High temperature glass powder for electronic cigarette nickel paste and preparation method thereof

Abstract

The present invention discloses a high-temperature glass powder and a preparation method thereof, and in particular, relates to a high-temperature glass powder for nickel paste of electronic cigarettes and a preparation method thereof. The glass powder comprises a base glass and a second component, the base glass comprises CaO, Al2O3, SiO2, B2O3 and Na2CO3, and the second component comprises one or more of TiO2, CeO2, ZrO2, Nb2O5 or WO3. The preparation method thereof is as follows: the base glass powder raw material is mixed uniformly and then preheated, placed in a glass frit furnace for high-temperature insulation, the second component is added to the mixture and then subjected to high-temperature smelting, water quenching, and crushing. The present invention makes the glass powder have a high softening temperature by adding the second component and smelting in steps, thereby improving the bonding strength between the nickel-based alloy layer and the porous ceramic substrate, reducing the vitrification penetration into the ceramic substrate, and improving the cycle life and stability.

Description

Technical Field

[0001] The invention relates to a high-temperature glass powder and a preparation method thereof, and in particular to a high-temperature glass powder for electronic cigarette nickel paste and a preparation method thereof. Background Art

[0002] Electronic atomizers are becoming more and more popular among young people, and their acceptance is getting higher and higher. The heating elements used in atomizers mainly include metal heating elements and ceramic heating elements. The metal heating elements use porous ceramics as the atomization core, which heats up quickly and has low cost. However, during the inhalation process of electronic cigarettes using atomization cotton atomization cores, it is easy to produce the burnt smell of atomization cotton and the metallic taste produced by the heating of metal heating wires, which seriously affect the user experience. The porous ceramic atomization core can well avoid such problems and gradually become the mainstream technology.

[0003] The porous ceramic atomization core is a heating layer printed with nickel-based slurry on the surface of porous ceramics to achieve the atomization effect. Glass powder, as an important component, can promote the densification sintering of the conductive layer, improve the bonding strength between the nickel-based metal layer and the porous ceramic, and improve the thermal conductivity and atomization effect. The sintering temperature of nickel-based slurry is generally between 1000 and 1150°C, but the softening point of the current mainstream glass powder is within 850°C, which is much lower. At this sintering temperature, the glass liquid has low viscosity, high fluidity, and strong erosion and penetration, resulting in poor linearity of the nickel-based heating layer after sintering, and a deepening of the ceramic glass layer. During the use of cyclic heating, the resistance fluctuation gradually increases, the metal layer falls off, and the ceramic glass layer intensifies (fragility increases, resulting in fragility and cracking). Therefore, increasing the softening temperature of nickel slurry glass powder has great application significance.

[0004] In the existing technology, the melting temperature of high-temperature glass powder is high, generally 1500-1700℃. At present, most of them use corundum crucibles and single melting methods. The corundum crucible needs to be hot in and hot out / cold in and hot out. Due to the size of the corundum crucible, it cannot be used multiple times, resulting in high production costs, low production capacity, batch instability and other problems. The glass melting furnace used in ultra-large-scale mass production melting equipment uses natural gas as a heat source. It is a large-scale industrial equipment with large investment and strict environmental assessment requirements. It is not suitable for large-scale mass production in this field. Summary of the invention

[0005] To achieve the above objectives, the present invention adopts the following specific technical solutions:

[0006] The present invention provides a high-temperature glass powder for nickel paste of electronic cigarettes, comprising a base glass and a second component, wherein the base glass comprises CaO, Al2O3, SiO2, B2O3 and Na2CO3, etc., and the second component comprises one or more of TiO2, CeO2, ZrO2, Nb2O5 or WO3, etc.

[0007] TiO2 is a peroxide, usually with an octahedral structure as the network outer oxide. 4+ Ce can connect the broken Si-O bonds and strengthen the glass network structure. TiO2 can act as a crystallization inducing agent and induce the formation of silicate glass nuclei above 600°C, thus increasing the softening temperature. 4+ and Zr 4+ High field strength and high coordination can also increase the strength of the glass network structure, improve stability, and increase softening temperature. In addition, Nb2O5 and WO3, as high-coordination oxides, can react with free O 2- It has stronger bonding strength and can simultaneously increase softening temperature and high temperature stability.

[0008] Furthermore, the mass percentage of the matrix glass is 95-99%; the mass percentage of the second component is 1-5%; preferably, the mass percentages of CaO, Al2O3, SiO2, B2O3 and Na2CO3 are 20-40%, 10-20%, 35-50%, 10-20% and 1-3% respectively.

[0009] Furthermore, the softening temperature of the glass powder is 850-1000°C, and the D 50 The particle size is 3.0-5.0μm, which has good water resistance, high temperature stability and high temperature acid and alkali resistance, and is more compatible with the co-firing temperature of the nickel-based slurry. It can increase the service life of the nickel-based heating layer under high-temperature atomization of different smoke oils, improve the bonding strength with porous ceramics, reduce the vitrification of porous ceramics and the cyclic heating process, and increase the service life.

[0010] The present invention also provides a method for preparing high-temperature glass powder for electronic cigarette nickel paste, comprising the following steps:

[0011] S10: After the matrix glass powder raw materials are mixed evenly, they are preheated to remove moisture and make the materials compact for easy feeding.

[0012] Preferably, the mixing comprises mixing the matrix glass powder raw materials, and then performing secondary mixing after sieving.

[0013] Preferably, the preheating treatment temperature is 200-300° C., and the preheating treatment time is 30-60 min.

[0014] S20: placing the product of step S10 in a glass frit furnace and keeping it at 1000-1200° C. for 10-30 minutes.

[0015] Preferably, before adding the product in step S10, the glass frit furnace is first loaded with an empty crucible and heated to 1000-1200°C at a heating rate of 3-5°C / min and kept warm for 10-30 minutes, and then the product in step S10 is added to the crucible, and the operation of step S20 is performed. At this temperature, the operation is safer for personnel, and the crucible has better resistance to cold and hot shocks, and will not crack due to excessive temperature difference of the added materials, and further avoid the boiling and splashing of some materials with lower temperatures due to excessive temperature of the preheated materials.

[0016] S30: adding the second component into the glass frit furnace, mixing with the product in step S20 and then melting at high temperature.

[0017] Furthermore, the temperature of the high temperature smelting is 1300-1400° C., and the time of the high temperature smelting is 30-60 minutes.

[0018] Preferably, stirring is performed during the high-temperature smelting process.

[0019] Preferably, step S21 is further included between step S20 and step S30: heating the product in step S20 to 1500-1650° C. at a heating rate of 5-10° C. / min in the glass frit furnace for pre-high temperature melting for 30-120 min.

[0020] More preferably, in step S21, the product after the previous high-temperature smelting is cooled to 1300-1400°C at a rate of 3-5°C / min, and then step S30 is performed.

[0021] S40: the product in step S30 is discharged and water quenched, and then the glass frit furnace is cooled to 1000-1200° C., and then the S10 product prepared in advance is added so that the next batch of materials can be continuously produced.

[0022] The processes of adding materials, smelting and water quenching are repeated to realize continuous production. The smelting process realizes step-by-step smelting, which can effectively improve the safety of personnel operation, avoid the risks and difficulties of personnel operation at 1500-1600°C, meet the performance requirements of high-temperature smelting, and at the same time, increase the service life of the crucible and reduce production costs.

[0023] The structure of the glass frit furnace is that the material is added at the top and discharged at the bottom. The weight of a single smelting is 15-25kg. The crucible is placed in the middle of the furnace body. There is a material port at the bottom of the crucible, which is blocked with a plug for smelting. At the same time, there is a stirring device at the top. After the smelting is completed, the plug is pulled out and the material is discharged and water quenched to obtain glass slag.

[0024] S50: After crushing the product of step S40, a glass powder with a D50 particle size of 3.0 to 5.0 μm is obtained.

[0025] In the preparation method, the matrix glass powder raw materials used include CaO, Al2O3, SiO2, B2O3 and Na2CO3, and the second component includes one or more of TiO2, CeO2, ZrO2, Nb2O5 or WO3.

[0026] Furthermore, the mass percentage of the matrix glass is 95-99%; the mass percentage of the second component is 1-5%; preferably, the mass percentages of CaO, Al2O3, SiO2, B2O3 and Na2CO3 are 20-40%, 10-20%, 35-50%, 10-20% and 1-3% respectively.

[0027] In the present invention, by adding the second component and melting in steps, a gain glass network structure is obtained, the softening temperature is increased, and it becomes the second phase in the glass, inhibiting the softening of the glass and the degree of vitrification of the matrix ceramic; a part of the second component exists independently in the form of oxide, which further increases the softening temperature and can also inhibit the vitrification of the ceramic matrix, thereby increasing its cycle life.

[0028] In addition, the preparation method of the present application can achieve large-scale mass production with a stable process and has reduced production costs.

[0029] The obtained glass powder has a high softening temperature, improves the bonding force between the nickel-based alloy layer and the porous ceramic matrix, reduces the vitrification penetration into the ceramic matrix, and improves the cycle life and stability. DETAILED DESCRIPTION

[0030] The embodiments of the present invention will be described in detail below in conjunction with specific examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. In the examples, if specific conditions are not specified, the conditions are carried out according to normal conditions or manufacturer recommendations. If the manufacturer is not specified for reagents or instruments used, they are all conventional products that can be obtained by commercial purchase. In addition, the component ratio or content not specified in the present invention can be any ratio or content.

[0031] Example 1

[0032] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0033] S10: mixing the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieving, remixing and preheating at 260°C for 40min;

[0034] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1000° C. at a heating rate of 3° C. / min and kept at this temperature for 30 minutes, and then the product in step S10 is added to the crucible and kept at 1000° C. for 20 minutes;

[0035] S21: heating the product of step S20 to 1550° C. at a heating rate of 5° C. / min in the glass frit furnace for pre-high temperature smelting for 60 min, and cooling the product after pre-high temperature smelting to 1350° C. at a rate of 3° C. / min;

[0036] S30: adding the second components TiO2 and CeO2 into the glass frit furnace according to the ratio in Table 1, mixing with the product in step S21, and then high-temperature melting at 1350° C. for 60 minutes under stirring;

[0037] S40: discharging the product in step S30 and quenching it with water, then heating the glass frit to 1000° C., and then adding the S10 product prepared in advance, so that the next batch of materials can be continuously produced;

[0038] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of glass powder with a particle size of 3.25 μm are 750°C and 850°C respectively.

[0039] Example 2

[0040] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0041] S10: Mix the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieve and perform secondary mixing, and preheat at 220°C for 60 minutes;

[0042] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1100° C. at a heating rate of 5° C. / min and kept at this temperature for 20 min, and then the product in step S10 is added to the crucible and kept at 1100° C. for 20 min;

[0043] S21: heating the product of step S20 to 1580° C. in the glass frit furnace at a heating rate of 5° C. / min for pre-high temperature melting for 120 min, and cooling the product after pre-high temperature melting to 1380° C. at a rate of 5° C. / min;

[0044] S30: adding the second component ZrO2 and Nb2O5 into the glass frit furnace according to the ratio in Table 1, mixing with the product in step S21, and then high-temperature melting at 1380° C. for 50 minutes under stirring;

[0045] S40: discharging the product in step S30 and quenching it with water, then heating the glass frit to 1100° C., and then adding the S10 product prepared in advance, so that the next batch of materials can be continuously produced;

[0046] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of the glass powder with a particle size of 4.33 μm are 790°C and 910°C respectively.

[0047] Example 3

[0048] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0049] S10: Mix the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieve and perform secondary mixing, and preheat at 280°C for 30 minutes;

[0050] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1150° C. at a heating rate of 5° C. / min and kept at this temperature for 20 minutes, and then the product in step S10 is added to the crucible and kept at 1150° C. for 20 minutes;

[0051] S21: heating the product of step S20 to 1520° C. in the glass frit furnace at a heating rate of 5° C. / min for pre-high temperature melting for 90 min, and cooling the product after pre-high temperature melting to 1330° C. at a rate of 5° C. / min;

[0052] S30: adding the second components TiO2 and WO3 into the glass frit furnace according to the ratio in Table 1, mixing with the product in step S21, and then high-temperature melting at 1330° C. for 60 minutes under stirring;

[0053] S40: discharging the product in step S30 and quenching it with water, then heating the glass frit furnace to 1150° C., and then adding the S10 product prepared in advance, so that the next batch of materials can be continuously produced;

[0054] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of glass powder with a particle size of 4.35 μm are 780°C and 860°C respectively.

[0055] Example 4

[0056] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0057] S10: mixing the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieving, remixing and preheating at 250°C for 30 minutes;

[0058] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1200° C. at a heating rate of 5° C. / min and kept at this temperature for 10 min, and then the product in step S10 is added to the crucible and kept at 1200° C. for 20 min;

[0059] S21: heating the product of step S20 to 1600° C. in the glass frit furnace at a heating rate of 5° C. / min for pre-high temperature smelting for 120 min, and cooling the product after pre-high temperature smelting to 1400° C. at a rate of 5° C. / min;

[0060] S30: adding the second component TiO2 and ZrO2 into the glass frit furnace according to the ratio in Table 1, mixing with the product in step S21, and then high-temperature melting at 1400° C. for 50 minutes under stirring;

[0061] S40: discharging the product in step S30 and quenching it with water, then heating the glass frit to 1200° C., and then adding the S10 product prepared in advance, so that the next batch of materials can be continuously produced;

[0062] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of the glass powder with a particle size of 3.88 μm are 810°C and 960°C respectively.

[0063] Example 5

[0064] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0065] S10: mixing the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieving, remixing and preheating at 200°C for 30min;

[0066] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1050° C. at a heating rate of 5° C. / min and kept at this temperature for 30 minutes, and then the product in step S10 is added to the crucible and kept at 1050° C. for 20 minutes;

[0067] S21: heating the product of step S20 to 1550° C. at a heating rate of 5° C. / min in the glass frit furnace for pre-high temperature smelting for 30 min, and cooling the product after pre-high temperature smelting to 1300° C. at a rate of 5° C. / min;

[0068] S30: adding the second component ZrO2 and WO3 into the glass frit furnace according to the ratio in Table 1, mixing with the product in step S21, and then high-temperature melting at 1300° C. for 60 minutes under stirring;

[0069] S40: discharging the product in step S30 and quenching it with water, then heating the glass frit furnace to 1050° C., and then adding the S10 product prepared in advance, so that the next batch of materials can be continuously produced;

[0070] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass powder with a particle size of 4.23 μm has a glass transition temperature Tg and a softening temperature Tf of 730° C. and 830° C. respectively.

[0071] Comparative Example 1

[0072] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0073] S10: Mix the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieve and perform secondary mixing, and preheat at 260°C for 30 minutes;

[0074] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1000° C. at a heating rate of 5° C. / min and kept at this temperature for 30 minutes, and then the product in step S10 is added to the crucible and kept at 1000° C. for 20 minutes;

[0075] S21: heating the product in step S20 to 1550° C. at a heating rate of 5° C. / min in the glass frit furnace for high temperature smelting for 60 min, then cooling the temperature to 1350° C. at a rate of 5° C. / min and keeping the temperature for 30 min;

[0076] S40: discharging and water quenching the product in step S21;

[0077] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of glass powder with a particle size of 3.25 μm are 590°C and 680°C respectively.

[0078] Comparative Example 2

[0079] A method for preparing high-temperature glass powder for electronic cigarette nickel paste:

[0080] S10: Mix the matrix glass powder raw materials CaO, Al2O3, SiO2, B2O3 and Na2CO3 according to the ratio in Table 1, sieve and perform secondary mixing, and preheat at 260°C for 30 minutes;

[0081] S20: firstly, the glass frit furnace is loaded with an empty crucible and heated to 1000° C. at a heating rate of 5° C. / min and kept at this temperature for 30 minutes, and then the product in step S10 is added to the crucible and kept at 1000° C. for 20 minutes;

[0082] S21: heating the second component TiO2 and CeO2 according to the ratio in Table 1 and the product in step S20 in the glass frit furnace at a heating rate of 5°C / min to 1550°C for high temperature smelting for 60min, cooling the temperature to 1350°C at a rate of 5°C / min, and keeping the temperature for 30min;

[0083] S40: discharging and water quenching the product in step S21;

[0084] S50: After the product of step S40 is crushed, it is passed through a 50-mesh sieve and then subjected to air flow crushing to obtain D 50 The glass transition temperature Tg and softening temperature Tf of glass powder with a particle size of 3.25 μm are 630°C and 780°C respectively.

[0085] Table 1 Parameters and performance comparison of Examples 1-5 and Comparative Examples 1-2

[0086]

[0087] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; although the present invention is described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the above embodiments, or replace some or all of the technical features therein by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention. In addition, those skilled in the art can understand that although some embodiments herein include certain features included in other embodiments instead of other features, the combination of features of different embodiments means being within the scope of the present invention and forming different embodiments. For example, in the above claims, any one of the embodiments claimed for protection can be used in any combination. The information disclosed in this background technology section is only intended to deepen the understanding of the overall background technology of the present invention, and should not be regarded as admitting or suggesting in any form that the information constitutes prior art known to those skilled in the art.

Claims

1. A method for preparing high-temperature glass powder for electronic cigarette nickel paste, characterized in that: The steps include: S10: mixing the matrix glass powder raw materials uniformly and then preheating them; S20: placing the product of step S10 in a glass frit furnace and keeping it at 1000-1200° C. for 10-30 min; S21: heating the product of step S20 to 1500-1650° C. in the glass frit furnace at a heating rate of 5-10° C. / min for pre-high temperature smelting for 30-120 min, and cooling the product after the pre-high temperature smelting to 1300-1400° C. at a rate of 3-5° C. / min; S30: adding the second component into the glass frit furnace, mixing with the product in step S20, and then performing high temperature melting at a temperature of 1300-1400° C. for 30-60 min; S40: discharging and water quenching the product in step S30, and then cooling the glass frit furnace to 1000-1200° C.; S50: After the product of step S40 is crushed, D 50 Glass powder with a particle size of 3.0~5.0μm; The matrix glass powder raw materials include CaO, Al2O 3、 SiO 2、 B2O3 and Na2CO3; Wherein, the CaO, Al2O 3、 SiO 2、 The mass percentages of B2O3 and Na2CO3 are 20~40%, 10~20%, 35~50%, 10~20% and 1~3% respectively; The second component includes one or more of TiO2, CeO2, ZrO2, Nb2O5 or WO3; The mass percentage of the matrix glass powder is 95-99%; the mass percentage of the second component is 1-5%.

2. The method for preparing high-temperature glass powder for electronic cigarette nickel paste according to claim 1, characterized in that: In step S10, the mixing includes mixing the matrix glass powder raw materials, and performing secondary mixing after sieving.

3. The method for preparing high temperature glass powder for electronic cigarette nickel paste according to claim 1, characterized in that: The temperature of the preheating treatment is 200-300° C., and the time of the preheating treatment is 30-60 minutes.

4. The method for preparing high temperature glass powder for electronic cigarette nickel paste according to claim 1, characterized in that: In step S20, before adding the product of step S10, the glass frit furnace is loaded with an empty crucible and heated to 1000-1200° C. at a heating rate of 3-5° C. / min and kept warm for 10-30 min, and then the product of step S10 is added to the crucible.

5. The method for preparing high temperature glass powder for electronic cigarette nickel paste according to claim 1, characterized in that: In step S30, stirring is performed during the high-temperature smelting process.

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