CN116420942A - Infrared heater, preparation method thereof and aerosol generating device - Google Patents
Infrared heater, preparation method thereof and aerosol generating device Download PDFInfo
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- CN116420942A CN116420942A CN202211533212.7A CN202211533212A CN116420942A CN 116420942 A CN116420942 A CN 116420942A CN 202211533212 A CN202211533212 A CN 202211533212A CN 116420942 A CN116420942 A CN 116420942A
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Abstract
The invention discloses an infrared heater, a preparation method thereof and an aerosol generating device, wherein the preparation method of the infrared heater comprises the following steps: snCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution; repeatedly depositing the mixed solution on the outer surface of the insulating matrix for 3-10 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, wherein the deposition temperature is 650-750 ℃, and the deposition residence time is 20-100s each time; printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain an infrared heater; the infrared radiation layer of the phosphorus-doped tin oxide film layer formed by multiple CVD reactions has good film forming uniformity and high bonding strength between the film layer and the insulating matrix; phosphor in the infrared radiation layer of the phosphor doped tin oxide film layer contributes to the modificationThe infrared radiation layer has good conductivity and infrared radiation efficiency, and the infrared radiation layer of the phosphorus-doped tin oxide film layer is more environment-friendly and safer.
Description
Technical Field
The invention relates to the technical field of smoking sets, in particular to an infrared heater, a preparation method thereof and an aerosol generating device.
Background
The existing heating non-burning smoking set mainly generates heat through a heating element and transmits the heat to an aerosol generating matrix in a cavity so that at least one component volatilizes to generate aerosol for a user to inhale, and the heating element used by the smoking set is an infrared heater, and the infrared heater has the advantages of higher heating speed but low heat conduction efficiency, so that the aerosol generating matrix is slowly preheated, and the internal matrix material is difficult to effectively heat, so that the problems of poor taste and poor experience of the aerosol are caused, and the infrared heater needs to be improved.
The chinese patent application No. CN202110979610.0 discloses a heater and a method for preparing the same, and an aerosol-generating device comprising the same, and specifically discloses a method for preparing the same, comprising the steps of: a. mixing isopropanol or water, stannic chloride and antimony trichloride to obtain a mixed solution; b. repeatedly depositing the mixed solution on the outer surface of the insulating matrix for 3-10 times to form a deposited infrared radiation layer, wherein the deposition temperature is 600-800 ℃, and the deposition residence time is 15-360s each time; c. printing an electrode layer on the surface of the infrared radiation layer obtained after deposition, and performing high-temperature sintering to obtain the heater; the infrared radiation layer of the antimony-doped tin oxide film layer is adopted in the application, although the infrared radiation rate of the infrared radiation layer of the antimony-doped tin oxide film layer is higher, antimony and compounds thereof are global pollutants, antimony is one of the most internationally focused toxic metal elements, and antimony and compounds thereof are management substances, so that the dosage of the antimony is limited, and therefore, the finding of a dopant which is environment-friendly and can enable the infrared radiation layer to have higher infrared radiation rate has important research significance.
Disclosure of Invention
The invention aims to provide an infrared heater, a preparation method thereof and an aerosol generating device, which are used for solving the problem that an infrared radiation layer of an antimony-doped tin oxide film layer pollutes the environment in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
in a first aspect, the present invention provides a method for manufacturing an infrared heater, comprising:
SnCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution;
repeatedly depositing the mixed solution on the outer surface of the insulating matrix for 3-10 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, wherein the deposition temperature is 650-750 ℃, and the deposition residence time is 20-100s each time;
and printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain the infrared heater.
Further, in the mixed solution, snCl 4 The concentration of H is 0.5-3 mol/L 3 PO 4 The concentration of the isopropyl alcohol is 0.05 to 0.5mol/L, the concentration of the isopropyl alcohol is 0.15mol/L, and the concentration of the CaCl is 0.15mol/L 2 The concentration of (C) was 0.03mol/L.
Further, the mole ratio of tin to phosphorus of the phosphorus-doped tin oxide film layer is 20:1-2
Further, the infrared radiation layer has a resistivity of 1×10 -6 ～15×10 -6 Ω·m。
Further, the insulating substrate is one or more of germanium single crystal, silicon single crystal, gallium arsenide, gallium phosphide, sapphire, alumina polycrystal, spinel, magnesium oxide, yttrium oxide, quartz, yttrium aluminum garnet, zinc sulfide, zinc selenide, silicon carbide, silicon nitride, magnesium fluoride, calcium fluoride and arsenic trisulfide.
In a second aspect, the present invention provides an infrared heater made by the method described above.
In a third aspect, the present invention provides an aerosol-generating device comprising a housing assembly and an infrared heater as described above, the infrared heater being disposed within the housing assembly.
Tin oxide (SnO) 2 ) Is a very important metal oxide semiconductor material with a wide forbidden band (the forbidden band width is 3.7-4.3 eV). Common single crystal SnO 2 In the tetragonal rutile structure, in a tin oxide unit cell, a Sn atom is positioned at the center of an oxygen octahedron, and 6O atoms are arranged around each Sn atom; similarly, 3 Sn atoms are attached around each O atom. Polycrystalline SnO 2 The film is composed of crystal grains with a tetragonal cassiterite structure or a tetragonal rutile structure, and the growing SnO is prepared by a film process 2 The preferred orientation of the crystal grain of the film has close relation with the parameters of the crystal structure, the surface state, the growth temperature and the like of the substrate material.
At a proper doping concentration, a phosphorus-doped tin oxide film layer (SnO 2 P film) is a polycrystalline degenerate semiconductor, P is typically found in SnO 2 As pentavalent donor atoms in the lattice. The conductivity of the phosphorus doped tin oxide film layer increases with the increase of the P concentration, and when the P concentration reaches a certain value, the conductivity decreases with the increase of the P concentration. This is because, when P is initially incorporated, P serves as a donor atom to increase the carrier concentration, thereby causing SnO to be formed 2 The conductivity of the P film is increased; when a certain value is reached, the concentration of P is further increased, so that the ionized impurity concentration and the lattice defect density are increased, and the carrier mobility is decreased, thereby causing a decrease in conductivity.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the infrared heater, the infrared radiation layer of the phosphorus-doped tin oxide film layer is formed through multiple CVD reactions, so that film forming uniformity is good, and the bonding strength of the film layer and an insulating substrate is high; the phosphorus element in the infrared radiation layer of the phosphorus-doped tin oxide film layer is beneficial to improving the conductivity and the infrared radiation efficiency of the infrared radiation layer, and the infrared radiation layer of the phosphorus-doped tin oxide film layer is more environment-friendly and safer.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method of making an infrared heater comprising:
s1: snCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution; in the mixed solution, snCl 4 The concentration of (C) is 0.5mol/L, H 3 PO 4 The concentration of (C) is 0.05mol/L, the concentration of isopropanol is 0.15mol/L, caCl 2 The concentration of (C) was 0.03mol/L.
S2, performing S2; the mixed solution is repeatedly deposited on the outer surface of the insulating matrix for 3 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, and the specific method is as follows:
setting the heating temperature of the CVD (Chemical Vapour Deposition, chemical vapor deposition) reaction chamber to 650 ℃, and starting a heating power supply; clamping an insulating substrate on a coating jig, wherein the insulating substrate is quartz, and starting an automatic coating mode; the coating jig is conveyed forward along with an online CVD coating conveyor belt; the insulating substrate is heated to a temperature of 650 ℃ required for the reaction during the transfer in the CVD coating chamber.
The CVD coating process adopts an online CVD coating device, wherein the online CVD coating device is a CVD continuous coating device and is provided with one or more CVD deposition positions, and the online deposition is carried out for a plurality of times, so that the uniformity of the film thickness is ensured, and a certain film thickness is achieved; one end is a charging end, and the other end is a semi-finished product discharging end; the rod-shaped coating jig penetrates through the insulating substrate and fixes the insulating substrate at a specific position; after the film plating jig is clamped on the CVD film plating equipment, the jig can rotate, so that the film plating uniformity of the outer surface of the insulating substrate is ensured in the film plating process; the coating jig transfers the sample from one end of the coating apparatus to the other end by a rotation and transport mechanism on the CVD coating apparatus.
The suction pump sucks the mixed solution up and atomizes the mixed solution through the ultrasonic atomizing head, and the mixed solution is uniformly dispersed in a CVD deposition area under the high-temperature heating condition; when the insulating substrate reaches the atomization deposition area and the insulating substrate is in the rotating process, the phosphorus-doped tin oxide film layer is uniformly deposited.
In the CVD reaction deposition process, the residence time of each deposition of the insulating matrix is 20s; if the residence time is too long, ultrasonic atomization is continuously carried out, the temperature of a deposition area is far lower than the temperature required by the reaction, and at the moment, the film forming quality is poor or film forming cannot be carried out.
The insulating matrix is subjected to primary deposition, continuously runs to a next deposition area, is heated to be recovered to a temperature suitable for reaction, and then continuously runs to the next deposition area; the infrared radiation layer of the phosphorus-doped tin oxide film layer can reach the required thickness and the proper resistance range after the process is repeated for 3 times.
The CVD reaction is as follows:
SnCl 4 +O 2 +H 2 O→SnO 2 +HCl↑+CO↑
p and Ca doping ions occupy part of SnO 2 Sn in lattice 4+ The location of the ions.
The reaction product molecules stay on the surface of the insulating substrate, and the reaction byproduct molecules are desorbed from the surface of the insulating substrate and discharged outside the CVD reaction chamber along with the gas flow.
After the insulating matrix is deposited for the last time, the insulating matrix passes through a section of high-temperature area and is heated, the CVD deposited film and the insulating matrix are firmly combined, then the insulating matrix enters a cooling area and is gradually cooled to below 300 ℃, and the insulating matrix can be discharged from a furnace and enters the atmosphere to be directly cooled to the room temperature.
The mole ratio of tin to phosphorus of the phosphorus-doped tin oxide film layer is 20:1, and the resistivity of the infrared radiation layer of the formed phosphorus-doped tin oxide film layer is 1 multiplied by 10 -6 Omega.m, resistivity can be controlled by dopingThe content of the impurity elements is controlled.
S3, performing S3; printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain the infrared heater, wherein the specific method comprises the following steps:
printing a silver electrode thick film on the insulating substrate on which the infrared radiation layer is deposited by adopting a printing screen with customized electrode patterns, wherein the film thickness is about 20 mu m;
placing the insulating substrate printed with the thick film silver electrode pattern into a sintering furnace, wherein the sintering temperature is 1130 ℃, and the sintering time is 9 hours;
testing the insulating matrix of the sintered silver electrode, detecting the silver electrode film and the phosphorus doped tin oxide film layer deposited by CVD, and screening out qualified products.
Example 2
A method of making an infrared heater comprising:
s1: snCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution; in the mixed solution, snCl 4 The concentration of (C) is 1.5mol/L, H 3 PO 4 The concentration of (C) is 0.3mol/L, the concentration of isopropanol is 0.15mol/L, caCl 2 The concentration of (C) was 0.03mol/L.
S2, performing S2; the mixed solution is repeatedly deposited on the outer surface of the insulating matrix for 7 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, and the specific method is as follows:
setting the heating temperature of a CVD (Chemical Vapour Deposition, chemical vapor deposition) reaction chamber to 700 ℃, and starting a heating power supply; clamping an insulating substrate on a coating jig, wherein the insulating substrate is silicon carbide, and starting an automatic coating mode; the coating jig is conveyed forward along with an online CVD coating conveyor belt; the insulating substrate is heated to a temperature required for the reaction to 700 ℃ during the transfer in the CVD coating chamber.
The CVD coating process adopts an online CVD coating device, wherein the online CVD coating device is a CVD continuous coating device and is provided with one or more CVD deposition positions, and the online deposition is carried out for a plurality of times, so that the uniformity of the film thickness is ensured, and a certain film thickness is achieved; one end is a charging end, and the other end is a semi-finished product discharging end; the rod-shaped coating jig penetrates through the insulating substrate and fixes the insulating substrate at a specific position; after the film plating jig is clamped on the CVD film plating equipment, the jig can rotate, so that the film plating uniformity of the outer surface of the insulating substrate is ensured in the film plating process; the coating jig transfers the sample from one end of the coating apparatus to the other end by a rotation and transport mechanism on the CVD coating apparatus.
The suction pump sucks the mixed solution up and atomizes the mixed solution through the ultrasonic atomizing head, and the mixed solution is uniformly dispersed in a CVD deposition area under the high-temperature heating condition; when the insulating substrate reaches the atomization deposition area and the insulating substrate is in the rotating process, the phosphorus-doped tin oxide film layer is uniformly deposited.
In the CVD reaction deposition process, the residence time of each deposition of the insulating matrix is 70s; if the residence time is too long, ultrasonic atomization is continuously carried out, the temperature of a deposition area is far lower than the temperature required by the reaction, and at the moment, the film forming quality is poor or film forming cannot be carried out.
The insulating matrix is subjected to primary deposition, continuously runs to a next deposition area, is heated to be recovered to a temperature suitable for reaction, and then continuously runs to the next deposition area; the infrared radiation layer of the phosphorus-doped tin oxide film layer can reach the required thickness and the proper resistance range after 7 times of reciprocating.
The CVD reaction is as follows:
SnCl 4 +O 2 +H 2 O→SnO 2 +HCl↑+CO↑
p and Ca doping ions occupy part of SnO 2 Sn in lattice 4+ The location of the ions.
The reaction product molecules stay on the surface of the insulating substrate, and the reaction byproduct molecules are desorbed from the surface of the insulating substrate and discharged outside the CVD reaction chamber along with the gas flow.
After the insulating matrix is deposited for the last time, the insulating matrix passes through a section of high-temperature area and is heated, the CVD deposited film and the insulating matrix are firmly combined, then the insulating matrix enters a cooling area and is gradually cooled to below 300 ℃, and the insulating matrix can be discharged from a furnace and enters the atmosphere to be directly cooled to the room temperature.
The mol ratio of tin to phosphorus of the phosphorus-doped tin oxide film layer is 20:1.5, and the infrared radiation layer of the phosphorus-doped tin oxide film layer is formedHas a resistivity of 8X 10 -6 The resistivity of Ω·m can be controlled by doping elements and the content.
S3, performing S3; printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain the infrared heater, wherein the specific method comprises the following steps:
printing a silver electrode thick film on the insulating substrate on which the infrared radiation layer is deposited by adopting a printing screen with customized electrode patterns, wherein the film thickness is about 20 mu m;
placing the insulating substrate printed with the thick film silver electrode pattern into a sintering furnace, wherein the sintering temperature is 1130 ℃, and the sintering time is 9 hours;
testing the insulating matrix of the sintered silver electrode, detecting the silver electrode film and the phosphorus doped tin oxide film layer deposited by CVD, and screening out qualified products.
Example 3
A method of making an infrared heater comprising:
s1: snCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution; in the mixed solution, snCl 4 The concentration of (C) is 3mol/L, H 3 PO 4 The concentration of (C) is 0.5mol/L, the concentration of isopropanol is 0.15mol/L, caCl 2 The concentration of (C) was 0.03mol/L.
S2, performing S2; the mixed solution is repeatedly deposited on the outer surface of the insulating matrix for 10 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, and the specific method is as follows:
setting the heating temperature of the CVD (Chemical Vapour Deposition, chemical vapor deposition) reaction chamber to 750 ℃, and starting a heating power supply; clamping an insulating substrate on a coating jig, wherein the insulating substrate is germanium monocrystal, and starting an automatic coating mode; the coating jig is conveyed forward along with an online CVD coating conveyor belt; the insulating substrate is heated to a temperature of 750 ℃ required for the reaction during the transfer in the CVD coating chamber.
The CVD coating process adopts an online CVD coating device, wherein the online CVD coating device is a CVD continuous coating device and is provided with one or more CVD deposition positions, and the online deposition is carried out for a plurality of times, so that the uniformity of the film thickness is ensured, and a certain film thickness is achieved; one end is a charging end, and the other end is a semi-finished product discharging end; the rod-shaped coating jig penetrates through the insulating substrate and fixes the insulating substrate at a specific position; after the film plating jig is clamped on the CVD film plating equipment, the jig can rotate, so that the film plating uniformity of the outer surface of the insulating substrate is ensured in the film plating process; the coating jig transfers the sample from one end of the coating apparatus to the other end by a rotation and transport mechanism on the CVD coating apparatus.
The suction pump sucks the mixed solution up and atomizes the mixed solution through the ultrasonic atomizing head, and the mixed solution is uniformly dispersed in a CVD deposition area under the high-temperature heating condition; when the insulating substrate reaches the atomization deposition area and the insulating substrate is in the rotating process, the phosphorus-doped tin oxide film layer is uniformly deposited.
In the CVD reaction deposition process, the residence time of each deposition of the insulating substrate is 100s; if the residence time is too long, ultrasonic atomization is continuously carried out, the temperature of a deposition area is far lower than the temperature required by the reaction, and at the moment, the film forming quality is poor or film forming cannot be carried out.
The insulating matrix is subjected to primary deposition, continuously runs to a next deposition area, is heated to be recovered to a temperature suitable for reaction, and then continuously runs to the next deposition area; the infrared radiation layer of the phosphorus-doped tin oxide film layer can reach the required thickness and the proper resistance range after 10 times of reciprocating.
The CVD reaction is as follows:
SnCl 4 +O 2 +H 2 O→SnO 2 +HCl↑+CO↑
p and Ca doping ions occupy part of SnO 2 Sn in lattice 4+ The location of the ions.
The reaction product molecules stay on the surface of the insulating substrate, and the reaction byproduct molecules are desorbed from the surface of the insulating substrate and discharged outside the CVD reaction chamber along with the gas flow.
After the insulating matrix is deposited for the last time, the insulating matrix passes through a section of high-temperature area and is heated, the CVD deposited film and the insulating matrix are firmly combined, then the insulating matrix enters a cooling area and is gradually cooled to below 300 ℃, and the insulating matrix can be discharged from a furnace and enters the atmosphere to be directly cooled to the room temperature.
The mole ratio of tin and phosphorus in the phosphorus-doped tin oxide film layerThe resistivity of the infrared radiation layer of the formed phosphor-doped tin oxide film layer is 15 multiplied by 10 at 20:2 -6 The resistivity of Ω·m can be controlled by doping elements and the content.
S3, performing S3; printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain the infrared heater, wherein the specific method comprises the following steps:
printing a silver electrode thick film on the insulating substrate on which the infrared radiation layer is deposited by adopting a printing screen with customized electrode patterns, wherein the film thickness is about 20 mu m;
placing the insulating substrate printed with the thick film silver electrode pattern into a sintering furnace, wherein the sintering temperature is 1130 ℃, and the sintering time is 9 hours;
testing the insulating matrix of the sintered silver electrode, detecting the silver electrode film and the phosphorus doped tin oxide film layer deposited by CVD, and screening out qualified products.
The infrared heaters prepared in examples 1 to 3 are arranged in a shell component of an aerosol generating device, then the actual working condition is detected, the two ends of the infrared heating tube are equal to the middle heating temperature after being electrified, the temperature difference is controlled within 5 ℃, and the test result shows that the infrared heater with the infrared radiation layer of the phosphorus-doped tin oxide film layer has better heating performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A method of manufacturing an infrared heater, comprising:
SnCl is added 4 ·5H 2 O, dense H 3 PO 4 Isopropanol, caCl 2 Mixing with water to obtain a mixed solution;
repeatedly depositing the mixed solution on the outer surface of the insulating matrix for 3-10 times to form an infrared radiation layer of the phosphorus-doped tin oxide film layer, wherein the deposition temperature is 650-750 ℃, and the deposition residence time is 20-100s each time;
and printing an electrode layer on the surface of the infrared radiation layer, and sintering to obtain the infrared heater.
2. The method for producing an infrared heater according to claim 1, wherein SnCl is contained in the mixed solution 4 The concentration of H is 0.5-3 mol/L 3 PO 4 The concentration of the isopropyl alcohol is 0.05 to 0.5mol/L, the concentration of the isopropyl alcohol is 0.15mol/L, and the concentration of the CaCl is 0.15mol/L 2 The concentration of (C) was 0.03mol/L.
3. The method for preparing an infrared heater according to claim 1, wherein the mole ratio of tin to phosphorus in the phosphorus-doped tin oxide film layer is 20:1-2.
4. The method of manufacturing an infrared heater according to claim 1, wherein the infrared radiation layer has a resistivity of 1 x 10 -6 ～15×10 -6 Ω·m。
5. The method of manufacturing an infrared heater according to claim 1, wherein the insulating substrate is one or more of germanium single crystal, silicon single crystal, gallium arsenide, gallium phosphide, sapphire, alumina polycrystal, spinel, magnesium oxide, yttria, quartz, yttrium aluminum garnet, zinc sulfide, zinc selenide, silicon carbide, silicon nitride, magnesium fluoride, calcium fluoride, arsenic trisulfide.
6. An infrared heater made by the method of any one of claims 1 to 5.
7. An aerosol-generating device comprising a housing assembly and the infrared heater of claim 6 disposed within the housing assembly.
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| CN202211533212.7A CN116420942A (en) | 2022-12-02 | 2022-12-02 | Infrared heater, preparation method thereof and aerosol generating device |
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| CN202211533212.7A CN116420942A (en) | 2022-12-02 | 2022-12-02 | Infrared heater, preparation method thereof and aerosol generating device |
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