Preparation method of spherical sealing glass powder and spherical sealing glass powder

Abstract

The invention provides a preparation method of spherical sealing glass powder and the spherical sealing glass powder, and relates to the technical field of sealing materials. The preparation method of the spherical sealing glass powder comprises the following steps: adding polyvinyl alcohol into deionized water to obtain a binder precursor liquid; placing deionized water, a dispersing agent, the original glass powder and grinding balls in a ball milling tank for ball milling to obtain first glass slurry; mixing the binder precursor liquid with the first glass slurry according to a mass ratio of 1: 4 to 1: 6 to obtain a second glass slurry; sieving the second glass slurry to obtain third glass slurry; and carrying out spray granulation by using the third glass slurry to obtain the spherical sealing glass powder. According to the invention, the sphericity degree of the sealing glass powder can be improved, so that the performance of the sealing material is improved.

Description

Technical Field

[0001] The present disclosure relates to the technical field of sealing materials, and in particular to a preparation method of a spherical sealing glass powder and the spherical sealing glass powder. Background Art

[0002] With the rapid development of electronic information technology, various sensors and semiconductor metal substrates are widely used in specific working environments, such as aerospace, aviation, national defense, military, power and other fields, which have higher and higher performance requirements for electrical connectors. However, in order to connect these devices to give full play to their performance, sealing materials that can work stably in specific environments are required, and glass powder is a commonly used sealing material.

[0003] Before glass powder is used for sealing, it often needs to be pressed into a glass blank. In order to better press the blank, the glass powder needs to be prepared into spherical granular powder with good fluidity. The pressed glass blank can prevent bubbles from being generated inside during sealing and ensure the sealing performance.

[0004] At present, there is a common problem that the sphericity of sealing glass powder is poor, resulting in poor performance of sealing materials.

[0005] It should be noted that the information disclosed in the above background technology section is only used to enhance the understanding of the background of the present disclosure, and therefore may include information that does not constitute the prior art known to ordinary technicians in the field. Summary of the invention

[0006] The purpose of the present disclosure is to provide a method for preparing a spherical sealing glass powder and a spherical sealing glass powder, thereby overcoming the problem of poor sphericity of the sealing glass powder at least to a certain extent.

[0007] According to the first aspect of the present disclosure, a method for preparing a spherical sealing glass powder is provided, comprising: adding polyvinyl alcohol to deionized water to obtain a binder precursor liquid; placing deionized water, a dispersant, original glass powder and grinding balls in a ball mill for ball milling to obtain a first glass slurry; mixing the binder precursor liquid with the first glass slurry in a mass ratio of 1:4 to 1:6 to obtain a second glass slurry; sieving the second glass slurry to obtain a third glass slurry; and spray granulating the third glass slurry to obtain a spherical sealing glass powder.

[0008] Optionally, polyvinyl alcohol is added to deionized water to obtain a binder precursor liquid, including: adding polyvinyl alcohol to deionized water to obtain a first intermediate solution; placing the intermediate solution in a magnetic stirring heating furnace, and magnetically stirring at 40°C to 80°C to obtain a second intermediate solution; wherein the rotation speed of the magnetic stirring heating furnace is 150r / min to 200r / min, and the heating stirring time is 2h to 3h; the second intermediate solution is allowed to stand until no binder is precipitated and the solution is transparent to obtain a binder precursor liquid.

[0009] Optionally, the mass percentage of polyvinyl alcohol in the binder precursor liquid is 10% to 18%.

[0010] Optionally, in the process of obtaining the first glass slurry, the ball milling speed is 100 r / min to 200 r / min, and the ball milling time is 50 min to 70 min.

[0011] Optionally, the particle size of the original glass powder is 10 μm to 20 μm.

[0012] Optionally, the ball mill is an alumina ceramic ball mill, and the grinding balls are zirconia balls; wherein, in the process of obtaining the first glass slurry, the ball-to-material ratio is 2:1 to 2.5:1.

[0013] Optionally, the dispersant is a combination of one or more of polyacrylamide, polyvinyl alcohol, polyethylene glycol, and polyethylene glycol; wherein the mass ratio of the dispersant to the original glass powder is 1:100 to 3:100.

[0014] Optionally, the binder precursor liquid and the first glass slurry are mixed in a mass ratio of 1:4 to 1:6 to obtain a second glass slurry, including: placing the binder precursor liquid and the first glass slurry in a mass ratio of 1:4 to 1:6 in a ball mill for ball milling to obtain the second glass slurry; wherein, in the process of obtaining the second glass slurry, the ball milling speed is 200 r / min to 300 r / min, and the ball milling time is 90 min to 120 min.

[0015] Optionally, spray granulation is performed using a third glass slurry to obtain a spherical sealing glass powder, including: using a spray granulator and performing spray granulation using a third glass slurry to obtain a spherical sealing glass powder; wherein, for the spray granulation process, the spray granulation inlet temperature is 200°C to 280°C, the outlet temperature is 100°C to 150°C, the feed pump speed is 10mL / min to 30mL / min, the frequency is 20 times / min to 40 times / min, and the nozzle atomization pressure is 0.1MPa to 0.5MPa.

[0016] According to a second aspect of the present disclosure, a spherical sealing glass powder is provided. The spherical sealing glass powder is prepared by any of the above-mentioned methods for preparing a spherical sealing glass powder.

[0017] In the scheme of the exemplary embodiment of the present disclosure, on the one hand, the process of forming the spherical sealing glass powder is simple and easy to implement through the configuration of the binder and the dispersant. When the binder is added, the ball milling and spray granulation processes are combined to greatly improve the sphericity of the sealing glass powder, which helps to improve the performance of the sealing material. On the other hand, the scheme of the present disclosure can achieve controllable particle size of the spherical sealing glass powder by adjusting the proportion of raw materials such as polyvinyl alcohol to meet the application requirements of different scenarios.

[0018] It is to be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present disclosure. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The accompanying drawings herein are incorporated into the specification and constitute a part of the specification, illustrate embodiments consistent with the present disclosure, and together with the specification are used to explain the principles of the present disclosure. Obviously, the accompanying drawings described below are only some embodiments of the present disclosure, and for ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without creative work.

[0020] Figure 1 The flowchart of the method for preparing the spherical sealing glass powder according to the exemplary embodiment of the present disclosure is schematically shown.

[0021] Figure 2 The scanning electron microscope image of the spherical sealing glass powder prepared in Example 1 of the present disclosure is schematically shown.

[0022] Figure 3 The scanning electron microscope image of the spherical sealing glass powder prepared in Comparative Example 1 of the present disclosure is schematically shown. DETAILED DESCRIPTION

[0023] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in a variety of forms and should not be construed as being limited to the examples set forth herein; on the contrary, these embodiments are provided so that the present disclosure will be more comprehensive and complete, and the concepts of the example embodiments are fully conveyed to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, many specific details are provided to provide a full understanding of the embodiments of the present disclosure. However, those skilled in the art will appreciate that the technical solutions of the present disclosure may be practiced while omitting one or more of the specific details, or other methods, processes, steps, etc. may be adopted. In other cases, known technical solutions are not shown or described in detail to avoid obscuring various aspects of the present disclosure.

[0024] In addition, the accompanying drawings are only schematic illustrations of the present disclosure and are not necessarily drawn to scale. The same reference numerals in the figures represent the same or similar parts, and thus their repeated descriptions will be omitted. The flowcharts shown in the accompanying drawings are only exemplary illustrations and do not necessarily include all the steps. For example, some steps can also be decomposed, while some steps can be combined or partially combined, so the actual execution order may change according to actual conditions. In addition, all the terms "first", "second", "third", etc. below are only for the purpose of distinction and should not be used as limitations of the present disclosure.

[0025] Among some technologies for preparing spherical sealing glass powder, paraffin granulation or mixed granulator can be used. Although these methods can prepare sealing glass powder, these methods generally have the problems of low preparation efficiency and poor sphericity, which affects the quality of sealing materials.

[0026] In view of this, the embodiments of the present disclosure provide a new method for preparing spherical sealing glass powder.

[0027] Figure 1 The flowchart of the method for preparing the spherical sealing glass powder according to the exemplary embodiment of the present disclosure is schematically shown. Figure 1 The method for preparing the spherical sealing glass powder according to the embodiment of the present disclosure may include the following steps: S10. Add polyvinyl alcohol into deionized water to obtain a binder precursor liquid.

[0028] According to some embodiments of the present disclosure, first, polyvinyl alcohol can be added to deionized water to obtain a first intermediate solution. Next, the intermediate solution can be placed in a magnetic stirring heating furnace and magnetically stirred at 40°C to 80°C to obtain a second intermediate solution; wherein the rotation speed of the magnetic stirring heating furnace is 150r / min to 200r / min, and the heating stirring time is 2h to 3h. Next, the second intermediate solution can be allowed to stand until no binder is precipitated and the solution is transparent to obtain a binder precursor liquid. In addition, a predetermined standing time can also be specified, and the present disclosure does not limit this.

[0029] For the binder precursor liquid, the mass percentage of polyvinyl alcohol is 10% to 18%.

[0030] S12. Deionized water, a dispersant, original glass powder and grinding balls are placed in a ball mill for ball milling to obtain a first glass slurry.

[0031] In an exemplary embodiment of the present disclosure, the dispersant may be an active polymer dispersant soluble in deionized water. Specifically, the dispersant may be a combination of one or more of polyacrylamide, polyvinyl alcohol, polyethylene glycol, and polyethylene glycol.

[0032] The particle size of the original glass powder in the embodiment of the present disclosure may be 10 μm to 20 μm. The mass ratio of the dispersant to the original glass powder may be controlled to be 1:100 to 3:100.

[0033] The ball mill used in the embodiment of the present disclosure may be an alumina ceramic ball mill, and the grinding balls may be zirconium oxide balls. In the process of obtaining the first glass slurry, the ball-to-material ratio may be 2:1 to 2.5:1. The loading height is not higher than one-third of the ball mill. In addition, at this stage, the ball milling speed is 100 r / min to 200 r / min, and the ball milling time is 50 min to 70 min.

[0034] S14. The binder precursor liquid is mixed with the first glass paste in a mass ratio of 1:4 to 1:6 to obtain a second glass paste.

[0035] According to some embodiments of the present disclosure, the binder precursor liquid and the first glass slurry can be placed in a ball milling jar at a mass ratio of 1:4 to 1:6 for ball milling to obtain a second glass slurry. In this stage, the ball milling speed is 200 to 300 r / min, and the ball milling time is 90 to 120 min.

[0036] The pH of the second glass paste of the embodiment of the present disclosure is 7 to 8.

[0037] S16. Screening the second glass slurry to obtain a third glass slurry.

[0038] In an exemplary embodiment of the present disclosure, the third glass slurry may be sieved with a 150-400 mesh sieve, for example, the second glass slurry is sieved with a 200 mesh sieve, and the obtained third glass slurry is placed in a clean beaker.

[0039] S18. Use the third glass slurry to perform spray granulation to obtain a spherical sealing glass powder.

[0040] In an exemplary embodiment of the present disclosure, a spray granulator can be used to perform spray granulation using the third glass slurry to obtain a spherical sealing glass powder. Specifically, the spray granulator is a centrifugal granulation spray dryer.

[0041] For the spray granulation process, the spray granulation inlet temperature is 200°C to 280°C, the outlet temperature is 100°C to 150°C, the feed pump speed is 10mL / min to 30mL / min, the frequency is 20 times / min to 40 times / min, and the nozzle atomization pressure is 0.1MPa to 0.5MPa.

[0042] Through the above process, the particle size distribution range of the prepared spherical sealing glass powder is 60 μm to 160 μm. That is, by adjusting the process parameters in the above preparation process, especially the content of the binder, the particle size of the spherical sealing glass powder can be adjusted within the range of 60 μm to 160 μm.

[0043] The above preparation process is described below by way of examples and comparative examples.

[0044] Example 1 First, 45 g of polyvinyl alcohol was added to 205 g of deionized water, and then placed in a magnetic stirring heating furnace at 80° C., with a rotation speed of 200 r / min, heated and stirred for 2 h, and after standing for a period of time, no binder was precipitated and the solution was clear and transparent, to obtain a binder precursor liquid.

[0045] Next, 80 g of deionized water was added to the alumina ceramic ball mill, and then 3 g of dispersant was added, and after being fully stirred with a glass rod, 250 g of grinding balls and 100 g of the prepared original glass powder were added for ball milling to obtain the first glass slurry. The ball milling speed was adjusted to 100 r / min, and the ball milling time was 70 min.

[0046] Subsequently, the binder precursor liquid and the first glass slurry were placed in a ball milling jar at a ratio of 1:6 to obtain a second glass slurry. In this stage, the ball milling speed was adjusted to 200 r / min and the ball milling time was 120 min.

[0047] Then, the second glass slurry was passed through a 200-mesh sieve to obtain a third glass slurry, and the third glass slurry was used for spray granulation, wherein the spray granulation inlet temperature was 280° C., the outlet temperature was 150° C., the feed pump speed was 30 mL / min, the frequency was 20 times / min, and the nozzle atomization pressure was 0.5 MPa.

[0048] Figure 2 The scanning electron microscope image of the spherical sealing glass powder prepared in Example 1 of the present disclosure is schematically shown. Figure 2 It can be seen that the sealing glass powder prepared by the solution of Example 1 of the present disclosure has a better sphericity.

[0049] Example 2 First, 40 g of polyvinyl alcohol was added to 360 g of deionized water, and then placed in a magnetic stirring heating furnace at 40° C., with a rotation speed of 150 r / min, and heated and stirred for 3 hours. After standing for a period of time, no binder was precipitated and the solution was clear and transparent, so as to obtain a binder precursor liquid.

[0050] Next, 80 g of deionized water was added to the alumina ceramic ball mill, and then 1 g of dispersant was added, and after being fully stirred with a glass rod, 200 g of grinding balls and 100 g of the prepared original glass powder were added for ball milling to obtain the first glass slurry. The ball milling speed was adjusted to 150 r / min, and the ball milling time was 50 min.

[0051] Subsequently, the binder precursor liquid and the first glass slurry were placed in a ball mill at a ratio of 1:4 to obtain a second glass slurry. In this stage, the ball milling speed was adjusted to 300 r / min and the ball milling time was 90 min.

[0052] Then, the second glass slurry was passed through a 200-mesh sieve to obtain a third glass slurry, and the third glass slurry was used for spray granulation, wherein the spray granulation inlet temperature was 200° C., the outlet temperature was 100° C., the feed pump speed was 10 mL / min, the frequency was 40 times / min, and the nozzle atomization pressure was 0.1 MPa.

[0053] Example 3 First, 36 g of polyvinyl alcohol was added to 260 g of deionized water, and then placed in a magnetic stirring heating furnace at 60°C, with a rotation speed of 150 r / min, heated and stirred for 2.5 h, and after standing for a period of time, no binder was precipitated and the solution was clear and transparent, to obtain a binder precursor liquid.

[0054] Next, 100 g of deionized water was added to the alumina ceramic ball mill, and then 1.3 g of dispersant was added, and after being fully stirred with a glass rod, 250 g of grinding balls and 100 g of the prepared original glass powder were added for ball milling to obtain the first glass slurry. The ball milling speed was adjusted to 180 r / min, and the ball milling time was 60 min.

[0055] Subsequently, the binder precursor liquid and the first glass slurry were placed in a ball mill at a ratio of 1:5 to obtain a second glass slurry. In this stage, the ball milling speed was adjusted to 260 r / min and the ball milling time was 100 min.

[0056] Then, the second glass slurry was passed through a 200-mesh sieve to obtain a third glass slurry, and the third glass slurry was used for spray granulation, wherein the spray granulation inlet temperature was 200° C., the outlet temperature was 110° C., the feed pump speed was 15 mL / min, the frequency was 30 times / min, and the nozzle atomization pressure was 0.1 MPa.

[0057] Comparative Example 1 First, 80 g of deionized water was added to an alumina ceramic ball mill, and then 1.3 g of a dispersant was added. After being fully stirred with a glass rod, 200 g of grinding balls and 100 g of the prepared original glass powder were added for ball milling. The ball milling speed was adjusted to 100 r / min, and the ball milling time was 60 min.

[0058] Next, the ball-milled slurry was passed through a 200-mesh sieve and spray granulated. The process parameters included: the spray granulation inlet temperature was 200°C, the outlet temperature was 110°C, the feed pump speed was 15 mL / min, the frequency was 22 times / min, and the nozzle atomization pressure was 0.2 MPa.

[0059] Figure 3 The scanning electron microscope image of the spherical sealing glass powder prepared in Comparative Example 1 of the present disclosure is schematically shown. Figure 3 and Figure 2 By comparison, it can be seen that the sealing glass powder prepared in Comparative Example 1 without a binder has poor spherical forming degree.

[0060] Furthermore, the embodiments of the present disclosure also provide a spherical sealing glass powder, which is prepared by the above-mentioned method for preparing the spherical sealing glass powder.

[0061] It should be noted that although the steps of the method in the present disclosure are described in a specific order in the drawings, this does not require or imply that the steps must be performed in this specific order, or that all the steps shown must be performed to achieve the desired results. Additionally or alternatively, some steps may be omitted, multiple steps may be combined into one step, and / or one step may be decomposed into multiple steps, etc.

[0062] In addition, the above-mentioned figures are only schematic illustrations of the processes included in the method according to the exemplary embodiments of the present disclosure, and are not intended to be limiting. It is easy to understand that the processes shown in the above-mentioned figures do not indicate or limit the time sequence of these processes. In addition, it is also easy to understand that these processes can be performed synchronously or asynchronously, for example, in multiple modules.

[0063] Those skilled in the art will readily appreciate other embodiments of the present disclosure after considering the specification and practicing what is disclosed herein. This application is intended to cover any variations, uses, or adaptations of the present disclosure that follow the general principles of the present disclosure and include common knowledge or customary technical means in the art that are not disclosed in the present disclosure. The specification and embodiments are to be considered merely as exemplary, and the true scope and spirit of the present disclosure are indicated by the claims.

[0064] It should be understood that the present disclosure is not limited to the exact structures that have been described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.

Claims

1. A method for preparing spherical sealing glass powder, characterized in that: include: adding polyvinyl alcohol to deionized water to obtain a binder precursor liquid; Deionized water, a dispersant, original glass powder and grinding balls are placed in a ball mill for ball milling to obtain a first glass slurry; Mixing the binder precursor liquid with the first glass paste in a mass ratio of 1:4 to 1:6 to obtain a second glass paste; Screening the second glass slurry to obtain a third glass slurry; The third glass slurry is used for spray granulation to obtain a spherical sealing glass powder.

2. The preparation method according to claim 1, characterized in that: Polyvinyl alcohol is added to deionized water to obtain a binder precursor solution, comprising: adding polyvinyl alcohol to deionized water to obtain a first intermediate solution; The intermediate solution is placed in a magnetic stirring heating furnace and magnetically stirred at 40° C. to 80° C. to obtain a second intermediate solution; wherein the rotation speed of the magnetic stirring heating furnace is 150 r / min to 200 r / min, and the heating stirring time is 2 h to 3 h; The second intermediate solution is allowed to stand until no binder is precipitated and the solution is transparent, so as to obtain a binder precursor solution.

3. The preparation method according to claim 1 or 2, characterized in that: The mass percentage of the polyvinyl alcohol in the binder precursor liquid is 10% to 18%.

4. The preparation method according to claim 1, characterized in that: In the process of obtaining the first glass slurry, the ball milling speed is 100 r / min to 200 r / min, and the ball milling time is 50 min to 70 min.

5. The preparation method according to claim 1, characterized in that: The particle size of the original glass powder is 10 μm to 20 μm.

6. The preparation method according to claim 1, characterized in that: The ball mill is an alumina ceramic ball mill, and the grinding balls are zirconia balls; Wherein, in the process of obtaining the first glass slurry, the ball-to-material ratio is 2:1 to 2.5:

1.

7. The preparation method according to claim 1, characterized in that: The dispersant is a combination of one or more of polyacrylamide, polyvinyl alcohol, polyethylene glycol, and polyethylene glycol; Wherein, the mass ratio of the dispersant to the original glass powder is 1:100 to 3:

100.

8. The preparation method according to claim 1, characterized in that: The binder precursor liquid is mixed with the first glass paste in a mass ratio of 1:4 to 1:6 to obtain a second glass paste, comprising: The binder precursor liquid and the first glass slurry are placed in a ball mill at a mass ratio of 1:4 to 1:6 for ball milling to obtain a second glass slurry; Wherein, in the process of obtaining the second glass slurry, the ball milling speed is 200 r / min to 300 r / min, and the ball milling time is 90 min to 120 min.

9. The preparation method according to claim 1, characterized in that: The third glass slurry is used for spray granulation to obtain a spherical sealing glass powder, comprising: Using a spray granulator and the third glass slurry to perform spray granulation to obtain a spherical sealing glass powder; Among them, for the spray granulation process, the spray granulation inlet temperature is 200℃ to 280℃, the outlet temperature is 100℃ to 150℃, the feed pump speed is 10mL / min to 30mL / min, the frequency is 20 times / min to 40 times / min, and the nozzle atomization pressure is 0.1MPa to 0.5MPa.

10. A spherical sealing glass powder, characterized in that: The spherical sealing glass powder is prepared by the method for preparing a spherical sealing glass powder according to any one of claims 1 to 9.

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