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WO2024234163A1 - Produit générateur d'aérosol - Google Patents

Produit générateur d'aérosol Download PDF

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Publication number
WO2024234163A1
WO2024234163A1 PCT/CN2023/093981 CN2023093981W WO2024234163A1 WO 2024234163 A1 WO2024234163 A1 WO 2024234163A1 CN 2023093981 W CN2023093981 W CN 2023093981W WO 2024234163 A1 WO2024234163 A1 WO 2024234163A1
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WO
WIPO (PCT)
Prior art keywords
soft magnetic
aerosol
aerosol generating
magnetic alloy
generating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/CN2023/093981
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English (en)
Chinese (zh)
Inventor
缪金波
孙搴慧
容辉
唐志强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Huabao Collaborative Innovation Technology Research Institute CoLtd
Original Assignee
Shenzhen Huabao Collaborative Innovation Technology Research Institute CoLtd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Huabao Collaborative Innovation Technology Research Institute CoLtd filed Critical Shenzhen Huabao Collaborative Innovation Technology Research Institute CoLtd
Priority to CN202380024224.3A priority Critical patent/CN119486612A/zh
Priority to PCT/CN2023/093981 priority patent/WO2024234163A1/fr
Publication of WO2024234163A1 publication Critical patent/WO2024234163A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A24D1/20—Cigarettes specially adapted for simulated smoking devices

Definitions

  • the present invention relates to the technical field of heat-not-burn tobacco, and in particular to an aerosol generating product.
  • the aerosol generating system includes an aerosol generating device and an aerosol generating product.
  • the resonant wireless power transfer system Magnetic Coupling Resonance Wireless Power Transfer, referred to as MCR-WPT
  • MCR-WPT Magnetic Coupling Resonance Wireless Power Transfer
  • Developing an aerosol generating device based on the principle of resonant wireless power transmission is a preferred solution.
  • the sensor is set in the aerosol generating device or the receptor is set in the aerosol generating product, and the receptor heats the aerosol generating product based on the principle of resonant wireless power transmission.
  • the material of the sensor needs to meet the appropriate high-frequency magnetic permeability, resistivity, and material size to match the specific coil parameters and external circuit characteristics, so as to maintain a resonant state in the basic constant temperature stage to achieve the purpose of heating non-burning cigarettes.
  • the heating process of the aerosol-generating product using the sensor includes a preheating stage and a basic constant temperature stage. In order to meet the user experience, it is often necessary to quickly increase the temperature in the preheating stage to achieve the purpose of efficiently releasing volatile smoke substances.
  • the temperature of the core material can continue to rise to the Curie point, and then the core material loses magnetism, and the core material cools down because it can no longer absorb energy from the external magnetic field.
  • the temperature of the core material drops significantly due to the influx of cold air, and the magnetic properties of the material are restored, thereby forming a heating-cooling cycle and achieving the purpose of automatic temperature control.
  • the present application provides an aerosol generating product that meets the requirements of the aerosol generating device receptor for magnetic properties and Curie temperature, ensures rapid temperature rise during the preheating stage, and undergoes ferromagnetic to paramagnetic transition and complete demagnetization before 400°C, thereby alleviating the behavior of the heater overheating the aerosol generating substrate.
  • the present application provides an aerosol generating product for generating an inhalable aerosol when heated, comprising an aerosol generating matrix segment, the aerosol generating matrix segment comprising an aerosol generating matrix and a receptor assembly, the receptor assembly inductively heats the aerosol forming matrix under the influence of an alternating magnetic field, the material of the receptor assembly is a soft magnetic alloy, the soft magnetic alloy is a single-layer structure with uniform element distribution; the average particle size of the soft magnetic alloy grains is 50 to 70 ⁇ m, and the grain size grade is 5.5 to 4.5.
  • the components of the soft magnetic alloy include iron, molybdenum and nickel, the mass of molybdenum accounts for 3.5% to 6% of the total mass of the soft magnetic alloy, and the mass of nickel accounts for 77% to 81% of the total mass of the soft magnetic alloy.
  • the soft magnetic alloy also includes chromium, and the mass of chromium accounts for 0.2-0.5% of the total mass of the soft magnetic alloy.
  • the soft magnetic alloy also includes manganese, and the mass of manganese accounts for 0.1-0.5% of the total mass of the soft magnetic alloy.
  • the soft magnetic alloy also includes silicon and aluminum, the silicon content is 0.1% to 0.4%, and the weight of aluminum accounts for 1.3% of the soft magnetic alloy. 0.15-0.7% of the total mass of gold.
  • the soft magnetic alloy comprises the following components in mass fractions: 77-81 parts of nickel, 3.5-6.0 parts of molybdenum, 0.2-0.5 parts of chromium, 0.1-0.5 parts of manganese, 0.1-0.4 parts of silicon, 0.15-0.7 parts of aluminum, and the balance is approximately 11-18 parts of iron.
  • the aerosol-generating substrate segment has an applied thickness of 0.03 to 0.18 mm, a width of 1.5 to 4.5 mm and a length of 9 to 18 mm.
  • the aerosol generating product for generating an inhalable aerosol when heated also has a filter segment and a cooling segment, wherein the cooling segment is located between the aerosol generating substrate segment and the filter segment;
  • the aerosol generating substrate is made of tobacco material or non-tobacco material and is distributed in filamentary, sheet-like or granular form, and the receptor assembly is wrapped by the aerosol generating substrate.
  • the preparation method of the sensor assembly comprises the following steps:
  • the annealing temperature is 1000-1200°C
  • the holding time is 70-120min
  • the cooling rate is 150-220°C/h
  • the mixed powder is a 100-300 mesh mixed powder, comprising a mixture of Fe2O3 , MnO, SiO2 , Al2O3 , MgO, and C powders ; the volume ratio of the mixed powder to the cold-rolled material is 0.05-0.15:100.
  • the present invention provides an aerosol generating product for generating an inhalable aerosol when heated, comprising an aerosol generating substrate segment, the aerosol generating substrate segment comprising an aerosol generating substrate and a sensor component, the sensor component inductively heats the homogeneous tobacco material of the aerosol generating substrate segment under the influence of an alternating magnetic field to form an aerosol for a user to inhale,
  • the sensor component is a soft magnetic alloy having only a single-layer homogeneous structure, and realizes application in the field of heating tobacco without burning
  • the soft magnetic alloy can realize non-contact heating of the aerosol generating substrate based on the principle of resonant wireless power transmission
  • the soft magnetic alloy with a single-layer homogeneous structure has a stable Curie temperature range, and can be used for heating tobacco without burning
  • the soft magnetic alloy can be used for heating tobacco without burning
  • the soft magnetic alloy with a single-layer homogeneous structure has a stable Curie temperature range, and can be used for heating tobacco without burning
  • the saturation magnetic induction intensity is greatly affected.
  • the magnetization mode mainly being the rotation of magnetic domains
  • the larger the grain size of the sensor component the greater the saturation magnetic induction intensity.
  • the appropriate magnetic permeability, lower coercive force and appropriate resistivity at high frequencies ensure rapid heating in the preheating stage and can completely demagnetize the sensor component before 400°C, thereby stopping the heating of the aerosol generating matrix. While satisfying the user experience, it minimizes the risk of users using aerosol products and alleviates the behavior of the heater overheating the aerosol generating matrix.
  • FIG1 is a 100X metallographic microscope identification diagram of a soft magnetic alloy component
  • FIG2 is a 200X metallographic microscope identification image of a soft magnetic alloy component
  • FIG3 is a field emission scanning electron microscope identification image of a typical area of a soft magnetic alloy component
  • FIG4 is an element analysis energy spectrum diagram of a characteristic point at a defect in region A of FIG3 ;
  • FIG5 is an element analysis energy spectrum diagram of a characteristic point at a defect in region B of FIG3 ;
  • FIG6 is an element analysis energy spectrum diagram of a characteristic point at a defect in region C of FIG3 ;
  • FIG7 is a field emission scanning electron microscope identification image of a typical area of a soft magnetic alloy component
  • FIG8 is a hysteresis B-H curve diagram of a soft magnetic alloy component
  • FIG9 is a hysteresis B-H curve diagram of a soft magnetic alloy component
  • FIG10 is a schematic diagram of the grayscale cross section of a soft magnetic alloy
  • FIG11 is a schematic diagram of a magnetization intensity-temperature curve and its derivative curve of a soft magnetic alloy
  • FIG12 is a schematic diagram of the magnetization intensity-temperature curve and its derivative curve of the soft magnetic alloy
  • FIG13 is a ternary structure aerosol generating product
  • FIG14 is a quaternary structure aerosol generating product
  • FIG15 is a schematic diagram of a time-temperature curve of a soft magnetic alloy in an aerosol generating device
  • Aerosol generation matrix section In the figure: 1. Aerosol generation matrix section; 2. Cooling section; 3. Mouth section; 4. Anti-leakage section.
  • the aerosol generating device has the characteristic of being able to automatically control the temperature according to the soft magnetic core material.
  • the sensor material continues to heat up to the Curie point, and then the sensor material loses magnetism.
  • air enters the cigarette core section and contacts the sensor material to reduce the temperature of the sensor material and restore the magnetic conductivity, thereby forming a heating-cooling cycle and achieving the purpose of automatic temperature control.
  • the existing alloy technology cannot have magnetic properties, Curie temperature and magnetic permeability that can meet the design requirements, and the prepared alloy materials are all multi-layer materials.
  • the present invention provides a homogeneous cigarette core material with only a single-layer structure, which realizes non-contact heating of aerosol generating products based on the principle of resonant wireless power transmission.
  • the temperature rises rapidly during the preheating stage, and heating is stopped after the ferromagnet-paramagnet transformation occurs before 400°C and the magnetism is completely lost. This helps to improve the user experience while effectively reducing the release of harmful substances and combustion risks of aerosol products.
  • the present application provides an aerosol generating product for generating an inhalable aerosol when heated, comprising an aerosol generating matrix section, the matrix section comprising an aerosol generating matrix and a receptor assembly, the receptor assembly inductively heats the aerosol to form the matrix under the influence of an alternating magnetic field, the material of the receptor assembly is a soft magnetic alloy, the soft magnetic alloy is a uniform single-layer structure; the average grain size of the soft magnetic alloy is 50 to 70 ⁇ m, and the grain size grade is 5.5 to 4.5.
  • Soft magnetic alloys have both the magnetic properties and Curie temperature requirements of the aerosol generating device receptor, ensuring rapid temperature rise during the preheating stage, and undergoing ferromagnetic-paramagnetic transformation and complete demagnetization before 400°C, so that they can be used in the field of electromagnetic induction heating of non-combustible tobacco with automatic temperature control under the principle of non-contact radio transmission, and significantly reduce the risk of releasing harmful substances and burning when heating homogenized tobacco materials.
  • the grain size of soft magnetic alloys affects the saturation magnetic induction intensity of the receptor. For magnetization methods that are mainly magnetic domain rotation, the larger the grain size of the soft magnetic alloy, the greater the saturation magnetic induction intensity.
  • the single-layer structure defined in the present invention satisfies the following two conditions: the manufacturing process of the soft magnetic alloy only includes smelting, remelting, hot forging, hot rolling, cold rolling, and annealing processes, and does not include any of the following processes: electroplating, coating, welding, and coating; in the grayscale image of the soft magnetic alloy taken under a scanning electron microscope, in the range of 100 to 3000 times, the overall image contrast is basically uniform and can be identified by the naked eye, and the color area with the widest area in the main part of the soft magnetic alloy accounts for at least 95% of the area value of the entire area of the soft magnetic alloy.
  • the components of the soft magnetic alloy include molybdenum and nickel.
  • the mass of molybdenum accounts for 3.5% to 6% of the total mass of the soft magnetic alloy, the mass of nickel accounts for 77% to 81% of the total mass of the soft magnetic alloy, and the balance is iron.
  • the mass ratio of nickel to molybdenum is 15.2 to 16.5:1.
  • the soft magnetic alloy of the present application includes, in addition to iron, nickel, and molybdenum, one or more of Al, Cr, Mn, and Cu, and other metals or non-metals that can be used for alloying, and the elements that can be included are not limited to Si, C, O, S, and P.
  • the surface of the soft magnetic alloy of the present solution is locally treated to form defects.
  • the Curie temperature of soft magnetic alloys is mainly related to the spatial arrangement structure of magnetic atoms and non-magnetic atoms.
  • the soft magnetic alloy of this scheme controls the composition ratio of nickel and molybdenum, and adds a certain proportion of molybdenum to reduce the relative content of nickel, which is beneficial to increase the initial magnetic permeability and resistivity of the alloy; in addition, molybdenum is a paramagnetic element, and a solid solution is formed between paramagnetic molybdenum and ferromagnetic Ni and Fe elements.
  • molybdenum Due to the solid solution behavior of molybdenum, the outer electrons of molybdenum atoms are transferred to ferromagnetic atoms, and the spins are reversed and filled, and the magnetic exchange effect of ferromagnetic atoms is weakened. At the same time, the solid solution behavior increases the crystal lattice of ferromagnetic material crystals, increases the distance between ferromagnetic elements, and also weakens the magnetic exchange effect of ferromagnetic atoms, reduces the remanence and coercive force of the material, and improves the initial magnetic permeability. Molybdenum is added in the following two ways: adding it during the initial batching; or adding molybdenum in the later stage of refining. Through the appropriate nickel-molybdenum ratio, it is beneficial to control the Curie temperature of the soft magnetic alloy and keep it between 350 and 400 ° C.
  • the soft magnetic alloy also includes chromium, which accounts for 0.2-0.5% of the total mass of the soft magnetic alloy.
  • chromium accounts for 0.2-0.5% of the total mass of the soft magnetic alloy.
  • the addition of chromium reduces the relative content of nickel, which is beneficial to improve the initial magnetic permeability, enhance the oxidation resistance of the alloy, and effectively reduce the correction Stubbornness.
  • the components of the soft magnetic alloy also include manganese, which accounts for 0.1 to 0.5% of the total mass of the soft magnetic alloy. It can be added during the refining process to achieve the purpose of alloying. At the same time, the Mn element is easily combined with the S element, avoiding the formation of FeS by Fe and S elements to increase the hot brittleness of the alloy.
  • the soft magnetic alloy also includes silicon and aluminum, with the silicon content being 0.1% to 0.4% and the aluminum content being 0.15% to 0.7%.
  • the mass ratio of manganese to silicon is 0.9 to 2.95: 1.
  • Manganese, silicon and aluminum elements effectively reduce the high proportion of oxides inside the alloy, effectively reduce its coercivity, and offset the increase in the coercivity of the soft magnetic alloy caused by the introduction of some oxides in the annealing process.
  • the addition of a small amount of Al elements can easily cause lattice distortion of the arrangement of metal atoms, enhance the solid solution behavior of Mo elements to ferromagnetic Ni and Fe elements, strengthen the solid solution behavior to increase the lattice of ferromagnetic material crystals, increase the distance between ferromagnetic elements, and weaken the magnetic exchange effect of ferromagnetic atoms, reduce the remanence and coercive force of the material, and increase the initial magnetic permeability.
  • the increase in initial magnetic permeability is conducive to maintaining good magnetic properties after the introduction of surface oxidation in the later stage of annealing.
  • the mass ratio of nickel to iron in the soft magnetic alloy is 4.5 to 5:1, which is conducive to forming an optimal short-range ordered structure near Ni 3 Fe, at which time it has the smallest magnetocrystalline anisotropy constant and saturation magnetostriction coefficient.
  • the soft magnetic alloy comprises the following components in mass fractions: 77-81 parts of nickel, 3.5-6.0 parts of molybdenum, 0.2-0.5 parts of chromium, 0.1-0.5 parts of manganese, 0.1-0.4 parts of silicon, 0.15-0.7 parts of aluminum, and the balance is approximately 11-18 parts of iron.
  • the thickness of the sensor component is 0.03-0.18 mm, the width is 1.5-4.5 mm, and the length is 9-18 mm.
  • the thickness is 0.105-0.15 mm, and the width is 2-4 mm.
  • the length of the material is 10-14 mm.
  • the Curie temperature of the soft magnetic alloy is 350-400°C.
  • the Curie temperature of the soft magnetic alloy is 380-395°C.
  • the magnetic permeability of the soft magnetic alloy component of the present application will significantly decrease and approach 0, and the power loss of the soft magnetic alloy component will be significantly reduced and approach 0.
  • a Curie temperature not higher than 400°C can avoid the release of harmful components and the potential risk of combustion.
  • the soft magnetic alloy has a saturation magnetic induction intensity of 7000-10000 Gs at a thickness of 0.1-0.18 mm and a magnetic field frequency of 60 Hz between 0.4 and 20 Oe.
  • the saturation magnetic induction intensity is 7000-9000 Gs, and more preferably, the saturation magnetic induction intensity is 7000-8500 Gs.
  • the saturation magnetic induction intensity of this scheme is used to meet the rapid heating process of the preheating stage of the aerosol generation matrix section, and significantly improve the magnetic flux value in the coil.
  • the maximum magnetic permeability of the soft magnetic alloy is 120-275 mH/m when the thickness is 0.1-0.18 mm and the magnetic field frequency is 60 Hz.
  • the maximum magnetic permeability is 150-220 mH/m, and more preferably, the maximum magnetic permeability is 190-200 mH/m.
  • a certain skin depth can be guaranteed, thereby ensuring that a certain amount of eddy current loss is effectively converted into heat energy and absorbed by the aerosol generating matrix to produce aerosol.
  • the soft magnetic alloy has a coercive force of 0.1 to 4 A/m when the thickness is 0.1 to 0.18 mm and the magnetic field frequency is 60 Hz. More preferably, the coercive force is 0.1 to 2 A/m. More preferably, the coercive force is 0.1 to 1.5 A/m. Within this range, the magnetic properties of the soft magnetic alloy component are highly stable.
  • the soft magnetic alloy has a room temperature resistivity of 40 to 100 ⁇ cm when the thickness is 0.1 to 0.18 mm and the magnetic field frequency is 60 Hz.
  • the room temperature resistivity is 40 to 80 ⁇ cm, and more preferably, the room temperature resistivity is 40 to 70 ⁇ cm.
  • the present application provides an aerosol generating product, which also has a filter segment 3 and a cooling segment 2, and the cooling segment 2 is located between the aerosol generating matrix segment 1 and the filter segment 3;
  • the aerosol generating matrix is made of tobacco material or non-tobacco material and is distributed in a filamentary, sheet-like or granular form, and the sensor component is wrapped by the aerosol generating matrix.
  • the sheet-like or filamentary tobacco or non-tobacco material surrounds and wraps the sensor component, and the granular tobacco or non-tobacco material buries the sensor component in a stacked manner.
  • Figure 14 is a ternary structure aerosol generating product, including a filter segment 3, a cooling segment 2, and an aerosol generating matrix segment 1;
  • Figure 15 is a quaternary structure aerosol generating product, including a filter segment 3, a cooling segment 2, an aerosol generating matrix segment 1 and an anti-leakage segment 4;
  • the aerosol generating matrix segment 1 includes an aerosol generating matrix and the above-mentioned soft magnetic alloy component, and the soft magnetic alloy heats the aerosol generating matrix based on the principle of electromagnetic induction heating.
  • the aerosol-generating substrate can be tobacco flakes, tobacco shreds, stem shreds, expanded tobacco shreds, expanded stem shreds, and tobacco particles, and is characterized by containing smoke-generating substances such as glycerin, propylene glycol, nicotine, and cannabis-like substances, and flavor substances such as flavors and fragrances can also be added.
  • smoke-generating substances such as glycerin, propylene glycol, nicotine, and cannabis-like substances
  • flavor substances such as flavors and fragrances can also be added.
  • the volatile smoking substances, nicotine, cannabis, flavor substances, etc. are released to form steam, which is then cooled during the suction process. Due to the nucleation mechanism, the steam condenses to form droplets. When the temperature is low enough, the number of droplets is large enough, and they condense with each other to form aerosol droplets with large particle size.
  • the cooling section 2 has the function of reducing the temperature of the smoke to further support the cooling of the volatile substances from the aerosol generating matrix section to form an aerosol. It usually has a smooth airway to transmit steam substances or aerosols.
  • the cooling mechanism can be convection heat transfer or phase change of the cooling material.
  • a mouth section is provided away from the aerosol generating matrix section shown. The mouth section contacts the oral cavity to support lung suction and plays a role in filtering harmful substances.
  • the mouth section is often made of fiber bundles, and the dense fiber bundles can effectively intercept harmful substances in the smoke.
  • an anti-leakage section 4 is provided to prevent aerosol or steam substances from escaping to avoid contaminating the aerosol generating device and play a role in maintaining cleanliness.
  • the preparation method of the sensor assembly comprises the following steps:
  • the annealing temperature is 1000-1200°C
  • the holding time is 70-120 minutes
  • the cooling rate is 150-220°C/h
  • the mixed powder includes a mixture of Fe, MnO, SiO2 , Al2O3 , and C powders .
  • the annealing process has a significant effect on the magnetic properties of soft magnetic alloys, including magnetic permeability and saturation magnetic induction intensity.
  • the annealing temperature is higher and the holding time is longer, the purity of the soft magnetic alloy will increase and the grain size will increase, which will lead to an increase in the maximum magnetic permeability and an increase in the saturation magnetic induction intensity.
  • the above annealing temperature and holding time are conducive to the proper adjustment of the maximum magnetic permeability and saturation magnetic induction intensity, and by controlling the cooling rate, especially the cooling rate of the secondary cooling starting at about 600°C, the rapid cooling method of air cooling can significantly increase the initial magnetic permeability of the alloy, while only causing a slight increase in the maximum relative magnetic permeability, and finally achieving a slightly higher saturation magnetic induction intensity and an appropriate maximum magnetic permeability.
  • the mixed powder serves the purpose of oxidizing the alloy surface.
  • the oxidation process of the alloy surface will cause a significant decrease in the maximum magnetic permeability of the material, an increase in coercive force, and a decrease in resistivity.
  • the production process is stable, and on the other hand, the inclusions on the alloy surface can be effectively controlled.
  • inclusion elements may be introduced into the alloy, including but not limited to Al, Si, C, O, Mn, S, and P. These inclusion elements exist mainly in the form of metal oxides or sulfides. These non-metallic inclusions will cause the increase of alloy grain size, produce pinning effects, cause the increase and complexity of magnetic domains, and cause the alloy's magnetic permeability to decrease, the saturation magnetic induction intensity to increase slightly, and the coercive force to increase.
  • a special surface oxidation treatment method is used in the annealing process to reduce the magnetic permeability of the soft magnetic alloy while maintaining the Curie temperature, saturation magnetic induction intensity, coercive force and resistivity without significant changes, so as to meet the application in the field of heated cigarettes under the automatic temperature control electromagnetic heating process under the principle of non-contact radio transmission.
  • the alloy raw materials in step S1 include but are not limited to iron, nickel, molybdenum, chromium, manganese, and silicon. Iron and nickel are added in the smelting step, and nickel or other alloy raw materials are added in the smelting and/or remelting step.
  • step S1 the smelting process of step S1 is as follows:
  • iron, nickel and molybdenum are weighed, and coke equivalent to half of the total mass of iron, nickel and molybdenum is added and placed in the feeding area.
  • the vacuum induction melting furnace is added from the feeding area and vacuumized, and the furnace is smelted at a smelting temperature of 1500-1600°C and a smelting time of 60-100min. After melting, continue to refine, and add 0.5 parts of manganese ore with a manganese content of 25% during the refining process to achieve the purpose of alloying.
  • the refining time is 0.5-1.5h and the refining temperature is 1550-1650°C.
  • step S1 After the refining is completed, pouring is carried out at 1400-1500°C, and then demolding and furnace numbering are performed to obtain ingots.
  • Other alloys include but are not limited to molybdenum, chromium, manganese and silicon that meet the requirements of the total composition of the soft magnetic alloy product; in some embodiments, the mass ratio of iron, nickel and molybdenum in step S1 is 2-3:9-10:0.5-1, and other components can be supplemented or adjusted in the subsequent remelting step.
  • step S1 the remelting process of step S1 is as follows:
  • the ingot is cut into small pieces of 5*5*5mm and polished to remove oil and rust on the surface; a graphite crucible is lined in a magnesia crucible, a 0.8-1.5wt% electrolytic nickel plate is placed at the bottom of the graphite crucible, and a block ingot is placed, and 0-0.1wt% of fused magnesia is stuffed into the gap of the ingot. Then it is added to a vacuum induction melting furnace and evacuated, and then the furnace is combined for smelting, 10KW power is sent for melting, the smelting temperature is 1500-1600°C, and the smelting time is 50-80min.
  • the refining time is 20 to 40 minutes
  • the heating power is adjusted to 2KW, and after the heating is completed, when the temperature drops to 300°C, the circuit is turned off, the vacuum is maintained, and the sample is allowed to cool with the furnace to obtain a remelted ingot.
  • the alloy After the alloy is melted and refined for the first time through the vacuum induction furnace (i.e., the melting process), its surface is cleaned and remelted for the second time, which is conducive to the removal of elements such as P and S in the alloy, and the reduction of the proportion of non-metallic elements in the alloy to stabilize the composition of the alloy and the stability of the subsequent processing technology; in the process of remelting, the controllable addition of materials or adjustment of the process can effectively control the proportion of non-metallic and metallic elements in the alloy, and make secondary adjustments to the alloy composition; at this stage, the alloy composition is sampled and tested to ensure that the alloy composition is within the set range.
  • the vacuum induction furnace i.e., the melting process
  • the soft magnetic alloy is made into a material with a thickness of 0.03 to 0.18 mm through hot forging, hot rolling, and cold rolling processes, and the cold rolled material is sampled to test its magnetic properties, Curie temperature, and resistivity.
  • the specific contents are as follows.
  • the soft magnetic alloy component includes 77 to 81 parts of nickel, 11 to 18 parts of iron, 3.5 to 6.0 parts of molybdenum, 0.2 to 0.5 parts of chromium, 0.1 to 0.5 parts of manganese, and 0.1 to 0.4 parts of silicon.
  • the hot forging process of step S1 is as follows:
  • the pressure of the smelting furnace is relieved, the crucible and the remelted ingot are taken out, and the remelted ingot is placed in a chamber furnace.
  • the temperature in the furnace is raised to 1250-1300°C in 50-70 minutes. After 5-15 minutes, it is hot forged into a 20-35 mm flat billet under the action of a 2-ton steam hammer, and the billet is obtained after surface grinding with a grinding wheel.
  • the hot rolling process of step S1 is as follows:
  • a four-roll reversible hot rolling mill is used for three insulation cycles, with the insulation time being 30-60min, 20-40min, and 15-30min respectively.
  • the thickness after three hot rolling cycles is 15-20mm, 8-15mm, and 3-8mm respectively.
  • the deformation temperature range of the hot rolling process is 900-1200°C, and further 1000-1200°C.
  • the surface temperature of the hot-rolled plate is tested with an infrared thermometer. When the temperature is lower than 1000°C, preferably 900°C, the hot rolling is stopped to obtain a hot-rolled material.
  • the cold rolling process of step S1 is as follows:
  • the hot rolled material is cold rolled using a four-roll reversible cold rolling mill, and the thickness is initially cold rolled to 1-1.5 mm.
  • the cold rolled material is further rolled to a thickness of 0.03-0.18 mm using a four-roll reversible cold rolling mill to obtain a cold rolled material.
  • the semi-finished materials are then subjected to an annealing process, which is beneficial for removing impurities and eliminating internal stresses in the alloy, while allowing the alloy to recrystallize and obtain a disordered and uniform crystal structure.
  • the annealing process of step S2 is:
  • the cold-rolled material is annealed, and a mixed powder of 100-300 mesh is prepared and placed in a vacuum hydrogen annealing furnace together with the cold-rolled material.
  • the temperature in the furnace is raised to 1000-1200°C in 60-120 minutes, kept warm for 70-120 minutes, and then reduced to 580-630°C at 150-220°C/h. It is then air-cooled or cooled with the furnace to 100-200°C before being taken out of the furnace.
  • the temperature is reduced from 600°C to 300°C for 30-60 minutes, and the cooling rate is 300-600°C/h; for the method of air cooling, the temperature is reduced from 600°C to 300°C for 8-20 minutes, and the cooling rate is 900-2250°C/h.
  • the annealing temperature, holding time, cooling rate and air cooling method selected in the annealing process of this scheme are conducive to controlling the average grain size of 50-70mm and the grain size level between 5.5 and 4.5.
  • the grain size of the material affects the saturation magnetic induction intensity of the material. For the magnetization method mainly based on the rotation of magnetic domains, the larger the alloy grain size, the greater the saturation magnetic induction intensity.
  • the alloy composition due to the influence of raw material purity, partial metal deoxidation during the smelting process, and pollutants on the furnace wall surface and other complex factors, a certain proportion of oxides will exist in the alloy composition.
  • the oxides generally present include MnO, SiO 2 , Al 2 O 3 , etc.
  • the magnetization modes of soft magnetic alloys mainly include reversible magnetic domain rotation and irreversible domain wall movement. Since the magnetic field strength is generally not higher than 50Oe in the magnetothermal conversion application in the field of heating tobacco, the main magnetic domain rotation and relatively few domain wall movements occur in soft magnetic alloys.
  • the soft magnetic alloy when the soft magnetic alloy is magnetized, a demagnetization field is generated, and a magnetic domain structure is generated inside the soft magnetic alloy, making magnetization difficult; secondly, the oxides produce a pinning effect inside the soft magnetic alloy, increasing the hysteresis loss and the coercive force, which increases the external force work required for domain wall movement and makes it difficult to magnetize.
  • the presence of oxides during the preparation process usually makes it difficult to magnetize the soft magnetic alloy, such as causing a decrease in the maximum magnetic permeability and an increase in the coercive force.
  • the soft magnetic alloy of the present application has a large grain size, a large saturation magnetic induction intensity, and a low magnetic permeability, which cooperates with the molybdenum-nickel component ratio to jointly improve the magnetic properties of the soft magnetic alloy.
  • the magnetic permeability of the sensor component is low and the saturation magnetic induction intensity is large, the average grain size is controlled to be between 50 and 70 ⁇ m, and the grain size level is between 5.5 and 4.5, thereby achieving the most preferred properties.
  • the mixed powder includes the following components in parts by mass: 30-50 parts of Fe powder, 25-30 parts of SiO 2 , 10-15 parts of C powder, 15-19 parts of Al 2 O 3 , and 1-5 parts of MnO.
  • the particle size of the mixed powder is 100-300 meshes.
  • the volume ratio of the mixed powder to the cold-rolled material is 0.05-0.15:100.
  • the soft magnetic alloy obtained by the above process steps has a Curie temperature of 350-400°C for induction heating of the aerosol generation matrix segment; the saturation magnetic induction intensity of the soft magnetic alloy between 0.4 and 20Oe is 7000-10000Gs when the thickness is 0.1-0.18mm and the magnetic field frequency is 60Hz; the maximum magnetic permeability of the soft magnetic alloy is 120-275mH/m when the thickness is 0.1-0.18mm and the magnetic field frequency is 60Hz; the coercive force of the soft magnetic alloy is 0-4A/m when the thickness is 0.1-0.18mm and the magnetic field frequency is 60Hz; the room temperature resistivity of the soft magnetic alloy is 40-100 ⁇ cm when the thickness is 0.1-0.18mm and the magnetic field frequency is 60Hz.
  • An aerosol generating product for generating an inhalable aerosol when heated comprising an aerosol generating matrix section, the matrix section comprising an aerosol generating matrix and a receptor assembly, the receptor assembly being used for induction heating the aerosol forming matrix under the influence of an alternating magnetic field, the material of the receptor assembly being a soft magnetic alloy, the soft magnetic alloy being a single-layer structure with uniform element distribution; the average grain size of the soft magnetic alloy is 50 to 70 ⁇ m, the grain size grade is 5.5 to 4.5, the composition of the soft magnetic alloy is shown in Table 1, and the preparation method of the receptor assembly is as follows:
  • the smelting process is as follows:
  • iron, nickel, molybdenum and aluminum with a mass ratio of 2:9.5:0.6:0.025 are weighed, and coke equivalent to half of the total mass of iron, nickel, molybdenum and aluminum is added and placed in the charging area.
  • the vacuum induction melting furnace is added from the charging area and vacuumized, and then the furnace is combined for smelting.
  • the smelting temperature is 1500°C and the smelting time is 70min. After melting, continue to refine.
  • the refining process 2.8wt% of the raw material nickel, manganese ore with a manganese content of 25% and 0.5wt% of the raw material nickel, low-carbon ferrochrome with a chromium content of 55% are added to achieve the purpose of alloying.
  • the refining time is 1h and the refining temperature is 1600°C.
  • pouring is carried out at 1450°C, and then demolding and furnace numbering are performed to obtain ingots.
  • the remelting process is as follows:
  • the ingot is cut into small pieces of 5*5*5mm and the small pieces are polished to remove the oil and rust on the surface; a graphite crucible is lined in a magnesia crucible, and a 1wt% electrolytic nickel plate is placed at the bottom of the graphite crucible to put the block ingot, and 0.5wt% of fused magnesia is stuffed into the gap of the ingot. Then it is added to the vacuum induction melting furnace and evacuated, and then the furnace is smelted, 10KW is sent for melting, the smelting temperature is 1560°C, and the smelting time is 60min.
  • 0.1wt% of graphite carbon powder and 0.05wt% of Si ⁇ Ca ⁇ Ba powder with a particle size less than 1.0mm are added in a ratio of 2:1 in 3 times, and the interval between the two additions is 8min, and 0.05wt% of molybdenum strips are added for the last time.
  • the refining time is 20min, and the power is adjusted to 2KW.
  • the temperature is reduced to 300°C, the circuit is turned off, the vacuum is maintained, and the sample is allowed to cool with the furnace to obtain a remelted ingot.
  • the hot forging process is as follows:
  • the smelting furnace was depressurized, the crucible and the remelted ingot were taken out, and the remelted ingot was placed in a chamber furnace.
  • the temperature in the furnace was raised to 1270°C in 60 minutes. After 10 minutes, it was hot forged into a 30mm flat billet under the action of a 2-ton steam hammer, and the billet was obtained after surface grinding with a grinding wheel.
  • the hot rolling process is as follows:
  • a four-roll reversible hot rolling machine is used. After three hot rollings with insulation time of 40min, 30min and 20min respectively, the thickness is reduced to 15mm, 10mm and 4mm respectively.
  • the deformation temperature range of hot rolling is 1000-1200°C.
  • the surface temperature of the hot-rolled plate is tested with an infrared thermometer. When the temperature is lower than 1000°C, the hot rolling is stopped to obtain the hot-rolled material.
  • the cold rolling process is as follows: the hot rolled material is cold rolled using a four-roller reversible cold rolling machine, the thickness is initially cold rolled to 1.2 mm, and the cold rolled material is further rolled to 0.1 mm using a four-roller reversible cold rolling machine to obtain a cold rolled material;
  • the annealing process is as follows: anneal the cold-rolled material, prepare the 100-mesh mixed powder, place it in a vacuum hydrogen annealing furnace together with the cold-rolled material, raise the temperature in the furnace to 1030°C in 100 minutes, keep it warm for 90 minutes, then reduce it to 600°C at 200°C/h, and cool it to 150°C at a cooling rate of 1800°C/h for secondary cooling.
  • the mixed powder includes the following components by mass: 45 parts of Fe powder, 20 parts of SiO 2 , 13 parts of C powder, 16 parts of Al 2 O 3 , and 6 parts of MnO.
  • the volume ratio of the mixed powder to the cold-rolled material is 0.05:100.
  • the mixed powder and hydrogen form a powder gas flow, which causes local oxidation on the alloy surface during the annealing process. Limited atomic exchange occurs between the elements in the mixed powder and the elements on the alloy surface. Since the atomic diameter is at the order of 0.1 nm, the effect of this local oxidation on the alloy composition is negligible.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that, when the sensor component is prepared, the mass ratio of the smelting raw materials iron, nickel, molybdenum and aluminum is controlled to be 2:10.5:0.65:0.025 during the smelting process.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that, when the sensor component is prepared, the mass ratio of the smelting raw materials iron, nickel, molybdenum and aluminum is controlled to be 2:8.5:0.5:0.025 during the smelting process.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that during the preparation of the sensor component, the annealing conditions and the annealing temperature are 1300°C.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that during the preparation of the sensor component, the secondary cooling condition is that the secondary cooling is carried out at 400°C/h and the temperature is cooled to 150°C before being taken out of the furnace.
  • An aerosol generating article for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the annealing conditions during the preparation of the susceptor assembly are 200 minutes.
  • An aerosol generating article for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that when the sensor component is prepared, no mixing powder is added during the annealing process.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the sensor component is a commercially available alloy material, and its international brand is Hymu 80 alloy.
  • An aerosol generating article for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the receptor component is a commercially available alloy material, whose international grade is 1J77 alloy.
  • An aerosol generating article for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the receptor component is a commercially available alloy material, whose international grade is 1J79 alloy.
  • An aerosol generating article for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the receptor component is a commercially available alloy material, whose international grade is 1J85 alloy.
  • An aerosol generating product for generating an inhalable aerosol when heated the other contents of which are substantially the same as those of Example 1, except that the receptor assembly is a multilayer receptor composed of two layers of Hymu80 alloy and Fe-Cr alloy.
  • the alloy composition was analyzed by inductively coupled plasma mass spectrometry combined with a sulfur-carbon analyzer.
  • the composition ratio of the sensor component obtained according to the above method is shown in Table 1.
  • the surface of the soft magnetic alloy (sensor component) prepared in Example 1 was tested and observed using a metallographic microscope, and schematic diagrams thereof are shown in Figures 1 (100X) and 2 (200X). According to the GB ⁇ T ⁇ 6394 ⁇ 2017 metal average grain size determination method, the grain size grade of the alloy in Example 1 was calculated to be 5.3 and the average grain diameter was 50.2 ⁇ m.
  • FIG3 a field emission scanning electron microscope was used to test the surface morphology and an energy spectrometer was used to perform elemental analysis on local feature points; in Examples 1 to 6, the prepared soft magnetic alloy was scanned over a wide area on the surface, and multiple types and multi-component defects on the surface of the material could be easily found.
  • Region 1 cluster defects were present, and the elemental composition of the four defects was basically similar.
  • Its elemental analysis was shown in FIG4 .
  • the main inclusion elements included Fe, C, and O, and the oxide that could be formed was Fe 3 O 4 .
  • Region 2 of FIG3 triangular defects were present, and its elemental analysis was shown in FIG5 .
  • Example 1 There is a significant difference in magnetic permeability between Example 1 and Comparative Example 1, and the maximum magnetic permeability in Example 1 decreased by about 50 mH/m. However, the two are not much different in saturation magnetic flux density, and the saturation magnetic flux density of Example 1 is slightly higher than that of Comparative Example 1 by about 330 Gs.
  • the soft magnetic alloy component of Example 1 and a commercially available multilayer receptor whose material composition is a combination of Hymu80 and 430, were tested for Curie temperature. It was found that the Curie temperature of the multilayer receptor was 402°C, and the magnetization intensity of the corresponding material was 61emu/g; in comparison, the Curie temperature of the single-layer iron core material was 385C, and the magnetization intensity of the corresponding material was 10emu/g; this means that the demagnetization phenomenon of the single-layer iron core material near the Curie temperature is more significant, thereby alleviating the behavior of overheating the aerosol generating matrix.

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  • Soft Magnetic Materials (AREA)

Abstract

L'invention concerne un produit générateur d'aérosol, comprenant une section matrice de génération d'aérosol (1). La section matrice de génération d'aérosol (1) comprend une matrice de génération d'aérosol et un ensemble suscepteur ; l'ensemble suscepteur chauffe par induction une matrice de formation d'aérosol sous l'influence d'un champ magnétique alternatif, le matériau de l'ensemble suscepteur est un alliage magnétique souple, et l'alliage magnétique souple est une structure monocouche ayant des éléments uniformément répartis ; la granulométrie moyenne des grains de l'alliage magnétique souple est de 50 à 70 µm, et le niveau de granulométrie est de 5,5 à 4,5. L'ensemble suscepteur de la microstructure satisfait les exigences d'un suscepteur de dispositif de génération d'aérosol pour la performance magnétique et la température de Curie, et garantit que la température augmente rapidement lors d'une étape de préchauffage, et à une température inférieure à 400 °C, la conversion ferromagnétique-paramagnétique se produit et le magnétisme est complètement perdu, de sorte que le produit générateur d'aérosol peut être appliqué dans le domaine des cigarettes chauffées dans un processus de chauffage électromagnétique automatique à température régulée selon un principe de transmission radio sans contact et le risque de chauffage de cigarettes dans ce mode est remarquablement réduit.
PCT/CN2023/093981 2023-05-12 2023-05-12 Produit générateur d'aérosol Pending WO2024234163A1 (fr)

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PCT/CN2023/093981 WO2024234163A1 (fr) 2023-05-12 2023-05-12 Produit générateur d'aérosol

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180317286A1 (en) * 2015-10-22 2018-11-01 Philip Morris Products S.A. Particle and aerosol-forming system comprising such particles
WO2018228131A1 (fr) * 2017-06-14 2018-12-20 中国健康养生集团有限公司 Appareil de chauffage électrique, ses applications, cigarette, appareil et système de production d'aérosol
CN209058134U (zh) * 2018-09-18 2019-07-05 深圳市卓力能电子有限公司 一种电子烟发热体
CN113967738A (zh) * 2020-07-24 2022-01-25 四川三联新材料有限公司 气雾生成装置、感受器及制备方法
WO2022129272A1 (fr) * 2020-12-17 2022-06-23 Philip Morris Products S.A. Capsule comprenant des particules de suscepteur et un excipient
CN115191670A (zh) * 2022-08-19 2022-10-18 深圳麦克韦尔科技有限公司 一种复合感应加热感受器及其制备方法和应用
WO2023280991A1 (fr) * 2021-07-07 2023-01-12 Philip Morris Products S.A. Substrat de formation d'aérosol à conductivité thermique améliorée

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180317286A1 (en) * 2015-10-22 2018-11-01 Philip Morris Products S.A. Particle and aerosol-forming system comprising such particles
WO2018228131A1 (fr) * 2017-06-14 2018-12-20 中国健康养生集团有限公司 Appareil de chauffage électrique, ses applications, cigarette, appareil et système de production d'aérosol
CN209058134U (zh) * 2018-09-18 2019-07-05 深圳市卓力能电子有限公司 一种电子烟发热体
CN113967738A (zh) * 2020-07-24 2022-01-25 四川三联新材料有限公司 气雾生成装置、感受器及制备方法
WO2022129272A1 (fr) * 2020-12-17 2022-06-23 Philip Morris Products S.A. Capsule comprenant des particules de suscepteur et un excipient
WO2023280991A1 (fr) * 2021-07-07 2023-01-12 Philip Morris Products S.A. Substrat de formation d'aérosol à conductivité thermique améliorée
CN115191670A (zh) * 2022-08-19 2022-10-18 深圳麦克韦尔科技有限公司 一种复合感应加热感受器及其制备方法和应用

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