A metal heating film, its preparation method and application

Abstract

The present invention belongs to the technical field of metal heating materials, and particularly relates to a metal heating film, a preparation method thereof, and an application. By introducing at least one element of Ru, Pt, and Pd into a nickel-chromium alloy or nickel metal and forming an alloy with the 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 contents of elements such as Ni and Cr in the flue gas. In addition, after introducing the elements of Ru, Pt, and 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 denser, having a stronger resistance to thermal 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, resulting in better taste consistency.

Description

Technical Field

[0001] The present invention belongs to the technical field of metal heating materials, and particularly relates to a metal heating film, a preparation method thereof, and an application thereof. Background Art

[0002] An electronic cigarette is an electronic product that imitates a cigarette. Although the electronic cigarette 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 other means to turn nicotine and the like into vapor.

[0003] 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 generations of updates from glass fiber, cotton to porous honeycomb ceramics. Among them, the glass fiber 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 good taste, does not wick, does not explode oil, but also has a long lifespan. Especially after using a heating film with better lipophilicity instead of a 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.

[0004] 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 flue gas. In order to further improve the safety of the flue gas, we hope to further reduce the content of Ni and Cr elements in the flue gas, so as to avoid the harm of Ni and Cr elements in the flue gas to the body and ensure the inhalation safety of users.

[0005] In view of this, there is an urgent need to develop a metal heating film and a preparation method thereof that can further reduce the content of Ni and Cr elements in the flue gas. Summary of the Invention

[0006] 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 flue gas in the prior art needs to be further reduced, so as to provide a metal heating film, a preparation method thereof, and an application thereof.

[0007] To this end, the present invention provides the following technical solutions:

[0008] The present invention provides a metal heating film, 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.

[0009] 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;

[0010] Optionally, the three metal elements Ru, Pt, and Pd coexist.

[0011] 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%.

[0012] 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%.

[0013] The present invention also provides a method for preparing a metal heating film, including the following steps,

[0014] Based on the total mass of the raw materials, mix 60-90% of the metal components, 0.5-9% of the glass powder, and 8-40% of the organic carrier to obtain a slurry;

[0015] Coat the obtained slurry onto a substrate, and after drying and sintering, obtain the metal heating film;

[0016] 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.

[0017] Optionally, it further includes the step of making the metal components into metal powder. Weigh each metal component in proportion, mix, melt, and atomize to obtain metal powder.

[0018] Optionally, the melting temperature of the metal components is 1400°C - 1600°C.

[0019] Optionally, make the metal components other than Ru, Pt, and Pd in the metal components into metal powder.

[0020] Optionally, the method for preparing the metal heating film satisfies at least one of the following (1)-(10):

[0021] (1) Based on the total mass of the glass powder, the composition of the glass powder includes: 30-73% of silicon oxide, 2-23% of boron oxide, 0.5-8% of aluminum oxide, 0-7% of calcium oxide, 4-12% of zinc oxide, 0-5% of magnesium oxide, 1-5% of titanium oxide, 0-11% of sodium oxide, 0-3% of potassium oxide, 0.2-4% of zirconium oxide;

[0022] (2) Based on the total mass of the metal components and the glass powder, it also includes 0-2% of B, 0-1% of Al, 0-1% of Ca, 0-1.5% of Zn, 0-1% of Mg, 0-0.5% of Ti, 0-1.5% of Na, 0-0.5% of K, 0-0.5% of Zr;

[0023] (3) The preparation method of the glass powder includes: mixing the required oxides in proportion, melting, water quenching, and grinding to obtain the glass powder;

[0024] Optionally, the melting temperature of the glass powder is 1450-1550 °C.

[0025] (4) The particle size of the glass powder is 1-15 μm;

[0026] (5) The organic carrier is a mixture of ethyl cellulose, acrylic resin, tributyl citrate, terpineol, butyl carbitol, and butyl carbitol acetate;

[0027] 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.

[0028] Optionally, the organic carrier can be mixed under heated conditions, and the heating temperature can be 75-90 °C.

[0029] (6) The slurry is coated onto the substrate by screen printing;

[0030] (7) The substrate is a ceramic substrate;

[0031] (8) The drying temperature is 100-300 °C;

[0032] (9) The sintering temperature is 800-1500 °C;

[0033] (10) The sintering time is 0.5-3 h;

[0034] (11) The sintering atmosphere is a vacuum, nitrogen, or argon atmosphere.

[0035] 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.

[0036] The present invention also provides an electronic cigarette, which includes the above-mentioned electronic cigarette atomization core.

[0037] The present invention does not particularly limit other structures and preparation methods of the electronic cigarette atomization core and the electronic 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 method.

[0038] 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.

[0039] The technical solution of the present invention has the following advantages:

[0040] 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, and Pd. By introducing at least one of the elements Ru, Pt, and Pd into the nickel-chromium alloy or nickel metal and forming an alloy with the 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, and 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, and the ability to resist the thermal shock of tobacco oil stronger. 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 tobacco oil can be atomized more coordinately, resulting in better taste consistency.

[0041] 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, and Pd exist simultaneously, the high-temperature corrosion resistance of the metal heating film to tobacco oil is the best, and the content of elements such as Ni and Cr in the smoke is the lowest.

[0042] The preparation method of the metal heating film provided by the present invention can introduce elements such as Ru, Pt, or Pd into the 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 smoke. In addition, these elements can also play a fluxing effect, making the sintering of the heating film more dense, and the ability to resist the thermal shock of tobacco oil stronger. 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 tobacco oil can be atomized more coordinately, resulting in better taste consistency.

[0043] The preparation method of the metal heating film provided by the present invention further defines the preparation steps, and makes the metal components other than Ru, Pt, and Pd in the metal components into metal powders. In this way, elements such as Ru, Pt, and Pd can be introduced into the nickel-based alloy or nickel metal, so that these highly corrosion-resistant metals are enriched on the surface of the metal powder, and finally a structure with low content of elements such as Ru, Pt, and Pd inside the heating film and high content outside is formed, 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 elements such as Ru, Pt, and Pd. When the contents of elements such as Ni and Cr in the flue gas reach a comparable level, the demand for elements such as Ru, Pt, and Pd is low, reducing the economic cost. Description of the Drawings

[0044] 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 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.

[0045] Figure 1 It is a picture of the heating film provided in Embodiment 1 of the present invention after the cracking test;

[0046] Figure 2 It is a picture of the heating film provided in Embodiment 2 of the present invention after the cracking test;

[0047] Figure 3 It is a picture of the heating film provided in Embodiment 3 of the present invention after the cracking test;

[0048] Figure 4 It is a picture of the heating film provided in Embodiment 4 of the present invention after the cracking test;

[0049] Figure 5 It is a picture of the heating film provided in Embodiment 5 of the present invention after the cracking test;

[0050] Figure 6 It is a picture of the heating film provided in Embodiment 6 of the present invention after the cracking test;

[0051] Figure 7 It is a picture of the heating film provided in Embodiment 7 of the present invention after the cracking test;

[0052] Figure 8 It is a picture of the heating film provided in Comparative Example 1 of the present invention after the cracking test. Detailed Embodiments

[0053] The following embodiments are provided to better understand the present invention further. They are not limited to the best mode, and do 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.

[0054] 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.

[0055] Example 1

[0056] This embodiment provides a metal heating film and its preparation method. The specific steps are as follows:

[0057] The raw material composition is: 80 wt% of metal components, 5 wt% of glass powder, and 15% of organic carrier;

[0058] 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;

[0059] 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.

[0060] Heating film preparation method:

[0061] Preparation of metal powder: After mixing the purchased Ni, Cr, Fe, Ru, Pt, Pd, Nb, Mn, Mo, W, and Si materials according to the above proportions, they are 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 protruding 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;

[0062] 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 1520 °C for melting, then poured into deionized water, water quenched into glass slag, and then the glass slag is broken to 1 - 15 μm by mechanical ball milling for standby;

[0063] Organic carrier: Ethyl cellulose (manufacturer: Sinopharm, model EC200), acrylic resin (manufacturer: Sinopharm, model 4086), tributyl citrate, terpineol, butyl carbitol, butyl carbitol acetate (manufacturer: Sinopharm) were weighed according to the mass ratio of 1:0.2:0.5:8:7.5:4, placed in a beaker, heated to 85 °C to completely dissolve, and set aside;

[0064] 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.

[0065] The heating film slurry was used to print and prepare a heating film circuit on the surface of a ceramic substrate (manufacturer: SMOK, AT02) by screen printing. The pattern is as Figure 1 shown, 9 mm long × 3.5 mm wide; after drying at 200 °C, it was then sintered at 1200 °C for 2 h to form a ceramic substrate heating film.

[0066] Example 2

[0067] This example provides a metal heating film and its preparation method. The specific steps are as follows:

[0068] The raw material composition is: Metal component No. 1 60 wt%, Metal component No. 2 26 wt%, glass powder 6 wt%; organic carrier 8%;

[0069] Among them, the composition of Metal component No. 1 is: Ni 85 wt%, Cr 15 wt%;

[0070] The composition of Metal component No. 2 is 100 wt% Ru powder;

[0071] 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%.

[0072] Heating film preparation method:

[0073] Preparation of Metal powder No. 1: After mixing the purchased Ni and Cr materials according to the above ratio, they were melted at 1500 °C and then metal powder was prepared by gas atomization. The injection apex angle α = 46°, the length of the liquid guide tube protruding z = 2 mm, the inner diameter of the liquid guide tube d = 4 mm, and nitrogen was selected for atomization powder making and set aside;

[0074] Preparation of glass powder: After weighing the required oxides according to the above ratio, they were mixed evenly, placed in an alumina crucible and heated to 1480 °C for melting, then poured into deionized water, water quenched into glass slag, and then the glass slag was broken to 1 - 15 μm by mechanical ball milling and set aside;

[0075] 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 up to 80 °C to completely dissolve them, and set aside;

[0076] Preparation of the 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.

[0077] Print the heating film slurry on the surface of the ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare the heating film circuit. The pattern is as Figure 2 shown, with dimensions or parameters of length 9 mm × width 3.5 mm; after drying at 160 °C, and then sintering at 1250 °C for 2 h to form the ceramic substrate heating film.

[0078] Example 3

[0079] This example provides a metal heating film and its preparation method. The specific steps are as follows:

[0080] 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%;

[0081] Among them, the composition of Metal Component No. 1 is: Ni 100 wt%;

[0082] The composition of Metal Component No. 2 is: Pt powder 100 wt%;

[0083] 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%.

[0084] Heating film preparation method:

[0085] Preparation of Metal Powder No. 1: After mixing the purchased Ni materials according to the above proportions, melt them at 1500 °C and then 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, and set aside;

[0086] Preparation of glass powder: Weigh the required oxides according to the above proportions, mix them evenly, place them in an alumina crucible, heat to 1450 °C to melt, pour them into deionized water, quench them into glass slag, and then crush the glass slag to 1 - 15 μm by mechanical ball milling, and set aside;

[0087] 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 up to 75°C to completely dissolve them, and set aside for later use;

[0088] Preparation of the 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.

[0089] Print the heating film slurry on the surface of the ceramic substrate (manufacturer: SMOK, AT02) by screen printing to prepare the heating film circuit. The pattern is as shown in Figure 3 shown, with dimensions or parameters of length 9 mm × width 3.5 mm; after drying at 160°C, then sinter at a high temperature of 1150°C for 0.5 h to form the ceramic substrate heating film.

[0090] Example 4

[0091] This example provides a metal heating film and its preparation method. The specific steps are as follows:

[0092] The raw material composition is: Metal Component No. 1 60 wt%, Metal Component No. 2 15.2 wt%, glass powder 4.8 wt%, and organic carrier 20%;

[0093] Among them, the composition of Metal Component No. 1 is: Ni 85 wt%, Cr 15%;

[0094] The composition of Metal Component No. 2 is 100 wt% Pt powder;

[0095] The composition of the glass powder is: silica 46%, boron oxide 20%, alumina 3%, calcium oxide 6%, zinc oxide 11%, magnesium oxide 4%, titanium oxide 3%, sodium oxide 3%, potassium oxide 2%, zirconium oxide 2%.

[0096] Heating film preparation method:

[0097] Preparation of Metal Powder No. 1: After mixing the purchased Ni, Cr and other materials according to the above proportions, melt them at 1500°C and then 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, and set aside for later use;

[0098] 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, water-quench to form glass slag, and then crush the glass slag to 1-15 μm by mechanical ball milling for standby;

[0099] 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 88 °C to completely dissolve them for standby;

[0100] 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.

[0101] 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 4 shown, with dimensions or parameters of length 9 mm × width 3.5 mm; after drying at 100 °C, then sinter at 1000 °C for 3 h to form a ceramic substrate heating film.

[0102] Example 5

[0103] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0104] 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;

[0105] Among them, the composition of metal component No. 1 is: 85 wt% of Ni and 15 wt% of Cr;

[0106] The composition of metal component No. 2 is 100 wt% of Pd powder;

[0107] 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.

[0108] Heating film preparation method:

[0109] Preparation of metal powder No. 1: After mixing the purchased Ni and Cr 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;

[0110] Preparation of glass powder: After weighing the required oxides in the above proportions, mix them evenly, place them in an alumina crucible, heat to 1480 °C until molten, pour into deionized water, quench into glass slag, and then crush the glass slag to 1 - 15 μm by mechanical ball milling for standby;

[0111] 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 them for standby;

[0112] 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.

[0113] 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 5 shown, with dimensions or parameters of length 9 mm × width 3.5 mm; after drying at 120 °C, then sinter at 1050 °C for 2.5 h to form a ceramic substrate heating film.

[0114] Example 6

[0115] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0116] 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;

[0117] Among them, the composition of metal component No. 1 is: 85 wt% Ni, 15 wt% Cr;

[0118] The composition of metal component No. 2 is: 30 wt% Ru powder; 35% Pt powder; 35 wt% Pd powder;

[0119] The composition of the glass powder is: 70% silicon oxide, 8% boron oxide, 2% aluminum oxide, 1% calcium oxide, 8% zinc oxide, 2% magnesium oxide, 3% titanium oxide, 4% sodium oxide, 1% potassium oxide, 1% zirconium oxide.

[0120] Heating film preparation method:

[0121] Preparation of Metal Powder No. 1: After mixing the purchased Ni and Cr 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 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 for standby;

[0122] Metal Powder No. 2 is provided by Hunan Reyin Rhenium Alloy Materials Co., Ltd.

[0123] Preparation of glass powder: After weighing the required oxides according to the above proportions and mixing them evenly, they are 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;

[0124] 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;

[0125] Preparation of heating film slurry: Weigh the required proportions of Metal Powder No. 1, Metal Powder No. 2, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0126] The heating film slurry is printed on the surface of the ceramic substrate (manufacturer: McWell, AT02) by screen printing to prepare the heating film circuit, and the pattern is as Figure 6 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 the ceramic substrate heating film.

[0127] Example 7

[0128] This example provides a metal heating film and its preparation method, and the specific steps are as follows:

[0129] The raw material composition is: metal component 80 wt%, glass powder 5 wt%, organic carrier 15 wt%;

[0130] Among them, the composition of the metal component is: Ni 65 wt%, Cr 10 wt%, Fe 5 wt%, Ru 5 wt%, Pt 2 wt%, Pd 3 wt%, Nb 2 wt%, Mn 3 wt%, Mo 3 wt%, W 1 wt%, Si 1 wt%;

[0131] 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.

[0132] Preparation method of the heating film:

[0133] 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 ratios, 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 protruding is 2 mm, the inner diameter d of the liquid guide tube is 4 mm, and nitrogen is selected for atomization powder making for standby;

[0134] 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 them into deionized water, quench into glass slag, and then crush the glass slag to 1 - 15 μm by mechanical ball milling for standby;

[0135] 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 82 °C to completely dissolve for standby;

[0136] Preparation of the heating film slurry: Weigh the required proportions of Metal Powder No. 1, Ru powder, Pt powder, glass powder, and organic carrier, mix them evenly, and use a three-roll mill to prepare the heating film slurry.

[0137] 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. 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.

[0138] Comparative Example 1

[0139] This comparative example provides a metal heating film and its preparation method. The specific steps are as follows:

[0140] The raw material composition is: 86 wt% metal component, 6 wt% glass powder; 8% organic carrier;

[0141] Among them, the composition of the metal component is: 85 wt% Ni, 15 wt% Cr;

[0142] The composition of the glass powder is as follows: 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%.

[0143] Preparation method of the heating film:

[0144] Preparation of the metal powder: After mixing the purchased Ni and Cr materials according to the above ratios, 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 delivery tube extending out is 2 mm, the inner diameter d of the liquid delivery tube is 4 mm, and nitrogen is selected for atomization to prepare powder for standby;

[0145] Preparation of the glass powder: After weighing the required oxides according to the above ratios, they are mixed evenly, placed in an alumina crucible, heated to 1480 °C for melting, then poured into deionized water, and water quenched into glass slag. Then the glass slag is broken to 1 - 15 μm by mechanical ball milling for standby;

[0146] 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 80 °C to completely dissolve for standby;

[0147] Preparation of the heating film slurry: Weigh the metal powder, glass powder, and organic carrier in the required ratios, mix them evenly, and use a three - roll mill to prepare the heating film slurry.

[0148] 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 parameters 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.

[0149] Test examples

[0150] The metal heating films provided in the examples and comparative examples of the present invention are tested. The specific test method is as follows:

[0151] Flue gas component test: Collect the electronic cigarette aerosol gel and analyze its components using a gas chromatography - mass spectrometry (GC - MS).

[0152] Taste and puffing experiment

[0153] 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-cycle puffing method, the 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), smoke volume, sweetness, throat hit, smoke humidity, 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.

[0154] The meanings of the 8 indicators are as follows: aroma concentration: the thickness 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 the e-cigarette liquid in the oral cavity, throat, and nasal cavity, such as granularity, needle prick feeling, and off-flavors, etc.; smoke volume: the total amount of aerosol formed after atomization of the e-cigarette liquid, and the size of the smoke volume visually observed through oral feeling and exhalation; sweetness: the strength of the sweet taste perceived in the oral cavity after atomization of the e-cigarette liquid and the strength of the sweet fragrance 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; smoke humidity: the dry and wet degree of the smoke particle droplets sensed by the oral cavity and nasal cavity; coordination: the mixing uniformity and coordination degree of the aroma after atomization of the 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.

[0155] Table 1 Sensory quality evaluation criteria for e-cigarette liquid

[0156]

[0157] Cracking test method and steps:

[0158] Cracking test plan: The heating film was tested by energization at a power of 6.5 W, the energization time was 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.

[0159] Specific test results are shown in the following table:

[0160] Table 2

[0161]

[0162] Note: ND indicates below the lower limit of instrument testing.

[0163] Table 3

[0164]

[0165]

[0166] Note: The e-liquid used in the test was provided by an American tobacco company, and the model was BAT-204567.

[0167] 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, from the data comparison between 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.

[0168] 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 still fall 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 also includes the metal elements Ru, Pt, and Pd; The three metal elements Ru, Pt, and Pd coexist.

2. The metal heating film according to claim 1, wherein 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 zero.

3. The metal heating film according to claim 1 or 2, 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%.

4. The metal heating film according to claim 3, wherein Based on the total mass of the metal heating film, it also includes: Fe 0-18%; Nb 0-4%; Mn 0-3%; Mo 0-2%; W 0-2%; Si 0-2.5%.

5. 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 zero.

6. The preparation method of the metal heating film according to claim 5, wherein, It also includes the step of making the metal components into metal powder. Weigh each metal component according to the proportion, mix, melt, and atomize to obtain metal powder.

7. The method for preparing a metal heating film according to claim 6, wherein Make 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: silica 30-73%, boron oxide 2-23%, alumina 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 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%; (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 1-15μm; (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 on 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 0.5-3h; The sintering atmosphere is a vacuum, nitrogen or argon atmosphere.

9. An e-cigarette atomization core, characterized in that, It includes the metal heating film described in any one of claims 1-4 or the metal heating film prepared by the preparation method described in any one of claims 5-8.

10. An electronic cigarette, characterized in that, It includes the electronic cigarette atomizing core described in claim 9.

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