CN111138081A

CN111138081A - Improved preparation method of glass sealing material

Info

Publication number: CN111138081A
Application number: CN201911413346.3A
Authority: CN
Inventors: 乔星; 华斯嘉; 王哲; 冯庆; 贾波; 刘卫红; 杨文波
Original assignee: Xian Seal Electronic Material Technology Co Ltd
Current assignee: Xian Seal Electronic Material Technology Co Ltd
Priority date: 2019-12-31
Filing date: 2019-12-31
Publication date: 2020-05-12

Abstract

The invention discloses an improved preparation method of a glass sealing material, which selects borosilicate glass produced by the company as a main body, dopes a small amount (3%, 5%, 8% and 10%) of micron Al2O3 and nano Al2O3 in the process of preparing slurry, then prepares doped glass granulation powder by a spray drying method, tests the recovery rate of powder, the fluidity, the apparent density and other properties, simultaneously prepares a corresponding glass blank, and tests the mechanical strength and the corrosion resistance of the glass blank. Test results show that the addition of the Al2O3 powder can effectively improve the overall performance of the borosilicate glass, and the recovery rate of the original powder in the spray granulation process is obviously improved along with the increase of the content of Al2O 3; the mechanical strength and the corrosion resistance of the corresponding glass product are also improved; for Al2O3 doped with the same content, the nano Al2O3 has higher performance improvement than the micron Al2O 3. The method has good effects on the preparation of the high-performance glass granulated powder and the improvement of the sealing performance.

Description

Improved preparation method of glass sealing material

Technical Field

The invention relates to the technical field of electronic glass, in particular to a preparation method of an improved glass sealing material.

Background

With the automation and scale of electronic component production, the requirement for the consistency of sealing glass and electronic component sealing precision is increasingly strict, and the past sealing glass powder wax-doped forming is gradually replaced by sealing glass spray granulation powder forming. The sealing glass powder has the advantages of good fluidity, uniform particles and easy operation after being subjected to spray granulation, and is suitable for precise sealing of electronic components with different sizes and various structures. Particularly for components with small size or complex structure, the precision consistency of the filling amount of a blank mold can be ensured only by spraying the granulated powder of the sealing glass with good fluidity, and the batch precision of glass and metal packaging is ensured.

How to optimize the sealing precision of electronic components and further improve the overall quality of sealing glass is always the focus of research and development personnel in recent years. Chinese patent (application No. CN102070300A) discloses a glass sealing material for a thermal battery and a method for preparing the same, which introduces the basic preparation process of the glass sealing material more fully through a series of specific examples, and there is still room for further optimization of the preparation technology mentioned in the patent.

Disclosure of Invention

The invention aims to optimize the prior preparation technology of the glass sealing material, and then the production efficiency and the overall performance of the glass sealing material. The invention mainly aims to solve the problems of low powder granulation recovery rate, poor blank making compactness, poor glass chemical stability and the like.

The invention adopts a method of mixing and pulping a plurality of powders in the slurry preparation stage to improve various performances of the glass powder and the glass blank while continuously optimizing parameters in the whole preparation process of the glass sealing material.

Experiments prove that the glass sealing material produced by the preparation technology provided by the invention has good comprehensive performance. The recovery rate of the granulated powder is improved, the powder fluidity is enhanced, and the mechanical strength is obviously improved.

Drawings

The present invention will be described in further detail with reference to the accompanying drawings.

FIG. 1 is a schematic flow chart of the preparation technique of the present invention.

FIG. 2 is a graph showing a comparison of the recovery rates of powders in the present invention.

FIG. 3 is a graph showing a comparison of powder flowability in the present invention.

FIG. 4 is a graph comparing the percent of pass of samples after mechanical impact on a glass gob of the present invention.

Detailed Description

The values and preparation methods of the components of the present invention are further described in detail by the following examples:

example (b):

preparing materials: 500g of raw materials are prepared according to the following component molar ratio, 600g of agate balls are added and mixed evenly.

SiO2：60-80％；BaO：3-15％；Na2O：5-15％；

K2O：4-15％；Al2O3：0-6％；B2O3：0-6％；

Li2O：0-5％；La2O3：0-5％。

Melting: and (3) placing the uniformly mixed ceramic powder in a high-temperature furnace, heating to 1600 ℃, preserving heat for a certain time, taking out, pouring into water, and quenching to obtain the glass slag.

Milling: and melting the obtained glass slag according to a ball-to-feed ratio of 1.2: 1, crushing and grinding for 2 hours in a ball mill, and then selecting a 150-mesh sieve for vibration screening to obtain the glass raw powder with a certain granularity.

Pulping: mixing the glass raw powder, the dispersant, the binder and the water according to a certain proportion, simultaneously adding Al2O3 with a certain content, and placing the mixture in a ball mill for fully stirring. The solid content of the slurry is controlled to be 60% in the whole process, and 3%, 5%, 8% and 10% of aluminum oxide powder (conventional powder and nano powder) are respectively added, so that nine experiments are performed.

And (3) granulation: taking out the slurry prepared in the step S4 and introducing the slurry into a centrifugal spray granulator to prepare granulated powder; wherein the spraying pressure is 15kg/cm 3; the aperture of the nozzle is 0.6 mm; the inlet temperature was 220 ℃ and the outlet temperature was 90 ℃.

Blank preparation: and pouring the prepared granulation powder into a briquetting machine to prepare a glass blank.

Vitrification: the glass gob prepared in S6 was placed in a vitrification furnace to be fully reacted.

Sealing: assembling the glass blank and placing the glass blank in a sintering furnace to prepare a product.

And (3) testing:

1. and respectively measuring the mass of the granulation powder by using an electronic balance, and calculating the recovery rate.

2. Selecting several kinds of granulation powder, and testing the flowability of the granulation powder by using a powder comprehensive tester.

3. And (3) performing an impact test of P & lt1200N on a plurality of products, measuring the air tightness of the products after impact, and calculating the final qualified rate, wherein the leakage rate is less than 1.0 multiplied by 10-10Pa.m 3/s.

As can be seen from fig. 2, the recovery rate of the granulated powder is significantly improved with the increase in the amount of alumina added, and as can be seen from fig. 3, the powder flowability can be improved by appropriately adding nano alumina powder. Fig. 4 shows the airtight pass rate of the product after mechanical impact of the sealed product, and as can be seen from fig. 4, the addition of alumina can effectively improve the mechanical strength of the glass product and further improve the impact resistance of the glass product.

The basic principles and the main features of the invention and the advantages of the invention have been shown and described above, it being obvious to a person skilled in the art that the invention is not limited to the details of the above-described exemplary embodiments.

The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims

1. The improved preparation method of the glass sealing material is characterized by comprising the following steps:

step 1), batching: preparing raw materials according to the mol ratio of the specific components, adding the raw materials into a ball mill, and uniformly mixing;

step 2) melting: placing the ceramic powder prepared in the step 2) in a high-temperature furnace to be heated to a liquid state, keeping the temperature for a certain time, taking out the ceramic powder, pouring the ceramic powder into water, and quenching the ceramic powder to obtain glass slag;

step 3) pulverizing: crushing, grinding and vibrating screening the glass slag obtained in the step 2) to obtain glass raw powder with a certain granularity;

step 4), pulping: mixing glass raw powder, a dispersing agent, a binder and water according to a certain proportion, simultaneously adding Al2O3 with a certain content, and placing the mixture in a ball mill for fully stirring;

step 5) granulation: taking out the slurry prepared in the step 4) and introducing the slurry into a spray granulator to prepare granulated powder;

step 6), blank making: pouring the granulation powder prepared in the step 5) into a briquetting machine to prepare a glass blank;

step 7) vitrification: placing the glass blank prepared in the step 6) in a vitrification furnace for full reaction;

step 8) sealing: assembling the glass blank and placing the glass blank in a sintering furnace to prepare a product.

2. The method for preparing an improved glass sealing material according to claim 1, wherein the ingredients in step 1) are based on SiO2, Al2O3 and B2O3, and are mixed with an appropriate alkali metal oxide.

3. The method for preparing an improved glass sealing material according to claim 1, wherein the Al2O3 added in the pulping in step 4) does not chemically react with the melted glass powder, and the main purpose is to improve the granulation efficiency and enhance the comprehensive performance of the glass.

4. The method for preparing an improved glass sealing material according to claim 1, wherein the dispersant and the binder used in the step 4) of pulping are both organic high molecular polymers.

5. The method for producing an improved glass sealing material according to claim 1, wherein the diameter of the nozzle is 0.6 to 0.7mm when the spray granulation is performed in the step 5); the spraying pressure was 15kg/cm 3.

6. The method for preparing an improved glass sealing material according to claim 1, wherein the inlet temperature is 200-240 ℃, the outlet temperature is 80-100 ℃ and the negative pressure is 25MPa during spray granulation in the step 5).