KR20200117770A - Ceramic glass bonding method in which paste is used - Google Patents

Abstract

The present invention can provide a ceramic glass bonding method, where paste coated on a bonding surface of ceramic glass is provided, wherein the paste includes ceramic glass powder, which is the same material as the ceramic glass to be bonded. A resin, a solvent, and the ceramic glass are mixed to form the paste, and the paste is applied to the ceramic glass bonding surface. After the solvent contained in the paste applied to the bonding surface is evaporated, the ceramic glass to which the paste is applied is brought into contact, so a bonding part of the ceramic glass can be made stronger. Also, precise bonding is possible by preventing the occurrence of optical spots, unbonded areas and surface devitrification in the bonding part. Since no welding device is used, the ceramic glass can be enlarged at an economical cost. In addition, by completely burning the resin contained in the paste, it is possible to eliminate the cause of impurities.

Description

Ceramic glass bonding method using paste {CERAMIC GLASS BONDING METHOD IN WHICH PASTE IS USED}

The present invention relates to a ceramic glass bonded by using a paste. In order to facilitate the manufacture of a large ceramic glass, the paste is applied to the bonding surface of the ceramic glass and heat is applied to remove the resin present in the paste on the bonding surface. The method relates to a ceramic glass in which it is used.

In recent years, according to the trend of increasing the size of the wearer in the semiconductor process and the size of the display in the display process, the need for a larger size and shape diversification of the ceramic glass used in the process is also increasing.

In general, in order to manufacture parts of various shapes of ceramic glass, ceramic glass is welded and used. In addition, as a method of welding ceramic glass, a method of bonding ceramic glass members to each other by melting the welding rod using a welding rod made of ceramic glass is used. This method has the advantage of being relatively easy to manufacture ceramic glass. have. However, on the other hand, the welding rod must be sufficiently welded to the welding area by melting the welding rod, and the experience and function of a skilled worker are also required, and the working time is long.

In addition, as another method, welding has been performed in which ceramic glass is fixed on a flat surface and heated and melted while the ceramic glass is in contact with each other. However, when the ceramic glass is placed on a flat surface and both sides of the ceramic glass are heated and melted from the top and bottom, there is a tendency that the ceramic glass falls downward due to its own weight in the melting step.

Of course, in the prior patent technology (Publication No. 10-2007-0027490), "It is a welding method using a device for welding both ends of a pair of quartz glass members facing each other, and the quartz glass members are vertically placed at regular intervals. A process of uniformly heating and melting the welded portion of the end face of the quartz glass member by the burner means from both sides of the welded portion; pressing the welded portion of the melted end face of the pair of quartz glass members with a predetermined pressure so as to face each other At the same time, a step of pushing and welding each other; a step of dispersing thermal deformation by heating and softening the bulging convex portion of the welded portion of the welded quartz glass member; and the bulging convex after the welded quartz glass member is cooled It proposes to include a process of "making it flat by grinding the (concave) part,

Further, in the prior patent technology (Publication No. 10-2019-0005441), "(a) providing an electrostatic plate made of a ceramic material; (b) forming an electrostatic adsorption electrode on one surface of the electrostatic plate; (c) Providing a base plate corresponding to the electrostatic plate; And (d) bonding the electrostatic plate on which the formation of the electrostatic adsorption electrode is completed and the base plate to each other using a low temperature liquid bonding paste; Manufacturing method."

However, in the above method, since the ceramic glass may be deformed, the ceramic glass cannot be precisely enlarged, and the low-temperature liquid bonding paste method may also cause problems such as containing impurities.

Therefore, it is a low cost method, it is possible to manufacture a ceramic glass of a complex shape, it is a situation that requires the development of a bonding method that can be solidly and precisely bonded to increase the size of the ceramic glass.

Prior Art 1: Korean Patent Laid-Open Patent 10-2007-0027490, Publication Date (Mar. 9, 2007) Prior Art 2: Korean Patent Publication 10-2019-0005441, Publication Date (January 16, 2019)

The present invention makes it possible to bond the joint part of the ceramic glass more firmly and strongly, but does not use a welding method so that the ceramic glass does not deform, and since no filler is added, the physical properties and properties of the mother agent are not different, and complex Since the device is not used, the ceramic glass can be enlarged and bonded at an economical cost.

The object is to provide a paste coated on the bonding surface of the ceramic glass, the paste includes ceramic glass powder, the ceramic glass powder is the same material as the ceramic glass to be bonded, resin, solvent, and powder of the ceramic glass This is achieved by mixing to form a paste, the paste is applied to the ceramic glass bonding surface, the solvent contained in the paste applied to the bonding surface evaporates, and then the ceramic glass on which the face is applied comes into contact. do.

In addition, when the ceramic glass to be bonded is mounted with a heating furnace and the temperature of the ceramic glass bonding surface becomes the melting temperature of the ceramic glass, pressure is applied in the bonding direction.

In addition, a thermoplastic resin is included in the paste, and the resin is burned and vaporized while the paste is heated in a heating furnace to reach the maximum temperature.

On the other hand, the surface roughness of the bonding surface is within 0.03 μm, and the surface flatness is within 0.02 mm.

In addition, the thickness of the paste applied to the bonding surface of the ceramic glass is 5 mm or less, and toluene is used as a solvent for the paste.

In the present invention, the bonded portion of the ceramic glass can be made stronger and stronger, and the bonded portion can be precisely bonded by preventing the occurrence of optical stains, unbonded portions, and surface devitrification, and the ceramic glass at an economical cost because no welding device is used. It is possible to provide a ceramic glass bonding method capable of increasing the size of the glass and completely burning the solvent and the resin contained in the paste, thereby eliminating the cause of the impurities.

1 is a view showing a method of bonding ceramic glass in the present invention.
2 is a diagram of an embodiment showing conditions in a process process.
3 shows a photograph of observing the bonding interface after etching the bonding portion.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. The configuration of the present invention and its effect will be clearly understood through the detailed description below.

In addition, detailed descriptions of known technical configurations may be omitted.

In the present invention, for uniform and effective bonding, a bonding method is performed by applying heat and maintaining a vacuum while a pair of ceramic glasses facing each other after applying the paste to the bonding portion at a constant pressure, It relates to a method of bonding ceramic glass that does not deform the ceramic glass and does not use a filler.

On the other hand, the ceramic glass applied in the present invention can be applied in various ways without limitation in thickness, length, or shape, and when the weight of the upper base material is 0.5 kg or more per unit area, bonding by its own weight is possible.

In addition, ceramic glass reflects not only infrared rays but also communication waves in the communication wavelength range. However, a bonded ceramic glass of a type that transmits communication waves and absorbs infrared rays is also required. In addition, ceramic glass is required not only to have high heat shielding properties, but also to have high visible light transmittance (Visible Transmittance). For example, it is preferable that the visible light transmittance is 80% or more. That is, it is required to increase the heat shielding property while maintaining the visible light transmittance high.

In general, ceramic glass based on alumino silica (Al2O3-SiO2) is a material that forms an essential part in processes such as semiconductors, displays, and mobile phone cover glasses due to its high chemical durability, thermal stability, and a coefficient of thermal expansion close to zero. It is a key entity in the industry.

In addition, there are also MgO-based and Li2O-based ceramic glasses, which are basic materials capable of manufacturing transparent ceramic glass used in semiconductor and display processes and opaque ceramic glass applicable to electronics and construction industries.

On the other hand, ceramic glass is an essential material for the front and rear industries as a jig for all processes of semiconductors and displays based on excellent properties such as high heat resistance, chemical resistance, and thermal safety at a commercial temperature of 700℃. Ceramic glass represented by Neoceram is thermally expandable. Since its coefficient is close to 0, it is translucent, has excellent airtightness and electrical insulation, it is applied to high-precision heat treatment and etch facilities for semiconductors and displays.

Therefore, there is a demand in the industry for a large or complex ceramic glass in which a bonding method that allows any type of ceramic glass to be stably bonded without deformation is required in the industry. Therefore, in the present invention, a ceramic glass that meets these needs To provide a method of bonding of

1 is a view showing a method of bonding ceramic glass in the present invention.

As shown in (A) of FIG. 1, a pair of ceramic glass 10 to which the paste 100 is applied on the bonding surface is positioned to face each other. In addition, a pair of ceramic glass 10 to which the paste 100 is applied may be positioned in the heating furnace 200.

At this time, at this time, the heating furnace 200 is a conventional sealed furnace capable of raising the temperature, and a vacuum pump may be connected to maintain a vacuum therein. Of course, a vacuum function is not required. And, since the heating furnace 200 uses a conventional furnace, its description will be omitted in the detailed description of the present invention.

In addition, when applying the paste 100, it may be applied to only one side of the bonding portion of the ceramic glass 10, or may be applied to both surfaces of the bonding portion of the ceramic glass 10.

As shown in Fig. 1(B), the ceramic glass 10 on which the paste 100 is applied is brought into contact with each other, and the heating furnace 200 is heated while applying pressure in the direction of the arrow shown in the drawing (abutting direction). To maintain a certain temperature.

In that case, as shown in FIG. 1C, the two ceramic glasses 10 are bonded like one ceramic glass 10.

Of course, the powder melted in the paste during the bonding process by pressure may be represented as the protrusion 11. That is, the powder melted in the paste may escape from the joint and become the protrusion 11.

In this case, when the protrusion 11 is polished, the bonded ceramic glass is completed as shown in (D) of FIG. 1.

--- Paste ingredients -----

(1) powder

The powder mixed in the paste of the present invention is a powder having the same components as the ceramic glass mother agent to be bonded.

For example, in order to bond a ceramic glass based on alumino silica (Al2O3-SiO2), a powder of ceramic glass based on alumino silica (Al2O3-SiO2) is used, and a ceramic glass based on MgO In order to bond the MgO-based ceramic glass powder, it can be said that the Li2O-based ceramic glass powder is used to bond the Li2O-based ceramic glass.

And, the diameter of the powder particles mixed in the paste can be manufactured in various sizes of 5 ㎛ to 30 ㎛.

(2) Paste Preparation First Example

6.25 parts by weight and 12.5 parts by weight of polyvinyl butyral binder B-76 (molecular weight 90,000 to 120,000; Kuraray Co., Ltd.) and B-98 (molecular weight 40,000 to 70,000), respectively, based on 100 parts by weight of ceramic glass powder ; Kuraray Co. Ltd.) was added.

In addition, 16.25 parts by weight of a plasticizer dioctyl phthalate (Samchun Pure Chemical Co. Ltd.) was added to 100 parts by weight of the slurry of the mixed powder. In addition, 100 parts by weight of toluene was further mixed as a solvent to prepare a slurry form.

The slurry was ball milled again for 24 hours, and gas was removed at a pressure of 160 torr for 15 minutes.

(3) Paste production second example

Based on the mass, 40 to 59% of ceramic glass powder and 40 to 59% of polyvinyl acetal, a thermoplastic resin, are mixed, and 1 to 2% of a phthalocyanine compound or a naphthalocyanine compound is added as an additive.

Toluene is added as a solvent, and toluene is added and mixed in a weight equivalent to 50% of the total weight of ceramic glass powder, thermoplastic resin, and additives.

After mixing the materials, the ball mill was again performed until sufficiently mixed, and gas was removed at a pressure of 160 torr for 15 minutes.

When the paste thus prepared is dried, the infrared reflecting layer has a property of having an infrared transmittance of 50% or less in at least one wavelength in the range of 780 to 2100 nm, and the bonding agent is made, and the infrared transmittance at a wavelength of 780 to 2100 nm is made. Also, the second resin layer has a characteristic higher than the infrared transmittance at a wavelength of 780 to 2100 nm.

(3) Paste production third example

"Ceramic glass powder 100 g, Trition X-100 3 cc, polyvinyl butyral 20 g, bibutylphthalate 9 cc, toluene 25 ± 10 cc, isopropanol 50 ± 200 cc" are mixed with each other and ball milled.

At this time, Trition X-100 is C ₈ H ₁₇ C ₈ H ₄ (OCH ₂ CH ₂ ) _n OH,

Then, the material was mixed with an ultrasonic disperser and a 3-zone mill to prepare a paste. When the viscosity of the paste does not fall within the range of 2000pcs/2000rpm or 50000pcs/5000rpm, it was left to volatilize or the amount of toluene and iso-propanol solution was added or subtracted to adjust the rheological properties. The voids contained between the fine particles were repeatedly degassed in a vacuum chamber.

------- fair ---------

Step 1: the paste application step,

One of the pastes made by the above three methods is applied to the bonding surface of the ceramic glass 10. The thickness to which the paste is applied is within 5 mm, and the most optimal is about 2 to 3 mm.

Step 2: paste drying step

As shown in (A) of FIG. 1, the ceramic glass 10 to be bonded to which the paste 100 is applied is mounted in the heating furnace 200. When heat is applied to the other heating furnace, toluene, which is a solvent, is evaporated in the paste, and the paste is dried, and impurities such as solvent are not left even after bonding by this drying process.

At this time, the temperature is gradually increased.

Step 3: step of butting ceramic glass

A pair of ceramic glass 10 to be bonded is brought into contact with each other and maintained until a certain temperature is reached. In this case, the predetermined temperature is increased only from 50° C. to 100° C. from a temperature at which the ceramic glass is not completely melted, that is, a phase transition temperature from solid to liquid. Therefore, in the process of the present invention, the constant temperature is about 1500 to 1550°C (when it is assumed that 1600°C is the temperature at which the ceramic glass is melted). However, since the melting temperature varies depending on the ceramic glass used, the predetermined temperature may vary depending on the ceramic glass.

Step 4: pressing and bonding step

When the temperature of the heating furnace 200 reaches the constant temperature of 1500 to 1550 °C, the ceramic glass 10 is raised to the phase transition temperature of 1600 °C through the additional heater 210 only at the junction, and Fig. 1(B) The pressure is applied in the direction of the arrow indicated in. At this time, the pressure is preferably a pressure that is not as strong as 0.2 to 0.4 kg/cm 2,

That is, the temperature is raised to the phase transition temperature of the ceramic glass through the additional heater 210, and the time to pressurize is within 1 minute.

Step 5: polishing step

When the above step 4 is achieved, the bonding is completed, but due to the pressing process in which pressure is applied in the direction of the arrow indicated in FIG. 1B, the ceramic glass powder (powder in a phase transition state) is pushed out of the bonding portion of the ceramic glass. Comes out.

That is, the protrusion 11 in the bonding process exists, and when the protrusion 11 is polished, the ceramic glass 10 having the bonding completed is made as shown in (D) of FIG. 1.

Advantages of the ceramic glass bonding method of the present invention are as follows.

Due to the drying of the paste in the second step, the resin is completely removed from the paste, so that no resin impurities are present.

Since the temperature rises to a maximum of 1500 ~ 1550 ℃ through the heating furnace 200, the resin mixed with the ceramic powder to make a paste is also burned and evaporated to disappear in the paste.

By instantaneous heating of the additional heater 200 and pressing in the direction of the bonding surface, the resin and the solvent are evaporated and the pores in the paste are filled with ceramic glass powder. As a result, when the process goes through, the solvent and the resin disappear in the paste, only ceramic powder of the same material as the ceramic glass base material exists, and the ceramic powder is also melted to form a ceramic glass, thereby forming a complete assembly.

That is, by instantaneous heating of the additional heater 200 and pressing in the direction of the bonding surface, the ceramic powder is also melted and then cured, thereby becoming integral with the ceramic glass.

In conclusion, the powder in the paste is made of the same material as the ceramic glass to be bonded, and there is no difference in physical properties at the interface of the ceramic glass even after bonding.

On the other hand, by giving a vacuum function, the resin existing in the paste is burned so that the gaseous material is exhausted, thereby minimizing impurities.

2 is a diagram of an embodiment showing conditions in a process process.

As shown in the figure, the maximum temperature reaches 1500° C. at a rate of 5° C./min in a vacuum state, and is maintained at the maximum temperature for 5 hours. And. After the 5 hour holding time is over, natural cooling is performed in a vacuum.

Then, when the temperature of the heating furnace reaches about 200°C, the solvent is completely evaporated and the paste is sufficiently dried, so that the ceramic glass to be bonded is brought into contact with each other. That is, when it is first mounted on the furnace, the ceramic glass is mounted without contacting each other, and when the solvent is sufficiently evaporated, the ceramic glass is brought into contact with each other.

On the other hand, while the maximum temperature is maintained for 5 hours, the additional heater 210 is heated at the midpoint of the maximum temperature, that is, 2 hours and 30 minutes after the start of the maximum temperature (7 hours and 30 minutes at the beginning of the process), Heat the joint part to 1600 ℃, which is the phase transition temperature, and keep it for 30 seconds to 1 minute. During the phase transition temperature period, a pressure of 0.2 to 0.4 ㎏/㎠ is applied to the joint surface.

- Preparation of glass ceramic and mounting process in the furnace ---

The cross-section of the ceramic glass 10 to be bonded is polished to prepare a bonded base material (ceramic glass to be bonded), and pickled to remove impurities from the cross-section of the ceramic glass 10. Only when impurities are removed, bonding is effectively performed and surface devitrification does not occur.

Then, it is checked whether the tilt of the ceramic glass to be bonded is precisely horizontal. Then, after loading the base material (a ceramic glass that has undergone a process of polishing a cross section and removing impurities), the level is checked. That is, even after mounting the base material, it is checked whether it is precisely leveled in order to apply a uniform pressure.

Then, to apply pressure, a graphite punch is charged and then unloading is performed.

The bonding temperature is 1500°C or 1550°C, but the actual bonding temperature is 1600°C, which is the melting temperature, the vacuum degree is from 1.00E-03torr to 1.00E-05torr, the surface roughness of the bonding surface is within 0.03 μm, and the surface flatness is 0.02㎜. Is within.

In addition, in the bonding process, when the process temperature is between 1650°C and 1750°C, the process time can be shortened, but the mother agent may be deformed and there may be no reproducibility. However, when the process temperature is 1000°C to 1300°C, the process time is long, but there is no deformation and a relatively high pressure is required.

On the other hand, in the brazing process using filler material, the physical properties and properties of the mother agent are different due to the use of filler material, so it is not a recommended method.

As a result of bonding the ceramic glass with the present invention, devitrification occurred on the surface of the base material (no devitrification inside the bonding), but there was no devitrification inside the bonding, and the devitrification was confirmed as an impurity inside the bonding surface (presumed to be graphite).

In addition, there was about 0.25% of weight loss estimated due to the influence on the surface deflection, and the dimensional deformation was confirmed to be within the measurement error at a maximum of 0.02 mm.

3 shows a photograph of observing the bonding interface after etching the bonding portion.

When looking at the photograph of FIG. 3 showing the ceramic glass bonded by the method of the present invention, it can be seen that the bonded portion also shows a uniform shape.

10 ceramic glass 100 paste
200: heating furnace 210: additional heater

Claims (6)

A paste coated on the bonding surface of the ceramic glass is provided, and the paste contains ceramic glass powder, the ceramic glass powder is the same material as the ceramic glass to be bonded, and a resin, a solvent, and the powder of the ceramic glass are mixed to form a paste. Is made, and the paste is applied to the ceramic glass bonding surface,
Ceramic glass bonding method using a paste, characterized in that after the solvent contained in the paste applied to the bonding surface is evaporated, the ceramic glass on which the face is applied is brought into contact with each other. The method of claim 1,
A ceramic glass bonding method using a paste, characterized in that when the ceramic glass to be bonded is mounted with a heating furnace and the temperature of the ceramic glass bonding surface becomes the melting temperature of the ceramic glass, pressure is applied in the bonding direction. The method of claim 1,
Ceramic glass bonding method using a paste, characterized in that the paste contains a thermoplastic resin and is heated in a heating furnace to reach the maximum temperature while the resin is burned and vaporized. The method of claim 1,
Ceramic glass bonding method using a paste, characterized in that the surface roughness of the bonding surface is within 0.03 µm and the surface flatness is within 0.02 mm. The method of claim 1,
Ceramic glass bonding method using a paste, characterized in that the thickness of the paste applied to the bonding surface of the ceramic glass is 5 mm or less. The method of claim 1,
Ceramic glass bonding method using a paste, characterized in that toluene is used as a solvent for the paste.

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