CN112167727A

CN112167727A - Heating element, preparation method thereof and electronic smoking set

Info

Publication number: CN112167727A
Application number: CN201910599004.9A
Authority: CN
Inventors: 周宏明; 刘宇嵘; 程振乾; 张蛟; 金鹤
Original assignee: Shenzhen Smoore Technology Ltd
Current assignee: Shenzhen Smoore Technology Ltd
Priority date: 2019-07-04
Filing date: 2019-07-04
Publication date: 2021-01-05
Anticipated expiration: 2039-07-04

Abstract

The invention relates to a heating element, a preparation method thereof and an electronic smoking set. The heating body comprises a substrate, a heating layer and a protective layer, wherein the heating layer is arranged on the substrate, the protective layer is arranged on one side, away from the substrate, of the heating layer, and the heating layer is made of silver alloy. The heating body generates heat stably.

Description

Heating element, preparation method thereof and electronic smoking set

Technical Field

The invention relates to the technical field of electronic cigarettes, in particular to a heating body, a preparation method of the heating body and an electronic smoking set.

Background

An electronic cigarette is an electronic product simulating a cigarette, has the appearance and taste similar to a cigarette, and generally does not contain tar, suspended particles and other harmful ingredients in the cigarette.

The electronic cigarette mainly releases tobacco tar or tobacco through heating of a heating body of the electronic smoking set, so that aromatic substances and nicotine in the tobacco tar or the tobacco are released, smoke close to the taste of real cigarettes is generated, and meanwhile, the generation of harmful substances is reduced. However, the conventional heat generating element often has a problem of unstable heat generation.

Disclosure of Invention

Accordingly, it is necessary to provide a heat generating body which generates heat stably.

The heating body comprises a substrate, a heating layer and a protective layer, wherein the heating layer is arranged on the substrate, the protective layer is arranged on one side, away from the substrate, of the heating layer, and the heating layer is made of silver alloy.

A large number of researches show that when a single metal such as silver is used as a heating layer of a heating body, the pure metal is easy to generate electrochemical migration phenomenon, so that the heating layer generates heat unevenly and is easy to short circuit. The heating body comprises a substrate, a heating layer and a protective layer, the heating layer is made of silver alloy, the silver alloy can form continuous solid solution, the electrochemical migration resistance of silver is enhanced, the heating layer can generate heat more uniformly, short circuit is not easy to occur, and the circulating heating stability of the heating body is improved. In addition, the protective layer is laminated on the heating layer, so that the heating layer is isolated from the external environment, the influence of the external environment on the heating of the heating layer is reduced, and the circulating thermal stability of the heating body is further enhanced.

In one embodiment, the material of the protective layer is selected from ZrO₂And Al₂O₃At least one of; and/or

The thickness of the protective layer is 2-5 μm.

In one embodiment, the material of the heat generating layer is selected from at least one of AgAu, AgPd and AgPt; and/or

The thickness of the heating layer is 1-6 μm.

In one embodiment, the heat-generating layer is laminated on one side of the transition layer far away from the substrate, and the material of the transition layer is selected from at least one of Ti or ZrNi; and/or

The thickness of the transition layer is 50 nm-200 nm.

In one embodiment, the material of the heating layer is AgPd, and the thickness of the heating layer is 1-3.5 μm; the protective layer is made of ZrO₂The thickness of the protective layer is 2-5 μm.

In one embodiment, the side of the protection layer far away from the heat generating layer is formed with a mastoid-like structure.

In one embodiment, the heat generating device further comprises a conductive layer, wherein the conductive layer is arranged on one side of the substrate close to the heat generating layer and is electrically connected with the heat generating layer.

In one embodiment, the substrate further comprises a bonding layer, the bonding layer is laminated between the substrate and the conductive layer, and the material of the bonding layer is at least one selected from titanium, nickel, tantalum and nickel alloy

A method for preparing a heating element comprises the following steps:

depositing a heating layer on a substrate, wherein the heating layer is made of silver alloy; and

and forming a protective layer on one side of the heat generating layer far away from the substrate.

An electronic smoking set comprises the heating element or the heating element prepared by the preparation method.

Drawings

FIG. 1 is a schematic view of a structure of a heat generating body according to an embodiment;

FIG. 2 is a schematic view showing a structure of a heat-generating body according to another embodiment;

fig. 3 is a substrate deposited with a heat generating layer prepared by step S130;

fig. 4 is a substrate deposited with a conductive layer prepared by step S150;

fig. 5 is a substrate deposited with a protective layer prepared by step S160;

FIG. 6 is a schematic view of an electronic smoking article and use according to one embodiment;

FIG. 7 is a SEM image of example 2 before treatment;

FIG. 8 is a SEM image of the treated steel sheet of example 2.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Some embodiments of the invention are presented in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

Referring to fig. 1, a heat generating body 100 according to an embodiment includes a base 110, a transition layer 120, a heat generating layer 130, a bonding layer 140, and a conductive layer 150. The heating element 100 has strong circulating heating stability and is applied to electronic smoking set.

The substrate 110 is a carrier of other film layers on the heating element 100. Specifically, the substrate 110 is a ceramic substrate. Further, the substrate 110 is a zirconia ceramic substrate or an alumina ceramic substrate. Further, the substrate 110 is a zirconia ceramic substrate. The zirconia ceramics have high strength and hardness, high temperature resistance and high chemical stability. Of course, in other embodiments, the material of the substrate 110 is not limited to ceramic, but may be other high temperature resistant materials, such as stainless steel. Compared with a stainless steel substrate, the zirconia ceramic substrate has high hardness and good toughness, is not easy to break when inserted into a smoke bomb, can avoid the corrosion of organic matters such as nicotine and the like generated in the smoking process to the substrate due to high temperature resistance and corrosion resistance, is non-conductive, avoids the manufacture of an insulating layer, and simplifies the process flow.

In the illustrated embodiment, the substrate 110 is substantially V-shaped sheet. Of course, in other embodiments, the shape of the substrate 110 is not limited to the V-shaped sheet, but may be other shapes, such as a circular sheet, a rectangular sheet, a bar, and the like.

The transition layer 120 is stacked on the substrate 110. The transition layer 120 can improve the heat generation stability of the heat generating body 100. It is understood that a material capable of forming a chemical bond (e.g., a metallic bond, a covalent bond, or an ionic bond) between the substrate 110 and the heat generating layer 130 may be used as the material of the transition layer 120. Of course, in some embodiments, the bonding of the transition layer 120 to the substrate 110 is not limited to the chemical bond formed by the transition layer 120 and the substrate 110, and may be in other forms. For example, the inter-diffusion layer is formed by two substances to improve the bonding force of the transition layer 120 and the substrate 110.

The material of the transition layer 120 is a metal, a metal oxide, or an alloy. When the material of the transition layer 120 is metal, the material is nickel or titanium. When the material of the transition layer 120 is a metal oxide, the material is specifically zirconia or alumina. When the transition layer 120 is an alloy, a specific material is a titanium alloy or a nickel alloy. The thermal expansion coefficient of the alloy is between that of the substrate 110 and that of the heat generating layer 120, and a firm chemical bond can be formed between the alloy and the substrate 110 and the heat generating layer 120, so that the whole system generates heat more stably. Of course, the transition layer 120 can also improve the bonding capability of the substrate 110 and the heat generating layer 130, so that the heat generating layer 130 is not easy to fall off from the substrate 110.

Further, the material of the transition layer 120 includes at least one of Ti, ZrNi, ZrTi, NiCr, and TiN.

Further, the material of the transition layer 120 includes NiCr and at least one of ZrNi, ZrTi, and TiN. Further, the NiCr in the transition layer 120 gradually increases from the side close to the substrate 110 to the side far from the substrate 110. Specifically, the material of the transition layer 120 includes ZrNi and NiCr, and the NiCr in the transition layer 120 gradually increases from the side close to the substrate 110 to the side away from the substrate 110. The NiCr of the transition layer 120, which gradually increases from the side close to the substrate 110 to the side away from the substrate 110, enables better cyclic thermal stability of the heat generating layer 130.

The thickness of the transition layer 120 is 50nm to 200 nm. The transition layer 120 is too thin to provide a bonding force with the substrate 110, but the transition layer 120 for improving the bonding force is not too thick, and the excessively thick transition layer 120 not only causes a large internal stress but also wastes material. Further, the thickness of the transition layer 120 is 100nm to 200 nm. Setting the thickness of the transition layer 120 to be 100 nm-200 nm can buffer the stress between the substrate 110 and the heating layer 120, obviously improve the bonding force between the substrate 110 and the heating layer 120, and save the cost as much as possible.

The heat generating layer 130 is stacked on the transition layer 120 to generate heat. The material of the heating layer 130 is a material with low resistivity and stable structural performance after high-temperature heating. In the illustrated embodiment, the heat generating layer 130 is laminated on a side of the second transition layer 123 remote from the first transition layer 121. It is understood that in some embodiments, the transition layer may be omitted. When the transition layer is omitted, the heat generating layer 130 is laminated on the substrate 110.

The research shows that when the heating layer 130 is made of alloy, the oxidation of the heating layer 130 can be reduced, the electrochemical migration of metal of the heating layer 130 is reduced, the heating layer 130 is not easy to be short-circuited, and the heating body 100 can generate heat uniformly and stably. In addition, the other metals except the base body in the alloy can also adjust the resistance temperature coefficient of the heating system, so that the temperature control of the heating layer 130 is more accurate. Of course, when the material of the heat generating layer 130 is an alloy and the material of the transition layer 120 is also an alloy, the material of the heat generating layer 130 is different from the material of the transition layer 120.

Specifically, when the material of the heat generating layer 130 is an alloy, the material of the heat generating layer 130 includes a silver alloy. Through a great deal of research, the silver alloy, such as AgPd, AgAu, AgPt, can form a continuous solid solution, so that the heat generating layer 130 is more stable, thereby enhancing the electrochemical migration resistance of silver. For example, it was found that Ag-15% Pd and pure Ag electrodes were tested for electromigration failure time in a constant 400 deg.C high temperature environment at 200V DC voltage. When the electrochemical migration time is 241min, a silver bridge connecting the cathode and the anode is formed between the silver electrodes, and the anode edge of the silver electrode has mass loss and is not complete. However, at 241min of electrochemical migration time, no "silver bridge" was formed between the Ag-15% Pd electrodes, but it was observed that a silver-lustrous layer of material was deposited at the cathode edge, causing movement of the silver atoms due to the current transport and ultimately mass transport. When the electrochemical migration time is 472min, a silver bridge connecting the anode and the cathode is also formed between the Ag-15% Pd electrodes. The electrochemical migration failure life value of the Ag-15% Pd electrode is far higher than that of a silver electrode, and the addition of Pd plays a good role in inhibiting the electrochemical migration behavior of silver in a high-temperature dry environment.

On the other hand, the temperature coefficient of resistance of pure silver is high, about 3800 ppm/DEG C, and the temperature rise is relatively slow under the condition of constant voltage input. When the silver alloy is used as the heating layer 130, other metals can adjust the Temperature Coefficient of Resistance (TCR) of the material, the temperature rise speed is higher than that of pure silver when constant voltage is electrified, and high-precision temperature control can be realized.

Further, the material of the heat generating layer 130 is at least one selected from the group consisting of AgAu, AgPd, and AgPt. Further, the material of the heat generating layer 130 is selected from one of AgAu, AgPd, and AgPt. The AgAu, AgPd, and AgPt may form a continuous solid solution, so that the heat generating layer 130 is more stable, thereby enhancing the electrochemical migration resistance and high temperature stability of silver.

The thickness of the heat generating layer 130 is 1 μm to 6 μm. Further, the thickness of the heat generating layer 130 is 1 μm to 3.5 μm. Or the thickness of the heat generating layer 130 is 3 μm to 6 μm.

The bonding layer 140 is stacked on the substrate 110, and the bonding layer 140 serves to improve the bonding force between the conductive layer 150 and the substrate 110. In the illustrated embodiment, the bonding layer 140 is laminated to the substrate 110 on a side thereof adjacent to the transition layer 120.

Specifically, the material of the bonding layer 140 is selected from at least one of titanium, nickel, tantalum, and nickel alloy. Further, the material of the bonding layer 140 is selected from one of titanium, nickel, tantalum, and nickel alloy. Further, the material of the bonding layer 140 is titanium. The bonding layer 140 is formed of a titanium layer, so that stress between the substrate 110 and the conductive layer 150 is buffered, and the bonding force between the substrate 110 and the conductive layer 150 is significantly improved.

The thickness of the bonding layer 140 is 100nm to 500 nm. Further, the method is carried out. The thickness of the bonding layer 140 is 300nm to 400 nm. Setting the thickness of the bonding layer 140 to 300nm to 400nm enables the conductive layer 150 to have a strong bonding force with the substrate without affecting the conductive performance of the conductive layer 150.

The conductive layer 150 is disposed on the bonding layer 140 and connected to the heat generating layer 130. The conductive layer 150 is used to connect the heat generating layer 130 and the power supply, so that a current loop is formed among the conductive layer 150, the heat generating layer 130 and the power supply.

Specifically, the conductive layer 150 is stacked on the bonding layer 140. The conductive layer 150 has two end surfaces, one end surface of the conductive layer 150 is electrically connected to the heat generating layer 130, and the other end surface is electrically connected to a power supply. Further, the conductive layer 150 is connected to a power source by a solder lead. The conductive layer 150 is manufactured in a magnetron sputtering mode and formed in a lead soldering mode as a conductive electrode, high temperature is not needed, and process efficiency is improved.

The material of the conductive layer 150 is selected from one of silver, copper, aluminum, and gold.

The thickness of the conductive layer 150 is 1 μm to 4 μm. Further, the conductive layer 150 has a thickness of 1.5 to 2.5 μm. The thickness of the conductive layer 150 is set to 1.5 μm to 2.5 μm, which enables the power supply and the heat generating layer 130 to form a path, and the resistance value of the conductive layer 150 is minimized, and the material cost increases when the conductive layer 150 is too thick.

Of course, it is understood that in some embodiments, the bonding layer 140 may be omitted. When the bonding layer 140 is omitted, the conductive layer 150 is disposed on the substrate 110 and electrically connected to the heat generating layer 130. Further, the conductive layer 150 is stacked on one side of the substrate 110 close to the heat generating layer 130.

The heating body 100 comprises a substrate 110, a transition layer 120 and a heating layer 130, the heating layer 130 is made of silver alloy, and the silver alloy can form a continuous solid solution, so that the whole heating layer 130 is more stable, the electrochemical migration resistance of silver is enhanced, and the circulating heating stability of the heating body 100 is improved.

Referring to fig. 2 and 3, a heating element 200 according to another embodiment is substantially the same as the heating element 100, except that the heating element 200 further includes a protective layer 260; the base 210 is generally pentagonal in shape. Of course, it is understood that in other embodiments, the shape of the substrate 210 is not limited to a pentagonal sheet, but may be any other shape. Such as needle, rectangular sheet, rod, etc.

Specifically, the protection layer 260 is disposed on the heating layer 230, and is used for the protection layer 260 to isolate the heating layer 230 from the external environment (air, tobacco leaves, tobacco tar), so as to avoid the external environment from affecting the heating layer 230, and to enable the heating layer 230 to generate heat more stably. Specifically, the protection layer 260 prevents soot deposition on the heat generating layer 230, resulting in uneven heat generation. In addition, the protection layer 260 prevents oxygen and impurities from corroding the heat generating layer 230, and reduces damage to the heat generating layer 230, so that the heat generating layer 230 generates heat more uniformly and stably. In the illustrated embodiment, the protection layer 260 is laminated on a side of the heat generating layer 230 away from the substrate 210.

The material of the protective layer 260 includes ZrO₂、Al₂O₃And Si₃N₄At least one of (1). ZrO (ZrO)₂、Al₂O₃And Si₃N₄The surface hardness of the heating element 200 is high, the thermal stability is good, the cleaning is easy, the corrosion resistance is good, and the protection layer 260 can make the heating element have the advantages of high surface hardness, high stability, cleaning and corrosion resistance.

Further, the material of the protective layer 260 includes ZrO₂And Al₂O₃At least one of (1). ZrO (ZrO)₂And Al₂O₃The coefficient of expansion of the silver alloy of the heat generating layer 230 is well matched. ZrO 2 is mixed with₂And Al₂O₃At least one of the materials of the protection layer 260 can make the binding force between the protection layer 260 and the heat generating layer 230 strong, so that the protection layer 260 can be stably bound to the heat generating layer 230 and is not easily dropped from the heat generating layer 230, thereby exerting the function of the protection layer 260.

Further, the material of the protective layer 260 includes ZrO₂And Al₂O₃。

Further, a side of the protection layer 260 away from the heat generating layer 230 is formed with a mastoid-like structure. The papillary-like structure may reduce adhesion to the surface of protective layer 260, making dirt less likely to adhere to the surface of protective layer 260. Further, a plurality of mastoid-like structures are formed at intervals on the side of the protection layer 260 away from the heat-generating layer 230.

The thickness of the protective layer 260 is 2 μm to 5 μm. Furthermore, the sum of the thicknesses of the transition layer, the heat generating layer 230 and the protective layer 260 is 2 to 5 μm. The total thickness of the heating body 200 is thinner, and tobacco insertion is more convenient. Of course, the possibility of increasing the thickness of the substrate 210 is provided, which is more advantageous in improving the bending strength of the heat-generating body 200.

In the embodiment, the material of the transition layer is Ti or ZrNi, and the thickness of the transition layer is 50nm to 200 nm; the material of the heating layer 230 is AgPd, and the thickness of the heating layer 230 is 1-3.5 μm; the material of the protective layer 260 is ZrO₂The thickness of the protective layer 260 is 2 μm to 5 μm.

Since the heating element 200 has substantially the same structure as the heating element 100, the heating element 200 has similar effects. In addition, above-mentioned heat-generating body 200 still sets up protective layer 260, and the setting of protective layer 260 can make heat-generating body 200 generate heat more stably, and anti erosion capacity is strong, difficult deposit cigarette dirt, easy cleanness, improves heat-generating body 200's life.

Referring to fig. 3 to 5, the method for manufacturing the heating element 200 includes steps S110 to S170.

And step S110, preprocessing.

Specifically, the substrate 210 is acid-base cleaned, and then the surface of the substrate 210 is ion-cleaned. The substrate 210 is a ceramic substrate, and specifically, the substrate 210 is a zirconia ceramic substrate or an alumina ceramic substrate.

And (3) placing the substrate 210 cleaned by the acid and the alkali in a film plating machine, vacuumizing, and performing ion cleaning on the surface of the substrate 210. Further, the surface of the substrate 210 is ion-cleaned.

The purpose of the pretreatment is to remove various dirt such as grease, dust, oxide, etc. on the substrate 210 and to improve the bonding force between the subsequent film layer and the substrate 210.

Step S120, depositing a transition layer on the substrate 210.

Specifically, a transition layer is deposited on the pre-treated substrate 210 using a vapor deposition technique. Further, a transition layer mask is additionally arranged on the substrate 210 layer, and argon is introduced until the atmospheric pressure of the coating environment is 1 multiplied by 10^-1Pa～10×10^-1Pa, power density of ZrNi target material is 6W/cm²～8W/cm²Coating for 10-20 min at 18-26 deg.C to obtain the final productA transition layer. The material of the transition layer is ZrNi, and the thickness of the transition layer is 100 nm-200 nm.

In other embodiments, a plurality of targets may be co-sputtered, and the sputtering power of at least one of the targets is gradually increased, and the sputtering power of the other targets is gradually decreased, so as to form a transition layer with a concentration gradient. The transition layer having the concentration gradient can significantly improve the cyclic heating stability of the heating layer 230. Specifically, a ZrNi target and a NiCr target are adopted for double-target co-sputtering to form a transition layer with a concentration gradient. The specific operation is as follows: introducing argon until the working pressure of the coating is 2 multiplied by 10^-1Pa～10×10^-1Pa; the power density of the ZrNi target material is 6W/cm²～8W/cm²Plating the film for 1-5 min at the temperature of 18-26 ℃; reducing the power density of the ZrNi target material to 4W/cm²～6W/cm²Opening a NiCr target until the power density of the target is 0W/cm²～2W/cm²Coating for 0-5 min; then reducing the power density of the ZrNi target material to 2W/cm²～4W/cm²And increasing the power density of the NiCr target material to 2W/cm²～4W/cm²Coating for 1-5 min; then reducing the power density of the ZrNi target material to 0W/cm²～2W/cm²And increasing the power density of the NiCr target material to 4W/cm²～6W/cm²And plating the film for 1-5 min.

Further, argon is introduced until the atmospheric pressure of the coating environment is 5 multiplied by 10^-1Pa; the power density of the ZrNi target material is 6.5W/cm²～7.5W/cm²Coating for 3-5 min at normal temperature; reducing the power density of the ZrNi target material to 4.5W/cm²～5.5W/cm²And opening a NiCr target until the power density of the target is 0.5W/cm²～1.5W/cm²Coating for 3-5 min; then reducing the power density of the ZrNi target material to 2.5W/cm²～3.5W/cm²And increasing the power density of the NiCr target material to 2.5W/cm²～3.5W/cm²Coating for 3-5 min; then reducing the power density of the ZrNi target material to 0.5W/cm²～1.5W/cm²And increasing the power density of the NiCr target material to 4.5W/cm²～5.5W/cm²And plating the film for 3-5 min.

A transition layer with a concentration gradient is formed between the substrate 210 and the heat generating layer 230 by adopting dual-target co-sputtering of a ZrNi target and a NiCr target. Namely, ZrNi with a certain thickness is sputtered firstly, then the power of the double targets is adjusted to form high-power sputtering ZrNi and low-power sputtering NiCr, and the power of the ZrNi target is gradually reduced and the power of the NiCr target is improved subsequently. The transition layer having the concentration gradient greatly improves the cyclic heating stability of the heat generating layer 230.

In the embodiment, argon is introduced into the coating cavity until the working pressure is 0.1 Pa-1 Pa, and the power density of the Ti target or ZrNi target at the target is 3.5W/cm²～15W/cm²Coating for 10-30 min at normal temperature to form a transition layer with a thickness of 50-200 nm.

Of course, in other embodiments, the target material of the transition layer may be adaptively selected according to the material of the desired transition layer; for example, when the material of the transition layer is ZrTi, a ZrTi target is selected as the target in sputtering the transition layer. The thickness of the transition layer can be adjusted according to the requirement on the coating time, the power density of the target material and the film binding force. It is understood that in other embodiments, step S120 may be omitted. When the step 120 is omitted, the heat generating layer may be deposited on the pre-processed substrate 210.

Step S130, forming a heat generating layer 230 on the transition layer.

Specifically, after the transition layer is formed on the substrate 210, the ZrNi target is turned off, and the power density of the AgPd target is 4W/cm²～20W/cm²And coating at the temperature of 20-400 ℃ for 60-180 min to form the heating layer 230, wherein the thickness of the heating layer 230 is 1-3.5 mu m.

Further, after the transition layer is formed on the substrate 210, the ZrNi target is turned off, and the power density of the AgPd target is 4W/cm²～8W/cm²Coating film for 90-120 min at normal temperature to form a heating layer 230; the thickness of the heat generating layer 230 is 1.5 μm to 2.5 μm.

In the illustrated embodiment, the heat generating layer 230 is deposited on a plurality of spaced apart transition layers.

In the embodiment, argon is introduced until the working pressure in the chamber is 0.1-1 Pa, and the silver-palladium alloy target works at the target workThe specific density is 4W/cm²～20W/cm²Then, the film plating is carried out for 60min to 150min, the substrate temperature is normal temperature to 400 ℃, the heat generating layer 230 is formed by deposition, then the products plated with the transition layer and the heat generating layer 230 are subjected to vacuum heat treatment at the high temperature of 300 ℃ to 500 ℃ for 5min to 20min, and the sum of the thicknesses of the formed transition layer and the heat generating layer 230 is 1 mu m to 3.5 mu m.

Of course, in other embodiments, the target of the heat generating layer 230 may be adaptively selected according to the material of the heat generating layer 230; for example, when the material of the heat generating layer 230 is AgAu, a target for sputtering the heat generating layer 230 is AgAu target. The thickness of the heating layer 230 can be adjusted according to the requirement, the coating time, the power density of the target material and the film bonding force.

Step S140, preparing a bonding layer on the substrate 210 prepared with the transition layer and the heat generating layer 230.

Specifically, a substrate 210 with a transition layer and a heating layer 230 is provided with a bonding layer mask and then placed in a coating machine; introducing argon until the air pressure of the coating environment is 2 multiplied by 10^-1Pa～10×10^-1Pa, power density of 6W/cm in titanium target material²～8W/cm²Plating a film for 15-30 min at the temperature of 20-400 ℃ to form a bonding layer of 100-500 nm.

Further, argon is introduced until the atmospheric pressure of the coating environment is 5 multiplied by 10^-1Pa, power density of 6W/cm in titanium target material²～8W/cm²And coating the film for 15-30 min to form a bonding layer with the thickness of 300-450 nm under the condition of normal temperature.

In the present embodiment, a bonding layer is deposited on each of the plurality of spaced-apart layers of the substrate 210, the bonding layer being located on the end face side of the heat generating layer 230. Of course, in other embodiments, the target material of the bonding layer may be adaptively selected according to the material of the desired bonding layer; the thickness of the bonding layer can be adjusted according to the requirement on the power density, the coating time and the film bonding force of the target.

It is understood that in some embodiments, step S140 may be omitted. When the step S140 is omitted, the conductive layer 250 may be deposited on the substrate 210 with the heat generating layer 230.

Step S150 of preparing the conductive layer 250 on the substrate 210 prepared with the transition layer, the heat generating layer 230 and the bonding layer.

Specifically, after the bonding layer is prepared, the titanium target is turned off, and the silver target is turned on; the power density of the silver target material is 4W/cm²～8W/cm²And coating for 60-120 min at the temperature of 20-400 ℃ to obtain the conductive layer 250 with the thickness of 1-3 mu m.

Further, the power density of the silver target material was 4.5W/cm²～6W/cm²And coating the film for 60-90 min at 20-200 ℃ to obtain the conductive layer with the thickness of 1.5-2.5 mu m.

In the illustrated embodiment, the conductive layer 250 is deposited on each of a plurality of spaced apart bonding layers, and the conductive layer 250 is electrically connected to the heat generating layer 230.

Of course, in other embodiments, the target material of the conductive layer may be adaptively selected according to the material of the bonding layer required; for example; when the conducting layer is made of Au, the Au target is selected as the target material during sputtering of the conducting layer; the thickness of the conducting layer can be adjusted according to the requirement on the power density, the coating time and the resistance value of the target.

Step S160, preparing a protective layer 260 on the substrate 210 prepared with the conductive layer 250 and the heat generating layer 230.

Specifically, a protective layer mask is added on the substrate 210 with the prepared heating layer 230, and then the substrate is placed in a coating machine; introducing argon to the working pressure of the film coating machine of 0.1-1 Pa in ZrO₂The sputtering power density of the target radio frequency power supply is 4W/cm²～8W/cm²Sputtering to form a film at the temperature of 25-500 ℃ to form a protective layer 260 with the thickness of 2-5.5 μm.

Further, in ZrO₂The sputtering power density of the target radio frequency power supply is 5W/cm²～7W/cm²Sputtering to form a film at the temperature of 25-200 ℃ to form a protective layer 260 with the thickness of 2-5.5 μm.

In other embodiments, the step of forming the protective layer 260 having a thickness of 2 μm to 5.5 μm is followed by increasing ZrO level₂The power density of the target material is up to 6W/cm²～8W/cm²Sputtering for 1-5 min to form mastoid-like structure (scattered large particles) on the surface of the protective layer 260.

In the illustrated embodiment, the protective layer 260 is deposited on each of the plurality of spaced heat generating layers 230, and the protective layer 260 covers a portion of the conductive layer 250.

In this embodiment, a protective layer mask is added to the substrate 210 on which the heat generating layer 230 is prepared, and then the substrate is placed in a coating machine; introducing argon to the working pressure of the film coating machine of 0.1-1 Pa in ZrO₂The sputtering power density of the target radio frequency power supply is 3.5W/cm²～15W/cm²Sputtering to form a film at the temperature of 25-500 ℃ to form a protective layer 260 with the thickness of 2-5 mu m.

Of course, in other embodiments, the target material of the protection layer 260 may be adaptively selected according to the desired material of the protection layer 260; for example; the material of the protective layer 260 is ZrO₂And Al₂O₃When the protective layer 260 is sputtered, ZrO is selected as the target₂Target material and Al₂O₃A target material; the thickness of the protective layer 260 may be adjusted as desired for target power density, coating time, and high temperature stability of the material.

Step S170, cutting the substrate 210 with the protective layer 260.

Specifically, after the preparation of the protective layer 260 is completed, the substrate 210 on which the protective layer 260 is prepared is cut to obtain a plurality of heat-generating bodies 200. In the present embodiment, the cutting method is laser cutting.

Of course, in some embodiments, only one transition layer and corresponding other film layer may be prepared on the substrate 210, and in this case, the step S170 is omitted.

It is understood that in some embodiments, the bonding layer and the conductive layer 250 may be prepared first, and then the transition layer and the heat generating layer 230 may be prepared, as long as the conductive layer 250 is electrically connected to the heat generating layer 230.

According to the preparation method of the heating body 200, each film layer is prepared by adopting a magnetron sputtering method and a mask method, so that the film thickness consistency of each film layer and the position accuracy of the film layer pattern are greatly improved. The thickness deviation of the film of the heating layer is less than or equal to 5%, the position accuracy of the pattern of the heating layer can reach +/-3 mu m, the resistance consistency of the heating layer is better, and the consistency of the smoking taste of the electronic cigarette is greatly improved.

It is understood that in other embodiments, the method for forming each film layer pattern on the substrate 210 is not limited to a mask method, and other methods commonly used in the art, such as an ion etching method, may also be used to form the film layer pattern.

As shown in fig. 6, the electronic smoking set 10 according to one embodiment includes the heating element 100, an insulator 300, a power supply 400, and an electrical connector 500.

Specifically, the insulator 300 is provided on a side of the conductive layer 150 of the heat generating body 100 away from the heat generating layer 130 for isolating the heat generating body 100 from other components (e.g., the power supply 400) of the electronic smoking set 10.

In the present embodiment, the electrical connector 500 is in a linear shape, and one end of the electrical connector 500 is electrically connected to the conductive layer 150 through the insulator 300, and the other end is electrically connected to the power supply 400, so that the heat generating layer 130, the conductive layer 150, and the power supply 400 can form a current loop.

When the electronic smoking set 10 is used, the heating element 100 is inserted into the tobacco 20, and a current circuit between the heating element 100 and the power supply 400 is turned on, so that the heating element 100 generates heat, thereby heating the tobacco 20.

The electronic smoking set 10 includes the heating element 100, and has the advantages of stable heating, strong corrosion resistance and long service life.

The electronic smoking set 10 is applied to preparing tobacco flavor or tobacco fragrance aerosol.

The electronic smoking set 10 uses a relatively low temperature heat source to heat tobacco, and can be applied to the preparation of tobacco flavor or tobacco flavor aerosol.

DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION

The following detailed description is given with reference to specific examples. The following examples are not specifically described, and other components except inevitable impurities are not included. Reagents and instruments used in the examples are all conventional in the art and are not specifically described. The experimental procedures, in which specific conditions are not indicated in the examples, were carried out according to conventional conditions, such as those described in the literature, in books, or as recommended by the manufacturer.

Example 1

The structure of the heating body of embodiment 1 includes the base, the transition layer, the layer that generates heat, protective layer, anchor coat and conducting layer, and the transition layer is laminated on the base, and the layer that generates heat is laminated in the one side that the base was kept away from to the transition layer, and the anchor coat is laminated on the base, and the anchor coat meets with the transition layer, and the conducting layer is laminated in the anchor coat and keeps away from one side of base, and the conducting layer is connected with the layer that generates heat, and the protective layer is laminated on the layer that. The substrate is a zirconia ceramic substrate, the transition layer is made of ZrNi, the thickness of the transition layer is 170nm, the heating layer is made of AgPd, the heating layer is 1.8 mu m, the bonding layer is made of titanium, the bonding layer is 200nm, the conducting layer is made of silver, the conducting layer is 2 mu m, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm. The specific production steps of the heat-generating body of example 1 were as follows:

(1) pretreatment: using 8% NaOH solution by mass concentration and 23% mixed acid by volume concentration (HF and HNO) on the zirconia ceramic substrate₃The volume ratio of 1:4), putting the substrate into a coating machine cavity, and then carrying out ion cleaning on the surface of the substrate by adopting an ion beam flow.

(2) Taking two pretreated zirconia ceramic substrates, respectively carrying out the following operations to obtain two substrates plated with a transition layer and a heating layer and subjected to vacuum heat treatment at 800 ℃ for 12 min: adding a transition layer mask on the pretreated zirconia ceramic substrate, and introducing argon until the working pressure in the cavity is 5 multiplied by 10^-1Pa, setting the power density of the ZrNi target material to be 7W/cm²And coating at normal temperature (25 ℃) for 15min to obtain a transition layer with the thickness of 170 nm. Then the ZrNi target is closed, and the power density of the AgPd target is set to be 7W/cm²And coating the film for 120min at normal temperature to form a heating layer with the thickness of 1.8 mu m on the transition layer.

(3) One of the substrates plated with the transition layer and the heating layer is circularly heated 6000 times at 400 ℃ in the air according to the heating rule of 2 min/stop for 1 min. Comparing and processing the resistance change of the front heating layer and the rear heating layer by adopting a bridge method; and comparing the surface appearance changes of the heating layer before and after treatment by using a scanning electron microscope.

(4) Adding a bonding layer mask on the other substrate plated with the transition layer and the heating layer, placing in a sputtering furnace, introducing argon until the atmospheric pressure of the coating environment is 5 × 10^-1Pa, the power density of the titanium target material is set to be 7W/cm²And plating a film for 15min at normal temperature to form a 200nm binding layer. Then closing the titanium target material, and controlling the power density of the silver target material to be 4W/cm²And coating for 60min at normal temperature to obtain a conductive layer with the thickness of 2 mu m.

(5) Adding a protective layer mask on the substrate with the heating layer and the conducting layer obtained in the step (4), then placing the substrate in a film coating machine, introducing argon until the working pressure of the film coating machine is 0.5Pa, and placing ZrO₂The sputtering power density of the target radio frequency power supply is 5W/cm²A protective layer having a thickness of 3 μm was formed by sputtering at a temperature of 25 ℃ to obtain a heating element of example 1.

(6) And (4) measuring the thermal stability of the heating element prepared in the step (5) by adopting a dry burning method.

The resistance change rate of the heat-generating layer of example 1 before and after the cyclic heat-generating treatment was not more than 3% as measured by the bridge method.

The measurement shows that the heating element of example 1 has an electric field strength of 2X 10 at a temperature of 250 ℃ to 500 DEG C⁵V/m～10×10⁵Within the range of V/m, the electrode spacing is below 0.4mm and lasts for more than 500h, and the resistance value change is less than 3%. The silver in the heating layer does not generate electrochemical migration between the electrodes under the environment of normal temperature and humidity or high temperature atmosphere of 250-500 ℃. The heating body has no bubbling and dropping phenomena and no obvious damage.

Example 2

The heating body of embodiment 2 has a structure including a base, a transition layer, a heating layer, a protective layer, a bonding layer and a conductive layer, wherein the transition layer is stacked on the base, the heating layer is stacked on one side of the transition layer away from the base, the bonding layer is stacked on the base, the bonding layer is connected with the transition layer, the conductive layer is stacked on one side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is stacked on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate; the transition layer is made of ZrNi and NiCr and is arranged close to the substrateFrom one side of the transition layer to the side far away from the substrate, the NiCr in the transition layer is gradually increased, and the thickness of the transition layer is 170 nm; the heating layer is made of AgPd, the heating layer is 1.8 μm thick, the bonding layer is made of titanium, the bonding layer is 200nm thick, the conductive layer is made of silver, the conductive layer is 2 μm thick, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm.

Example 2 a method of producing a heat-generating body was substantially the same as in example 1, except that the transition layer of example 2 was produced differently from example 1. The preparation steps of the transition layer of example 2 were:

adding a transition layer mask on the pretreated zirconia ceramic substrate, and introducing argon until the working pressure in the cavity is 5 multiplied by 10^-1Pa, power density of ZrNi target material is 7W/cm²Coating film for 4min at normal temperature; then reducing the power density of the ZrNi target to 5W/cm²And opening a NiCr target until the power density of the target is 1W/cm²Coating the film for 4 min; then reducing the power density of the ZrNi target to 3W/cm²And increasing the NiCr target power density to 3W/cm²Coating the film for 4 min; then reducing the power density of the ZrNi target to 1W/cm²And increasing the NiCr target power density to 5W/cm²And plating a film for 4min to obtain a transition layer with the thickness of 170 nm.

The resistance change rate of the heat-generating layer of example 2 before and after the cyclic heating treatment was not more than 3% as measured by the bridge method.

The surface topography changes of the heat-generating layer before and after the cyclic heating treatment are shown in FIGS. 7 to 8. FIG. 7 is an image of the substrate coated with the transition layer and the heat generating layer before being processed at a scanning electron microscope of 3K times; fig. 8 is an image of the treated substrate plated with the transition layer and the heat generating layer under a scanning electron microscope of 3K times.

As can be seen from fig. 7 and 8, the shapes of the substrates plated with the transition layer and the heat-generating layer before and after the cyclic heating treatment are not significantly changed, and excellent cyclic heating stability is exhibited.

The heating element of example 2 was measured to have a temperature of 250 to 500 ℃ and an electric field strength of 2X 10⁵V/m～10×10⁵Within the range of V/m, the electrode spacing is less than 0.4mm and lasts for more than 550h, and the resistance value change is less than 3 percent.The silver in the heating layer does not generate electrochemical migration between the electrodes under the environment of normal temperature and humidity or high temperature atmosphere of 250-500 ℃. The heating body has no bubbling and dropping phenomena and no obvious damage.

Example 3

The heating body of embodiment 3 has a structure including a base, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer, wherein the transition layer is stacked on the base, the heating layer is stacked on one side of the transition layer away from the base, the bonding layer is stacked on the base, the bonding layer is connected to the transition layer, the conductive layer is stacked on one side of the bonding layer away from the base, the conductive layer is electrically connected to the heating layer, and the protective layer is stacked on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the transition layer is made of ZrNi, the thickness of the transition layer is 170nm, the heating layer is made of Ag, the heating layer is 1.8 mu m, the bonding layer is made of titanium, the bonding layer is 200nm, the conducting layer is made of silver, the conducting layer is 2 mu m, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm.

The method for producing the heat-generating body of example 3 was substantially the same as the method for producing the heat-generating body of example 1, except that the material of the heat-generating layer of example 3 was silver.

The heat-generating layer of example 3 exhibited a resistance change rate of > 3% before and after the cyclic heat-generating treatment as measured by the bridge method.

The measurement shows that the heating element of example 3 has an electric field strength of 2X 10 at a temperature of 250 ℃ to 500 DEG C⁵V/m～10×10⁵Within the range of V/m, the electrode distance is less than 0.4mm, the resistance value is changed by more than 3 percent for 100 hours, and the silver in the heating layer can generate electrochemical migration between the electrodes under the environment of normal temperature and humidity or high temperature atmosphere of 250-500 ℃, thereby causing short circuit. The heating body has no bubbling and dropping phenomena and no obvious damage.

Example 4

The heating unit of embodiment 4 has a structure including a base, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer, wherein the transition layer is stacked on the base, the heating layer is stacked on the transition layer on the side away from the base, the bonding layer is stacked on the base, the bonding layer is connected to the transition layer, and the conductive layer is connected to the bonding layerThe bonding layer is stacked on one side of the substrate, the conducting layer is electrically connected with the heating layer, and the protective layer is stacked on the heating layer and partially covers the conducting layer. The substrate is a zirconia ceramic substrate, the transition layer is made of Ti, the thickness of the transition layer is 170nm, the heating layer is made of AgPd, the heating layer is 1.8 mu m, the bonding layer is made of titanium, the bonding layer is 200nm, the conducting layer is made of silver, the conducting layer is 2 mu m, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm.

The method for producing the heat-generating body of example 4 was substantially the same as the method for producing the heat-generating body of example 1, except that the target material for producing the transition layer of example 4 was a titanium target, and the thickness of the transition layer of example 4 was 170 nm.

The resistance change rate of the heat-generating layer of example 4 before and after the cyclic heat-generating treatment was not more than 3% as measured by the bridge method.

The heating element of example 4 was measured to have a temperature of 250 to 500 ℃ and an electric field strength of 2X 10⁵V/m～×10⁵Within the range of V/m, the electrode spacing is below 0.4mm, the electrode spacing lasts for more than 300h, the resistance value change is less than 3%, and the silver in the heating layer does not generate electrochemical migration between the electrodes under the environment of normal temperature and humidity or high temperature atmosphere of 250-500 ℃. However, when the heating element is continuously dried, the edges of the heating element patterns are stripped off by a small amount of films, and the adhesive force is poor.

Example 5

The heating unit of embodiment 5 has a structure including a substrate, a heating layer, a protective layer, a bonding layer and a conductive layer, wherein the heating layer is stacked on the substrate, the bonding layer is connected to the heating layer, the conductive layer is stacked on the side of the bonding layer away from the substrate, the conductive layer is electrically connected to the heating layer, and the protective layer is stacked on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the heating layer is made of AgPd, the heating layer is 1.8 mu m thick, the bonding layer is made of titanium, the bonding layer is 200nm thick, the conducting layer is made of silver, the conducting layer is 2 mu m thick, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm.

The method of producing the heat-generating body of example 5 was substantially the same as the method of producing the heat-generating body of example 1, except that example 5 had no step of producing a transition layer, and the heat-generating layer was produced on the substrate after the pretreatment.

As a result of measurement, the heat-generating layer of the heat-generating body of example 5 was peeled off, and the adhesion force was poor.

Example 6

The structure of the heating body of embodiment 6 includes the basement, the transition layer, generate heat the layer, the protective layer, the anchor coat and the conducting layer, and the transition layer is laminated on the basement, and the one side of basement is kept away from to the layer that generates heat range upon range of transition layer, and the anchor coat is laminated on the basement, and the anchor coat meets with the transition layer, and the conducting layer is laminated in the anchor coat and keeps away from one side of basement, and the conducting layer is connected with the layer that generates heat, and the protective layer is laminated on the. The substrate is a zirconia ceramic substrate, the transition layer is made of ZrNi, the thickness of the transition layer is 170nm, the heating layer is made of AgAu, the thickness of the heating layer is 1.8 mu m, the bonding layer is made of titanium, the thickness of the bonding layer is 200nm, the conducting layer is made of silver, the conducting layer is made of 2 mu m, and the protective layer is made of ZrO₂The thickness of the protective layer was 3 μm.

The method for producing the heat-generating body of example 6 is substantially the same as the method for producing the heat-generating body of example 1, except that the material of the heat-generating layer of example 6 is a silver-gold alloy.

The resistance change rate of the heat-generating layer of example 6 before and after the cyclic heat-generating treatment was not more than 3% as measured by the bridge method.

The heating element of example 6 was measured to have a temperature of 250 to 500 ℃ and an electric field strength of 2X 10⁵V/m～10×10⁵Within the range of V/m, the electrode distance is less than 0.4mm, the resistance value is changed by less than 3 percent after the electrode distance lasts for more than 600 hours, and the silver in the heating layer does not generate electrochemical migration between the electrodes under the environment of normal temperature and humidity or high temperature atmosphere of 250-500 ℃. The heating body has no bubbling and dropping phenomena and no obvious damage.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims

1. The heating body is characterized by comprising a substrate, a heating layer and a protective layer, wherein the heating layer is arranged on the substrate, the protective layer is arranged on one side, away from the substrate, of the heating layer, and the heating layer is made of silver alloy.

2. A heat-generating body as described in claim 1, characterized in that the material of the protective layer is selected from ZrO₂And Al₂O₃At least one of; and/or

The thickness of the protective layer is 2-5 μm.

3. A heat-generating body as described in claim 2, wherein a material of the heat-generating layer is at least one selected from the group consisting of AgAu, AgPd, and AgPt; and/or

The thickness of the heating layer is 1-6 μm.

4. A heat-generating body as described in claim 1, further comprising a transition layer laminated on said substrate, said heat-generating layer being laminated on a side of said transition layer remote from said substrate, a material of said transition layer being selected from at least one of Ti or ZrNi; and/or

The thickness of the transition layer is 50 nm-200 nm.

5. A heat-generating body as described in claim 4, wherein a material of the heat-generating layer is AgPd, and the heat-generating layer is made of AgPdThe thickness of the heating layer is 1-3.5 μm; the protective layer is made of ZrO₂The thickness of the protective layer is 2-5 μm.

6. A heat-generating body as described in any one of claims 1 to 5, characterized in that a mastoid-like structure is formed on the side of the protective layer away from the heat-generating layer.

7. A heat-generating body as described in claim 6, further comprising a conductive layer which is provided on a side of the substrate close to the heat-generating layer and is electrically connected to the heat-generating layer.

8. A heat-generating body as described in claim 7, further comprising a bonding layer laminated between said substrate and said conductive layer, a material of said bonding layer being at least one selected from the group consisting of titanium, nickel, tantalum, and a nickel alloy.

9. A method for preparing a heating element is characterized by comprising the following steps:

10. An electronic smoking set comprising the heating element according to any one of claims 1 to 8 or the heating element produced by the heating element production method according to claim 9.