A glass powder and a method of making the same

Abstract

The application provides a glass powder and a preparation method thereof, wherein the glass powder comprises SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5% and Fe2O3 1-4% based on the total weight of the glass powder. The glass powder and the preparation method thereof have the advantages that the glass powder obtained by the preparation method has no pollution to the environment, the thermal expansion coefficient can be controlled, and the glass powder has good particle size distribution, sintering property and water chemical stability. The application further provides a heating resistance paste comprising the glass powder and an electronic device comprising the glass powder.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of glass, in particular to a glass powder and a preparation method thereof. BACKGROUND

[0002] Electronic paste contains inorganic non-metallic, metal, organic material, is the basic material for manufacturing thick film elements, according to the use, sintering temperature and so on, can be subdivided into conductor paste, resistance paste and high temperature, medium temperature, low temperature sintering paste and so on. In recent years, with the rapid development of electronic information industry, the demand for electronic paste is increasing. However, the research on electronic paste in China is not much, especially the research on electric heating resistance paste is very little, not to mention the research and development of key material glass powder, the relevant research results and technology are mastered by foreign enterprises such as Dupont, 3M, Japan Sanjian and so on. The excellent performance of the heating electronic paste used in China is mostly imported, and the glass powder used therein is almost not sold separately, which seriously restricts the rise of domestic industrial technology and the dependence on foreign products, which is urgent.

[0003] The basic components of electronic cigarette are atomizer, control circuit, power supply circuit and battery. The atomizer includes oil storage, air flow channel and atomizing core. The oil storage contains tobacco tar. The atomizing core includes oil guide body and heating wire, and the heating wire is made of high-temperature sintering of heating resistance paste. The heating resistance paste used in the atomizing core is mainly stainless steel and nickel paste, which has obvious price advantage compared with silver paste. The performance of the heating resistance paste requires that after sintering at 900-1200℃, it has strong bonding force with the ceramic porous atomizing core and provides high resistance value. The stainless steel powder and nickel powder alone are difficult to sinter together at high temperature, and even if they are sintered together, the resistance value is very low, and they have poor bonding force with the ceramic atomizing core. However, these problems can be solved by glass powder. Lead-free glass not only meets the environmental protection requirements of electronic cigarette, but also has high resistivity, can bond metal powder together after sintering, and the softened glass can be deposited below to tightly combine with the ceramic atomizing core. Therefore, the research and development of related glass powder is very important. SUMMARY

[0004] The purpose of the present application is to provide a glass powder and a preparation method thereof, so as to obtain a glass powder which is pollution-free to the environment, has adjustable thermal expansion coefficient, and has good particle size distribution, sintering property and water chemical stability. The specific technical scheme is as follows:

[0005] The first aspect of the present application provides a glass powder, wherein, based on the total weight of the glass powder, the glass powder comprises: SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, Fe2O3 1-4%.

[0006] The second aspect of the present application provides a preparation method of the glass powder provided by the first aspect of the present application, comprising the following steps:

[0007] (1) weighing raw materials of the glass powder, mixing to obtain a mixture;

[0008] (2) melting the mixture to obtain a melt, and water quenching to obtain a glass slag;

[0009] (3) annealing the glass slag to obtain an annealed glass slag;

[0010] (4) ball milling the annealed glass slag in a planetary ball mill, filtering, and spray drying to obtain the glass powder;

[0011] wherein, based on the total weight of the glass powder, the glass powder comprises: SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, and Fe2O3 1-4%.

[0012] The third aspect of the present application provides a heating resistance paste comprising the glass powder provided by the first aspect of the present application.

[0013] The fourth aspect of the present application provides an electronic device comprising the glass powder provided by the first aspect of the present application.

[0014] The glass powder and the preparation method thereof provided by the present application adopt the use amount of the raw materials of the glass powder, and obtain the glass powder with no environmental pollution, adjustable thermal expansion coefficient, and good particle size distribution, sintering property, and water chemical stability through the preparation method of the present application. When the glass powder provided by the present application is used in an electronic cigarette atomizing core, the thermal expansion coefficient thereof matches that of a ceramic atomizing core, and meanwhile, it is beneficial to the combination of the glass powder with stainless steel powder and nickel powder.

[0015] Of course, implementing any product or method of the present application does not necessarily require achieving all the advantages described above at the same time. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art based on the present application belong to the scope of protection of the present application.

[0017] The first aspect of the present application provides a glass powder, wherein, based on the total weight of the glass powder, the glass powder comprises: SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, and Fe2O3 1-4%.

[0018] The glass powder of the present application, by reasonably adjusting the amount of SiO2, B2O3, Na2O, Al2O3, Ni2O3 and Fe2O3, makes the silicon-oxygen tetrahedron, boron-oxygen triangle and boron-oxygen tetrahedron as the basic structural unit of the glass network more closely connected, the structure more compact and stable, thereby reducing the thermal expansion coefficient of the glass system and improving the acid and alkali resistance; wherein, Na2O not only makes the silicon-oxygen bond break and easily enter the gap of the silicon-oxygen tetrahedron, boron-oxygen triangle and boron-oxygen tetrahedron as the basic structural unit, but also forms a eutectic with other oxides, thereby reducing the softening temperature and melting temperature of the glass system, which is beneficial to the clarification of the glass; the content of Al2O3 is between 1-8%, which not only plays a role in improving the chemical stability of the glass powder, but also stabilizes the glass body within the sealing temperature range, avoiding the occurrence of crystallization; appropriate amounts of Ni2O3 and Fe2O3 not only can reinforce the glass network and link the broken chains in the network, thereby enhancing the acid resistance of the glass powder, but also are beneficial to the combination of the glass powder with stainless steel powder and nickel powder when the glass powder is used in the electronic cigarette atomizing core.

[0019] The glass powder provided by the present application has good performance, is free of lead and does not pollute the environment, and has a good particle size distribution, sintering property and water chemical stability by adjusting the component amount of the glass powder of the present application to control the thermal expansion coefficient of the glass powder; when the glass powder of the present application is used in the electronic cigarette atomizing core, the thermal expansion coefficient thereof matches that of the ceramic atomizing core (the thermal expansion coefficient is 20x10 -7 -35x10 -7 / ℃), and is beneficial to the combination of the glass powder with stainless steel powder and nickel powder.

[0020] In some embodiments of the first aspect of the present application, the particle size D50 of the glass powder is 1-2 μm, the thermal expansion coefficient is 35x10 -7 -45x10 -7 / ℃, the softening temperature is 750-820℃, the glass transition temperature is 650-690℃, and the water chemical stability is not less than secondary.

[0021] The second aspect of the present application provides a preparation method of the glass powder provided by the first aspect of the present application, which comprises the following steps:

[0022] (1) weighing the raw materials of the glass powder, mixing to obtain a mixture;

[0023] (2) melting the mixture to obtain a melt, and water quenching to obtain a glass slag;

[0024] (3) annealing the glass slag to obtain an annealed glass slag;

[0025] (4) placing the annealed glass slag into a planetary ball mill, filtering, spray drying to obtain a glass powder;

[0026] The glass powder comprises, based on the total weight of the glass powder, SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, and Fe2O3 1-4%.

[0027] In the present application, the content of the raw material components of the glass powder is the same as the content of the components of the glass powder.

[0028] In the present application, the mixing in step (1) is uniform mixing, and the present application does not limit the mixing method as long as the purpose of the present application can be achieved. For example, the weighed raw materials can be placed into a zirconium oxide bottle and ball milled using zirconium balls in a planetary ball mill for 1-2 h to obtain a mixture.

[0029] In some embodiments of the second aspect of the present application, the melting in step (2) comprises: heating the mixture to 1400-1600°C and maintaining for 2-5 h to fully melt the mixture; and the present application does not limit the melting method as long as the purpose of the present application can be achieved. For example, a silicon-carbon rod resistance furnace can be used for melting operation.

[0030] In the present application, the water quenching in step (2) is to pour the melt into water for water quenching to rapidly cool the melt, and at the same time, the melt can be crushed by extremely cold crushing to obtain a glass slag; the water quenching can also appropriately break the large glass pieces.

[0031] In some embodiments of the second aspect of the present application, the annealing in step (3) comprises: heating the glass slag to 660-700°C and maintaining for 1-2 h, and then cooling to room temperature; annealing the glass slag can reduce hardness and residual stress, stabilize the size, reduce the tendency of deformation and cracking, and make the glass structure more stable.

[0032] The present application does not particularly limit the ball milling method in step (4) as long as the purpose of the present application can be achieved. For example, the ball milling can comprise: placing the annealed glass slag into a planetary ball mill, using water as the ball milling medium, and ball milling at a speed of 400-500 rap / min; the present application does not limit the ball milling time as long as the purpose of the present application can be achieved. For example, the ball milling time can be 15-20 h. The filtering can be performed using different mesh screens according to the needs, for example, after ball milling, the glass slurry can be obtained by passing the glass slag through a 200-400 mesh screen to remove the porcelain balls and larger glass slag, and then spray drying, wherein the glass powder with different particle sizes can be prepared according to the needs, for example, the particle size D50 can be 1-2 μm.

[0033] In some embodiments of the second aspect of the application, the glass powder has a particle size D50 of 1-2 μm, a coefficient of thermal expansion of 35x10 -7 -45x10 -7 / ℃, a softening temperature of 750-820℃, a glass transition temperature of 650-690℃, and a water chemical stability of no less than level II.

[0034] The third aspect of the application provides a heating resistance paste, which comprises the glass powder provided in the first aspect of the application.

[0035] The heating resistance paste of the application is not particularly limited, and can be used in thick film resistors, hybrid integrated circuits, resistance networks, electronic cigarettes, fast electric heating kettles, special-purpose resistors, electrodes, etc.; when the heating resistance paste of the application comprising the glass powder is used in an electronic cigarette atomizer, the heating resistance paste further comprises stainless steel powder and nickel powder, the glass powder is beneficial to the combination of the stainless steel powder and the nickel powder, and the coefficient of thermal expansion of the glass powder matches the ceramic atomizer.

[0036] The fourth aspect of the application provides an electronic device comprising the glass powder provided in the first aspect of the application.

[0037] The following examples and comparative examples are used to more specifically illustrate the embodiments of the application.

[0038] Example 1

[0039] (1) Weigh raw materials SiO2 65g, B2O3 12g, Na2O 8g, Al2O3 8g, Ni2O3 4g, Fe2O3 3g, and mix them thoroughly to obtain a mixture;

[0040] (2) Heat the mixture to 1400℃ and keep it at this temperature for 2h to make it melt thoroughly, obtain a melt, and pour the melt into water to quench it, obtaining a glass slag;

[0041] (3) Heat the glass slag to 660℃ and keep it at this temperature for 1h, and then cool it to room temperature to obtain an annealed glass slag;

[0042] (4) Put the annealed glass slag into a planetary ball mill, use water as the ball milling medium, ball mill at a speed of 400 rap / min for 15h, pass through a 300-mesh screen, and then pour it into the liquid tank of a spray granulator for spray drying to obtain a glass powder.

[0043] Examples 2-3

[0044] The preparation steps of the glass powder are the same as those in Example 1, and the changes in the relevant preparation parameters are shown in Table 1.

[0045] Comparative Examples 1-2

[0046] The preparation steps of the glass powder are the same as those of Example 1, and the changes of the related preparation parameters are shown in Table 1.

[0047] The glass powder of Examples 1-3 and Comparative Examples 1-2 is tested by the following performance test method, and the results are shown in Table 1.

[0048] Performance test:

[0049] Particle size distribution: tested by a laser particle size distribution instrument;

[0050] Thermal expansion coefficient test: SJ 689-83 test method for linear expansion coefficient of electric vacuum glass is used;

[0051] Glass transition temperature and softening temperature: tested by differential thermal analysis method DTA;

[0052] Water chemical stability: SJ 696-83 test method for water chemical stability of electric vacuum glass is used.

[0053] Table 1

[0054]

[0055]

[0056] The inventors of the present application found in the research that the glass powder of Comparative Example 1-2 of the present application cannot obtain a uniformly distributed glass powder, and the content range of each component of the glass powder of the present application is the limit range that can form a uniform glass.

[0057] Through the test, the thermal expansion coefficient of the glass powder of the present application is between 35x10 -7 -45x10 -7 / ℃, the glass transition temperature is between 650-690℃, the softening temperature is between 750-820℃, and the water chemical stability is not less than the second level.

[0058] In summary, the glass powder and the preparation method thereof provided by the present application, wherein, based on the total weight of the glass powder, the glass powder comprises: SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, Fe2O3 1-4%. The glass powder and the preparation method thereof provided by the present application, by using the amount of the glass powder raw material of the present application, through the preparation method of the present application, a glass powder with no environmental pollution, adjustable thermal expansion coefficient, and good particle size distribution, sintering property and water chemical stability is obtained.

[0059] The above merely provides the preferred embodiment of the present application, and not intended to limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A heat generating resistive paste comprising stainless steel powder and glass powder, wherein, The glass powder is composed of SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, Fe2O3 1-4% based on the total weight of the glass powder, The glass powder has a particle size D50 of 1-2 μm, a thermal expansion coefficient of 35x10 -7 -45x10 -7 -6 / ℃, a softening temperature of 750-820℃, and a glass transition temperature of 650-690℃.

2. The heat-generating resistive paste of claim 1, wherein, The preparation method of the glass powder comprises the following steps: (1) weighing the raw materials of the glass powder, mixing to obtain a mixture; (2) melting the mixture to obtain a melt, water quenching to obtain a glass slag; (3) annealing the glass slag to obtain an annealed glass slag; (4) placing the annealed glass slag in a planetary ball mill for ball milling, filtering, and spray drying to obtain the glass powder; The glass powder is composed of SiO2 65-75%, B2O3 10-14%, Na2O 5-10%, Al2O3 1-8%, Ni2O3 1-5%, Fe2O3 1-4% based on the total weight of the glass powder.

3. The heat-generating resistive paste of claim 2, wherein, The melting of step (2) comprises: heating the mixture to 1400-1600℃ and maintaining for 2-5h.

4. The heat-generating resistive paste of claim 2, wherein, The annealing of step (3) comprises: heating the glass slag to 660-700℃ and maintaining for 1-2h, and then cooling to room temperature.

5. The heat-generating resistive paste of claim 2, wherein, The ball milling of step (4) comprises: placing the annealed glass slag in a planetary ball mill, using water as the ball milling medium, and ball milling at a rotation speed of 400-500 rap / min.

6. An electronic device comprising the heat-generating resistance paste according to claim 1.

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