Metal heating film and preparation method and application thereof

Abstract

The invention belongs to the technical field of metal heating materials, and particularly relates to a metal heating film and a preparation method and application thereof. According to the metal heating film, at least one element of Ru, Pt and Pd is introduced into the nickel-chromium alloy or the nickel metal and forms an alloy with the nickel-chromium alloy or the nickel metal, so that the tobacco tar high-temperature corrosion resistance of the obtained metal heating film is improved, and the content of elements such as Ni and Cr in smoke is reduced. Besides, after Ru, Pt and Pd elements are introduced, the elements, Ni, Cr and other elements can form alloys, the fluxing effect is achieved, the heating film is sintered more compactly, the capacity of resisting cold and hot impact of tobacco tar is higher, and the heating film is not prone to cracking and losing efficacy in the smoking process. Meanwhile, the elements have a modification effect on the surface microstructure of the heating film, various components in the tobacco tar can be atomized more harmoniously, and the taste consistency is better.

Description

[0001] This application is a divisional application. The application number of its parent application is 202210420215.3, the application date is April 20, 2022, and the invention title is "A Metal Heating Film and Its Preparation Method and Application". Technical Field

[0002] The present invention belongs to the technical field of metal heating materials, and specifically relates to a metal heating film and its preparation method and application. Background Art

[0003] An electronic cigarette is an electronic product that imitates a cigarette. Although it does not contain tar, it has the same appearance, smoke, taste, and feeling as a cigarette. It is a product that allows users to inhale by means of atomization and turns nicotine into vapor.

[0004] The atomization core of an electronic cigarette is the core component of the electronic cigarette and plays a crucial role in the performance of the electronic cigarette, such as taste and smoke volume. The atomization core of the electronic cigarette has gone through an update from fiberglass, cotton to porous honeycomb ceramics. Among them, the fiberglass atomization core has a small smoke volume and poor taste; although the cotton core has improved in taste and smoke volume, it still has deficiencies such as short lifespan, easy wicking, and oil leakage; while the ceramic atomization core not only has a good taste, does not wick, does not explode oil, but also has a long lifespan. Especially after using a heating film with better lipophilicity to replace the heating wire to heat the e-liquid, the contact area between the heating component and the e-liquid is increased, and the atomization efficiency and taste are further improved.

[0005] However, at present, most of the heating film materials for ceramic atomization cores of electronic cigarettes use nickel-chromium alloys. At the atomization temperature of e-liquid, due to the high-temperature corrosion of the e-liquid, a very small amount of Ni and Cr elements will enter the smoke. In order to further improve the safety of the smoke, we hope to further reduce the content of Ni and Cr elements in the smoke, so as to avoid the harm of Ni and Cr elements in the smoke to the body and ensure the safety of users' inhalation.

[0006] In view of this, there is an urgent need to develop a metal heating film and its preparation method that can further reduce the content of Ni and Cr elements in the smoke. Summary of the Invention

[0007] Therefore, the technical problem to be solved by the present invention is to overcome the defect that the content of Ni and Cr elements in the smoke in the prior art needs to be further reduced, so as to provide a metal heating film and its preparation method and application.

[0008] For this reason, the present invention provides the following technical solutions:

[0009] The present invention provides a metal heating film, which is a nickel-chromium alloy-based metal heating film or a nickel-based metal heating film, and further includes at least one of the metal elements Ru, Pt, and Pd.

[0010] Optionally, the metal heating film includes the metal element Ru.

[0011] Optionally, the metal heating film includes the metal elements Ru, Pt, and Pd.

[0012] Optionally, based on the total mass of the metal heating film, the content of Ru is 0-24%, the content of Pt is 0-21%, the content of Pd is 0-19%, and the contents of the three metal elements Ru, Pt, and Pd are not all 0 at the same time;

[0013] Optionally, the content of the metal element Ru is not 0, and the contents of the metal elements Pt and Pd are 0; or, the three metal elements Ru, Pt, and Pd exist simultaneously.

[0014] Optionally, based on the total mass of the metal heating film, the content of Ni is 24-55%; the content of Cr is 0-23%.

[0015] Optionally, based on the total mass of the metal heating film, it further includes: Fe 0-18%; Nb 0-4%; Mn 0-3%; Mo 0-2%; W 0-2%; Si 0-2.5%.

[0016] The present invention also provides a preparation method of a metal heating film, including the following steps,

[0017] Based on the total mass of the raw materials, 60-90% of metal components, 0.5-9% of glass powder, and 8-40% of organic carrier are mixed to obtain a slurry;

[0018] The obtained slurry is coated on a substrate, and after drying and sintering, the metal heating film is obtained;

[0019] Among them, based on the total mass of the metal components and the glass powder, it includes Ni 24-55%, Cr 0-23%, Fe 0-18%, Ru 0-24%, Pt 0-21%, Pd 0-19%, Nb 0-4%, Mn 0-3%, Mo 0-2%, W 0-2%, Si 0-6%, and the contents of the three metal elements Ru, Pt, and Pd are not all 0 at the same time.

[0020] Optionally, it further includes the step of making the metal components into metal powder. Each metal component is weighed according to the proportion, mixed, melted, and atomized to obtain metal powder.

[0021] Optionally, the melting temperature of the metal components is 1400°C - 1600°C.

[0022] Optionally, the metal components other than Ru, Pt, and Pd in the metal component are made into metal powder.

[0023] Optionally, the method for preparing the metal heating film satisfies at least one of the following (1)-(10):

[0024] (1) Based on the total mass of the glass powder, the composition of the glass powder includes: silicon oxide 30-73%, boron oxide 2-23%, aluminum oxide 0.5-8%, calcium oxide 0-7%, zinc oxide 4-12%, magnesium oxide 0-5%, titanium oxide 1-5%, sodium oxide 0-11%, potassium oxide 0-3%, zirconium oxide 0.2-4%;

[0025] (2) Based on the total mass of the metal component and the glass powder, it also includes B 0-2%, Al 0-1%, Ca 0-1%, Zn 0-1.5%, Mg 0-1%, Ti 0-0.5%, Na 0-1.5%, K 0-0.5%, Zr 0-0.5%;

[0026] (3) The method for preparing the glass powder includes: mixing the required oxides in proportion, melting, water quenching, and grinding to obtain the glass powder;

[0027] Optionally, the melting temperature of the glass powder is 1450-1550 °C.

[0028] (4) The particle size of the glass powder is 1-15 μm;

[0029] (5) The organic carrier is a mixture of ethyl cellulose, acrylic resin, tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate;

[0030] Optionally, the mass ratio of ethyl cellulose, acrylic resin, tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate in the organic carrier is 1:0.1-0.3:0.4-0.6:7-9:6-9:3-5.

[0031] Optionally, the organic carrier can be mixed under heating conditions, and the heating temperature can be 75-90 °C.

[0032] (6) The slurry is coated onto the substrate by screen printing;

[0033] (7) The substrate is a ceramic substrate;

[0034] (8) The drying temperature is 100-300 °C;

[0035] (9) The sintering temperature is 800-1500 °C;

[0036] (10) The sintering time is 0.5 - 3 h;

[0037] (11) The sintering atmosphere is vacuum, nitrogen or argon atmosphere.

[0038] The present invention also provides an e - cigarette atomizing core, including the above - mentioned metal heating film or the metal heating film prepared by the above - mentioned preparation method.

[0039] The present invention also provides an e - cigarette, including the above - mentioned e - cigarette atomizing core.

[0040] The present invention has no special limitation on other structures and preparation methods of the e - cigarette atomizing core and the e - cigarette. The main improvement lies in the adoption of the metal heating film provided by the present invention or the metal heating film prepared by the above - mentioned method.

[0041] The nickel - chromium alloy - based metal heating film or nickel - based metal heating film described in the present invention refers to an alloy in which other metal components are doped in nickel - chromium alloy or nickel metal.

[0042] The technical solution of the present invention has the following advantages:

[0043] The metal heating film provided by the present invention, the metal heating film is a nickel - chromium alloy - based metal heating film or a nickel - based metal heating film, and further includes at least one of the metal elements Ru, Pt, Pd. By introducing at least one of the elements Ru, Pt, Pd into nickel - chromium alloy or nickel metal and forming an alloy with nickel - chromium alloy or nickel metal, the present invention improves the high - temperature corrosion resistance of the obtained metal heating film to tobacco oil, and reduces the content of elements such as Ni and Cr in the smoke. In addition, after introducing the elements Ru, Pt, Pd, these elements can form an alloy with elements such as Ni and Cr, playing a fluxing effect, making the sintering of the heating film more dense, enhancing the ability of the heating film to resist the thermal and cold shock of tobacco oil, and the heating film is not prone to cracking and failure during the suction process. At the same time, these elements have a modifying effect on the surface microstructure of the heating film, and various components in the tobacco oil can be atomized more coordinately, and the taste consistency is better.

[0044] By limiting the content of each component in the metal heating film, the metal heating film provided by the present invention can further improve the high - temperature corrosion resistance of the metal heating film to tobacco oil. Especially when the metal elements Ru, Pt, Pd exist simultaneously, the high - temperature corrosion resistance of the metal heating film to tobacco oil is optimal, and the content of elements such as Ni and Cr in the smoke is the lowest.

[0045] The preparation method of the metal heating film provided by the present invention can introduce elements such as Ru, Pt, or Pd into nickel-chromium alloy or nickel metal, and form an alloy with the nickel-chromium alloy, improving the high-temperature corrosion resistance of the obtained metal heating film to tobacco oil and reducing the content of elements such as Ni and Cr in the flue gas. In addition, these elements can also play a fluxing effect, making the sintering of the heating film more dense, enhancing the ability of the heating film to resist the thermal shock of tobacco oil, and making it less likely for the heating film to crack and fail during the suction process. At the same time, these elements have a modifying effect on the surface microstructure of the heating film, enabling various components in the tobacco oil to be atomized more coordinately and resulting in better taste consistency.

[0046] In the preparation method of the metal heating film provided by the present invention, through further limitation of the preparation steps, the metal components other than Ru, Pt, and Pd in the metal components are made into metal powders. In this way, elements such as Ru, Pt, and Pd can be introduced into the nickel-based alloy or nickel metal, enabling these highly corrosion-resistant metals to be enriched on the surface of the metal powder, and finally forming a structure with low content of elements such as Ru, Pt, and Pd inside the heating film and high content outside, which can further improve the corrosion resistance of the heating film; in addition, in this case, it is equivalent to covering the heating film with Ru, Pt, Pd, etc. When the content levels of elements such as Ni and Cr in the flue gas are equivalent, the demand for elements such as Ru, Pt, and Pd is low, reducing the economic cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for use in the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0048] Figure 1 It is a picture of the heating film provided in Example 1 of the present invention after the cracking test;

[0049] Figure 2 It is a picture of the heating film provided in Example 2 of the present invention after the cracking test;

[0050] Figure 3 It is a picture of the heating film provided in Example 3 of the present invention after the cracking test;

[0051] Figure 4 It is a picture of the heating film provided in Example 4 of the present invention after the cracking test;

[0052] Figure 5 It is a picture of the heating film provided in Example 5 of the present invention after the cracking test;

[0053] Figure 6 It is a picture of the heating film provided in Embodiment 6 of the present invention after the cracking test;

[0054] Figure 7 It is a picture of the heating film provided in Embodiment 7 of the present invention after the cracking test;

[0055] Figure 8 It is a picture of the heating film provided in Comparative Example 1 of the present invention after the cracking test. Detailed implementation manners

[0056] The following embodiments are provided to better further understand the present invention. It is not limited to the described best implementation manner, and does not limit the content and protection scope of the present invention. Any product that is the same as or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other prior art features falls within the protection scope of the present invention.

[0057] For those embodiments where specific experimental steps or conditions are not indicated, the operations or conditions of the conventional experimental steps described in the literature in this field can be followed. For reagents or instruments whose manufacturers are not indicated, they are all conventional reagent products that can be obtained through commercial purchase.

[0058] Embodiment 1

[0059] This embodiment provides a preparation method of a metal heating film, and the specific steps are as follows:

[0060] The raw material composition is: 80 wt% of metal components, 5 wt% of glass powder, and 15% of organic carrier;

[0061] Among them, the composition of the metal components is: 65 wt% of Ni, 10 wt% of Cr, 5 wt% of Fe, 5 wt% of Ru, 2 wt% of Pt, 3 wt% of Pd, 2 wt% of Nb, 3 wt% of Mn, 3 wt% of Mo, 1 wt% of W, and 1 wt% of Si;

[0062] The composition of the glass powder is: 65% of silicon oxide, 5% of boron oxide, 8% of aluminum oxide, 7% of calcium oxide, 6% of zinc oxide, 3% of magnesium oxide, 1% of titanium oxide, 4% of sodium oxide, 0.5% of potassium oxide, and 0.5% of zirconium oxide.

[0063] Heating film preparation method:

[0064] Preparation of metal powder: After the purchased Ni, Cr, Fe, Ru, Pt, Pd, Nb, Mn, Mo, W, and Si materials are prepared and mixed according to the above ratios, they are melted at 1500 °C and then metal powder is prepared by gas atomization method. The injection apex angle α = 46°, the length z of the liquid guide tube extending out is 2 mm, the inner diameter d of the liquid guide tube is 4 mm, and nitrogen is selected for atomization powder making, and it is reserved for use;

[0065] Preparation of glass powder: After weighing the required oxides according to the above ratios, mix them evenly, place them in an alumina crucible, heat to 1520 °C until melted, pour into deionized water, quench into glass slag, and then crush the glass slag to 1 - 15 μm by mechanical ball milling for standby;

[0066] Organic carrier: Weigh ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate (manufacturer: Sinopharm) according to a mass ratio of 1:0.2:0.5:8:7.5:4, place them in a beaker, heat to 85 °C to completely dissolve, and set aside for standby;

[0067] Preparation of heating film slurry: Weigh the required proportions of metal powder, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0068] Print the heating film slurry on the surface of a ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare a heating film circuit, and the pattern is as Figure 1 shown, with a length of 9 mm × a width of 3.5 mm; after drying at 200 °C, then sinter at 1200 °C for 2 h to form a ceramic substrate heating film.

[0069] Example 2

[0070] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0071] The raw material composition is: Metal component No. 1 60 wt%, Metal component No. 2 26 wt%, glass powder 6 wt%; organic carrier 8%;

[0072] Among them, the composition of Metal component No. 1 is: Ni 85 wt%, Cr 15 wt%;

[0073] The composition of Metal component No. 2 is 100 wt% Ru powder;

[0074] The composition of the glass powder is: silicon oxide 67%, boron oxide 8%, aluminum oxide 3%, calcium oxide 5%, zinc oxide 7%, magnesium oxide 3%, titanium oxide 2%, sodium oxide 3%, potassium oxide 1%, zirconium oxide 1%.

[0075] Heating film preparation method:

[0076] Preparation of Metal powder No. 1: After mixing the purchased Ni and Cr materials according to the above ratios, melt at 1500 °C and prepare metal powder by gas atomization method. The injection apex angle α = 46°, the length of the liquid guide tube extending out z = 2 mm, the inner diameter of the liquid guide tube d = 4 mm, and nitrogen is selected for atomization powder making for standby;

[0077] Preparation of glass powder: After weighing the required oxides according to the above proportions, mix them evenly, place them in an alumina crucible, heat to 1480 °C until melted, pour into deionized water, quench into glass slag, and then crush the glass slag to 1-15 μm by mechanical ball milling for standby;

[0078] Organic carrier: Weigh ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate (manufacturer: Sinopharm) according to a mass ratio of 1:0.2:0.5:8:7.5:4, place them in a beaker, heat to 80 °C to completely dissolve, and set aside for standby;

[0079] Preparation of heating film slurry: Weigh the required proportions of Metal Powder No. 1, Metal Component No. 2, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0080] Print the heating film slurry on the surface of a ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare a heating film circuit, and the pattern is as Figure 2 shown, with the size or parameter of length 9 mm × width 3.5 mm; after drying at 160 °C, sinter at 1250 °C for 2 h to form a ceramic substrate heating film.

[0081] Example 3

[0082] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0083] The raw material composition is: Metal Component No. 1 65 wt%, Metal Component No. 2 16 wt%, glass powder 5 wt%, and organic carrier 14%;

[0084] Among them, the composition of Metal Component No. 1 is: Ni 100 wt%;

[0085] The composition of Metal Component No. 2 is: Pt powder 100 wt%;

[0086] The composition of the glass powder is: silicon oxide 55%, boron oxide 18%, aluminum oxide 3%, calcium oxide 6%, zinc oxide 10%, magnesium oxide 3%, titanium oxide 1%, sodium oxide 3%, potassium oxide 0.5%, and zirconium oxide 0.5%.

[0087] Heating film preparation method:

[0088] Preparation of Metal Powder No. 1: After mixing the purchased Ni materials according to the above proportions, melt at 1500 °C and prepare metal powder by gas atomization method. The injection apex angle α = 46°, the length of the liquid guide tube extending out z = 2 mm, the inner diameter of the liquid guide tube d = 4 mm, and nitrogen is selected for atomization powder making for standby;

[0089] Preparation of glass powder: After weighing the required oxides according to the above ratios, mix them evenly, place them in an alumina crucible, heat to 1450 °C for melting, pour into deionized water, water-quench to form glass slag, and then crush the glass slag to 1 - 15 μm by mechanical ball milling for standby;

[0090] Organic carrier: Weigh ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate (manufacturer: Sinopharm) according to a mass ratio of 1:0.2:0.5:8:7.5:4, place them in a beaker, heat to 75 °C to completely dissolve, and set aside for standby;

[0091] Preparation of heating film paste: Weigh the required proportions of metal powder No. 1, metal component No. 2, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film paste.

[0092] Print the heating film paste on the surface of a ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare a heating film circuit, and the pattern is as shown in Figure 3 shown, with the size or parameters of length 9 mm × width 3.5 mm; after drying at 160 °C, then sinter at 1150 °C for 0.5 h to form a ceramic substrate heating film.

[0093] Example 4

[0094] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0095] The raw material composition is: 60 wt% of metal component No. 1, 15.2 wt% of metal component No. 2, 4.8 wt% of glass powder, and 20% of organic carrier;

[0096] Among them, the composition of metal component No. 1 is: 85 wt% Ni, 15% Cr;

[0097] The composition of metal component No. 2 is 100 wt% Pt powder;

[0098] The composition of the glass powder is: 46% silicon oxide, 20% boron oxide, 3% aluminum oxide, 6% calcium oxide, 11% zinc oxide, 4% magnesium oxide, 3% titanium oxide, 3% sodium oxide, 2% potassium oxide, and 2% zirconium oxide.

[0099] Heating film preparation method:

[0100] Preparation of Metal Powder No. 1: After mixing the purchased Ni, Cr and other materials according to the above proportions, they are melted at 1500 °C and then metal powder is prepared by gas atomization method. The injection apex angle α = 46°, the length z of the liquid delivery pipe extending out is 2 mm, the inner diameter d of the liquid delivery pipe is 4 mm, and nitrogen is selected for atomization powder making, and it is reserved for use;

[0101] Preparation of Glass Powder: After weighing the required oxides according to the above proportions, they are mixed evenly, placed in an alumina crucible and heated to 1480 °C for melting, then poured into deionized water, and water quenched into glass slag, and then the glass slag is broken to 1 - 15 μm by mechanical ball milling, and it is reserved for use;

[0102] Organic Carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, butyl carbitol acetate (manufacturer: Sinopharm) are weighed according to the mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, heated to 88 °C to completely dissolve it, and it is reserved for use;

[0103] Preparation of Heating Film Slurry: Weigh the required proportions of Metal Powder No. 1, Metal Component No. 2, glass powder, and organic carrier, and mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0104] The heating film slurry is printed on the surface of the ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare the heating film circuit, and the pattern is as Figure 4 shown, with the size or parameter of length 9 mm × width 3.5 mm; after drying at 100 °C, it is then sintered at 1000 °C for 3 h to form the ceramic substrate heating film.

[0105] Example 5

[0106] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0107] The raw material composition is: 72 wt% of Metal Component No. 1, 9 wt% of Metal Component No. 2, 9 wt% of glass powder, and 10% of organic carrier;

[0108] Among them, the composition of Metal Component No. 1 is: 85 wt% of Ni and 15 wt% of Cr;

[0109] The composition of Metal Component No. 2 is 100 wt% of Pd powder;

[0110] The composition of the glass powder is: 70% of silicon oxide, 8% of boron oxide, 2% of aluminum oxide, 1% of calcium oxide, 8% of zinc oxide, 2% of magnesium oxide, 3% of titanium oxide, 4% of sodium oxide, 1% of potassium oxide, and 1% of zirconium oxide.

[0111] Heating Film Preparation Method:

[0112] Preparation of Metal Powder No. 1: After mixing the purchased Ni and Cr materials according to the above - mentioned ratio, they are melted at 1500 °C and then metal powder is prepared by gas atomization method. The injection apex angle α = 46°, the extension length z of the liquid - guiding tube is 2 mm, the inner diameter d of the liquid - guiding tube is 4 mm, and nitrogen is selected for atomization powder preparation for standby;

[0113] Preparation of glass powder: After weighing the required oxides according to the above - mentioned ratio, they are mixed evenly, placed in an alumina crucible, heated to 1480 °C for melting, then poured into deionized water, quenched into glass slag, and then the glass slag is crushed to 1 - 15 μm by mechanical ball - milling for standby;

[0114] Organic carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, butyl carbitol acetate (manufacturer: Sinopharm) are weighed according to the mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, heated to 75 °C to completely dissolve for standby;

[0115] Preparation of heating film slurry: Weigh the required proportion of Metal Powder No. 1, Metal Component No. 2, glass powder, and organic carrier, and mix them evenly, and use a three - roll mill to prepare heating film slurry.

[0116] The heating film slurry is printed on the surface of a ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare a heating film circuit, and the pattern is as Figure 5 shown, with the size or parameters of length 9 mm × width 3.5 mm; after drying at 120 °C, it is then sintered at 1050 °C for 2.5 h to form a ceramic substrate heating film.

[0117] Example 6

[0118] This example provides a metal heating film and its preparation method. The specific steps are as follows:

[0119] The raw material composition is: Metal Component No. 1 72 wt%, Metal Component No. 2 9 wt%, glass powder 9 wt%, organic carrier 10%;

[0120] Among them, the composition of Metal Component No. 1 is: Ni 85 wt%, Cr 15 wt%;

[0121] The composition of Metal Component No. 2 is: Ru powder 30 wt%; Pt powder 35%; Pd powder 35%;

[0122] The composition of the glass powder is: silicon oxide 70%, boron oxide 8%, aluminum oxide 2%, calcium oxide 1%, zinc oxide 8%, magnesium oxide 2%, titanium oxide 3%, sodium oxide 4%, potassium oxide 1%, zirconium oxide 1%.

[0123] Preparation method of heating film:

[0124] Preparation of Metal Powder No. 1: After mixing the purchased Ni and Cr materials according to the above-mentioned ratio, they are melted at 1500 °C and then metal powder is prepared by gas atomization method. The injection apex angle α = 46°, the length z of the liquid guide tube extending out is 2 mm, the inner diameter d of the liquid guide tube is 4 mm, and nitrogen is selected for atomization powder preparation for standby;

[0125] Metal Powder No. 2 is provided by Hunan Laiyin Rhenium Alloy Materials Co., Ltd.

[0126] Preparation of glass powder: After weighing the required oxides according to the above-mentioned ratio, they are mixed evenly, placed in an alumina crucible and heated to 1480 °C for melting, then poured into deionized water, quenched into glass slag, and then the glass slag is broken to 1 - 15 μm by mechanical ball milling for standby;

[0127] Organic carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, butyl carbitol acetate (manufacturer: Sinopharm) are weighed according to the mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, and heated to 75 °C to completely dissolve for standby;

[0128] Preparation of heating film slurry: Weigh the required proportions of Metal Powder No. 1, Metal Powder No. 2, glass powder, and organic carrier, and mix them evenly, and then use a three-roll mill to prepare the heating film slurry.

[0129] The heating film slurry is used to print and prepare a heating film circuit on the surface of a ceramic substrate (manufacturer: McWell, AT02) by screen printing. The pattern is as Figure 6 shown, with the size or parameter of length 9 mm × width 3.5 mm; after drying at 120 °C, it is then sintered at 1050 °C for 2.5 h to form a ceramic substrate heating film.

[0130] Example 7

[0131] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0132] The raw material composition is: 80 wt% of metal components, 5 wt% of glass powder, and 15 wt% of organic carrier;

[0133] Among them, the composition of the metal components is: 65 wt% of Ni, 10 wt% of Cr, 5 wt% of Fe, 5 wt% of Ru, 2 wt% of Pt, 3 wt% of Pd, 2 wt% of Nb, 3 wt% of Mn, 3 wt% of Mo, 1 wt% of W, 1 wt% of Si;

[0134] The composition of the glass powder is as follows: 65% silicon oxide, 5% boron oxide, 8% aluminum oxide, 7% calcium oxide, 6% zinc oxide, 3% magnesium oxide, 1% titanium oxide, 4% sodium oxide, 0.5% potassium oxide, and 0.5% zirconium oxide.

[0135] Preparation method of the heating film:

[0136] Preparation of Metal Powder No. 1: The purchased Ni, Cr, Fe, Nb, Mn, Mo, W, Si (excluding Ru and Pt) materials are mixed according to the above proportions, melted at 1500 °C, and then metal powder is prepared by gas atomization. The injection apex angle α = 46°, the length z of the liquid guide tube extending out is 2 mm, the inner diameter d of the liquid guide tube is 4 mm, and nitrogen is selected for atomization to prepare powder for standby;

[0137] Preparation of glass powder: After weighing the required oxides according to the above proportions, they are mixed evenly, placed in an alumina crucible, heated to 1520 °C for melting, then poured into deionized water, quenched into glass slag, and then the glass slag is crushed to 1 - 15 μm by mechanical ball milling for standby;

[0138] Organic carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate (manufacturer: Sinopharm) are weighed according to a mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, and heated to 82 °C to completely dissolve for standby;

[0139] Preparation of the heating film slurry: Weigh the required proportions of Metal Powder No. 1, Ru powder, Pt powder, glass powder, and organic carrier, and mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0140] The heating film slurry is used to print and prepare the heating film circuit on the surface of the ceramic substrate (manufacturer: SMOK, AT02) by screen printing. The pattern is as Figure 7 shown, with the size or parameters of length 9 mm × width 3.5 mm; after drying at 120 °C, it is then sintered at 1200 °C for 2 h to form the ceramic substrate heating film.

[0141] Comparative Example 1

[0142] This comparative example provides a metal heating film and its preparation method. The specific steps are as follows:

[0143] The raw material composition is: 86 wt% metal component, 6 wt% glass powder; 8% organic carrier;

[0144] Among them, the composition of the metal component is: 85 wt% Ni, 15 wt% Cr;

[0145] The composition of the glass powder is as follows: 67% silicon oxide, 8% boron oxide, 3% aluminum oxide, 5% calcium oxide, 7% zinc oxide, 3% magnesium oxide, 2% titanium oxide, 3% sodium oxide, 1% potassium oxide, and 1% zirconium oxide.

[0146] Preparation method of the heating film:

[0147] Preparation of the metal powder: After mixing the purchased Ni and Cr materials according to the above-mentioned ratio, they are melted at 1500 °C and then the metal powder is prepared by gas atomization. The injection apex angle α = 46°, the length z of the liquid guide tube protruding is 2 mm, the inner diameter d of the liquid guide tube is 4 mm, and nitrogen is selected for atomization to prepare the powder for standby;

[0148] Preparation of the glass powder: After weighing the required oxides according to the above-mentioned ratio and mixing them evenly, they are placed in an alumina crucible, heated to 1480 °C and melted, then poured into deionized water, quenched into glass slag, and then the glass slag is broken to 1 - 15 μm by mechanical ball milling for standby;

[0149] Organic carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, butyl carbitol acetate (manufacturer: Sinopharm) are weighed according to the mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, heated to 80 °C to completely dissolve them for standby;

[0150] Preparation of the heating film slurry: Weigh the required proportions of metal powder, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0151] The heating film slurry is printed on the surface of the ceramic substrate (manufacturer: SMOK, AT02, AT02) by screen printing to prepare the heating film circuit. The pattern is as Figure 8 shown, with the size or parameter of length 9 mm × width 3.5 mm; after drying at 160 °C, it is then sintered at 1250 °C for 2 h to form the ceramic substrate heating film.

[0152] Test example

[0153] The metal heating films provided in the examples and comparative examples of the present invention are tested. The specific test method is as follows:

[0154] Test of flue gas components: Collect the electronic cigarette aerosol gel and analyze its components using a gas chromatography-mass spectrometer (GC-MS).

[0155] Taste and smoking experiment

[0156] The metal heating films provided in the above embodiments and comparative examples were tested at a power of 6.5 W. Using a blind evaluation scoring method and the large-loop puffing method, e-cigarette liquid was puffed. A 5-person taste puffing group conducted sensory evaluations respectively. The taste evaluation criteria are as described in the following table, mainly including the following evaluation indicators: aroma concentration, irritation (off-flavors), amount of smoke, sweetness, throat hit, humidity of smoke, coordination, and satisfaction. The maximum score for each evaluation indicator is 10 points, and each evaluation indicator is scored in units of 0.5 points.

[0157] The meanings of the 8 indicators are as follows: aroma concentration: the degree of richness of the overall flue gas sensed by the nasal cavity and oral cavity; irritation: the sensory perception of irritation of the flue gas after atomization of e-cigarette liquid in the oral cavity, throat, and nasal cavity, such as granularity, needle prick feeling, and off-flavors, etc.; amount of smoke: the total amount of aerosol formed after atomization of e-cigarette liquid, and the size of the amount of smoke visually observed through oral feeling and exhalation; sweetness: the strength of the sweet taste perceived in the oral cavity after atomization of e-cigarette liquid and the strength of the sweet aroma felt in the nasal cavity; throat hit: the physical sensory intensity of the impact of the flue gas on the throat after inhaling the aerosol; humidity of smoke: the dry-wet degree of the smoke particle droplets sensed by the oral cavity and nasal cavity; coordination: the degree of uniformity and coordination of the mixed aroma after atomization of e-cigarette liquid. Satisfaction: Under the same number of puffs, the feeling of short-term brain excitement reflected by the absorption of nicotine by the lungs, which can be symptoms such as numbness and dizziness in the head.

[0158] Table 1 Sensory Quality Evaluation Criteria for E-Cigarette Liquid

[0159]

[0160]

[0161] Cracking test method and steps:

[0162] Cracking test plan: The heating film was tested by energization at a power of 6.5 W for 3 s, and the energization test was carried out 40 times. Observe the fracture situation of the heating film. As Figures 1-8 shown, it can be seen from the figure that the heating film provided in Comparative Example 1 showed fractures after the cracking test, Figure 8 with cracks in the lower left corner, while no fractures occurred in Examples 1-7, Figures 1-3 and only the color deepened in the lower left corner, but no cracks appeared.

[0163] Specific test results are shown in the following table:

[0164] Table 2

[0165]

[0166] Note: ND indicates below the lower limit of instrument testing.

[0167] Table 3

[0168]

[0169]

[0170] Note: The e-liquid used in the test was provided by an American tobacco company, with the model number BAT-204567.

[0171] From the above test results, it can be seen that in the embodiments of the present invention, by introducing at least one element of Ru, Pt, and Pd into the nickel-chromium alloy, the high-temperature corrosion resistance of the obtained metal heating film to e-liquid is improved, and the contents of elements such as Ni and Cr in the flue gas are reduced. In addition, during the suction process, the heating film is not prone to cracking and failure. At the same time, these elements have a modifying effect on the surface microstructure of the heating film, and various components in the e-liquid can be atomized more coordinately, resulting in better taste consistency. Among them, by comparing the data of Example 6 and Example 5, it can be seen that when the metal elements Ru, Pt, and Pd coexist in Example 6, the high-temperature corrosion resistance of the metal heating film to e-liquid is the best, and the contents of elements such as Ni and Cr in the flue gas are the lowest.

[0172] Obviously, the above embodiments are merely examples given for clear illustration and are not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or modifications derived therefrom are still within the protection scope of the present invention.

Claims

1. A metal heating film, characterized in that, The metal heating film is a nickel-chromium alloy-based metal heating film or a nickel-based metal heating film, and further includes at least one of the metal elements Ru, Pt, and Pd.

2. The metal heating film according to claim 1, characterized in that, The metal heating film includes the metal element Ru.

3. The metal heating film according to claim 2, characterized in that, The metal heating film includes the metal elements Ru, Pt, and Pd.

4. The metal heating film according to claim 1, characterized in that, Based on the total mass of the metal heating film, the content of Ru is 0-24%, the content of Pt is 0-21%, the content of Pd is 0-19%, and the contents of the three metal elements Ru, Pt, and Pd are not 0 at the same time; Optionally, the content of the metal element Ru is not 0, and the contents of the metal elements Pt and Pd are 0; or, the three metal elements Ru, Pt, and Pd exist simultaneously.

5. The metal heating film according to any one of claims 1-4, characterized in that, Based on the total mass of the metal heating film, the content of Ni is 24-55%; the content of Cr is 0-23%; Optionally, based on the total mass of the metal heating film, it further includes: Fe 0-18%; Nb 0-4%; Mn 0-3%; Mo 0-2%; W 0-2%; Si 0-2.5%.

6. A preparation method of a metal heating film, characterized in that, It includes the following steps, Based on the total mass of the raw materials, 60-90% of the metal components, 0.5-9% of the glass powder, and 8-40% of the organic carrier are mixed to obtain a slurry; The obtained slurry is coated on a substrate, and after drying and sintering, the metal heating film is obtained; Among them, based on the total mass of the metal components and the glass powder, it includes Ni 24-55%, Cr 0-23%, Fe 0-18%, Ru 0-24%, Pt 0-21%, Pd 0-19%, Nb 0-4%, Mn 0-3%, Mo 0-2%, W 0-2%, Si 0-6%, and the contents of the three metal elements Ru, Pt, and Pd are not 0 at the same time.

7. The preparation method of the metal heating film according to claim 6, characterized in that, It further includes the step of making the metal components into metal powder, weighing each metal component according to the proportion, mixing, melting, and atomizing to obtain metal powder; Or, making the metal components other than Ru, Pt, and Pd in the metal components into metal powder.

8. The preparation method of the metal heating film according to any one of claims 5-7, characterized in that, Meet at least one of the following (1)-(11): (1) Based on the total mass of the glass powder, the composition of the glass powder includes: silicon oxide 30-73%, boron oxide 2-23%, aluminum oxide 0.5-8%, calcium oxide 0-7%, zinc oxide 4-12%, magnesium oxide 0-5%, titanium oxide 1-5%, sodium oxide 0-11%, potassium oxide 0-3%, zirconium oxide 0.2-4%; (2) Based on the total mass of the metal components and the glass powder, it further includes B 0-2%, Al 0-1%, Ca 0-1%, Zn 0-1.5%, Mg 0-1%, Ti 0-0.5%, Na 0-1.5%, K 0-0.5%, Zr 0-0.5%; (3) The preparation method of the glass powder includes: mixing the required oxides according to the proportion, melting, water quenching, and grinding to obtain the glass powder; (4) The particle size of the glass powder is 1-15 μm; (5) The organic carrier is a mixture of ethyl cellulose, acrylic resin, tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate; (6) The slurry is coated onto the substrate by screen printing; (7) The substrate is a ceramic substrate; (8) The drying temperature is 100 - 300 °C; (9) The sintering temperature is 800 - 1500 °C; (10) The sintering time is 0.5 - 3 h; (11) The sintering atmosphere is a vacuum, nitrogen or argon atmosphere.

9. An e-cigarette atomizing core, characterized in that, Comprising the metal heating film according to any one of claims 1 - 4 or the metal heating film prepared by the preparation method according to any one of claims 5 - 8.

10. An e-cigarette, characterized in that, Comprising the electronic cigarette atomizing core according to claim 9.

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