KR101470971B1 - Liquid hermetic sealant of heat-resistant, menufacturing and sealing method therof - Google Patents

Abstract

The present invention relates to a heat resistant liquid type hermetic sealant, a manufacturing method thereof, and a sealing method. The liquid type hermetic sealant of the present invention comprise: a raw material in which 0-50 parts by weight of metal oxide and 5-10 parts by weight of clay mineral are mixed; and a binder mixture in which 30-50 parts by weight of liquid phase inorganic binders and 4-12 parts by weight of metal oxide sol. The manufacturing method for the liquid type hermetic sealant comprises: a first step (S1) of manufacturing a raw material by mixing metal compounds and high purity clay mineral; a second step (S2) of manufacturing a binder mixture by mixing liquid phase inorganic binders and metal oxide sol; and a third step (S3) of adding an additive while mixing the raw material and the binder mixture. The sealing method according to the present invention comprises: a tenth step (S10) of injecting the liquid type hermetic sealant into a product requiring liquid type hermetic sealant sealing; a twentieth step (S20) of drying the liquid type hermetic sealant at room temperature; a thirtieth step (S30) of heating the dried liquid type hermetic sealant; a fortieth step (S40) of performing primary plasticization; a fiftieth step (S50) of injecting metal oxide sol; and a sixtieth step (S60) of performing secondary plasticization. Accordingly, the present invention markedly improves heat resistance and adhesion strength in order to be continuously used at a temperature of 600°C or more, prevents physical property change, combustion phenomenon and the like, and increases energy efficiency by a sintering temperature of 600°C or less.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hermetic sealing material,

The present invention relates to a hermetic sealing material, and more particularly, to a hermetic sealing material which comprises a raw material in which a metal oxide and a clay are mixed, an inorganic binder and a metal oxide sol Which comprises a binder mixture as a main component, to produce a liquid hermetic sealing material having heat resistance, a process for producing the hermetic sealing material, and a sealing method.

A hermetic sealing process is required to prevent water infiltration and oxidation that cause adhesion to the structure during packaging of electronic and optical devices and to improve the reliability of the device by keeping the atmosphere inside the device constant. Conventional hermetic sealing materials used herein include epoxy-based phenol-based organic materials and inorganic sealing materials such as glass and ceramics.

Here, in the case of the organic sealing material, the range of use is wide and the manufacturing and introduction process is good, but it is difficult to use in an environment of high temperature and high pressure. Particularly, most of the organic sealing materials have a problem that their physical properties are changed or burned at a high temperature of 300 ° C or more, resulting in a serious problem of heat resistance. To improve this, Aremco of the United States, Telnik Industrial of Japan and Toagosei of Japan developed and sold products with inorganic fillers such as alumina and magnesium oxide introduced into the processing process to improve heat resistance and bonding strength However, the price is very high and there are limitations in process application.

In addition, inorganic sealing materials such as glass and ceramics are excellent in heat resistance and airtightness but require a high sintering temperature of 900 ° C or higher in the manufacturing process, resulting in low energy efficiency.

In addition, the paste-type sealing material made of the inorganic sealing material can be used as a sealing material in which a crystal type package (hereinafter referred to as " PbO ") containing zinc oxide (ZnO) and boron (B ₂ O ₃ ) A glass-like mounting material powder containing lead powder, lead oxide (PbO), boron (B ₂ O ₃ ) and silicon dioxide (SiO ₂ ) as main components is mixed at a predetermined ratio, An additive such as a binder and a surfactant is added and mixed and dispersed.

However, such a paste-type sealing material has a problem that it is difficult to control pores and pores.

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In order to solve the above-described problems, the present invention provides a method of manufacturing a hermetic sealing material in the form of a liquid by adding an additive such as a defoaming agent and a dispersing agent while mixing a mixture of a metal oxide and a clay mineral and a mixture of an inorganic binder and a metal oxide sol A heat-resistant liquid-type hermetic sealing material which is improved in heat resistance and energy efficiency as compared with a conventional sealing material and is improved in airtightness and controllability by controlling the pores and bubbles during sealing by the liquid hermetic sealing material of the present invention, A manufacturing method thereof, and a sealing method.

In order to achieve the above object, the heat-resistant liquid-type hermetic sealing material according to the present invention comprises a raw material in which a metal oxide in a weight ratio of 40 to 50 and a clay mineral in a weight ratio of 5 to 10 are mixed; And a binder mixture of 30 to 50 weight ratio of an inorganic binder and 4 to 12 weight ratio of a metal oxide sol, wherein the inorganic binder is a liquid, and the hermetic sealing material comprising a mixture of a raw material and a binder mixture, .

The heat-resistant liquid-type hermetic sealing material according to the present invention further comprises an additive in a weight ratio of 5 to 10, and the additive is characterized by being composed of at least one of a defoaming agent, a dispersant, and a heat stabilizer.

Further, the metal oxide is in powder form, and is characterized by being any one of aluminum oxide, zirconium oxide, silicon oxide, and titanium oxide.

The clay mineral is characterized by being kaolin or bentonite.

Further, the inorganic binder is characterized by being a silicate-based material including sodium silicate or a phosphate-based material including aluminum phosphate.

The metal oxide sol is characterized by being zirconia sol, alumina sol, silica sol, or titania sol.

Meanwhile, a method of manufacturing a liquid type hermetic sealing material according to the present invention includes a first step (S1) of producing a raw material by mixing a metal compound at a weight ratio of 40 to 50 and a high purity clay mineral at a weight ratio of 5 to 10 by weight for 23 to 25 hours, ); A second step (S2) of mixing an inorganic binder in a liquid state at a weight ratio of 30 to 50 and a metal oxide sol at a rate of 4 to 12 by weight at 500 to 1,000 rpm for 30 to 60 minutes to form a binder mixture; And a third step (S3) of adding the additive of 5 to 10 weight ratio while mixing the raw material and the binder mixture and mixing the mixture at 500 to 1,000 rpm for 2 to 3 hours.

The sealing method using the liquid type hermetic sealing material according to the present invention may further include a tenth step (S10) of injecting a liquid type hermetic sealing material into a product requiring sealing; 20) S20 (S20) of drying the liquid type hermetic sealing material at room temperature for 11 to 13 hours; A thirty step S30 of heat-treating the dried liquid-like hermetic sealing material at 100 to 150 DEG C for 30 to 60 minutes; A forty-first step (S40) of subjecting the first heat-treated liquid type hermetic sealing material to a temperature of 150 to 300 DEG C for about 10 to 60 minutes; A 50th step (S50) of injecting a metal oxide sol at a weight ratio of 10 to 30 into a liquefied hermetic sealing material subjected to the first calcination as a void control material; And a 60th step (S60) of subjecting the liquid type hermetic sealing material having the metal oxide sol to a secondary firing treatment at 300 to 600 캜 for 10 to 60 minutes.

As described above, according to the present invention, by mixing a raw material material in which a metal oxide and a clay mineral are mixed, and a binder mixture in which an inorganic binder and a metal oxide sol are mixed, a small amount of an additive is added to produce a liquid type hermetic sealing material, The heat resistance and the bonding strength are remarkably improved so that they can be continuously used in an environment of 600 DEG C or more, the property change or the combustion phenomenon is prevented, and the energy efficiency is increased due to the sintering temperature of 600 DEG C or less.

In addition, when a sealing operation is performed using a liquid type hermetic sealing material, by injecting a metal oxide sol, the air gap and pores of the sealing material can be controlled to maximize airtightness.

In addition, since the liquid phase is strong against high temperature, the application range can be maximized.

BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate preferred embodiments of the invention and, together with the description, serve to further the understanding of the technical idea of the invention, It should not be interpreted.
1 is a process diagram for manufacturing a heat resistant liquid type hermetic sealing material according to the present invention.
2 is a process diagram showing a sealing operation using a heat-resistant liquid-type hermetic sealing material according to the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the detailed description of known functions and configurations incorporated herein will be omitted when it may unnecessarily obscure the subject matter of the present invention.

<Configuration>

The heat-resistant liquid type hermetic sealing material according to the present invention is made of raw materials, a binder mixture, and an additive including an antifoaming agent, a dispersant, and a heat stabilizer.

The raw material is composed of a mixture of metal oxide (40 to 50 wt%) and clay (5 to 10 wt%).

Here, the metal oxide is one of aluminum oxide (Al ₂ O ₃ ), zirconium oxide (ZrO ₂ ), silicon oxide, and titanium oxide as a material for improving heat resistance, and is in powder form.

Aluminum oxide is a compound of aluminum and oxygen, and is industrially called alumina. It is also the main component of aluminum light. This aluminum oxide is mechanically strong, and has excellent chemical resistance and heat resistance.

Zirconium oxide is a colorless powder, which is a monoclinic system at low temperature (1,000 ° C or less) and tetragonal system at high temperature. This zirconium oxide is excellent in corrosion resistance, has a high melting point of 2,677 ° C, and is used as a refractory material because of its low coefficient of thermal expansion. In addition, zirconium oxide has the highest strength among the ceramic materials, is excellent in aesthetics, and is resistant to abrupt temperature changes such as rapid heating and quenching. This zirconium oxide is used as an inorganic silicon sealing material.

Silicon oxide is a relatively simple compound of silicon and is used as a raw material for glass. This silicon oxide is used as an inorganic glass sealing material.

Titanium oxide is a material in which titanium metal is oxidized, and has the property of titanium. Titanium is a silver-white metal. Its strength is almost the same as that of carbon steel. Its thermal conductivity and thermal expansion coefficient are small, so it has excellent heat resistance.

Further, clay minerals are mixed with powdery metal oxides to improve the bonding strength with inorganic binders and additives. These clay minerals are high purity clay materials, either kaolin or bentonite.

On the other hand, the binder mixture is composed of an inorganic binder in a weight ratio of 30 to 50 and a metal oxide sol in a weight ratio of 4 to 12.

As the inorganic binder, a silicate-based or sodium phosphate-based phosphate system is used as the liquid material.

The metal oxide sol is selected from zirconia sol, alumina sol, silica sol, and titania sol.

On the other hand, the additive is added in an amount of 5 to 10 parts by weight, using any one or more of a defoaming agent, a dispersant and a heat stabilizer. Here, the antifoaming agent is a polyether-based agent and the dispersing agent is a polycarboxylic acid-based agent. The heat stabilizer is a conventional one.

<Manufacturing Method>

A method for manufacturing a heat-resistant liquid-type hermetic sealing material according to the present invention comprises first mixing a metal oxide and a clay mineral to form a raw material (S1). At this time, the raw material is prepared by mixing a metal compound of 40 to 50 weight ratio and a high purity clay mineral of 5 to 10 weight ratio for about 23 to 25 hours, preferably 24 hours. Here, the metal compound for improving the heat resistance is any one of aluminum oxide (Al ₂ O ₃ ), zirconium oxide (ZrO ₂ ), silicon oxide, and titanium oxide in powder form. Also, kaolin or kaolinite is used to improve the bonding force between the materials to be mixed.

Next, the inorganic binder and the metal oxide sol are mixed to prepare a binder mixture (S2). At this time, an inorganic binder in a liquid phase of 30 to 50 weight ratio and a metal oxide sol of 4 to 12 weight ratio are mixed at a speed of 500 to 1,000 rpm for 30 to 60 minutes. Here, the inorganic binder includes one selected from the group consisting of silicate containing sodium silicate and phosphoric acid containing aluminum phosphate. The metal oxide sol may be any one of zirconia sol, alumina sol, silica sol and titania sol.

Next, the additive is further mixed with the raw material and the binder mixture (S3). At this time, a mixture of the raw material and the binder is added, and an additive of at least one of a defoaming agent, a dispersant, and a heat stabilizer is further added and mixed. At this time, these raw materials, the binder mixture and the additive are mixed for 2 to 3 hours at a speed of 500 to 1,000 rpm. As a result, a liquid type Hermetic sealing material excellent in heat resistance is produced.

<Sealing method>

Meanwhile, in the sealing method using the heat resistant liquid hermetic sealing material according to the present invention, first, a liquid sealing material is put into a product requiring sealing (S10).

Next, drying is performed at room temperature (S20). At this time, it is allowed to stand at room temperature for about 11 to 13 hours, preferably for about 12 hours.

Next, heat treatment is performed at 100 to 150 占 폚 for 30 to 60 minutes (S30).

Next, the first firing process is performed at 150 to 300 DEG C for about 10 to 60 minutes (S40). It is easy to inject the void control material by the first firing process.

Next, a metal oxide sol in a weight ratio of 10 to 30 is introduced as a void control material (S50).

Finally, secondary firing is performed at 300 to 600 ° C for 10 to 60 minutes (S60). Thereby, the sealing to the sealed product is completed.

As described above, those skilled in the art will appreciate that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are to be considered in all respects as illustrative and not restrictive. The scope of the present invention is defined by the appended claims rather than the detailed description and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included within the scope of the present invention.

Claims (8)

A hermetic sealing material comprising: a raw material mixed with a metal oxide in a weight ratio of 40 to 50 and a clay mineral in a weight ratio of 5 to 10; And a binder mixture of 30 to 50 weight ratio of an inorganic binder and 4 to 12 weight ratio of a metal oxide sol, wherein the inorganic binder is a liquid phase, and the binder is a hermetic Wherein the sealing material is a liquid and the metal oxide is in the form of powder and is any one of aluminum oxide, zirconium oxide, silicon oxide and titanium oxide, the clay mineral is kaolin or bentonite, the inorganic binder is a silicate- Wherein the metal oxide sol is a phosphate compound including aluminum and the metal oxide sol is any one of zirconia sol, alumina sol, silica sol, and titania sol.
The method according to claim 1,
Further comprising 5 to 10 weight ratio of an additive,
Wherein the additive comprises at least one of a defoaming agent, a dispersant, and a heat stabilizer.
delete delete delete delete A method for producing a heat resistant liquid hermetic sealing material according to claim 1 or 2,
A first step (S1) of mixing a metal compound in a weight ratio of 40 to 50 and a high-purity clay mineral in a ratio of 5 to 10 by weight for 23 to 25 hours to prepare a raw material;
A second step (S2) of mixing an inorganic binder in a liquid state at a weight ratio of 30 to 50 and a metal oxide sol at a rate of 4 to 12 by weight at 500 to 1,000 rpm for 30 to 60 minutes to form a binder mixture; And
And a third step (S3) of mixing the raw material and the binder mixture together with additives at a weight ratio of 5 to 10 at 500 to 1,000 rpm for 2 to 3 hours (S3). Way.
A sealing method using the heat resistant liquid type hermetic sealing material according to claim 1 or 2,
A tenth step (SlO) of injecting a liquid type hermetic sealing material into a product requiring sealing;
20) S20 (S20) of drying the liquid type hermetic sealing material at room temperature for 11 to 13 hours;
A thirty step S30 of heat-treating the dried liquid type hermetic sealing material at 100 to 150 DEG C for 30 to 60 minutes;
A step (S40) of subjecting the liquid type hermetic sealing material subjected to the first heat treatment to a first firing treatment at 150 to 300 DEG C for about 10 to 60 minutes;
A 50th step (S50) of injecting a metal oxide sol at a weight ratio of 10 to 30 as a void control material into the liquid type hermetic sealing material subjected to the first calcination treatment; And
(60) (S60) a secondary firing step (S60) of the liquid type hermetic sealing material into which the metal oxide sol has been added at a temperature of 300 to 600 DEG C for about 10 minutes to 60 minutes (S60). Way.

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