CN114101827A - Ceramic heating element electrode brazing process - Google Patents
Ceramic heating element electrode brazing process Download PDFInfo
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- CN114101827A CN114101827A CN202111389679.4A CN202111389679A CN114101827A CN 114101827 A CN114101827 A CN 114101827A CN 202111389679 A CN202111389679 A CN 202111389679A CN 114101827 A CN114101827 A CN 114101827A
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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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
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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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
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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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
- B23K2103/52—Ceramics
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Abstract
The invention relates to the technical field of ceramic heating element welding, in particular to a ceramic heating element electrode brazing process, which comprises the following steps: 1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and noble metal slurry; 2) cutting into alumina ceramic substrates; 3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate; 4) printing a second layer of electrode metal slurry at the electrode; 5) superposing the aluminum oxide ceramic substrate and the green body or the substrate into a vacuum bag for vacuumizing and isostatic pressing treatment; 6) sintering the product subjected to isostatic pressing in the step 5), and preserving heat; 7) and (3) spot-welding the noble metal slurry on the electrode of the sintered product, then installing the required welding metal wire, and obtaining the ceramic heating element with the metal wire. The process is simple, the manufacturing cost is reduced, and the stability and the reliability of the product tension are improved; the tensile force of the product after brazing by the process can reach 5-12KG, and the tensile force is obviously improved.
Description
Technical Field
The invention relates to the technical field of ceramic heating element welding, in particular to a ceramic heating element electrode brazing process.
Background
The ceramic heating substrate is a new generation of upgraded heating element product developed in recent years, and due to the characteristics of environmental protection, high reliability, long service life and the like, the ceramic heating substrate replaces the PTC heating element containing the lead component which is commonly used in the past, and has wide application market prospect at home and abroad. Therefore, people pay more attention to the technology for researching the production process of the high-temperature alumina ceramic heating substrate product.
After the traditional welding method needs metallization, (ceramic metallization is a process of firmly adhering a layer of metal film on the surface of ceramic to realize the welding between ceramic and metal, and the existing molybdenum-manganese method, gold plating method, copper plating method, tin plating method, nickel plating method, LAP method (laser metal plating) and other ceramic metallization processes) are independently welded, however, the metallization strength is low, the film layer binding force is poor, the oxidation is easy, the sintering cost is high, and the problems of large resistivity fluctuation, unstable electrode welding, difficult electrode welding and the like of an internal printed circuit are easy to occur. Since these not only cause a decrease in yield but also affect the quality of the product, it is important to improve the quality of the product and promote the development of the ceramic heating element by continuously researching and improving the process level of the ceramic heating element.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the electrode brazing process for the ceramic heating element, which is simple, reduces the manufacturing cost, improves the tensile stability and reliability of a product, improves the ceramic printing slurry, increases a layer of electrode metal slurry on the electrode, combines the electrode with a noble metal solder for welding, welds a metal wire under the reducing atmosphere condition, improves the tensile stability and reliability of the product, can also reduce the previous nickel electroplating or chemical nickel plating process, avoids the pollution of heavy metal of electroplating liquid to a water source, and is safer and more environment-friendly; in addition, the tensile force of the product after brazing by the process can reach 5-12KG, and the tensile force is obviously improved.
The purpose of the invention is realized by the following technical scheme: a ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body or substrate into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition of 1500-1700 ℃, preserving heat for 1-4.5h, and discharging for later use;
7) and (3) dispensing the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding metal wire, brazing in a reducing atmosphere at the temperature of 800-1300 ℃, and preserving heat for 0.5-2.5h to obtain the ceramic heating element with the metal wire.
The ceramic heating element electrode brazing process is simple, the manufacturing cost is reduced, the stability and the reliability of the tensile force of the product are improved, the ceramic printing slurry is improved, a layer of electrode metal slurry is additionally printed at the electrode, and then the electrode is welded by adding the noble metal solder at the electrode, and the metal wire is welded under the reducing atmosphere condition, so that the stability and the reliability of the tensile force of the product are improved, the previous nickel electroplating or chemical nickel plating process can be reduced, the pollution of heavy metal of electroplating liquid to a water source is avoided, and the ceramic heating element electrode brazing process is safer and more environment-friendly; in addition, the tensile force of the product after brazing by the process can reach 5-12KG, and the tensile force is obviously improved; wherein the sintering temperature in the step 6) needs to be strictly controlled to be 1500-1700 ℃, if the temperature is too high, the ceramic heating element obtained by final sintering is easy to crack locally, and if the temperature is too low, the strength of the ceramic heating element obtained by final sintering is not favorable.
Preferably, the first layer metal slurry is prepared from a first tungsten slurry and a first porcelain slurry according to the following weight parts of 75-95: 5-25;
the first porcelain slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 0.1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-90 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-95 parts of tungsten powder.
Preferably, the first layer metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first ceramic slurry obtained in the step S1, uniformly mixing and stirring, baking for 2-4 hours, and performing ball milling for 7-16 hours through a ball mill to obtain a first layer of metal slurry.
Preferably, the second layer electrode metal slurry is prepared from a second tungsten slurry and a second ceramic slurry according to the following weight parts of 85-98: 1-15;
the second porcelain slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 0.1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-90 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-95 parts of tungsten powder.
According to the invention, the function of additionally printing a second layer of electrode metal slurry at the electrode is to increase the thickness of the electrode and facilitate the bonding force of metal solder, while terpineol, tributyl citrate, butyl carbitol and ethyl cellulose added in the second layer of electrode metal slurry can effectively improve the stability of the resistivity of a printed circuit, and the butyl carbitol is added in the tungsten slurry to improve the stability of later-stage welding electrode soldering.
Preferably, the second layer electrode metal paste is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 1-4 hours, and performing ball milling for 8-16 hours through a ball mill to obtain second layer electrode metal slurry.
Preferably, the precious metal slurry comprises the following raw materials in parts by weight: 1-15 parts of nickel powder, 70-90 parts of silver powder, 1-10 parts of copper powder, 0.1-10 parts of titanium powder and 1-30 parts of organic carrier; more preferably, the organic carrier is one or more of terpineol, tributyl citrate, butyl carbitol and ethyl cellulose.
Preferably, the noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The nickel powder and the copper powder added into the noble metal slurry have good high-temperature strength, the nickel powder and the copper powder are added by the solder so as to increase the wettability of the ceramic surface, and the bonding force between the solder and the metal wire of the electrode can be enhanced, so that the bonding force between the ceramic heating element and the metal wire is improved; when the noble metal slurry is dotted at the electrode of the ceramic heating element, the ceramic heating element and the noble metal solder are heated to a slightly higher temperature than the melting point of the solder, the solder is melted, and the liquid solder is filled into the gap between the ceramic heating element and the metal and is diffused and dissolved after being condensed, thereby being convenient for welding the metal wire.
Preferably, the reducing atmosphere is formed by mixing hydrogen and nitrogen in a ratio of 1-10: 1-10 of the composition of the mixed gas.
Preferably, the shape of the blank is any one of a flat plate shape, a cylindrical shape, or a round bar shape.
The moisture obtained after the hydrogen is ignited in the invention can effectively cool the sintered ceramic heating piece and can also relieve the problem that the green sheet is not sintered and has low strength in the sintering process.
The invention has the beneficial effects that: the ceramic heating element electrode brazing process is simple, the manufacturing cost is reduced, the stability and the reliability of the tensile force of a product are improved, the ceramic printing slurry is improved, a layer of electrode metal slurry is additionally printed at the electrode, and then the electrode is welded by adding the noble metal solder at the electrode, and a metal wire is welded under the reducing atmosphere condition, so that the stability and the reliability of the tensile force of the product are improved, the previous nickel electroplating or chemical nickel plating process can be reduced, the pollution of heavy metal of electroplating liquid to a water source is avoided, and the ceramic heating element electrode brazing process is safer and more environment-friendly; in addition, the tensile force of the product after brazing by the process can reach 5-12KG, and the tensile force is obviously improved.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
A ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use; the blank is shaped like a flat plate;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition at the temperature of 1500 ℃, preserving heat for 1h, and discharging for later use;
7) and (3) dotting the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding wire, brazing in a reducing atmosphere at the temperature of 800 ℃, and preserving heat for 0.5h to obtain the ceramic heating element with the metal wire.
The first layer of metal slurry is prepared from 75 parts by weight of first tungsten slurry and first ceramic slurry: 5, preparing a composition;
the first porcelain slurry comprises the following raw materials in parts by weight: 20 parts of terpineol, 1 part of tributyl citrate, 0.1 part of butyl carbitol, 1 part of ethyl cellulose and 50 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 20 parts of terpineol, 1 part of tributyl citrate, 1 part of butyl carbitol, 1 part of ethyl cellulose and 50 parts of tungsten powder.
The first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first ceramic slurry obtained in the step S1, uniformly mixing and stirring, baking for 2 hours, and performing ball milling for 7 hours through a ball mill to obtain a first layer of metal slurry.
The second layer of electrode metal slurry is prepared from a second tungsten slurry and a second ceramic slurry in parts by weight of 85: 1, preparing a composition;
the second porcelain slurry comprises the following raw materials in parts by weight: 20 parts of terpineol, 1 part of tributyl citrate, 0.1 part of butyl carbitol, 1 part of ethyl cellulose and 50 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 20 parts of terpineol, 1 part of butyl carbitol, 1 part of ethyl cellulose and 50 parts of tungsten powder.
The second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 1h, and performing ball milling for 8h through a ball mill to obtain second-layer electrode metal slurry.
The precious metal slurry comprises the following raw materials in parts by weight: 1 part of nickel powder, 70 parts of silver powder, 1 part of copper powder, 0.1 part of titanium powder and 1 part of organic carrier.
The organic carrier is terpineol.
The noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The reducing atmosphere is prepared by mixing hydrogen and nitrogen in a ratio of 1: 1, and a mixed gas.
Example 2
A ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the substrate into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition at the temperature of 1550 ℃, preserving heat for 2 hours, and discharging for later use;
7) and (3) dotting the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding wire, brazing in a reducing atmosphere at the temperature of 900 ℃, and preserving heat for 1.0h to obtain the ceramic heating element with the metal wire.
The first layer of metal slurry is prepared from a first tungsten slurry and a first ceramic slurry in parts by weight of 80: 10;
the first porcelain slurry comprises the following raw materials in parts by weight: 30 parts of terpineol, 2 parts of tributyl citrate, 2 parts of butyl carbitol, 2 parts of ethyl cellulose and 60 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 30 parts of terpineol, 2 parts of tributyl citrate, 3 parts of butyl carbitol, 2 parts of ethyl cellulose and 61 parts of tungsten powder.
The first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first ceramic slurry obtained in the step S1, uniformly mixing and stirring, baking for 2.5 hours, and performing ball milling for 9 hours through a ball mill to obtain a first layer of metal slurry.
The second layer of electrode metal slurry is prepared from 88 parts by weight of second tungsten slurry and second ceramic slurry: 5, preparing a composition;
the second porcelain slurry comprises the following raw materials in parts by weight: 30 parts of terpineol, 3 parts of tributyl citrate, 3 parts of butyl carbitol, 3 parts of ethyl cellulose and 60 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 30 parts of terpineol, 3 parts of butyl carbitol, 3 parts of ethyl cellulose and 61 parts of tungsten powder.
The second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 2 hours, and performing ball milling for 10 hours through a ball mill to obtain second-layer electrode metal slurry.
The precious metal slurry comprises the following raw materials in parts by weight: 4 parts of nickel powder, 75 parts of silver powder, 3 parts of copper powder, 3 parts of titanium powder and 7 parts of organic carrier.
The organic carrier is tributyl citrate.
The noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The reducing atmosphere is formed by mixing hydrogen and nitrogen in a ratio of 3: 3, and (3).
Example 3
A ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use; the blank body is cylindrical;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition at 1600 ℃, preserving heat for 3 hours, and discharging for later use;
7) and (3) dotting the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding wire, brazing in a reducing atmosphere at the temperature of 1000 ℃, and preserving heat for 1.5 hours to obtain the ceramic heating element with the metal wire.
The first layer of metal slurry is prepared from a first tungsten slurry and a first ceramic slurry in parts by weight of 85: 15;
the first porcelain slurry comprises the following raw materials in parts by weight: 40 parts of terpineol, 4 parts of tributyl citrate, 4 parts of butyl carbitol, 4 parts of ethyl cellulose and 70 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 40 parts of terpineol, 4 parts of tributyl citrate, 5 parts of butyl carbitol, 4 parts of ethyl cellulose and 72 parts of tungsten powder.
The first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first porcelain slurry obtained in the step S1, uniformly mixing and stirring, baking for 3 hours, and performing ball milling for 11 hours through a ball mill to obtain a first layer of metal slurry.
The second layer of electrode metal slurry is prepared from second tungsten slurry and second ceramic slurry in parts by weight of 91: 8, preparing a mixture;
the second porcelain slurry comprises the following raw materials in parts by weight: 40 parts of terpineol, 5 parts of tributyl citrate, 5 parts of butyl carbitol, 5 parts of ethyl cellulose and 70 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 40 parts of terpineol, 5 parts of butyl carbitol, 5 parts of ethyl cellulose and 72 parts of tungsten powder.
The second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 3 hours, and performing ball milling for 12 hours through a ball mill to obtain second layer electrode metal slurry.
The precious metal slurry comprises the following raw materials in parts by weight: 8 parts of nickel powder, 80 parts of silver powder, 5 parts of copper powder, 5 parts of titanium powder and 15 parts of organic carrier.
The organic carrier is butyl carbitol.
The noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The reducing atmosphere is prepared by mixing hydrogen and nitrogen in a ratio of 5: 4, and 4.
Example 4
A ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use; the blank body is in a round bar shape;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition of 1650 ℃, preserving heat for 4 hours, and discharging for later use;
7) and (3) dotting the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding wire, brazing in a reducing atmosphere at the temperature of 1200 ℃, and preserving heat for 2.0h to obtain the ceramic heating element with the metal wire.
The first layer of metal slurry is prepared from a first tungsten slurry and a first ceramic slurry in parts by weight of 90: 20;
the first porcelain slurry comprises the following raw materials in parts by weight: 50 parts of terpineol, 8 parts of tributyl citrate, 8 parts of butyl carbitol, 8 parts of ethyl cellulose and 80 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 50 parts of terpineol, 6 parts of tributyl citrate, 8 parts of butyl carbitol, 8 parts of ethyl cellulose and 83 parts of tungsten powder.
The first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first ceramic slurry obtained in the step S1, uniformly mixing and stirring, baking for 3.5 hours, and performing ball milling for 13 hours through a ball mill to obtain a first layer of metal slurry.
The second layer of electrode metal slurry is prepared from a second tungsten slurry and a second ceramic slurry in parts by weight of 94: 12;
the second porcelain slurry comprises the following raw materials in parts by weight: 50 parts of terpineol, 8 parts of tributyl citrate, 8 parts of butyl carbitol, 8 parts of ethyl cellulose and 80 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 50 parts of terpineol, 8 parts of butyl carbitol, 8 parts of ethyl cellulose and 83 parts of tungsten powder.
The second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 4 hours, and performing ball milling for 14 hours through a ball mill to obtain second layer electrode metal slurry.
The precious metal slurry comprises the following raw materials in parts by weight: 12 parts of nickel powder, 85 parts of silver powder, 8 parts of copper powder, 8 parts of titanium powder and 23 parts of organic carrier.
The organic carrier is ethyl cellulose.
The noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The reducing atmosphere is formed by mixing hydrogen and nitrogen in a ratio of 7: 8, and (c) a mixed gas.
Example 5
A ceramic heating element electrode brazing process comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use; the blank is shaped like a flat plate;
6) sintering the product subjected to isostatic pressing in the step 5) under the reducing atmosphere condition at the temperature of 1700 ℃, preserving heat for 4.5 hours, and discharging for later use;
7) and (3) dotting the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding wire, brazing in a reducing atmosphere at the temperature of 1300 ℃, and preserving heat for 2.5 hours to obtain the ceramic heating element with the metal wire.
The first layer of metal slurry is prepared from a first tungsten slurry and a first ceramic slurry in parts by weight of 95: 25;
the first porcelain slurry comprises the following raw materials in parts by weight: 60 parts of terpineol, 1-10 parts of tributyl citrate, 10 parts of butyl carbitol, 10 parts of ethyl cellulose and 90 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 60 parts of terpineol, 10 parts of tributyl citrate, 10 parts of butyl carbitol, 10 parts of ethyl cellulose and 95 parts of tungsten powder.
The first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first porcelain slurry obtained in the step S1, uniformly mixing and stirring, baking for 4 hours, and performing ball milling for 16 hours through a ball mill to obtain a first layer of metal slurry.
The second layer of electrode metal slurry is prepared from 98 parts by weight of second tungsten slurry and second ceramic slurry: 15;
the second porcelain slurry comprises the following raw materials in parts by weight: 60 parts of terpineol, 10 parts of tributyl citrate, 10 parts of butyl carbitol, 10 parts of ethyl cellulose and 90 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 60 parts of terpineol, 10 parts of butyl carbitol, 10 parts of ethyl cellulose and 95 parts of tungsten powder.
The second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 4 hours, and performing ball milling for 16 hours through a ball mill to obtain second layer electrode metal slurry.
The precious metal slurry comprises the following raw materials in parts by weight: 15 parts of nickel powder, 90 parts of silver powder, 10 parts of copper powder, 10 parts of titanium powder and 30 parts of organic carrier.
The organic carrier is a mixture of terpineol, tributyl citrate and butyl carbitol according to the weight ratio of 0.8:0.6: 0.7.
The noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
The reducing atmosphere is formed by mixing hydrogen and nitrogen in a ratio of 10: 10, and (b) a mixed gas.
The reliability test is respectively carried out on the ceramic heating parts prepared in the specific embodiments 1-5, a chest expander is adopted during the test, and the test standard is as follows: the welding strength of the lead in the vertical direction is more than or equal to 2kgf, the welding strength of the lead in the horizontal direction is more than or equal to 5kgf, and the tensile force of the product obtained by final testing can reach 5-12 KG.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A ceramic heating element electrode brazing process is characterized in that: the method comprises the following steps:
1) preparing a first layer of metal slurry, a second layer of electrode metal slurry and a noble metal slurry for later use;
2) cutting the aluminum oxide ceramic green body into an aluminum oxide ceramic substrate according to the required size for later use;
3) respectively printing a heating circuit and an electrode on an aluminum oxide ceramic substrate by using a first layer of metal slurry for later use;
4) printing a second layer of electrode metal slurry on the printed electrode in the step 3) for later use;
5) superposing the aluminum oxide ceramic substrate printed with the second layer of electrode metal slurry and the green body or substrate into a vacuum bag for vacuumizing, and then carrying out isostatic pressing treatment for later use;
6) sintering the product subjected to isostatic pressing in the step 5) under the condition of a reducing atmosphere furnace with the temperature of 1500-1700 ℃, preserving heat for 1-4.5h, and discharging for later use;
7) and (3) dispensing the noble metal slurry on the electrode of the product sintered in the step 6), then installing a required welding metal wire, brazing in a reducing atmosphere at the temperature of 800-1300 ℃, and preserving heat for 0.5-2.5h to obtain the ceramic heating element with the metal wire.
2. The electrode brazing process for a ceramic heating element according to claim 1, wherein: the first layer of metal slurry is prepared from 75-95 parts by weight of first tungsten slurry and first ceramic slurry: 5-25;
the first porcelain slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 0.1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-90 parts of porcelain powder;
the first tungsten slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-95 parts of tungsten powder.
3. The electrode brazing process for a ceramic heating element according to claim 2, wherein: the first layer of metal slurry is prepared by the following steps:
s1, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain first porcelain slurry for later use;
s2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and stirring to obtain first tungsten slurry for later use;
s3, adding the first tungsten slurry obtained in the step S2 into the first ceramic slurry obtained in the step S1, uniformly mixing and stirring, baking for 2-4 hours, and performing ball milling for 7-16 hours through a ball mill to obtain a first layer of metal slurry.
4. The electrode brazing process for a ceramic heating element according to claim 1, wherein: the second layer electrode metal slurry is prepared from 85-98 parts by weight of second tungsten slurry and second ceramic slurry: 1-15;
the second porcelain slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of tributyl citrate, 0.1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-90 parts of porcelain powder;
the second tungsten slurry comprises the following raw materials in parts by weight: 20-60 parts of terpineol, 1-10 parts of butyl carbitol, 1-10 parts of ethyl cellulose and 50-95 parts of tungsten powder.
5. The electrode brazing process for a ceramic heating element according to claim 4, wherein: the second layer electrode metal slurry is prepared by the following steps:
e1, adding terpineol, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding tungsten powder, and uniformly stirring to obtain a second tungsten slurry for later use;
e2, adding terpineol, tributyl citrate, butyl carbitol and ethyl cellulose into a reaction device according to the parts by weight, uniformly mixing and stirring, adding porcelain powder, and uniformly stirring to obtain second porcelain slurry for later use;
e3, adding the second tungsten slurry obtained in the step E1 into the second ceramic slurry obtained in the step E2, uniformly mixing and stirring, baking for 1-4 hours, and performing ball milling for 8-16 hours through a ball mill to obtain second layer electrode metal slurry.
6. The electrode brazing process for a ceramic heating element according to claim 1, wherein: the precious metal slurry comprises the following raw materials in parts by weight: 1-15 parts of nickel powder, 70-90 parts of silver powder, 1-10 parts of copper powder, 0.1-10 parts of titanium powder and 1-30 parts of organic carrier.
7. The electrode brazing process for a ceramic heating element according to claim 6, wherein: the noble metal slurry is prepared by the following steps: according to the weight parts, the nickel powder, the silver powder, the copper powder and the titanium powder are mixed and stirred uniformly, then the organic carrier is added and mixed and stirred to obtain mixed slurry, and then the mixed slurry is dispersed and ground on a three-roller machine to finally obtain the noble metal slurry.
8. The electrode brazing process for a ceramic heating element according to claim 6, wherein: the organic carrier is one or a mixture of more of terpineol, tributyl citrate, butyl carbitol and ethyl cellulose.
9. The electrode brazing process for a ceramic heating element according to claim 1, wherein: the reducing atmosphere is prepared by mixing hydrogen and nitrogen in a ratio of 1-10: 1-10 of the composition of the mixed gas.
10. The electrode brazing process for a ceramic heating element according to claim 1, wherein: the blank is in any shape of flat plate, cylinder or round bar.
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