阅读说明：本技术 一种电子烟雾化器石墨烯热导陶瓷发热体的制备方法 (Preparation method of graphene heat-conducting ceramic heating body of electronic cigarette atomizer ) 是由 张志旭 华艺存 郭海明 于 2020-07-13 设计创作，主要内容包括：本发明涉及一种电子烟雾化器发热体的制备方法,公开一种石墨烯热导涂层陶瓷发热体的制备工艺,该方法有效解决传统雾化器加热设备热反应速率慢、传热效率低的技术问题。该方法包含以下步骤：(1)石墨烯改性电热涂料的制备；(2)石墨烯改性热导涂料在特种陶瓷的涂覆工艺；(3)石墨烯改性热导陶瓷发热体的高温烧结技术。石墨烯材料快速电热特性能够实现雾化器快速助热,石墨烯材料优异的导热性能,有利于烟草的充分雾化,提升烟草口感,材料安全性高,可以过滤烟油的杂质,减少烟气的有害成分。(The invention relates to a preparation method of a heating body of an electronic cigarette atomizer, and discloses a preparation process of a graphene thermal conductive coating ceramic heating body. The method comprises the following steps: (1) preparing a graphene modified electric heating coating; (2) a coating process of the graphene modified thermal conductive coating on special ceramics; (3) high-temperature sintering technology of graphene modified heat-conducting ceramic heating body. The quick electrothermal property of graphite alkene material can realize that the atomizer helps heat fast, and the excellent heat conductivility of graphite alkene material is favorable to the abundant atomizing of tobacco, promotes the tobacco taste, and the material security is high, can filter the impurity of tobacco tar, reduces the harmful component of flue gas.)

1. The preparation method of the graphene heat-conducting ceramic heating body of the electronic cigarette atomizer is characterized by comprising the following steps of:

(1) the preparation process of the graphene modified thermal conductive coating comprises the step of carrying out amination modification on 5000-mesh graphene nanoplatelets by using plasma equipment. Adding the compounded 75-80% of tert-butyl alcohol graphene nano silver conductive agent dispersion liquid into a reaction kettle at the constant temperature of 25 ℃, adding 10-15% of waterborne polyurethane/acrylic resin mixed material and 5-10% of deionized water, fully mixing, mechanically stirring, vacuumizing, shearing at high speed and homogenizing, finishing the process treatment, filtering the material and discharging.

(2) Coating and fixing the graphene modified heat conduction coating on the ceramic, and carrying out substrate adhesion and adhesion on the graphene heat conduction coating in the step (1) by adopting a JY-IC-560D round thick film printer, coating the inner side and the outer side of the ceramic device in an annular structure, and drying and fixing the graphene heat conduction slurry.

(3) And (3) high-temperature sintering molding of the graphene modified heat conduction coating ceramic heating element, placing the graphene heat conduction ceramic heating element in the step (2) in an inert gas atmosphere in a carbonization furnace for high-temperature treatment for 2h, and preparing the graphene heat conduction ceramic heating element device of the electronic cigarette atomizer.

2. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein in the step (1) of preparing the graphene modified thermal conductive coating, the graphene is mainly filled with graphene nanoplatelets treated by plasma, and the volume fraction of ammonia and nitrogen in the nitrogen source environment is 4:1, so that the amination degree of the graphene is 3-5%.

3. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein in the graphene modified thermal conductive coating of step (1), the conductive filler is compounded in the form of "20-30 parts of modified graphene, 15-20 parts of nano silver, 5-10 parts of conductive carbon black, and 1-2 parts of defoaming agent".

4. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein in the graphene modified thermal conductive coating of step (1), a resin system connecting material compounded by aqueous polyurethane/acrylic resin is adopted, and the mass ratio of aqueous polyurethane/acrylic resin is 1: 3.

5. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein in the graphene modified thermal conductive coating of step (1), the fully mixed materials are mechanically stirred for 10min at a rotation speed of 30-50rpm, a vacuum device is started, vacuum pumping is performed for 20min during stirring, a homogenizing device is started for high-speed shearing, the stirring rotation speed is adjusted to 10-30rpm, homogenizing is performed for 60min, and the interval of 5min during soaking is performed.

6. The preparation of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein in the graphene modified thermal conductive coating of step (1), a 100-mesh and 500-mesh filter screen is used for material filtration, and a high-level self-flowing positive pressure discharge is used for discharge.

7. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer as claimed in claim 1, wherein the graphene modified thermal conductive coating in step (2) is applied and shaped on the ceramic, the material viscosity is 2000 and 8000Mpa · s, the printing stable air pressure is 0.54-0.56Mpa, the material coating thickness is 1-3mm, and the drying temperature is 70-90 ℃.

8. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer of claim 1, wherein the graphene modified thermal conductive coating in the step (2) is coated and shaped on the ceramic in a screen printing or spraying manner, the surface of the ceramic is a planar heating film, and the graphene coating film with a power supply wire and a ceramic lining has a rapid thermal conductive effect.

9. The preparation method of the graphene thermal conductive ceramic heating element of the electronic smoke atomizer according to claim 1, wherein the graphene modified thermal conductive coating ceramic heating element in the step (3) is sintered and molded at a high temperature, the processing temperature range is set to 500-.

Technical Field

The invention relates to a preparation method of a heating body of an electronic cigarette atomizer, in particular to a preparation process of a graphene thermal conduction coating ceramic heating body.

Background

Along with the attention of people to healthy life and the enhancement of smoking prohibition measures of all countries, the traditional cigarette market is lack of strength, and the electronic cigarette market taking young people as the consumption master has a trend of remarkably rising in the market. The production and manufacture of Chinese electronic cigarettes already form a mature industrial chain system, and the industrial prospect is wide. In 2017, the yield of the Chinese electronic cigarette is 16.51 hundred million, in 2018, 22.29 hundred million is achieved, 25.42 hundred million is expected to be achieved in 2020, the yield of the Chinese electronic cigarette is continuously increased, and the growth speed exceeds 30%.

At present, electronic cigarettes can be roughly divided into two categories, one is tobacco tar type electronic cigarettes, and the main components of the electronic cigarettes are edible or medical glycerin, tobacco essence, tobacco extract and the like. The materials are changed into steam by atomization means, and then the steam is sucked by a user. The tobacco tar type electronic cigarette can be divided into a closed system and an open system. The second category is the heating of non-combustible tobacco products, i.e. low temperature cigarettes, where the material of the cartridge is kept the same as the cut tobacco in a conventional cigarette, but heated in a non-combustible manner by an electronically controlled heating blade at a temperature below 350 ℃, thereby releasing (nicotine-containing) smoke for the user to smoke. Typical products are IQOS, fimo international, Glo, engme tobacco and ploom tech, japan tobacco.

Different types of electronic cigarettes have slight differences in structure, but the main structures of the electronic cigarettes are approximately the same. Four core elements of the electronic cigarette: tobacco tar, control chip, atomizer, battery. In the cost structure of the electronic cigarette, the battery accounts for the highest percentage, reaching 55% of the total cost, followed by the atomizer accounting for 35%. The atomizer is an important component of the electronic cigarette, and the smoke is obtained by heating a heating wire in the atomizer to evaporate tobacco tar on the inner oil guide cotton. The heating wire is the part of the electronic cigarette which directly contacts with the tobacco tar and is the most core part. The heating wire is powered by a battery, and the current can generate heat to heat through a coil made of the heating wire, and then the tobacco tar is atomized to generate steam. Generally, the resistance of the heating wire is not always fixed and can change along with the change of temperature.

The electronic cigarette technology has been developed to the fourth generation products, the most representative of which is that Feelm pushed by mivir combines a metal film and a ceramic conductor, and breaks through in the aspects of material and structure science, and represents an innovative technology in the field of steam atomization, and the ceramic heating element technology of the electronic cigarette technology leads the market by about 12-18 months. However, the metal sheet ceramic combination mode is also influenced by the impedance of the metal material along with the temperature change in the aspect of temperature accurate control, the metal sheet ceramic combination mode needs to be heated to a specified temperature within 30 seconds in the aspect of rapid thermal reaction rate, and the metal sheet ceramic combination mode is influenced by the impedance fluctuation of different positions of the metal film, and the temperature has certain difference, so that the atomization effect of the tobacco is influenced. According to the preparation method of the graphene heat conduction ceramic heating body of the electronic cigarette atomizer, the rapid thermal reaction efficiency, the good thermal stability and the heat conduction performance of the graphene material are realized, and the atomizer heating body is prepared in a manner of compounding with special ceramics, so that an extraordinary wide heating surface is created, the temperature can be accurately and intelligently applied, the generation of instant steam is ensured, harmful substances are reduced, and the service life of the heating body is effectively prolonged.

Disclosure of Invention

The invention aims to solve the technical problems of low thermal reaction efficiency of an electronic cigarette atomizer, influence of resistance of a heating element along with temperature change, insufficient heat conduction and the like, and discloses a preparation method of a graphene thermal conductive ceramic heating element of the electronic cigarette atomizer by combining the excellent characteristics of a graphene material.

The method comprises the following steps:

(1) the preparation process of the graphene modified thermal conductive coating comprises the step of carrying out amination modification on 5000-mesh graphene nanoplatelets by using plasma equipment. Adding the compounded 75-80% of tert-butyl alcohol graphene nano silver conductive agent dispersion liquid into a reaction kettle at the constant temperature of 25 ℃, adding 10-15% of waterborne polyurethane/acrylic resin mixed material and 5-10% of deionized water, fully mixing, mechanically stirring, vacuumizing, shearing at high speed and homogenizing, finishing the process treatment, filtering the material and discharging.

(2) Coating and fixing the graphene modified heat conduction coating on the ceramic, and carrying out substrate adhesion and adhesion on the graphene heat conduction coating in the step (1) by adopting a JY-IC-560D round thick film printer, coating the inner side and the outer side of the ceramic device in an annular structure, and drying and fixing the graphene heat conduction slurry.

(3) And (3) high-temperature sintering molding of the graphene modified heat conduction coating ceramic heating element, placing the graphene heat conduction ceramic heating element in the step (2) in an inert gas atmosphere in a carbonization furnace for high-temperature treatment for 2h, and preparing the graphene heat conduction ceramic heating element device of the electronic cigarette atomizer.

In the specific process preparation of the graphene modified thermal conductive coating in the step (1), the graphene microchip treated by plasma is adopted as the main filler graphene, and the volume fraction of ammonia gas and nitrogen gas in a nitrogen source environment is 4:1, so that the amination degree of the graphene is 3-5%.

Specifically, in the graphene modified thermal conductive coating in the step (1), the conductive filler is compounded according to the form of 20-30 parts of modified graphene, 15-20 parts of nano silver, 5-10 parts of conductive carbon black and 1-2 parts of defoaming agent.

Specifically, in the graphene modified thermal conductive coating in the step (1), a resin system connecting material compounded by aqueous polyurethane/acrylic resin is adopted, and the mass ratio of the aqueous polyurethane to the acrylic resin is 1: 3.

In the graphene modified thermal conductive coating in the step (1), fully mixing materials, mechanically stirring for 10min at a rotation speed of 30-50rpm, starting a vacuum device, vacuumizing for 20min during stirring, starting a homogenizing device for high-speed shearing, adjusting the stirring rotation speed to 10-30rpm, homogenizing for 60min, and performing bubble extraction at an interval of 5 min.

In the graphene modified heat conduction coating in the step (1), a 100-mesh filter screen is adopted for material filtration, and a high-level self-flowing positive-pressure discharging mode is adopted for discharging.

Specifically, the graphene modified heat conduction coating in the step (2) is coated and shaped on the ceramic, the material viscosity is 2000-.

Specifically, the graphene modified heat conduction coating in the step (2) is coated and shaped on the ceramic, the adopted coating mode is screen printing or spraying, the surface of the ceramic is a planar heating film and is connected with a power supply lead, and the graphene coating film with the ceramic lining has the effect of rapid heat conduction.

Specifically, in the step (3), the graphene modified heat conduction coating ceramic heating element is sintered and formed at a high temperature, the processing temperature interval is set to be 500-800 ℃, the heating rate is set to be 2-5 ℃/min, the temperature is kept for 2h in a constant temperature area, and the temperature is reduced in a natural cooling mode.

According to the preparation method of the graphene heat conduction ceramic heating element of the electronic cigarette atomizer, the preparation of the graphene modified heat conduction coating and the coating forming of the graphene modified heat conduction coating ceramic heating element are realized, 5V direct-current voltage electrifying simulation test of a heating element device is carried out, the temperature-sensitive area of the heating element can reach 350 ℃ in 25 seconds at the fastest speed, and the test impedance is 0.05 ohm; the adhesive force of the graphene modified thermal conductive coating of the heating body reaches 3B level; the heat conduction performance of the ceramic body coated with the graphene modified heat conduction coating is simulated by using a heat source at 300 ℃, and the surface temperature is 30 ℃ higher than that of the ceramic body without the coating.

Drawings

FIG. 1 is an SEM image of aminated modified graphene

FIG. 2 is an FTIR image of aminated modified graphene

FIG. 3 is a technical index legend of graphene thermal conductive coating

FIG. 4 shows data parameters of embodiments of the graphene thermal conductive ceramic heater

FIG. 5 is a TGA image of high temperature processing of a ceramic thermal conductive coating

FIG. 6 is a perspective cross-sectional view of a graphene thermal conductive ceramic heating element of an atomizer

FIG. 7 is an impedance spectrum of graphene thermal conductance ceramic heater for atomizer

FIG. 8 is a heat dissipation map of graphene thermal conductivity ceramics for a 300 deg.C heat source

FIG. 9 is a graph of temperature rise rate of a graphene thermal conductive ceramic heating element VS Macweil Feelm heating element

Detailed Description

The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the scope of the present invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.