtained in the step c) to 1300 ℃;
e) applying an electric field intensity of 2000V/cm and a current density of 100mAmm to the sample obtained in the step d)-2And the samples were welded together for 5 seconds.
And (4) conclusion: by using the solder with the mass ratio of 35 percent to 65 percent of zirconia to alumina, the high-efficiency welding of zirconia and alumina ceramics is realized, and the welding effect is good.
Example 5:
a) uniformly mixing 3% by mass of scandia-stabilized zirconia powder and 3% by mass of magnesia-doped alumina powder according to a mass ratio of 25% to 75%, then pressing and molding the obtained mixed powder, and sintering at 1500 ℃ to obtain the solder.
b) Polishing the surfaces of the solder, the stabilized zirconia and the alumina ceramics obtained in the step a) to 1 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying pressure of 5 MPa;
d) heating the sample obtained in the step c) to 800 ℃;
e) applying an electric field strength of 1500V/cm and a current density of 20mAmm to the sample obtained in the step d)-2And kept for 10min to weld the samples.
And (4) conclusion: by using the solder with the mass ratio of the zirconium oxide to the aluminum oxide being 25% to 75%, the zirconium oxide and the aluminum oxide are efficiently welded, and the welding effect is good.
Example 6:
a) uniformly mixing 3 mass percent of yttria-stabilized zirconia powder and 2 mass percent of magnesia-doped alumina powder according to the mass ratio of 30 to 70 percent, then pressing and molding the obtained mixed powder, and sintering at 1500 ℃ to obtain the solder.
b) Polishing the surfaces of the solder, the stabilized zirconia and the alumina ceramics obtained in the step a) to 1 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying a pressure of 2 MPa;
d) heating the sample obtained in the step c) to 1000 ℃;
e) applying an electric field strength of 1000V/cm and a current density of 15mAmm to the sample obtained in the step d)-2The samples were welded together in the direction from alumina to zirconia for 1 min.
And (4) conclusion: by using the solder with the mass ratio of 30% to 70% of zirconia and alumina, the efficient welding of the zirconia and the alumina is realized, and the welding effect is good.
Example 7:
a) uniformly mixing zirconia powder with stable yttria and magnesia-doped alumina powder with the mass fraction of 4% and magnesia-doped alumina powder with the mass fraction of 1% according to the mass ratio of 45% to 55%, then pressing and molding the obtained mixed powder, and sintering at 1450 ℃ to obtain the required solder.
b) Polishing the surfaces of the solder, the stabilized zirconia and the alumina ceramics obtained in the step a) to 1 mu m;
c) tightly attaching the surfaces of the samples obtained in the step b) together, and applying pressure intensity of 10 MPa;
d) heating the sample obtained in the step c) to 900 ℃;
e) applying an electric field strength of 1800V/cm and a current density of 10mAmm to the sample obtained in the step d)-2And kept for 10min to weld the samples.
And (4) conclusion: by using the welding flux with the mass ratio of the zirconium oxide to the aluminum oxide being 45% to 55%, the zirconium oxide and the aluminum oxide are efficiently welded, and the welding effect is good.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. A solder for low-temperature rapid soldering of heterogeneous ceramics, characterized in that: the solder consists of rare earth stabilized zirconia and magnesia doped alumina; the mass ratio of zirconia to alumina in the solder is as follows: 2:8 to 8: 2; uniformly mixing, pressing, forming and sintering zirconium oxide and aluminum oxide powder to obtain the solder; the sintering temperature is 1450-.
2. A method for rapidly welding zirconia and alumina heterogeneous ceramics in an electric field using a solder prepared by the method of claim 1, wherein: the method comprises the following steps:
polishing the surfaces of a solder, zirconia and alumina ceramics to be less than 10 mu m, placing the solder between the zirconia and the alumina, and enabling the polished surfaces of the zirconia and the alumina to be attached together to obtain a sample;
step two, applying pressure to the sample obtained in the step one; the pressure is more than or equal to 1MPa and is less than the compressive strength of the material; then heating the sample to a certain temperature; the temperature is 800-1300 ℃; finally, applying a certain electric field to the sample and keeping for a certain time to finish the welding of the sample; the electric field intensity is more than or equal to 30V/cm, and the current density is more than or equal to 5mA/mm2(ii) a The time is 1-300 s;
because the solder contains the components of zirconium oxide and aluminum oxide, the welded materials can respectively carry out mass transfer with the same components in the solder, thereby realizing the welding between the two; the higher the content of a certain phase in the solder, the higher the interface bonding strength between the solder and such ceramics.
3. A solder material prepared by the method of claim 1, wherein: the rare earth stabilized zirconia includes: stabilized zirconia such as yttria, ceria, calcia, or scandia.
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| CN116354708A (en) * | 2021-12-28 | 2023-06-30 | 财团法人工业技术研究院 | Ceramic material and ceramic article made of same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116354708A (en) * | 2021-12-28 | 2023-06-30 | 财团法人工业技术研究院 | Ceramic material and ceramic article made of same |
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