CN113860749A - Glass powder and preparation method thereof - Google Patents
Glass powder and preparation method thereof Download PDFInfo
- Publication number
- CN113860749A CN113860749A CN202111120202.6A CN202111120202A CN113860749A CN 113860749 A CN113860749 A CN 113860749A CN 202111120202 A CN202111120202 A CN 202111120202A CN 113860749 A CN113860749 A CN 113860749A
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- Prior art keywords
- glass
- glass powder
- glass frit
- slag
- powder
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
Abstract
The application provides a glass powder and a preparation method thereof, wherein the glass powder comprises the following components based on the total weight of the glass powder: SiO 22 65‑75％，B2O3 10‑14％，Na2O 5‑10％，Al2O3 1‑8％，Ni2O3 1‑5％，Fe2O31 to 4 percent. According to the glass powder and the preparation method thereof, the glass powder which is free of pollution to the environment, adjustable in thermal expansion coefficient and good in particle size distribution, sintering performance and water-resistant chemical stability is obtained by adopting the using amount of the glass powder raw material and the preparation method. The application also provides heating resistance paste comprising the glass powder, and an electronic device comprising the glass powder.
Description
Technical Field
The application relates to the technical field of glass, in particular to glass powder and a preparation method thereof.
Background
The electronic paste contains inorganic non-metal, metal and organic materials, is a basic material for manufacturing thick film elements, and can be further divided into conductor paste, resistance paste, high-temperature, medium-temperature and low-temperature sintering paste and the like according to different purposes, sintering temperatures and the like. With the rapid development of the electronic information industry in recent years, the demand of electronic paste is increasingly vigorous. However, the research on domestic electronic paste is not much, especially the research on electric heating resistance paste is very little, and in addition, the research and development of the key material glass powder are carried out, related research results and technologies are mastered in foreign enterprises, such as Dupont, 3M, Japan triple bond and the like, domestic heating electronic paste with excellent performance is mostly imported, and the used glass powder is hardly sold alone, so that the rise of domestic industrial technology is severely restricted, and the dependence on foreign products is eliminated.
The electronic cigarette comprises basic components of an atomizer, a control circuit, a power supply circuit and a battery, wherein the atomizer comprises an oil storage bin, an airflow channel and an atomization core, tobacco tar is filled in the oil storage bin, the atomization core comprises an oil guide body and a heating wire, and the heating wire is made by high-temperature sintering of heating resistor slurry. The existing heating resistance paste for the atomization core is mainly stainless steel and nickel paste, and has obvious price advantage compared with silver paste. The performance of the heating resistance slurry requires that the slurry has stronger binding force with the ceramic porous atomizing core and provides higher resistance value after being sintered at the temperature of 900-1200 ℃. The stainless steel powder and the nickel powder alone are difficult to sinter together in a high temperature state, the resistance value is low even if they are sintered together, and their binding force with the ceramic atomizing core is poor, however, these problems can be solved by the glass powder. The lead-free glass not only meets the environmental protection requirement of the electronic cigarette, but also has high resistivity, the metal powder can be bonded together after sintering, and the softened glass can be deposited below and also can be tightly combined with the ceramic atomizing core. Therefore, the development of the related glass powder is very important.
Disclosure of Invention
The application aims to provide glass powder and a preparation method thereof, so as to obtain the glass powder which has no pollution to the environment, adjustable and controllable thermal expansion coefficient, good particle size distribution, good sintering property and good water-resistant chemical stability. The specific technical scheme is as follows:
a first aspect of the present application provides a glass frit, wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
A second aspect of the present application provides a method for preparing a glass frit according to the first aspect of the present application, which comprises the steps of:
(1) weighing raw materials of glass powder, and mixing to obtain a mixture;
(2) melting the mixture to obtain a melt, and performing water quenching to obtain glass slag;
(3) annealing the glass slag to obtain annealed glass slag;
(4) placing the annealed glass slag in a planetary ball mill for ball milling, filtering and spray drying to obtain glass powder;
wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
A third aspect of the present application provides a heat-generating resistor paste including the glass frit provided according to the first aspect of the present application.
A fourth aspect of the present application provides an electronic device comprising the glass frit provided according to the first aspect of the present application.
According to the glass powder and the preparation method thereof, the glass powder which is free of pollution to the environment, adjustable in thermal expansion coefficient and good in particle size distribution, sintering performance and water-resistant chemical stability is obtained by adopting the consumption of the raw materials of the glass powder and the preparation method; when the glass powder is used for the electronic cigarette atomizing core, the thermal expansion coefficient of the glass powder is matched with that of the ceramic atomizing core, and the glass powder is simultaneously favorable for combining with stainless steel powder and nickel powder.
Of course, not all advantages described above need to be achieved at the same time in the practice of any one product or method of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the description herein are intended to be within the scope of the present disclosure.
A first aspect of the present application provides a glass frit, wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
The glass powder of the application is prepared by reasonably adjusting SiO2、B2O3、Na2O、Al2O3、Ni2O3、Fe2O3The usage amount of the silicon-oxygen tetrahedron, the boron-oxygen triangle and the boron-oxygen tetrahedron are used as basic structural units, so that the mutual connection of glass networks is tighter, the structure is more compact and stable, the thermal expansion coefficient of a glass system is reduced, and the acid-base resistance is improved; wherein, Na2O can form eutectic with other oxides in addition to breaking silicon-oxygen bonds and easily entering into the gaps of silicon-oxygen tetrahedron, boron-oxygen trigone and boron-oxygen tetrahedron as basic structural units, thereby reducingThe softening temperature and the melting temperature of a glass system are low, so that the clarification of glass is facilitated; al (Al)2O3The content is between 1 and 8 percent, on one hand, the glass powder has the function of improving the chemical stability of the glass powder, and the glass body can be stabilized within the range of sealing temperature to avoid the occurrence of crystallization; proper amount of Ni2O3And Fe2O3The glass powder can be reinforced to link broken chains in the network, so that the acid resistance of the glass powder is enhanced, and when the glass powder is used for the electronic cigarette atomization core, the glass powder is also favorably combined with stainless steel powder and nickel powder.
The glass powder provided by the application has good performance, does not contain lead and has no pollution to the environment, and has good particle size distribution, sintering property and water-resistant chemical stability by adjusting the component dosage of the glass powder and regulating and controlling the thermal expansion coefficient of the glass powder; when the glass powder is used for the electronic cigarette atomizing core, the thermal expansion coefficient of the glass powder is 20 multiplied by 10 with the ceramic atomizing core-7-35×10-7/° c) while facilitating the bonding with the stainless steel powder and the nickel powder.
In certain embodiments of the first aspect of the present application, the glass frit has a particle size D50 of 1-2 μm and a coefficient of thermal expansion of 35X 10-7-45×10-7The softening temperature is 750-820 ℃, the glass transition temperature is 650-690 ℃, and the water-resistant chemical stability is not lower than two levels.
A second aspect of the present application provides a method for preparing a glass frit according to the first aspect of the present application, which comprises the steps of:
(1) weighing raw materials of glass powder, and mixing to obtain a mixture;
(2) melting the mixture to obtain a melt, and performing water quenching to obtain glass slag;
(3) annealing the glass slag to obtain annealed glass slag;
(4) placing the annealed glass slag in a planetary ball mill for ball milling, filtering and spray drying to obtain glass powder;
wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
In the application, the raw material component content of the glass powder is the same as the component content of the glass powder.
In this application, step (1) the mixing is the homogeneous mixing, and this application does not do the restriction to the mode of mixing, as long as can realize the purpose of this application can, exemplarily, can use the zirconium ball-milling through putting the raw materials of weighing into zirconia bottle, ball-milling for 1-2h at the planet ball mill, intensive mixing obtains the mixture.
In some embodiments of the second aspect of the present application, wherein the melting of step (2) comprises: heating the mixture to 1400-1600 ℃ and preserving heat for 2-5h to fully melt the mixture; the melting method is not limited as long as the object of the present invention can be achieved, and the melting operation may be performed by using a silicon carbide rod resistance furnace, for example.
In the application, the water quenching in the step (2) is to pour the melt into water for water quenching so as to rapidly cool the melt, and simultaneously, the melt can be crushed through ultra-cooling so as to obtain glass slag; the water quenching can also properly crush the large glass.
In some embodiments of the second aspect of the present application, wherein the annealing of step (3) comprises: heating the glass slag to 660-700 ℃, preserving the heat for 1-2h, and cooling to room temperature; the glass slag is annealed, so that the hardness and the residual stress can be reduced, the size is stabilized, the deformation and crack tendency is reduced, and the glass structure is more stable.
The manner of the ball milling in the step (4) is not particularly limited as long as the purpose of the present invention can be achieved, and for example, the ball milling may include: placing the annealed glass slag in a planetary ball mill, taking water as a ball milling medium, and carrying out ball milling at a rotating speed of 400-500 rap/min; the ball milling time is not limited in the present application as long as the purpose of the present application can be achieved, and the ball milling time may be, for example, 15 to 20 hours. The filtering can be performed by selecting screens with different mesh numbers according to requirements, and for example, the ball milling can be performed by passing through a 200-400-mesh screen to remove porcelain balls and larger glass slag to obtain glass slurry, and then the glass slurry is subjected to spray drying, wherein glass powder with different particle sizes can be prepared according to requirements, for example, the particle size D50 can be 1-2 μm.
In certain embodiments of the second aspect of the present application, the glass frit has a particle size D50 of 1-2 μm and a coefficient of thermal expansion of 35X 10-7-45×10-7The softening temperature is 750-820 ℃, the glass transition temperature is 650-690 ℃, and the water-resistant chemical stability is not lower than two levels.
A third aspect of the present application provides a heat-generating resistor paste including the glass frit provided according to the first aspect of the present application.
The heating resistor paste of the present application is not particularly limited, and can be used for thick film resistors, hybrid integrated circuits, resistor networks, electronic cigarettes, rapid electric heating kettles, special-purpose resistors, electrodes, and the like; this application includes when the resistance to heat thick liquids of glass powder are used for electron smog core, the resistance to heat thick liquids still include stainless steel powder, nickel powder, the glass powder is favorable to the combination of stainless steel powder, nickel powder, the coefficient of thermal expansion and the pottery atomizing core of glass powder match.
A fourth aspect of the present application provides an electronic device comprising the glass frit provided according to the first aspect of the present application.
The embodiments of the present application will be described in more detail below with reference to examples and comparative examples.
Example 1
(1) Weighing raw material SiO2 65g、B2O3 12g、Na2O 8g、Al2O3 8g、Ni2O3 4g、Fe2O33g, fully mixing to obtain a mixture;
(2) heating the mixture to 1400 ℃, preserving heat for 2h to fully melt the mixture to obtain a melt, and pouring the melt into water for water quenching to obtain glass slag;
(3) heating the glass slag to 660 ℃, preserving heat for 1h, and cooling to room temperature to obtain annealed glass slag;
(4) and (3) placing the annealed glass slag in a planetary ball mill, taking water as a ball milling medium, performing ball milling for 15h at the rotating speed of 400rap/min, sieving by a 300-mesh sieve, and pouring into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Examples 2 to 3
The glass frit was prepared in the same manner as in example 1, and the relevant preparation parameters were varied as shown in Table 1.
Comparative examples 1 to 2
The glass frit was prepared in the same manner as in example 1, and the relevant preparation parameters were varied as shown in Table 1.
The glass frits of examples 1-3 and comparative examples 1-2 were tested using the following performance test methods, and the results are shown in table 1.
And (3) performance testing:
particle size distribution: testing by a laser particle size distribution instrument;
testing the thermal expansion coefficient: adopting a method for testing the linear expansion coefficient of SJ 689-83 electric vacuum glass;
glass transition temperature, softening temperature: testing by differential thermal analysis DTA;
and (3) water-resistant chemical stability: a test method of the water-chemical resistance stability of the electric vacuum glass SJ 696-83 is adopted.
TABLE 1
The inventors of the present application found in their studies that comparative examples 1 to 2 of the present application did not give a glass frit having a uniform distribution, and the content ranges of the components of the glass frit of the present application were the limit ranges capable of forming a uniform glass.
Through tests, the coefficient of thermal expansion of the glass powder is 35 multiplied by 10-7-45×10-7The glass transition temperature is between 650 ℃ and 690 ℃, and the softening temperature is between 750 ℃ and 820 DEG CAnd the water-resistant chemical stability is not lower than the second level.
In summary, the glass frit and the preparation method thereof provided by the present application, wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O31 to 4 percent. According to the glass powder and the preparation method thereof, the glass powder which is free of pollution to the environment, adjustable in thermal expansion coefficient and good in particle size distribution, sintering performance and water-resistant chemical stability is obtained by adopting the using amount of the glass powder raw material and the preparation method.
The above description is only for the preferred embodiment of the present application and is not intended to limit the scope of the present application. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application are included in the protection scope of the present application.
Claims (9)
1. A glass frit, wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O310-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
2. The glass frit according to claim 1, wherein the glass frit has a particle size D50 of 1-2 μm and a thermal expansion coefficient of 35 x 10-7-45×10-7The softening temperature is 750-820 ℃, and the glass transition temperature is 650-690 ℃.
3. A method for producing the glass frit according to any one of claims 1 to 2, comprising the steps of:
(1) weighing raw materials of glass powder, and mixing to obtain a mixture;
(2) melting the mixture to obtain a melt, and performing water quenching to obtain glass slag;
(3) annealing the glass slag to obtain annealed glass slag;
(4) placing the annealed glass slag in a planetary ball mill for ball milling, filtering and spray drying to obtain glass powder;
wherein the glass frit comprises, based on the total weight of the glass frit: SiO 22 65-75％，B2O3 10-14％，Na2O 5-10％，Al2O3 1-8％，Ni2O3 1-5％，Fe2O3 1-4％。
4. The production method according to claim 3, wherein the melting of step (2) includes: heating the mixture to 1400-1600 ℃ and preserving the heat for 2-5 h.
5. The production method according to claim 3, wherein the annealing of step (3) includes: heating the glass slag to 660-700 ℃, preserving the heat for 1-2h, and cooling to room temperature.
6. The preparation method of claim 3, wherein the ball milling of step (4) comprises: and placing the annealed glass slag in a planetary ball mill, and ball-milling at the rotating speed of 400-500rap/min by using water as a ball-milling medium.
7. The production method according to any one of claims 3 to 6, wherein the glass frit has a particle size D50 of 1 to 2 μm and a thermal expansion coefficient of 35 x 10-7-45×10-7The softening temperature is 750-820 ℃, and the glass transition temperature is 650-690 ℃.
8. A heat-generating resistor paste comprising the glass frit according to any one of claims 1 to 2.
9. An electronic device comprising the glass frit according to any one of claims 1 to 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111120202.6A CN113860749A (en) | 2021-09-24 | 2021-09-24 | Glass powder and preparation method thereof |
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| CN202111120202.6A CN113860749A (en) | 2021-09-24 | 2021-09-24 | Glass powder and preparation method thereof |
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| CN113860749A true CN113860749A (en) | 2021-12-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636590A (en) * | 2022-10-08 | 2023-01-24 | 中建材玻璃新材料研究院集团有限公司 | Antibacterial glass powder, preparation method thereof and plastic antibacterial material |
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