CN107399909B - Preparation method of glass microspheres for solid-phase converter - Google Patents
Preparation method of glass microspheres for solid-phase converter Download PDFInfo
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- CN107399909B CN107399909B CN201710796701.4A CN201710796701A CN107399909B CN 107399909 B CN107399909 B CN 107399909B CN 201710796701 A CN201710796701 A CN 201710796701A CN 107399909 B CN107399909 B CN 107399909B
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
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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
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Abstract
The invention discloses a preparation method of glass microspheres for a solid phase converter, which comprises the following specific steps: putting the raw materials into a mixer according to a certain proportion and uniformly mixing to obtain a glass mixture; melting the glass mixture at a high temperature; pouring the molten glass mixed solution into a cold water pool for water quenching; drying the water-quenched glass mixture, then feeding the dried glass mixture into a crusher for crushing, and screening by utilizing a multi-stage linear sieve to obtain glass powder; feeding the glass powder into a sintering furnace for sintering to form glass microspheres; and (3) selecting the hollow glass microspheres by utilizing buoyancy, discarding the hollow glass microspheres, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter. The preparation method can realize the control of the grain diameter of the glass microspheres by controlling the grain diameter of the glass powder and the control of the roundness of the glass microspheres by controlling the sintering temperature, so that the solid content of the glass microspheres is improved to more than 99 percent, and the softening point and the expansion coefficient of the prepared glass microspheres meet the requirements of preparing solid-phase converters.
Description
Technical Field
The invention relates to a preparation method of glass microspheres for a solid phase converter.
Background
With the development of science and technology, in the control and monitoring systems of most moving objects in the fields of military industry and aerospace, not only the information of angular displacement and angular velocity, but also the related information of angular acceleration is needed. With the rapid development of industrial automatic control technology, the application requirements of the angular acceleration sensor become more and more.
The liquid ring type angular acceleration sensor is mainly composed of a reference plate, an amplifying circuit and a liquid ring, wherein the liquid ring is a core part and consists of a liquid cavity, liquid, an electrode and a solid phase converter. The solid phase converter is a porous net structure, when the liquid ring moves, a series of changes can occur at the internal and external solid-liquid interfaces of the converter, and the formed potential difference is connected to the amplifying circuit through the electrode of the liquid ring terminal for amplifying and then outputting, so that the solid phase converter is an important factor influencing the performance of the whole angular acceleration sensor.
The softening point and the expansion coefficient of the glass microspheres for the solid phase converter in the liquid ring type angular acceleration sensor need to be strictly controlled, and the composition of the glass is designed according to the expansion coefficient and the softening point corresponding to the glass microspheres in a selected component range and the proportion of each component. In addition, the solubility of gas products generated in the melting process of glass raw materials in a glass system is different, and the clarification effect and the solubility of the glass directly influence the performance of the glass after balling, so that the density of glass microspheres is influenced, the actual heart rate of the glass microspheres is influenced, the preparation performance of a converter is directly influenced, and the glass components directly influence key parameters such as the density, the softening point, the expansion coefficient and the like of the glass microspheres after balling.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of glass microspheres for a solid phase converter, which can realize the control of the particle size of the glass microspheres by controlling the particle size of glass powder and the roundness of the glass microspheres by controlling sintering temperature, improve the solid content of the glass microspheres to 99 percent, ensure that the softening point of the prepared glass microspheres reaches 740 +/-20 ℃ and the expansion coefficient reaches (80 +/-5) multiplied by 10－7And the preparation of the solid phase converter is more suitable.
In order to solve the technical problems, the invention provides a preparation method of glass microspheres for a solid-phase converter, which comprises the following steps:
(1) preparing a glass mixture: putting 60-65% of silicon dioxide, 0.5-1.5% of boric acid, 8-12% of limestone, 18-22% of soda ash, 1-3% of alumina, 0.5-1.5% of potassium carbonate and 1-1.5% of magnesium oxide into a mixer according to the weight percentage, and uniformly mixing to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 80-90 min; the temperature rise time of 700-1100 ℃ is 110-120 min, and the temperature is kept for 100-120 min; heating for 60-70 min at 1100-1500 ℃, and keeping the temperature for 100-120 min to melt the glass mixture;
(3) after the glass mixture is melted, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a multi-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the sintering temperature is 1350-1500 ℃, and forming glass microspheres;
(6) and (3) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter.
The purpose of step (1) is to mix the various raw materials evenly. The purpose of the step (2) is to melt the glass mixture, and through gradient setting of the heating rate and heat preservation for a certain time in each heating process, the heating element of the high-temperature resistance furnace can be protected, the crucible can be protected from cracking to cause overflow of raw materials, the glass liquid can be fully homogenized, devitrification is avoided, the glass liquid with uniform components is formed, the solubility of a gas product generated in the melting process of the glass mixture can be controlled, the clarification temperature and the clarification time are controlled, and the purpose of controlling the density and the actual heart rate of the microspheres is achieved. And (3) performing water quenching crushing on the glass, wherein the high-temperature glass liquid can be broken into small fragments with the diameter of 5-10 mm after meeting water. And (4) putting the small fragments into a crusher for crushing to form glass powder with the particle size of 10-30 microns, and screening to classify the glass powder so as to control the particle size of the glass powder. And (5) spheroidizing the glass powder with irregular shape by high-temperature melting to form the glass microspheres. The step (6) is to sort out the hollow glass microspheres mixed in the solid glass microspheres, and because a certain proportion of hollow glass microspheres can be generated in the sintering process of the glass microspheres, the hollow glass microspheres can collapse to different degrees when meeting high temperature in the later process of preparing the solid phase converter, and certain influence is generated on performance parameters of the solid phase converter, the hollow glass microspheres need to be called out and discarded, water is used as a medium, and the hollow glass microspheres can be sorted out more conveniently and quickly by a floating method.
Preferably, during the mixing process of the glass batch in the step (1), 1% of water can be added to prevent part of raw materials from being lost due to dust during the mixing process, so that the glass components are not stable.
In a word, the invention can realize the control of the grain diameter of the glass microspheres by controlling the grain diameter of the glass powder and the control of the roundness of the glass microspheres by controlling the sintering temperature, the softening point of the glass microspheres prepared by the method of the invention reaches 740 +/-20 ℃, and the expansion coefficient reaches (80 +/-5) multiplied by 10－7And the preparation of the solid phase converter is more suitable.
Detailed Description
The invention will be further understood from the following examples, which are given by way of illustration and are not intended to be limiting.
Example 1
(1) Preparing a glass mixture: putting 65% of silicon dioxide, 1% of boric acid, 11% of limestone, 18% of soda ash, 3% of alumina, 0.5% of potassium carbonate and 1.5% of magnesium oxide into a mixer according to the weight percentage, and uniformly mixing to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 90 min; the temperature rise time of 700-1100 ℃ is 120min, and the temperature is kept for 120 min; heating for 70 min at 1100-1500 ℃, and keeping the temperature for 120min to melt the glass mixture;
(3) after the melting of the glass mixture is finished, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a three-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the temperature of the sintering furnace is 1350 ℃ to form glass microspheres;
(6) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter, wherein the spheroidization rate of the prepared glass microspheres reaches 95%.
Example 2
(1) Preparing a glass mixture: putting 60% of silicon dioxide, 1.5% of boric acid, 12% of limestone, 22% of soda ash, 2% of alumina, 1.5% of potassium carbonate and 1% of magnesium oxide into a mixer according to the weight percentage, and uniformly mixing to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 80 min; the temperature rise time of 700-1100 ℃ is 110 min, and the temperature is kept for 120 min; heating for 60 min at 1100-1500 ℃, and keeping the temperature for 120min to melt the glass mixture;
(3) after the melting of the glass mixture is finished, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a three-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the temperature of the sintering furnace is 1400 ℃, and forming glass microspheres;
(6) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter, wherein the spheroidization rate of the prepared glass microspheres reaches 98%.
Example 3
(1) Preparing a glass mixture: putting 65% of silicon dioxide, 0.8% of boric acid, 8% of limestone, 21% of soda ash, 3% of alumina, 1.1% of potassium carbonate and 1.1% of magnesium oxide into a mixer according to the weight percentage, and uniformly mixing to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 90 min; the temperature rise time of 700-1100 ℃ is 120min, and the temperature is kept for 100 min; heating for 70 min at 1100-1500 ℃, and keeping the temperature for 100min to melt the glass mixture;
(3) after the melting of the glass mixture is finished, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a three-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the temperature of the sintering furnace is 1450 ℃, and forming glass microspheres;
(6) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter, wherein the spheroidization rate of the prepared glass microspheres reaches 99%.
Example 4
(1) Preparing a glass mixture: putting 63% of silicon dioxide, 0.5% of boric acid, 12% of limestone, 20% of soda ash, 1% of alumina, 1% of potassium carbonate, 1.5% of magnesium oxide and 1% of water into a mixer according to the weight percentage, and uniformly mixing to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 90 min; the temperature rise time of 700-1100 ℃ is 110 min, and the temperature is kept for 100 min; heating for 70 min at 1100-1500 ℃, and keeping the temperature for 120min to melt the glass mixture;
(3) after the melting of the glass mixture is finished, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a three-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the temperature of the sintering furnace is 1500 ℃, and forming glass microspheres;
(6) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter, wherein the spheroidization rate of the prepared glass microspheres reaches 99%.
What has been described above is merely a preferred embodiment of the present invention. It should be noted that, for those skilled in the art, it is possible to make some adjustments to the raw material ratio without departing from the principle of the present invention, and these should be considered as falling within the protection scope of the present invention.
Claims (2)
1. The preparation method of the glass microspheres for the solid phase converter is characterized by comprising the following steps of:
(1) uniformly mixing 60-65% of silicon dioxide, 0.5-1.5% of boric acid, 8-12% of limestone, 18-22% of soda ash, 1-3% of alumina, 0.5-1.5% of potassium carbonate and 1-1.5% of magnesium oxide according to weight percentage to obtain a glass mixture;
(2) putting the glass mixture into a crucible, putting the crucible into a high-temperature resistance furnace, and setting a temperature rise curve of the high-temperature resistance furnace: the temperature rise time from room temperature to 700 ℃ is 80-90 min; the temperature rise time of 700-1100 ℃ is 110-120 min, and the temperature is kept for 100-120 min; heating for 60-70 min at 1100-1500 ℃, and keeping the temperature for 100-120 min to melt the glass mixture;
(3) after the glass mixture is melted, taking the crucible out of the high-temperature resistance furnace, and then pouring the crucible into a cold water pool for water quenching;
(4) drying the water-quenched glass mixture, then sending the dried water-quenched glass mixture into a crusher for crushing, and screening the crushed glass mixture by using a multi-stage linear screen to obtain glass powder;
(5) feeding the sieved glass powder with the diameter range of 10-30 mu m into a sintering furnace for sintering, wherein the sintering temperature is 1350-1500 ℃, and forming glass microspheres;
(6) and (3) putting the glass microspheres into a water tank, selecting and discarding the hollow glass microspheres by utilizing buoyancy, and drying the remaining solid glass microspheres to obtain the glass microspheres for the solid-phase converter.
2. The method for producing glass microspheres for a solid-phase converter according to claim 1, wherein: and (2) adding 1% of water into the mixer in the step (1).
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| CN102320743B (en) * | 2011-09-29 | 2013-07-31 | 蚌埠玻璃工业设计研究院 | High strength aluminosilicate hollow glass microsphere and preparation method thereof |
| CN103723910B (en) * | 2013-12-14 | 2016-06-29 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of porous glass beads |
| CN204079762U (en) * | 2014-07-24 | 2015-01-07 | 宁波大学 | A kind of preparation facilities of chalcogenide glass microballoon |
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