CN113336566A - Welding method for heating element, and aerosol generating apparatus - Google Patents
Welding method for heating element, and aerosol generating apparatus Download PDFInfo
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- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 3
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
- A24F40/46—Shape or structure of electric heating means
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F47/00—Smokers' requisites not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The application relates to a welding treatment method of a heating element, the heating element and an aerosol generating device, wherein the method comprises the following steps: taking a conductive ceramic substrate with a sunken electrode welding groove on the surface, and filling welding slurry into the electrode welding groove, wherein the alloy component in the welding slurry comprises at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy and silver-palladium-titanium alloy; arranging an electrode in an electrode welding groove, and pressing the electrode to enable at least part of welding slurry to overflow to the surface of the electrode; and drying the preliminarily fixed conductive ceramic substrate and the electrode, carrying out staged heating sintering, and cooling to obtain the heating element. The welding treatment method provided by the application can improve the welding strength of the electrode and the conductive ceramic base body, improve the use stability and effectively control the resistance variation of the heating body in the heating use process.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a welding treatment method of a heating element, the heating element and an aerosol generating device.
Background
At present, with the rapid development of a heating non-combustible aerosol generating device, a heating body of the aerosol generating device becomes a core component, and the overall design and performance quality level of the aerosol generating device are determined. The heating body of the ceramic material has the advantages of oxidation resistance, high temperature resistance, long service life and the like, and has gradually replaced the old heating resistance wire. At present, a heating element is generally formed by printing a resistance paste on a porous ceramic substrate to form a heating track. The inventor adopts the conductive ceramic as the heating body, but finds that the welding strength of the conductive ceramic base material and the electrode is low, the welding contact resistance is large, and in the cyclic heating use process, the welding point of the electrode is easy to loose and fall off under the action of thermal stress, so that the resistance is easy to increase.
Disclosure of Invention
The embodiment of the invention provides a welding treatment method of a heating element, the heating element and an aerosol generating device, which can improve the welding strength of an electrode and a conductive ceramic substrate, improve the use stability and effectively control the resistance variation of the heating element in the heating use process.
In a first aspect, the present application provides a welding processing method of a heat generating body, including the steps of:
taking a conductive ceramic substrate with a sunken electrode welding groove on the surface, and filling welding slurry into the electrode welding groove, wherein the alloy component in the welding slurry comprises at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy and silver-palladium-titanium alloy;
arranging an electrode plate in the electrode welding groove, and pressing the electrode plate to enable at least part of the welding slurry to overflow to the surface of the electrode plate;
and drying the preliminarily fixed conductive ceramic substrate and the electrode plate, carrying out staged heating sintering, and cooling to obtain the heating body.
With reference to the first aspect, in one possible embodiment, the method satisfies at least one of the following features a-b:
a. the conductive ceramic matrix material comprises at least one of silicon carbide, silicon nitride, aluminum oxide, silicon oxide, titanium diboride, titanium carbide and zirconium diboride;
b. the thickness of the conductive ceramic matrix is 0.3 mm-2 mm;
c. the resistivity of the conductive ceramic matrix is more than or equal to 1.0 multiplied by 10-6Ω·m。
With reference to the first aspect, in one possible embodiment, the electrode is a copper electrode or a silver electrode, and a surface of the copper electrode or the silver electrode is formed with at least one of a silver film, a gold film, or a nickel film.
In a possible embodiment, in combination with the first aspect, two electrode welding grooves are symmetrically arranged on the surface of the conductive ceramic substrate, and the two electrode welding grooves are a positive electrode welding groove and a negative electrode welding groove respectively.
With reference to the first aspect, in one possible embodiment, the method satisfies at least one of the following features a to c:
a. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove;
b. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove, the positioning groove comprises a bottom surface and a side guide surface with a slope, and the side guide surface with the slope is connected with the bottom surface and the surface of the conductive ceramic substrate;
c. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove, and the depth of the electrode welding groove is 0.25-0.45 mm.
With reference to the first aspect, in a possible implementation manner, the electrode includes an electrode tab and an electrode lead connected to the electrode tab, and at least a portion of the electrode tab is accommodated in the positioning slot and electrically connected to the conductive ceramic substrate; the electrode lead extends to the outside of the conductive ceramic base along the guide groove.
With reference to the first aspect, in a possible embodiment, before the taking the conductive ceramic substrate with the surface having the recessed electrode bonding groove, the method further includes:
carrying out surface polishing treatment on the conductive ceramic matrix;
and (3) placing the polished conductive ceramic matrix in a cleaning solution for ultrasonic cleaning.
In a possible embodiment in combination with the first aspect, the thickness of the welding paste in the electrode welding groove is 0.1mm to 0.3 mm.
With reference to the first aspect, in one possible embodiment, the method satisfies at least one of the following features a to c:
a. the viscosity of the welding slurry is 100 Pa.s-180 Pa.s;
b. the average grain diameter of alloy components in the welding slurry is 10-50 mu m;
c. the thickness of the welding slurry in the electrode welding groove is 0.1 mm-0.3 mm.
With reference to the first aspect, in one possible embodiment, the method satisfies at least one of the following features a to c:
a. the drying temperature is 150-250 ℃;
b. the drying time is 0.5-2 h;
c. the drying mode is air blast drying.
With reference to the first aspect, in one possible embodiment, the method satisfies at least one of the following features a to d:
a. the temperature rise rate of the staged temperature rise sintering is 8-12 ℃/min;
b. the step-type temperature-rising sintering is carried out in a vacuum environment, and the vacuum degree of the vacuum environment is less than or equal to 1.0 multiplied by 10- 2Pa；
c. The temperature of the stage type temperature rise sintering is between room temperature and 860 ℃;
d. the step-type heating sintering comprises three-stage heating treatment, wherein the temperature is increased to 290-320 ℃ in the first stage, and the temperature is kept for 13-18 min; in the second stage, the temperature is raised to 720-750 ℃, and the temperature is kept for 13-18 min; in the third stage, the temperature is raised to 830-860 ℃, and the temperature is kept for 8-12 min.
In a second aspect, the present application provides a heat-generating body produced by the welding method according to the first aspect.
In a third aspect, the present application provides an aerosol-generating device comprising the heat-generating body according to the second aspect.
Compared with the prior art, the technical scheme provided by the application has the following beneficial effects at least:
according to the welding treatment method of the heating body, the electrode welding groove is formed on the surface of the conductive ceramic substrate, so that on one hand, the welding area of the electrode and the conductive ceramic is greatly increased; on the other hand, pack welding slurry to the electrode welding inslot, utilize the bond strength of welding slurry and the gravity of electrode slice self, can realize the preliminary fixed of conductive ceramic base member and electrode slice through local pressing, realize quick location, dry and the sintering of staged intensification of rethread, improve electrode slice and conductive ceramic base member welding strength, improve the stability in use of heat-generating body, in heat-generating body heating process, can avoid electrode slice thermal stress effect to produce not hard up or drop, can effective control heat-generating body resistance variation in the heating use. In addition, the electrode is buried in the welding groove, can be well fixed, and is not easy to loosen or fall off.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive labor.
FIG. 1 is a schematic flow chart showing a welding treatment method of a heat-generating body according to an embodiment of the present application;
FIG. 2a is a schematic structural view of a conductive ceramic matrix according to an embodiment of the present application;
FIG. 2b is a schematic structural diagram of a conductive ceramic matrix according to an embodiment of the present application;
FIG. 2c is a schematic view of another structure of the conductive ceramic matrix according to an embodiment of the present application;
FIG. 3a is a cross-sectional view of an electrically conductive ceramic substrate provided in accordance with an embodiment of the present application;
FIG. 3b is an enlarged view of a portion of area A in a cross-sectional view of a conductive ceramic base provided in an embodiment of the present application;
FIG. 4a is an exploded schematic view of a heat-generating body provided in another embodiment of the present application;
FIG. 4b is an exploded schematic view of a heat-generating body provided in another embodiment of the present application;
FIGS. 5a and 5b are schematic views showing the state of the heating element prepared in comparative example 1 before and after electrode cycling, respectively.
Detailed Description
For better understanding of the technical solutions of the present invention, the following detailed descriptions of the embodiments of the present invention are provided with reference to the accompanying drawings.
It should be understood that the described embodiments are only some embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in the examples of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Furthermore, the features, operations, or characteristics described in the specification may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification and drawings are for the purpose of describing certain embodiments only and are not intended to imply a required sequence unless otherwise indicated where such sequence must be followed.
The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning. The term "coupled" as used herein includes both direct and indirect connections, unless otherwise indicated.
The term "aerosol-generating device" as used herein refers to an aerosol-generating article which is heated to a temperature below its combustion temperature to generate an aerosol, thereby avoiding the generation of noxious, harmful substances as a result of the combustion of the aerosol-generating article.
FIG. 1 is a schematic flow chart of a welding treatment method of a heat-generating body according to an embodiment of the present application, as shown in FIG. 1,
step S10, a conductive ceramic substrate with a sunken electrode welding groove on the surface is taken, welding slurry is filled into the electrode welding groove, and alloy components in the welding slurry comprise at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy and silver-palladium-titanium alloy;
step S20, arranging an electrode in the electrode welding groove, and pressing the electrode to enable at least part of the welding slurry to overflow to the surface of the electrode;
and step S30, drying the preliminarily fixed conductive ceramic base body and the electrode, carrying out staged heating sintering, and cooling to obtain the heating element.
In the scheme, the electrode welding groove is formed on the surface of the conductive ceramic substrate, so that on one hand, the welding area of the electrode and the conductive ceramic is greatly increased; on the other hand, pack welding slurry to electrode welding inslot, utilize welding slurry's adhesive strength and electrode self's gravity, can realize the preliminary fixed of conductive ceramic base member and electrode through local pressing, realize quick location, dry and the sintering of stage formula intensification of rethread, improve electrode and conductive ceramic base member welding strength, improve the stability in use of heat-generating body, in heat-generating body heating process, can avoid electrode thermal stress effect to produce not hard up or drop, can effective control heat-generating body resistance variation in the heating use. In addition, the electrode is buried in the welding groove, is well fixed by the positioning groove and is not easy to loosen or fall off.
The present solution is described in detail below by means of specific examples:
before step S10, a conductive ceramic base body having a recessed electrode bonding groove on the surface thereof is obtained by dry press molding a conductive ceramic base body material.
The conductive ceramic matrix material comprises at least one of silicon carbide, silicon nitride, aluminum oxide, silicon oxide, titanium diboride, titanium carbide and zirconium diboride. Preferably, the conductive ceramic matrix material is a composite material of silicon carbide and titanium diboride. The conductive ceramic matrix material is a novel material with ionic conduction and electron/hole conduction in the ceramic material, and has the characteristics of oxidation resistance, corrosion resistance, high temperature resistance, long service life and the like. The heating body made of the conductive ceramic matrix material can uniformly release heat in the repeated heating process, avoids local overheating of the non-combustible product, generates pungent tastes such as scorch and the like, and can prolong the service life of the heating body.
FIG. 2a is a schematic structural diagram of a conductive ceramic matrix according to an embodiment of the present application, and FIG. 2b is a schematic structural diagram of a conductive ceramic matrix according to another embodiment of the present application; as shown in fig. 2a and 2b, the conductive ceramic substrate 1 may be a long sheet, and the thickness of the conductive ceramic substrate 1 may be 0.3 to 2mm, specifically, 0.5mm, 0.7mm, 0.9mm, 1mm, 1.2mm, 1.5mm, 1.8mm, or 2mm, and the like, which is not limited herein; the thickness of the conductive ceramic base 1 is preferably 1 mm.
The resistivity of the conductive ceramic matrix 1 is more than or equal to 1.0 multiplied by 10-6Omega. m, specifically 1.0X 10-6Ω·m、1.5×10-5Ω·m、1.1×10-5Ω·m、1.2×10-4Ω · m, etc., without limitation.
It should be noted that the thickness of the conductive ceramic substrate is relatively thin, the generated thermal resistance is relatively large, and the solder joint is particularly easy to age, so that the soldering difficulty is high, and the requirement on the soldering strength is relatively high. In addition, the conductive ceramic with smaller resistivity of the conductive ceramic matrix is easier to weld, and the conductive ceramic has high resistivity, so the requirements on welding strength and anti-oxidation and anti-aging capability are higher. Therefore, by forming the recessed electrode welding groove on the surface of the conductive ceramic substrate, the welding area between the electrode and the conductive ceramic can be increased, and the welding strength can be improved.
The conductive ceramic base 1 includes an insertion portion 11 and a connection portion 12, and the insertion portion 11 and the connection portion 12 are integrally formed. Wherein the insert 11 is for insertion into an aerosol-forming substrate of an aerosol-generating device such that heat from the heat-generating body can cause the aerosol-forming substrate to form an aerosol. In this embodiment, the insertion portion 11 is a V-shaped tip, which facilitates insertion of the heating element into the aerosol-forming substrate. The edges of the insert 11 are sharpened to further facilitate insertion into the aerosol-forming substrate. The connecting portion 12 is used for mounting the heating element in the aerosol generating device shell, and specifically, the bottom of the conductive ceramic substrate 1 is provided with two connecting portions 12 protruding to both sides respectively, so that the heating element is clamped in the mounting cavity of the aerosol generating device shell. The conductive ceramic base 1 is obtained by dry-pressing a conductive ceramic material with a mold and sintering the same.
Further, in order to form the conductive loop, the conductive ceramic base 1 is provided with a through groove 13 along the longitudinal direction, and the through groove 13 enables the conductive ceramic base 1 to form the loop in the energized state. The through grooves 13 are also formed by dry pressing of a mold, and insulating materials can be filled in the through grooves 13.
Wherein, the electrode welding groove 2 extends to the edge of the conductive ceramic substrate 1, thereby facilitating the extraction of the electrode 3. Specifically, the depth of the electrode bonding groove 2 is 0.25mm to 0.45mm, specifically, 0.25mm, 0.26mm, 0.27mm, 0.28mm, 0.29mm, 0.30mm, 0.31mm, 0.32mm, 0.33mm, 0.34mm, 0.35mm, 0.40mm, or 0.45mm, and the like, and may be any other value within the above range, which is not limited herein.
In the present embodiment, as shown in fig. 2a or fig. 2b, two electrode welding grooves 2 are symmetrically disposed on the surface of the conductive ceramic substrate 1, and the two electrode welding grooves 2 are a positive electrode welding groove and a negative electrode welding groove, respectively. Specifically, two symmetrically arranged electrode welding grooves 2 are respectively arranged on two connecting portions 12 of the conductive ceramic substrate 1, so as to be conveniently connected with a power supply of the aerosol generating device. The distance between the two electrode welding grooves 2 which are symmetrically arranged is 5.65 mm-5.75 mm, specifically 5.65mm, 5.66mm, 5.67mm, 5.68mm, 5.7mm, 5.72mm, 5.75mm and the like, and the positive electrode welding groove and the negative electrode welding groove are respectively arranged at two sides of the conductive ceramic matrix 1, so that the interference of the positive electrode and the negative electrode can be avoided, and the heat generated by the electrodes can be favorably dissipated.
Further, the electrode welding groove 2 comprises a positioning groove 21 and a guide groove 22 communicated with the positioning groove 21, and at least part of the electrode 3 is contained in the positioning groove 21, so that the electrode 3 can be conveniently and quickly positioned. The guide groove 22 is communicated with the positioning groove 21 and extends to one end of the conductive ceramic substrate 1, and the guide groove 22 is used for accommodating an electrode lead of the electrode 3, so that the connection stability of the electrode can be improved. The positioning groove 21 of the electrode welding groove 2 may be any one of square, rectangular, diamond, circular, oval, and the like. The guide groove 22 of the electrode welding groove 2 may be a circular arc, a square, or the like. Specifically, the positioning groove 21 may be square, the width of the positioning groove 21 may be 1.55mm to 1.65mm, specifically 1.55mm, 1.58mm, 1.6mm, 1.62mm, or 1.65mm, and the width of the guide groove 22 may be 0.35mm to 0.45mm, specifically 0.35mm, 0.38mm, 0.4mm, 0.42mm, or 0.45mm, and the like, which is not limited herein.
As shown in fig. 2b, the positioning groove 21 may be circular, the diameter of the positioning groove 21 may be 1.45mm to 1.55mm, specifically 1.45mm, 1.48mm, 1.5mm, 1.52mm, or 1.55mm, and the width of the guide groove 22 may be 0.35mm to 0.45mm, specifically 0.35mm, 0.38mm, 0.4mm, 0.42mm, or 0.45mm, but is not limited thereto.
In other embodiments, as shown in fig. 2c, the electrode bonding groove 2 may also extend directly to the edge of the conductive ceramic base, i.e. without the guiding groove 22.
As shown in fig. 3a to 3b, the positioning groove 21 of the electrode soldering groove includes a bottom surface 211 and a side guide surface 212 having a slope, wherein the side guide surface 212 having a slope connects the bottom surface 211 and the surface 101 of the conductive ceramic substrate 1, and the design of the side guide surface 212 is advantageous for quick positioning of the electrode during mounting and for improving the assembly efficiency. Specifically, the angle between the side guide surface 212 and the bottom surface 211 is greater than 90 degrees, and may be, for example, 120 degrees, 130 degrees, 140 degrees, and the like, which is not limited herein. The side guide surface 212 may be a flat surface or an arc surface.
Prior to step S10, the method further comprises:
carrying out surface polishing treatment on the conductive ceramic matrix 1;
and (3) putting the polished conductive ceramic substrate 1 into a cleaning solution for ultrasonic cleaning.
It is understood that the surface of the conductive ceramic substrate is cleaned by polishing and ultrasonic washing.
In a specific embodiment, the conductive ceramic base 1 obtained by dry press molding is subjected to polishing treatment using an alumina polishing liquid. The average particle diameter of the metal particles in the alumina polishing slurry is 1 μm to 3 μm, and specifically, it may be 1 μm, 1.5 μm, 2 μm, 2.2 μm, 2.5 μm, 2.8 μm, or 3 μm, and the like, and is not limited thereto.
The cleaning liquid adopted in ultrasonic cleaning is acetone or ethanol liquid with the mass ratio of more than 99%, and dirt on the surface of the conductive ceramic matrix can be effectively removed. The ultrasonic cleaning time is 5-15 min, and dirt can be effectively removed.
Step S10, a conductive ceramic substrate with a sunken electrode welding groove on the surface is taken, welding slurry is filled into the electrode welding groove, and alloy components in the welding slurry comprise at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy and silver-palladium-titanium alloy.
The welding slurry can be extruded and filled into the electrode welding groove through the needle tube, and the operation is simple and rapid. The alloy component in the soldering paste may be at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy, and silver-palladium-titanium alloy. The wettability of the solder paste can be adjusted by adjusting the mass ratio of silver to copper. The indium metal in the silver, copper, titanium and indium is beneficial to reducing the melting point of alloy components and improving the welding stability of the electrode and the conductive ceramic. Illustratively, the silver-copper-titanium alloy may be Ag-Cu-Ti2The melting point is 780-805 ℃; the silver-copper-titanium alloy can also be Ag-Cu-Ti4.5The melting point is 780-810 ℃; the Ag-Cu-Ti-In alloy can also be Ag-Cu-In-Ti3The melting point is 540-650 ℃. It will be appreciated that the melting points of the alloy components can be adjusted by adjusting the mass ratios of the respective elemental metals in the alloy.
Further, the viscosity of the solder paste is 100Pa · s to 180Pa · s, and specifically may be 100Pa · s, 110Pa · s, 120Pa · s, 130Pa · s, 140Pa · s, 160Pa · s, 180Pa · s, or the like, and is not limited thereto. When the viscosity of the welding slurry is more than 180 Pa.s, the operation is not easy; when the viscosity of the welding paste is less than 100Pa s, the initial adhesion and fixation of the electrode and the conductive ceramic substrate are not facilitated.
The average grain diameter of the alloy component in the welding paste is 10 μm to 50 μm, and specifically may be 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, or 50 μm, and the like, and is not limited herein.
In the present embodiment, the thickness of the welding paste in the electrode welding groove 2 is 0.1mm to 0.3mm, and may be, for example, 0.1mm, 0.15mm, 0.18mm, 0.2mm, 0.22mm, 0.25mm, or 0.3mm, and is not limited thereto. The thickness of the welding slurry is too thick, the electrode is easy to protrude out of the surface of the conductive ceramic base body after being welded with the conductive ceramic base body, and the space for subsequent installation is easy to be influenced. The thickness of the welding slurry is too thin, the welding slurry is not easy to overflow to the surface of the electrode, and the bottom of the electrode is only welded with the conductive ceramic substrate, so that the welding strength is not improved.
Step S20, arranging an electrode in the electrode welding groove, and pressing the electrode to enable at least part of the welding slurry to overflow to the surface of the electrode;
FIG. 4a is an exploded schematic view of a heat-generating body provided in another embodiment of the present application, and FIG. 4b is an exploded schematic view of the heat-generating body provided in another embodiment of the present application; as shown in fig. 4a and 4b, the electrode 3 includes an electrode tab 31 and an electrode lead 32 connected to the electrode tab 31. At least part of the electrode sheet 31 is accommodated in the electrode welding groove 2 and is electrically connected with the conductive ceramic substrate 1; the electrode leads 32 extend to the outside of the conductive ceramic base 1.
When the electrode tab 31 is accommodated in the electrode welding groove 2, the electrode tab 31 may be completely accommodated in the positioning groove 21 of the electrode welding groove 2, or may be partially accommodated in the positioning groove 21 of the electrode welding groove 2, for example, a portion of the electrode tab 31 protrudes from the positioning groove 21.
Specifically, the electrode 3 is a copper electrode or a silver electrode, and at least one of a silver film, a gold film, or a nickel film is formed on the surface of the copper electrode or the silver electrode. The surface of the copper electrode or the silver electrode is coated with the film, so that the high-temperature oxidation of the electrode can be slowed down, and the service life of the electrode is prolonged.
Through slightly pressing, electrode slice 31 can be fixed with the bonding of welding thick liquids, in this embodiment, makes the welding thick liquids spill over to the surface of electrode slice 31 through pressing for the welding thick liquids can be filled to electrode slice around, can improve the welding strength of electrode slice 31 and conductive ceramic base member.
And step S30, drying the preliminarily fixed conductive ceramic base body and the electrode, carrying out staged heating sintering, and cooling to obtain the heating element.
The drying temperature is 150-250 ℃, specifically 180 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 245 ℃ or 250 ℃, and the drying time is 0.5-2 h, specifically 0.5h, 0.6h, 0.7h, 0.8h, 1.0h, 1.2h, 1.5h, 1.8h or 2.0h, and the like, which is not limited herein.
In a specific embodiment, the drying mode is air-blast drying. The assembled conductive ceramic substrate may be placed on a quartz or graphite boat and dried in a forced air drying oven.
Performing staged heating sintering on the dried conductive ceramic matrix and the electrode plate, wherein the staged heating sintering is performed in a vacuum environment, and the vacuum degree of the vacuum environment is less than or equal to 1.0 multiplied by 10-2Pa, specifically 1.0X 10-3Pa、5.0×10- 3Pa、7.0×10-4Pa、2.0×10-4Pa、1.4×10-3Pa, etc., and are not limited thereto.
The temperature range of the sintering peak of the stepwise temperature rise is 650 to 860 ℃, and the sintering peak temperature is 650 ℃, 680 ℃, 720 ℃, 750 ℃, 780 ℃, 820 ℃ or 860 ℃ according to the selection of the solder, and other values in the range can be of course. The temperature rise rate of the staged temperature rise sintering is 8-12 ℃/min, specifically 8 ℃/min, 9 ℃/min, 10 ℃/min, 11 ℃/min or 12 ℃/min, and the like, and can be other values within the range.
Specifically, the step-type heating sintering comprises three-stage heating treatment, wherein the temperature is increased to 290-320 ℃ in the first stage, and the temperature is kept for 13-18 min; in the second stage, the temperature is raised to 720-750 ℃, and the temperature is kept for 13-18 min; in the third stage, the temperature is raised to 830-860 ℃, and the temperature is kept for 5-12 min. Through the staged heating sintering, the firm welding of the conductive ceramic substrate and the electrode plate can be fully ensured, and the welding strength is improved.
And cooling the sintered conductive ceramic substrate to obtain a heating body, wherein the cooling can be furnace cooling, natural cooling or rapid cooling, and is not limited herein.
The following examples are intended to illustrate the invention in more detail. The embodiments of the present invention are not limited to the following specific embodiments. The present invention can be modified and implemented as appropriate within the scope of the main claim.
Example 1
(1) Dry-pressing conductive ceramic matrix material formed by compounding silicon carbide and titanium diboride to obtain conductive ceramic matrix with thickness of 1mm, wherein the resistivity of the conductive ceramic matrix is 3.0 multiplied by 10-5Omega.m. The conductive ceramic base body comprises two electrode welding grooves which are symmetrically arranged, the electrode welding grooves are square grooves, the width of each electrode welding groove is 0.6mm, and the depth of each electrode welding groove is 0.3 mm.
(2) And polishing the surface of the conductive ceramic matrix by using an alumina polishing solution, and ultrasonically cleaning the polished conductive ceramic matrix in an acetone solution with the mass of more than 99% for 10 min.
(3) And filling the welding slurry containing the silver-copper-titanium alloy into the electrode welding groove, and controlling the thickness of the welding slurry to be 0.2 mm.
(4) Arranging a copper electrode plate in the electrode welding groove, and pressing the electrode plate to enable at least part of welding slurry to overflow to the surface of the electrode plate;
(5) placing the preliminarily fixed conductive ceramic substrate and the electrode plate in a forced air drying oven for drying, controlling the temperature in the forced air drying oven to be 220 ℃, and controlling the drying time to be 2 hours; and then placing the mixture in a vacuum sintering furnace, heating to 300 ℃ at the speed of 10 ℃/min, preserving heat for 15min, heating to 750 ℃ and preserving heat for 15min, heating to 860 ℃ and preserving heat for 10min, and cooling the welded conductive ceramic substrate along with the furnace to obtain the heating element.
Example 2
Unlike example 1, the conductive ceramic base was obtained by dry press molding using a conductive ceramic base material containing silicon nitride.
Example 3
Different from the embodiment 1, the welding slurry containing the silver-copper-titanium-indium alloy is filled into the electrode welding groove; and in the sintering process, heating to 300 ℃ at the speed of 8 ℃/min, preserving heat for 15min, heating to 550 ℃ and preserving heat for 15min, heating to 700 ℃ and preserving heat for 10min, and cooling the welded conductive ceramic matrix along with a furnace to obtain the heating element.
Example 4
Unlike example 1, the thickness of the soldering paste was controlled to 0.2mm, and the sintering peak temperature was adjusted to 820 ℃.
Comparative example 1
Unlike example 1, a conventional silver paste containing glass frit was filled into the electrode soldering bath, and the thickness of the soldering paste was controlled to be 0.2 mm.
Comparative example 2
Unlike example 1, the thickness of the solder paste was controlled to be 0.05 mm.
Comparative example 3
Unlike example 1, the surface of the conductive ceramic substrate was directly coated with a solder paste containing silver, copper, and titanium alloy without providing an electrode soldering bath.
The heating elements obtained in examples 1 to 4 and comparative examples 1 to 3 were subjected to a resistance value test and a heat cycle performance test.
The thermal cycle performance test is as follows:
heating the heating element to 350 ℃ from room temperature within 10s, preserving the temperature for 3min, then naturally cooling for 3min, recording as 1 time, repeating the cycle for 600 times, and then testing the resistance value of the heating element, wherein the test results are shown in the following table 1:
TABLE 1
FIGS. 5a to 5b are schematic views showing the state before and after the electrode cycle of the heating element manufactured in comparative example 1; as shown in fig. 5a and 5b, in comparative example 1, the conventional silver paste was used, and the prepared electrode exhibited a cracking phenomenon at the junction between the electrode and the conductive ceramic base after the cycle, and the electrode was loose. And the resistance change value of the heating element is greatly improved compared with that of the embodiment 1, because the welding point of the electrode is easy to loose under the action of thermal stress in the cyclic heating use process of the traditional silver paste, and the resistance is easy to increase. In the embodiment 1 of the present application, the welding slurry containing silver-copper-titanium alloy is adopted, and the electrode sheet of the electrode is accommodated in the electrode welding groove, so that the welding strength can be improved, the stability of the electrode can be improved, the resistance change value is only 6.2%, and the resistance change amount of the heating element in the heating use process can be effectively controlled in the embodiment 1.
The thickness of the welding paste in the electrode welding groove of comparative example 2 is only 0.05mm, the welding strength of the electrode sheet and the conductive ceramic substrate is reduced due to too little welding paste, and the welding point of the electrode is easily loosened due to the action of thermal stress, so that the resistance is easily increased.
Comparative example 3 the welding paste containing silver, copper and titanium alloy is directly coated on the surface of the conductive ceramic substrate, the limiting and fixing effect of the electrode welding groove is avoided, the yield of the electrode welding spot is greatly reduced, about 30% of electrodes can fall off and become loose, and the resistance value fluctuates abnormally in the heating cycle process.
According to the test data of embodiments 1 to 3, it can be known that forming the electrode welding groove on the surface of the conductive ceramic base can greatly increase the welding area between the electrode and the conductive ceramic, improve the welding strength between the electrode plate and the conductive ceramic base, improve the stability of the heating element, avoid the loosening or falling of the electrode plate due to the action of thermal stress during the heating process of the heating element, and effectively control the resistance variation of the heating element during the heating process. In addition, the electrode is buried in the welding groove, can be well fixed, and is not easy to loosen or fall off.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the 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 (12)
1. A welding treatment method of a heating body is characterized by comprising the following steps:
taking a conductive ceramic substrate with a sunken electrode welding groove on the surface, and filling welding slurry into the electrode welding groove, wherein the alloy component in the welding slurry comprises at least one of silver-copper-titanium alloy, silver-copper-titanium-indium alloy and silver-palladium-titanium alloy;
disposing an electrode in the electrode welding groove, pressing the electrode such that at least a portion of the welding paste overflows to a surface of the electrode;
and drying the preliminarily fixed conductive ceramic substrate and the electrode, carrying out staged heating sintering, and cooling to obtain the heating element.
2. The welding processing method according to claim 1, characterized in that the method satisfies at least one of the following characteristics a to c:
a. the conductive ceramic matrix material comprises at least one of silicon carbide, silicon nitride, aluminum oxide, silicon oxide, titanium diboride, titanium carbide and zirconium diboride;
b. the thickness of the conductive ceramic matrix is 0.3 mm-2 mm;
c. the resistivity of the conductive ceramic matrix is more than or equal to 1.0 multiplied by 10-6Ω·m。
3. The welding processing method according to claim 1, wherein the electrode is a copper electrode or a silver electrode, and at least one of a silver film, a gold film, and a nickel film is formed on a surface of the copper electrode or the silver electrode.
4. The welding treatment method according to claim 1, wherein two electrode welding grooves are symmetrically formed on the surface of the conductive ceramic substrate, and the two electrode welding grooves are a positive electrode welding groove and a negative electrode welding groove.
5. The welding process according to claim 1 or 2, characterized in that the process satisfies at least one of the following characteristics a to c:
a. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove;
b. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove, the positioning groove comprises a bottom surface and a side guide surface with a slope, and the side guide surface with the slope is connected with the bottom surface and the surface of the conductive ceramic substrate;
c. the electrode welding groove comprises a positioning groove and a guide groove communicated with the positioning groove, and the depth of the electrode welding groove is 0.25-0.45 mm.
6. The welding process method according to claim 5, wherein the electrode includes an electrode tab and an electrode lead connected to the electrode tab, and at least a portion of the electrode tab is received in the positioning groove and electrically connected to the conductive ceramic base; the electrode lead extends to the outside of the conductive ceramic base along the guide groove.
7. The soldering processing method according to claim 1, wherein before the taking of the conductive ceramic base having the electrode soldering groove with the depression on the surface, the method further comprises:
carrying out surface polishing treatment on the conductive ceramic matrix;
and (3) placing the polished conductive ceramic matrix in a cleaning solution for ultrasonic cleaning.
8. The welding processing method according to claim 1, characterized in that the method satisfies at least one of the following characteristics a to c:
a. the viscosity of the welding slurry is 100 Pa.s-180 Pa.s;
b. the average grain diameter of alloy components in the welding slurry is 10-50 mu m;
c. the thickness of the welding slurry in the electrode welding groove is 0.1 mm-0.3 mm.
9. The welding processing method according to claim 1, characterized in that the method satisfies at least one of the following characteristics a to c:
a. the drying temperature is 150-250 ℃;
b. the drying time is 0.5-2 h;
c. the drying mode is air blast drying.
10. The welding process according to claim 1, wherein the method satisfies at least one of the following characteristics a to d:
a. the temperature rise rate of the staged temperature rise sintering is 8-12 ℃/min;
b. the step-type temperature-rising sintering is carried out in a vacuum environment, and the vacuum degree of the vacuum environment is less than or equal to 1.0 multiplied by 10-2Pa；
c. The temperature of the stage type temperature rise sintering is between room temperature and 860 ℃;
d. the step-type heating sintering comprises three-stage heating treatment, wherein the temperature is increased to 290-320 ℃ in the first stage, and the temperature is kept for 13-18 min; in the second stage, the temperature is raised to 720-750 ℃, and the temperature is kept for 13-18 min; in the third stage, the temperature is raised to 830-860 ℃, and the temperature is kept for 5-12 min.
11. A heat-generating body characterized by being produced by the welding treatment method according to any one of claims 1 to 10.
12. An aerosol-generating device comprising the heat-generating body according to claim 11.
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Application publication date: 20210903 |