WO2021000806A1

WO2021000806A1 - Heating body and manufacturing method therefor, and electronic cigarette utensil

Info

Publication number: WO2021000806A1
Application number: PCT/CN2020/098664
Authority: WO
Inventors: 周宏明; 程振乾; 张蛟; 金鹤; 刘宇嵘
Original assignee: 深圳麦克韦尔科技有限公司
Priority date: 2019-07-04
Filing date: 2020-06-29
Publication date: 2021-01-07
Also published as: CN112251723B; CN112251723A

Abstract

The present invention relates to a heating body and a manufacturing method therefor, and an electronic cigarette utensil. A heating body (100) comprises a substrate (110), a transition layer (120), and a heating layer (130). The transition layer (120) is stacked on the substrate (110), and the heating layer (130) is stacked on one side of the transition layer (120) away from the substrate (110); the substrate (110) is a ceramic substrate, and the transition layer (120) is made of alloy; a chemical bond is formed between the transition layer (120) and the substrate (110), and a chemical bond is also formed between the transition layer (120) and the heating layer (130).

Description

Heating body, preparation method thereof, and electronic cigarette

Technical field

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

Background technique

Electronic cigarettes are electronic products that imitate cigarettes. They have a similar appearance and taste to cigarettes, but generally do not contain other harmful ingredients such as tar and suspended particles in cigarettes.

E-cigarettes mainly release e-liquid or tobacco by heating the heating element of the e-cigarette, thereby releasing the aromatic substances and nicotine in the e-liquid or tobacco, producing smoke close to the taste of real smoke, and reducing the production of harmful substances. However, current heating elements often suffer from unstable heating.

Summary of the invention

Based on this, it is necessary to provide a heat generating body with stable heat generation.

A heating element comprising a substrate, a transition layer and a heating layer, the transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, the substrate is a ceramic substrate, The material of the transition layer is an alloy, the transition layer forms a chemical bond with the substrate, and the transition layer forms a chemical bond with the heating layer.

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

Depositing a transition layer on a substrate, the substrate is a ceramic substrate, the material of the transition layer is an alloy, and the transition layer forms a chemical bond with the substrate; and

A heating layer is formed on the transition layer, and the heating layer forms a chemical bond with the transition layer.

An electronic cigarette, the heating element or the heating element produced by the heating element preparation method.

The details of one or more embodiments of the present application are set forth in the following drawings and descriptions, and other features, purposes and advantages of the present application will become apparent from the description, drawings and claims.

Description of the drawings

Fig. 1 is a schematic diagram of the structure of a heating element according to an embodiment;

Fig. 2 is a schematic structural diagram of a heating element according to another embodiment;

Figure 3 is a substrate deposited with a heating layer prepared in step S130;

4 is a substrate deposited with a conductive layer prepared in step S150;

Fig. 5 is a substrate deposited with a protective layer prepared in step S160;

Fig. 6 is a schematic diagram of an electronic cigarette set and its use according to an embodiment;

Figure 7 is a scanning electron microscope image before processing in Example 2;

Figure 8 is a scanning electron microscope image after processing in Example 2;

Figure 9 is a heating element prepared in Example 6;

Figure 10 is a scanning electron micrograph of the heating element of Example 6 before processing;

Fig. 11 is a scanning electron micrograph of the heating element of Example 6 after processing.

In order to better describe and explain the embodiments and/or examples of the inventions disclosed herein, one or more drawings may be referred to. The additional details or examples used to describe the drawings should not be considered as limiting the scope of any of the disclosed inventions, the currently described embodiments and/or examples, and the best mode of these inventions currently understood.

Detailed ways

In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. The drawings show some embodiments of the present invention. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

It should be noted that when an element is referred to as being "fixed to" another element, it may be directly on the other element or a central element may also exist. When an element is considered to be "connected" to another element, it can be directly connected to the other element or an intermediate element may be present at the same time.

Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field of the present invention. The terms used in the description of the present invention herein are only for the purpose of describing specific embodiments, and are not intended to limit the present invention.

As shown in FIG. 1, the heating element 100 of an embodiment includes a substrate 110, a transition layer 120, a heating layer 130, a bonding layer 140 and a conductive layer 150. The heating element 100 has strong thermal stability.

The substrate 110 is a carrier for 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. Furthermore, the substrate 110 is a zirconia ceramic substrate. Zirconia ceramics have high strength, hardness, high temperature resistance and high chemical stability. Of course, in some other embodiments, the material of the substrate 110 is not limited to ceramics, and may also be other high temperature resistant materials, such as stainless steel. Compared with the stainless steel substrate, the zirconia ceramic substrate has high hardness and good toughness. It is not easy to break when inserted into the cartridge. At the same time, its high temperature resistance and corrosion resistance can avoid the corrosion of the substrate by organic substances such as nicotine generated during the smoking process. The zirconia ceramic substrate is not conductive, which avoids the production of an insulating layer and simplifies the process flow.

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

The transition layer 120 is laminated on the substrate 110. The transition layer 120 can form a stable chemical bond with the substrate 110 and the heating layer 130 at the same time, so that the heating element 100 has higher cycle heating stability. Further, the transition layer 120 can form a metal bond with the substrate 110 and the heating layer 130 at the same time. It is understandable that all materials capable of forming a chemical bond (such as a metal bond, a covalent bond or an ionic bond) between the substrate and the heating layer can be used as the material of the transition layer 120.

The material of the transition layer 120 is metal, metal oxide or alloy.

When the material of the transition layer 120 is metal, specifically, the material is nickel or chromium. When the material of the transition layer 120 is a metal oxide, the material is specifically zirconia or alumina.

When the material of the transition layer 120 is an alloy, specifically, the material of the transition layer 120 includes at least one of ZrNi, ZrTi, NiCr, and TiN. The thermal expansion coefficient of the alloy is between the substrate 110 and the heating layer 120, and can form a strong chemical bond with the substrate 110 and the heating layer 120, thereby making the entire system more stable. Of course, in some embodiments, the transition layer 120 can also improve the bonding ability of the substrate 110 and the heating layer 130, so that the heating layer 130 is not easy to fall off the substrate 110.

Further, the material of the transition layer 120 includes at least one of ZrNi, ZrTi and TiN and NiCr. Further, the material of the transition layer 120 is selected from at least one of ZrNi, ZrTi and TiN and NiCr. Specifically, from the side close to the substrate 110 to the side far from the substrate 110, the NiCr in the transition layer 120 gradually increases. The NiCr gradually increasing from the side close to the substrate 110 to the side far away from the substrate 110 in the transition layer 120 can make the cycle thermal stability of the heating layer 130 better. Furthermore, the material of the transition layer 120 includes ZrNi and NiCr. The material of the transition layer 120 is ZrNi and NiCr.

The thickness of the transition layer 120 is 100 nm to 500 nm. The transition layer 120 is too thin to provide the bonding force with the substrate 110, but the transition layer 120 to improve the bonding force should not be too thick. An overly thick transition layer 120 not only causes greater internal stress, but also wastes material. Further, the thickness of the transition layer 120 is 100 nm to 200 nm. Setting the thickness of the transition layer 120 to 100 nm to 200 nm can buffer the stress between the substrate 110 and the heating layer 120, significantly improve the bonding force between the substrate 110 and the heating layer 120, and save costs as much as possible.

The heating layer 130 is laminated on the transition layer 120 for heating. The material of the heating layer 130 is a material with a small resistivity and stable material structure performance after high temperature heating.

Specifically, the material of the heating layer 130 is a single metal or alloy.

When the material of the heating layer 130 is a single metal, the material of the heating layer 130 is gold, silver, copper, platinum or aluminum.

This study found that when the heating layer 130 is an alloy, the oxidation of the heating layer 130 can be reduced, and the electrochemical migration of the metal of the heating layer 130 can be reduced, so that the heating layer 130 is not easily short-circuited, and the heating of the heating element 100 is more uniform and stable. In addition, other metals in the alloy besides the matrix can also adjust the temperature coefficient of resistance of the heating system, so that the temperature control of the heating layer 130 is more accurate. Of course, when the material of the heating layer 130 is an alloy and the material of the transition layer 120 is also an alloy, the material of the heating layer 130 is different from the material of the transition layer 120.

Specifically, when the material of the heating layer 130 is an alloy, the material of the heating layer 130 includes at least one of a nickel alloy, a silver alloy, and a gold alloy. Further, the material of the heating layer 130 includes one of nickel alloy, silver alloy and gold alloy.

Specifically, the material of the heating layer 130 is selected from at least one of NiCr, NiCrAlY, AgAu, AgPd, AgPt, AuPt, and AuPd. The metal alloy is selected as the material of the heating layer 130, and the TCR fluctuation range of the heating layer 130 is small, which is more conducive to the precise temperature control of the heating layer 130. Further, the material of the heating layer 130 is selected from one of NiCr, NiCrAlY, AgAu, AgPd, AgPt, AuPt, and AuPd. NiCr, NiCrAlY, AgAu, AgPd, AgPt, AuPt and AuPd can make the heating layer 130 have extremely low resistivity, prevent short circuit caused by the migration of metal in the heating layer 130, and have good temperature oxidation and corrosion resistance. The high temperature stability of the heating layer 130 is improved as a whole. AgPd, NiCr and NiCrAlY also have good high temperature oxidation and corrosion resistance, which can extend the life of the heating element 100.

Further, the material of the heating layer is selected from at least one of NiCr, NiCrAlY, AgAu, AgPd, AgPt, AuPt, AuPd and platinum. Furthermore, the material of the heating layer 130 is silver alloy.

This study found that, on the one hand, silver alloys, such as AgPd, AgAu, and AgPt, can form a continuous solid solution to make the heating layer 130 more stable, thereby enhancing the electrochemical migration resistance of silver. For example, it has been found through research that Ag-15%Pd and pure Ag electrodes are tested for electromigration failure time under a constant 400°C high temperature environment and a 200V DC voltage. When the electrochemical migration time is 241 minutes, a "silver bridge" connecting the anode and cathode is formed between the silver electrodes, and the anode edge of the silver electrode has a mass loss and is no longer complete. However, when the electrochemical migration time is 241min, there is no "silver bridge" formed between the Ag-15%Pd electrodes, but it can be seen that a layer of silvery luster is deposited on the edge of the cathode, and silver atoms are caused by the transmission of current. The movement and ultimately led to the transmission of its mass. When the electrochemical migration time reaches 472 minutes, a "silver bridge" connecting the anode and cathode is also formed between the Ag-15%Pd electrodes. It shows that the electrochemical migration failure life of Ag-15%Pd electrode is much higher than that of silver electrode, indicating that the addition of Pd has a good inhibitory effect on the electrochemical migration behavior of silver in a high temperature and dry environment.

On the other hand, the temperature coefficient of resistance of pure silver is relatively high, about 3800ppm/℃, and the temperature rise is relatively slow in the case of constant voltage input. When silver alloy is used as the heating layer 130, other metals can adjust the temperature coefficient of resistance (TCR) of the material, and the temperature rise rate is faster than pure silver when the constant voltage is applied, and high-precision temperature control can be realized.

Specifically, the material of the heating layer 130 is selected from at least one of AgAu, AgPd, and AgPt. Further, the material of the heating layer 130 is selected from one of AgAu, AgPd and AgPt. Doping Au, Pd or Pt in silver to form an alloy can reduce the silver migration phenomenon of silver at high temperature, and at the same time can adjust the resistance of the heating film to the required range. Further, the material of the heating layer 130 is platinum.

The thickness of the heat generating layer 130 is 2 μm to 6 μm. Further, the sum of the thickness of the heating layer 130 and the thickness of the transition layer 120 is 2 μm-4 μm.

In other embodiments, the substrate 110 is a zirconia ceramic substrate, the material of the transition layer 120 includes at least one of ZrNi, ZrTi, and TiN and NiCr, and the material of the heating layer 130 includes at least one of NiCr, AgPd, and NiCrAlY .

In some other embodiments, the substrate 110 is a zirconia ceramic substrate, the material of the transition layer 120 includes at least one of ZrNi, ZrTi, and TiN and NiCr, and the material of the heating layer 130 includes one of NiCr, AgPd, and NiCrAlY. NiCr, AgPd and NiCrAlY have good high-temperature oxidation and corrosion resistance, which can extend the life of the heating element 100. Further, the material of the heating layer 130 includes NiCr. At high temperatures, NiCr will form a continuous dense chromium oxide layer on the surface of the heating layer 130, so that the heating film has good oxidation and corrosion resistance, and the price of NiCr is cheap, which can make the heating layer 130 resistant to oxidation and corrosion Improved capacity and lower cost.

The bonding layer 140 is laminated on the substrate 110, and the bonding layer 140 is used to improve the bonding force between the conductive layer 150 and the substrate 110. Specifically, the material of the bonding layer 140 is selected from at least one of titanium, chromium, aluminum, nickel, and nickel-based alloys. Further, the material of the bonding layer 140 is selected from one of titanium, nickel and nickel-based alloys. Furthermore, the material of the bonding layer 140 is titanium. Setting the bonding layer 140 as a titanium layer on the one hand can improve the bonding force between the conductive layer 150 and the substrate 110, on the other hand, it can prevent the high temperature corrosion of the metallized film during the soldering process, and improve the bonding of the bonding pads formed after soldering. The bonding force between the substrates.

The thickness of the bonding layer 140 is 200 nm to 700 nm. further. The thickness of the bonding layer 140 is 300 nm to 600 nm. Setting the thickness of the bonding layer 140 to 300 nm to 600 nm can make the bonding force of the conductive layer 150 and the substrate strong without affecting the conductive performance of the conductive layer 150.

The conductive layer 150 is disposed on the bonding layer 140 and is electrically connected to the heating layer 130. The conductive layer 150 is used to connect the heating layer 130 and the power source, so that a current loop is formed between the conductive layer 150, the heating layer 130 and the power source.

Specifically, the conductive layer 150 is laminated 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 heating layer 130, and the other end surface is electrically connected to the power source. Further, the conductive layer 150 and the power source are connected by soldering leads. The conductive layer 150 is used as a conductive electrode to be formed by magnetron sputtering and soldering leads, which does not need to go through high temperature and improves process efficiency.

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 8 μm. Further, the thickness of the conductive layer 150 is 3 μm to 6 μm. Setting the thickness of the conductive layer 150 to 3 μm to 6 μm enables the power supply and the heating layer 130 to form a path, and the resistance value of the conductive layer 150 is minimized. If the conductive layer 150 is too thick, the material cost increases. Furthermore, the sum of the thickness of the conductive layer and the thickness of the bonding layer is 2 μm-4 μm.

Of course, it can be understood that in some embodiments, the bonding layer 140 may be omitted. When the bonding layer 140 is omitted, the conductive layer 150 is provided on the substrate 110 and is electrically connected to the heating layer 130. Further, the conductive layer 150 is laminated on the side of the base 110 close to the heating layer 130.

The heating element 100 includes a substrate 110, a transition layer 120, and a heating layer 130. The transition layer 120 forms a stable chemical bond with the substrate 110, and the transition layer 120 and the heating layer 130 also form a stable chemical bond, thereby improving the cycle heat stability of the heating layer 130. Sex.

2 and 3, the heating element 200 of another embodiment is substantially the same as the heating element 100, except that the heating element 200 further includes a protective layer 260, and the shape of the base 210 is approximately a pentagonal sheet. Of course, it can be understood that in some other embodiments, the shape of the base 210 is not limited to a pentagonal sheet shape, and may also be any other shape. For example, disc shape, rectangular sheet shape, rod shape, etc.

Specifically, the protective layer 260 is provided on the heating layer 230 for the protective layer 260 to isolate the heating layer 230 from the external environment (air, tobacco leaves, smoke oil), to avoid the influence of the external environment on the heating layer 230, so that the heating layer 230 Fever is more stable. Specifically, the protective layer 260 is arranged to prevent soot deposits on the heating layer 230, which causes uneven heating. In addition, the setting of the protective layer 260 blocks the erosion of the heat generating layer 230 by oxygen and impurities, reduces the damage of the heat generating layer 230, and makes the heat generating layer 230 heat more uniformly and more stable. In the illustrated embodiment, the protective layer 260 is laminated on the side of the heating layer 230 away from the base 210.

The material of the protective layer 260 includes at least one of ZrO ₂ , Al ₂ O ₃ and Si ₃ N ₄ . ZrO ₂ , Al ₂ O ₃ and Si ₃ N ₄ have high surface hardness, good thermal stability, easy cleaning and good corrosion resistance. As the protective layer 260, the heating element 200 can have high surface hardness, high stability and easy cleaning. And good corrosion resistance.

Further, the material of the protective layer 260 is selected from at least one of ZrO ₂ and Al ₂ O ₃ . The expansion coefficients of ZrO ₂ and Al ₂ O ₃ and the silver alloy of the heating layer 230 are well matched. Using at least one of ZrO ₂ and Al ₂ O ₃ as the material of the protective layer 260 can make the protective layer 260 and the heating layer 230 have a strong bonding force, so that the protective layer 260 can be stably combined with the heating layer 230, and it is not easy to The heat generating layer 230 is peeled off, thereby playing the role of the protective layer 260. Further, the material of the protective layer 260 includes ZrO ₂ and Al ₂ O ₃ . Furthermore, the material of the protective layer 260 is ZrO ₂ and Al ₂ O ₃ .

Further, the protective layer 260 has a papilla-like structure formed on a side away from the heating layer 230. The papilla-like structure can reduce the adhesion on the surface of the protective layer 260, so that dirt is less likely to adhere to the surface of the protective layer 260. Further, the protective layer 260 has a plurality of papillary structures arranged at intervals on the side away from the heating layer 230.

The thickness of the protective layer 260 is 700 nm to 1000 nm.

The total thickness of the transition layer, the heating layer 230 and the protective layer 260 is 2 μm to 5 μm. The total thickness of the heating element 200 is thinner, and the tobacco insertion is more convenient. Of course, the possibility of increasing the thickness of the base 210 is more conducive to improving the flexural strength of the heating element 200.

In this embodiment, the substrate 110 is a zirconia ceramic substrate, the material of the transition layer is ZrNi, the material of the heating layer 230 is platinum, the thickness of the transition layer and the thickness of the heating layer 230 are 2 μm-4 μm, and the material of the bonding layer It is ZrNi or Ti, the material of the conductive layer 250 is silver, the thickness of the bonding layer and the thickness of the conductive layer 250 are 2 μm to 4 μm, the material of the protective layer 260 is ZrO ₂ , and the thickness of the protective layer 260 is 700 nm to 1000 nm.

The above-mentioned heating element 200 has substantially the same structure as the heating element 100, and therefore, has similar effects to the heating element 200. In addition, the heating element 200 is further provided with a protective layer 260. The provision of the protective layer 260 can make the heating element 200 generate more stable heat, have strong corrosion resistance, is not easy to deposit soot, and is easy to clean, thereby increasing the service life of the heating element 200.

Please refer to FIGS. 3 to 5, the method for preparing the heating element 200 includes steps S110 to S170.

Step S110, pre-processing.

Specifically, the substrate 210 is subjected to acid-base cleaning, and then the surface of the substrate 210 is subjected to ion cleaning. Furthermore, the substrate 210 after acid-base cleaning is placed in a coating machine, and vacuum is applied to ion-clean the surface of the substrate 210. Further, ion cleaning is performed on the surface of the substrate 210 at 30°C to 100°C.

The purpose of the pre-treatment is to remove grease, dust, oxides and other dirt on the substrate 210, and improve the bonding force between the subsequent film layer and the substrate 210.

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

Specifically, vapor deposition technology is used to deposit a transition layer on the pre-treated substrate 210. Furthermore, a transition layer mask is added on the 210 layer of the substrate, and argon gas is introduced until the pressure of the coating environment is 0.2Pa～1.5Pa, the power density of the ZrNi target material is 6W/cm ² ～8W/cm ² , and the temperature is 18 The film is plated at ℃～26℃ for 10min～20min to obtain the transition layer. The material of the transition layer is ZrNi, and the thickness of the transition layer is 100 nm to 200 nm.

In some embodiments, it is also possible to use multiple target materials for co-sputtering, gradually increasing the sputtering power of at least one target material, and gradually reducing the sputtering power of other target materials, thereby forming a transition layer with a concentration gradient . The transition layer with a concentration gradient can significantly improve the cycle heating stability of the heating layer 230.

Specifically, a ZrNi target and a NiCr target are used to co-sputter to form a transition layer with a concentration gradient. Furthermore, argon gas is introduced to the coating environment pressure of 0.2Pa～1.5Pa; the ZrNi target power density is 6W/cm ² ～8W/cm ² , the temperature is 18℃～26℃, and the film is coated for 0min～5min; Reduce the power density of the ZrNi target material to 4W/cm ² ～6W/cm ² , open the NiCr target material to the target power density of 0W/cm ² ～ 2W/cm ² , and coat the film for 0min～5min; then reduce the power density of the ZrNi target material to 2W/cm ² ～4W/cm ² and increase the power density of NiCr target material to 2W/cm ² ～4W/cm ² , coating 0min～5min; then reduce the power density of ZrNi target material to 0W/cm ² ～2W/cm ² And increase the power density of NiCr target material to 4W/cm ² ～6W/cm ² , coating 0min～5min. Furthermore, argon gas is introduced to the atmosphere pressure of the coating to be 5×10 ^-1 Pa; the power density of the ZrNi target material is 6.5W/cm ² ～7.5W/cm ² , and the coating is 3min～5min under normal temperature conditions; reduce the ZrNi target Material power density to 4.5W/cm ² ～5.5W/cm ² and NiCr target to target power density of 0.5W/cm ² ～1.5W/cm ² , coating 3min～5min; then reduce the power density of ZrNi target To 2.5W/cm ² ～3.5W/cm ² and increase the power density of NiCr target material to 2.5W/cm ² ～3.5W/cm ² , coating 3min～5min; then reduce the power density of ZrNi target material to 0.5W/cm ² ～1.5W/cm ² and increase the power density of NiCr target material to 4.5W/cm ² ～5.5W/cm ² , coating 3min～5min.

Using ZrNi target material and NiCr target material dual target co-sputtering to form a transition layer with a concentration gradient between the substrate 210 and the heating layer 230, that is, first sputtering a certain thickness of ZrNi, and then adjusting the power of the dual target material to form high-power sputtering ZrNi and low-power sputtering NiCr, then gradually reduce the power of the ZrNi target and increase the power of the NiCr target. The transition layer with a concentration gradient greatly improves the cycle heating stability of the heating layer 230.

It is understandable that in some other embodiments, the target material of the transition layer can be adaptively selected according to the material of the required transition layer; for example, when the material of the transition layer is ZrTi, the target material during the sputtering of the transition layer is selected as ZrTi Target. The thickness of the transition layer can be adjusted according to the needs of the coating time, the power density of the target and the bonding force of the film.

Step S130, forming a heating layer 230 on the transition layer.

Specifically, after the transition layer is formed on the substrate 210, the ZrNi target is closed, the power density of the NiCr target is increased to 6W/cm ² ～8W/cm ² , and the temperature is 25℃～500℃, and the coating is 60min～200min , The formed heating layer 230; then vented out of the furnace, the substrate 210 plated with the transition layer and the heating layer 230 is subjected to 500 ℃ ~ 1000 ℃ vacuum heat treatment for 5 min to 20 min, and the total thickness of the transition layer and the heating layer 230 is 2 μm ~ 3.5μm. The substrate 210 plated with the transition layer and the heating layer 230 is subjected to 500℃～1000℃ vacuum heat treatment for 5min～20min to make the bonding ability between the transition layer, the heating layer 230 and the substrate 210 stronger; and it can also improve the transition layer and heating The crystallinity of the layer 230 effectively eliminates the defects in the transition layer and the heating layer 230, so that the performance of the transition layer and the heating layer 230 is stable. Further, after the transition layer is formed on the substrate 210, the ZrNi target is closed, the power density of the NiCr target is increased to 6.5W/cm ² to 7.5W/cm ² , and the film is plated for 90 to 150 minutes under normal temperature conditions to form a film; Then, the gas is discharged out of the furnace, and the substrate 210 coated with the transition layer and the heating layer is subjected to a vacuum heat treatment at 600°C to 900°C for 12 to 18 minutes, and the total thickness of the transition layer and the heating layer 230 is 2.5 μm to 3.2 μm.

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

Of course, in some other embodiments, the target material of the heating layer 230 can be adaptively selected according to the material of the heating layer 230 required; for example, when the material of the heating layer 230 is NiCrAlY, the target material for the sputtering of the heating layer 230 is selected NiCrAlY target. The thickness of the heating layer 230 can be adjusted according to the needs of the coating time, the power density of the target and the bonding force of the film.

Step S140, preparing a bonding layer on the substrate 210 on which the transition layer and the heating layer 230 are prepared.

Specifically, the substrate 210 prepared with the transition layer and the heating layer 230 is equipped with a bonding layer mask, and then placed in the coating machine; the argon gas is introduced to the coating environment with a pressure of 0.2 Pa to 1.5 Pa, and the power density of the titanium target Under the condition of 6W/cm ² to 8W/cm ² and the temperature of 25°C to 300°C, the film is plated for 15 to 30 minutes to form a bonding layer of 100nm to 500nm. Furthermore, argon gas is introduced to the coating atmosphere pressure of 5×10 ^-1 Pa, the power density of the titanium target is set to 6W/cm ² ～8W/cm ² , and the coating is formed for 15min～30min to form 150nm～300nm under the condition of normal temperature The bonding layer.

In this embodiment, a bonding layer is deposited on a plurality of substrate 210 layers arranged at intervals, and the bonding layer is located on the end surface side of the heating layer 230. Of course, in some other embodiments, the target of the bonding layer can be adaptively selected according to the material of the required bonding layer; the thickness of the bonding layer can be adjusted according to the needs of the coating time, the power density of the target and the bonding force of the film. .

It can be understood that, in some embodiments, step S140 may be omitted. When step S140 is omitted, the conductive layer 250 can be deposited on the substrate 210 on which the heating layer 230 is prepared.

In step S150, a conductive layer 250 is prepared on the substrate 210 on which the transition layer, the heating layer 230 and the bonding layer are prepared.

Specifically, after preparing the bonding layer, turn off the titanium target and turn on the silver target; under the condition that the power density of the silver target is 4W/cm ² ～8W/cm ² and the temperature is 25℃～500℃, the coating For 60 minutes to 120 minutes, a conductive layer 250 with a thickness of 1 μm to 8 μm is obtained. Further, the power density of the silver target material is 5W/cm ² -7 W/cm ² , and the film is plated at 50° C. to 300° C. for 70 min to 100 min to obtain a conductive layer with a thickness of 3 μm to 5 μm.

In the illustrated embodiment, a conductive layer 250 is deposited on a plurality of bonding layers arranged at intervals, and the conductive layer 250 is electrically connected to the heating layer 230.

Of course, in some other embodiments, the target material of the conductive layer 250 can be adaptively selected according to the material of the required bonding layer; for example, when the material of the conductive layer 250 is Au, the target material during the sputtering of the conductive layer 250 is selected as Au Target; the thickness of the conductive layer 250 can be adjusted according to the needs of the coating time, power density and resistance of the target.

In step S160, a protective layer 260 is prepared on the substrate 210 on which the conductive layer 250 and the heating layer 230 are prepared.

Specifically, the substrate 210 prepared with the heating layer 230 is equipped with a protective layer mask, and then placed in the coating machine; argon gas is introduced to the working pressure of the coating machine at 0.5 Pa ~ 2 Pa, and sputtering is performed on the ZrO ₂ target radio frequency power supply The power density is 2 W/cm ² to 6 W/cm ² , and the temperature is 25° C. to 500° C., and the film is sputtered to form a protective layer 260 with a thickness of 700 nm to 1000 nm. Further, the sputtering film is formed under the conditions of a ZrO ₂ target radio frequency power supply sputtering power density of 3W/cm ² ～5W/cm ² and a temperature of 40℃～300℃ to form a protective layer 260 with a thickness of 750nm～950nm .

Further, after the step of forming the protective layer 260, it further includes increasing the power density of the ZrO ₂ target material to 6W/cm ² ～8W/cm ² sputtering for 2 to 5 minutes, so that scattered large particles (like milky particles) appear on the surface of the protective layer 260突结构).

In the illustrated embodiment, a conductive protective layer 260 is deposited on a plurality of heating layers 230 arranged at intervals, and the protective layer 260 covers a part of the conductive layer 250.

Of course, in some other embodiments, the target material of the protective layer 260 can be adaptively selected according to the material of the protective layer 260; for example, when the material of the protective layer 260 is ZrO ₂ and Al ₂ O ₃ , the conductive layer 260 is splashed. ZrO ₂ target and Al ₂ O ₃ target are selected as the target materials during shooting; the thickness of the conductive layer 250 can be adjusted according to the needs of the coating time, the power density of the target and the high temperature stability of the material.

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

Specifically, after the protective layer 260 is prepared, the substrate 210 on which the protective layer 260 is prepared is cut to obtain a plurality of heating elements 200. In this embodiment, the cutting method is laser cutting.

Of course, in some embodiments, it is also possible to prepare only one transition layer and corresponding other film layers on the substrate 210. In this case, step S170 is omitted.

It can be understood that, in some embodiments, the bonding layer and the conductive layer 250 can also be prepared first, and then the transition layer and the heating layer 230 are prepared, as long as the conductive layer 250 and the heating layer 230 are electrically connected.

The above-mentioned preparation method of the heating element 20 adopts magnetron sputtering and a mask method to prepare each film layer, so that the film thickness consistency of each film layer and the film layer pattern position accuracy are greatly improved. The thickness deviation of the heating layer is ≤5%, the position accuracy of the heating layer pattern can reach ±3μm, the resistance value of the heating layer is better, and the smoking taste consistency of the electronic cigarette is greatly improved.

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

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

Specifically, the insulator 300 is disposed on the side of the conductive layer 150 of the heating element 100 away from the heating layer 130 to isolate the heating element 100 from other components of the electronic cigarette 10 (for example, the power supply 400). The electrical connector 500 is linear. 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 heating layer 130, the conductive layer 150 and the power supply 400 can form a current loop.

When using the above-mentioned electronic cigarette 10, the heating element 100 is inserted into the tobacco 20, and the current loop between the heating element 100 and the power supply 400 is opened, so that the heating element 100 generates heat, thereby heating the tobacco 20.

The above-mentioned electronic cigarette 10 includes the above-mentioned heating element 100, which has stable heating, strong corrosion resistance and long service life.

Application of the above electronic cigarette 10 in preparing tobacco flavor or tobacco flavor aerosol.

The above-mentioned electronic cigarette 10 uses a relatively low temperature heat source to heat the tobacco, and can be applied to prepare tobacco flavor or tobacco flavor aerosol.

Specific embodiment

The detailed description will be given below in conjunction with specific embodiments. The following examples are not specifically stated, and do not include other components except unavoidable impurities. The drugs and instruments used in the examples are conventional choices in the art unless otherwise specified. The experimental methods that do not specify specific conditions in the examples should be implemented in accordance with conventional conditions, such as the conditions described in the literature, books, or the method recommended by the manufacturer.

Example 1

The structure of the heating element of Example 1 includes a substrate, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer. The transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, and the bonding layer is laminated on the substrate. Above, the bonding layer is connected with the transition layer, the conductive layer is laminated on the side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the material of the transition layer is ZrNi, the thickness of the transition layer is 170nm, the material of the heating layer is NiCr, the thickness of the heating layer is 3μm, the material of the bonding layer is titanium, the thickness of the bonding layer is 200nm, conductive The material of the layer is silver, the thickness of the conductive layer is 3.2 μm, the material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850 nm. The specific preparation steps of the heating element of Example 1 are as follows:

(1) Pretreatment: After cleaning the zirconia ceramic substrate with a NaOH solution with a mass concentration of 8% and a mixed acid with a volume concentration of 23% (the volume ratio of HF to HNO ₃ is 1:4), put it into the coating chamber Inside, evacuated and preheated to 100°C, and then ion-cleaned the substrate surface with ion beam.

(2) Take two pre-treated zirconia ceramic substrates and perform the following operations respectively to obtain two substrates coated with a transition layer and a heating layer that have undergone a vacuum heat treatment at 800°C for 10 minutes: add on the pre-treated zirconia ceramic substrate Install the transition layer mask, pass argon gas into the cavity to a working pressure of 5×10 ^-1 Pa, set the power density of the ZrNi target to 7W/cm ² , and conduct the coating for 15 minutes at room temperature (25°C) to obtain a thickness of 170nm Transition layer. Then close the ZrNi target, set the power density of the NiCr target to 7W/cm ² , and coat the film at room temperature for 120 minutes to form a heating layer with a thickness of 3 μm on the transition layer. Then vent the gas out of the furnace, and subject the base plated with the transition layer and the heating layer to 800°C vacuum heat treatment for 15 minutes.

(3) One of the substrates coated with the transition layer and the heating layer that has undergone a vacuum heat treatment at 800°C for 15 minutes is heated for 6000 times in the air at 400°C for 2 minutes/stop for 1 minute. The electrical bridge method was used to compare the resistance changes of the heating layer before and after the treatment; the scanning electron microscope was used to compare the topography changes of the heating layer surface before and after the treatment.

(4) Add a bonding layer mask to another substrate coated with a transition layer and a heating layer that has undergone a vacuum heat treatment at 800°C for 15 minutes, and then place it in a sputtering furnace, and pass argon gas to the coating environment pressure of 5×10 ^-1 Pa, the power density of the titanium target is set to 7W/cm ² , and the film is coated at room temperature for 15 minutes to form a bonding layer of 200 nm. Then the titanium target is closed, and the power density of the silver target is 4W/cm ² and the film is plated for 90 minutes under normal temperature conditions to obtain a conductive layer with a thickness of 3.2 μm.

(5) Install a protective layer mask on the substrate with the heating layer and the conductive layer obtained in step (4), and then place it in the coating machine, and pass argon gas to the working pressure of the coating machine at 1.5 Pa, and place it on the ZrO ₂ target The sputtering power density of the radio frequency power supply was 5 W/cm ² and the sputtering film was formed at a temperature of 50° C. to form a protective layer with a thickness of 850 nm to obtain the heating element of Example 1.

(6) The thermal stability of the heating element prepared in step (5) is measured by the cyclic energization method.

Measured by the bridge method, the resistance change rate of the heating layer of Example 1 before and after the cyclic heating treatment is ≤1%.

Measured by the cyclic energization method, the heating element of Example 1 has no obvious change in resistance value and surface morphology after heating at 400° C. for 6000 times.

Example 2

The structure of the heating element of Example 2 includes a substrate, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer. The transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, and the bonding layer is laminated on the substrate Above, the bonding layer is connected with the transition layer, the conductive layer is laminated on the side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate; the materials of the transition layer are ZrNi and NiCr. From the side close to the substrate to the side away from the substrate, the NiCr in the transition layer gradually increases, and the thickness of the transition layer is 170nm; the material of the heating layer is NiCr The thickness of the heating layer is 3μm, the material of the bonding layer is titanium, the thickness of the bonding layer is 200nm, the material of the conductive layer is silver, the thickness of the conductive layer is 3.2μm, the material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850nm.

The method for preparing the heating element in Example 2 is substantially the same as that in Example 1, except that the preparation of the transition layer in Example 2 is different from that in Example 1. The preparation steps of the transition layer of Example 2 are:

Add a transition layer mask on the pre-treated zirconia ceramic substrate, and pass argon gas to the chamber to a working pressure of 5×10 ^-1 Pa. The power density of the ZrNi target material is 7W/cm ^{2 and} the film is coated for 4 minutes at room temperature ; Then reduce the power density of the ZrNi target to 5W/cm ² , and open the NiCr target until the target power density is 1W/cm ² , and coat for 4 minutes; then reduce the power density of the ZrNi target to 3W/cm ² and increase the power density of the NiCr target to 3W / cm ^2, coating 4min; ZrNi was then reduced to a target power density of 1W / cm ² and power density to increase the target NiCr 5W / cm ^2, coating 4min, a thickness of the transition layer of 170nm.

The morphological changes of the surface of the heating layer before and after the cyclic heating treatment are shown in Figures 7-8. Fig. 7 is an image of the substrate coated with a transition layer and a heating layer before processing under 3K times of a scanning electron microscope; Fig. 8 is an image of a substrate plated with a transition layer and a heating layer after processing under 3K times of a scanning electron microscope.

It can be seen from Fig. 7 and Fig. 8 that the morphology of the substrate coated with the transition layer and the heating layer before and after the cyclic heating treatment does not change significantly, showing excellent cyclic heating stability.

Measured by the cyclic energization method, the heating element of Example 2 has no obvious change in resistance and surface morphology after heating at 400° C. for 6000 times.

Example 3

The structure of the heating element of Example 3 includes a base, a heating layer, a protective layer, a bonding layer, and a conductive layer. The heating layer is laminated on the base, the bonding layer is laminated on the base, the bonding layer is connected to the heat generating layer, and the conductive layer is laminated on the bonding On the side of the layer away from the substrate, the conductive layer is electrically connected to the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the heating layer material is NiCr, the heating layer thickness is 3μm, the bonding layer material is titanium, the bonding layer thickness is 200nm, the conductive layer material is silver, and the conductive layer thickness is 3.2μm. The material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850 nm.

The preparation method of the heating element of Example 3 is substantially the same as the preparation method of the heating element of Example 1, except that the transition layer of Example 3 is omitted, and the heating layer of Example 3 is laminated on the substrate.

Measured by the cyclic energization method, the heating element of Example 3 was circulated at 400°C for 50 times and the heating film fell off and failed.

Example 4

The structure of the heating element of Example 4 includes a substrate, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer. The transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, and the bonding layer is laminated on the substrate. Above, the bonding layer is connected with the transition layer, the conductive layer is laminated on the side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the material of the transition layer is Ti, the thickness of the transition layer is 170nm, the material of the heating layer is NiCr, the thickness of the heating layer is 3μm, the material of the bonding layer is titanium, the thickness of the bonding layer is 200nm, conductive The material of the layer is silver, the thickness of the conductive layer is 3.2 μm, the material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850 nm.

The preparation method of the heating element of Example 4 is substantially the same as the preparation method of the heating element of Example 1. The difference is that the target material for preparing the transition layer of Example 4 is a titanium target, and the thickness of the transition layer of Example 4 is 170 nm .

Measured by the cyclic energization method, the heating element of Example 4 was circulated at 400°C for 200 times and the heating film fell off and failed.

Example 5

The structure of the heating element of Example 5 includes a substrate, a transition layer, a heating layer, a protective layer, a bonding layer, and a conductive layer. The transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, and the bonding layer is laminated on the substrate. Above, the bonding layer is connected with the transition layer, the conductive layer is laminated on the side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the material of the transition layer is ZrTi, the thickness of the transition layer is 170nm, the material of the heating layer is NiCr, the thickness of the heating layer is 3μm, the material of the bonding layer is titanium, the thickness of the bonding layer is 200nm, conductive The material of the layer is silver, the thickness of the conductive layer is 3.2 μm, the material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850 nm.

The preparation method of the heating element of Example 5 is roughly the same as the preparation method of the heating element of Example 1. The difference is that the target material for preparing the transition layer of Example 5 is a ZrTi target, and the thickness of the transition layer of Example 5 is 170 nm .

Measured by the bridge method, the resistance change rate of the heating layer of Example 5 before and after the cyclic heating treatment is ≤1%; measured by the cyclic energization method, the heating element of Example 5 has been cyclically heated at 400°C for 6000 times in resistance and surface No obvious change in morphology.

Example 6

The structure of the heating element of Example 6 includes a substrate, a transition layer, a heating layer, a protective layer, a bonding layer and a conductive layer. The transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, and the bonding layer is laminated on the substrate. Above, the bonding layer is connected with the transition layer, the conductive layer is laminated on the side of the bonding layer away from the base, the conductive layer is electrically connected with the heating layer, and the protective layer is laminated on the heating layer and partially covers the conductive layer. The substrate is a zirconia ceramic substrate, the material of the transition layer is ZrNi, the thickness of the transition layer is 170nm, the material of the heating layer is platinum, the thickness of the heating layer is 3μm, the material of the bonding layer is titanium, the thickness of the bonding layer is 200nm, conductive The material of the layer is silver, the thickness of the conductive layer is 3.2 μm, the material of the protective layer is ZrO ₂ , and the thickness of the protective layer is 850 nm.

The preparation method of the heating element of Example 6 is substantially the same as the preparation method of the heating element of Example 1, except that the target for preparing the heating layer of Example 6 is a platinum target, and the thickness of the heating layer of Example 6 is 3 μm. .

The heating element prepared in Example 6 is shown in FIG. 9.

The thermal stability of the heating element prepared in Example 6 was measured by the cyclic energization method. The surface morphology of the heating element before and after the cyclic heating treatment is shown in Figures 10-11. Fig. 10 is a scanning electron microscope image of the heating element before treatment; Fig. 11 is a scanning electron microscope image of the heating element after treatment.

It can be seen from Fig. 10 and Fig. 11 that the morphology of the heating element does not change significantly before and after dry firing, and it shows excellent cyclic heating stability.

The resistance value of the heating element of Example 6 is in the range of 0.6Ω-1.2Ω, and the resistance value change rate is less than 1% after 4000 cycles of dry firing. The details are shown in Table 1.

Table 1

循环次数/次Cycle times/time	阻值/ΩResistance/Ω
初始值Initial value	0.770.77
10001000	0.770.77

20002000	0.770.77
30003000	0.770.77
40004000	0.770.77

The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, All should be considered as the scope of this specification.

The above-mentioned embodiments only express several embodiments of the present invention, and the descriptions are more specific and detailed, but they should not be understood as limiting the scope of the invention patent. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.

Claims

A heating element comprising a substrate, a transition layer and a heating layer, the transition layer is laminated on the substrate, the heating layer is laminated on the side of the transition layer away from the substrate, the substrate is a ceramic substrate, The material of the transition layer is an alloy, the transition layer forms a chemical bond with the substrate, and the transition layer also forms a chemical bond with the heating layer.
The heating element according to claim 1, wherein the transition layer and the base form a metal bond, and the transition layer and the heating layer also form a metal bond.
The heating element according to claim 1, wherein the material of the transition layer includes at least one of ZrNi, ZrTi, NiCr and TiN; and/or

The thickness of the transition layer is 100 nm to 200 nm.
The heating element according to claim 3, wherein the material of the transition layer includes ZrNi and NiCr.
The heating element according to claim 1, wherein the material of the heating layer includes at least one of nickel alloy, silver alloy, gold alloy and platinum; and/or

The thickness of the heating layer is 2 μm to 6 μm.
The heating element according to claim 5, wherein the material of the heating layer is selected from at least one of NiCr, NiCrAlY, AgAu, AgPd, AgPt, AuPt, AuPd, and platinum.
The heating element according to claim 5, wherein the material of the heating layer is a silver alloy.
The heating element according to claim 7, wherein the material of the heating layer is selected from at least one of AgAu, AgPd, and AgPt.
The heating element according to claim 1, wherein the substrate is a zirconia ceramic substrate, the material of the transition layer includes at least one of ZrNi, ZrTi and TiN and NiCr, and the material of the heating layer includes At least one of NiCr, AgPd, and NiCrAlY.
9. The heating element according to claim 9, wherein the NiCr in the transition layer gradually increases from the side close to the substrate to the side away from the substrate.
The heating element according to any one of claims 1 to 10, further comprising a protective layer laminated on the side of the heating layer away from the transition layer; the material of the protective layer is selected From at least one of ZrO 2 , Al 2 O 3 and Si 3 N 4 .
The heating element according to claim 11, wherein the material of the protective layer is selected from at least one of ZrO 2 and Al 2 O 3 ; and/or

The thickness of the protective layer is 700 nm to 1000 nm.
The heating element according to claim 11, wherein the protective layer has a papilla-like structure formed on a side of the protective layer away from the heating layer.
The heating element according to claim 11, further comprising a conductive layer, the conductive layer is located on a side of the substrate close to the transition layer, and is electrically connected to the heating layer.
The heating element according to claim 14, wherein the thickness of the conductive layer is 1 μm to 8 μm.
The heating element according to claim 14, further comprising a bonding layer laminated between the base and the conductive layer, and the bonding layer is made of materials selected from titanium, chromium, aluminum, At least one of nickel and nickel alloy.
The heating element according to claim 16, wherein the thickness of the bonding layer is 200 nm to 700 nm.
The heating element of claim 16, wherein the material of the transition layer is ZrNi, the material of the heating layer is platinum, and the sum of the thickness of the transition layer and the heating layer is 2 μm-4 μm; The material of the bonding layer is titanium or ZrNi, the material of the conductive layer is silver, the sum of the thickness of the bonding layer and the conductive layer is 2 μm-4 μm; the material of the protective layer is ZrO 2 , The thickness of the protective layer is 700 nm to 1000 nm.
A method for preparing a heating element includes the following steps:

Depositing a transition layer on a substrate, the substrate is a ceramic substrate, the material of the transition layer is an alloy, and the transition layer forms a chemical bond with the substrate; and

A heating layer is formed on the transition layer, and the heating layer forms a chemical bond with the transition layer.
An electronic cigarette, comprising the heating element according to any one of claims 1-18 or the heating element produced by the heating element preparation method according to claim 19.