WO2018147702A1 - Glass coating structure and method for forming same - Google Patents

Abstract

The present invention relates to a glass coating structure and a method for forming the same. A technical problem to be solved is to provide a glass coating structure having high light transmittance without grain boundary and a method of forming the same, by coating glass powder on a base material by a vacuum injection method at room temperature and then performing a heat treatment process. To this end, disclosed are a glass coating structure comprising: a base material; and a transparent coating layer without grain boundary formed by heat-treating an opaque coating layer with a grain boundary formed by mechanical impact of glass powder on the base material, and a method of forming the same.

Description

Glass coated structure and method of forming the same

The present invention relates to a glass coating structure and a method of forming the same.

At present, there is an increasing demand for the formation of a coating layer using a ceramic material in order to express characteristics such as chemical resistance, abrasion resistance, and water repellency in various industrial fields. In the process of forming a ceramic coating layer, a thermal spray coating process, a thin film process such as chemical vapor deposition (CVD) or physical vapor deposition (PVD), and a solution-based solution process are used.

However, the coating layer formed by such a conventional coating process has a grain boundary in most cases, the material properties inherent in the coating layer is lowered, and there is a problem of making the base material to be coated opaque.

The present invention is to overcome the above-mentioned conventional problems, an object of the present invention is to coat the glass powder on the base material by the vacuum injection method at room temperature, and then performing a heat treatment process, glass coating having a high light transmittance without grain boundary It is to provide a structure and a method of forming the same.

In addition, an object of the present invention is to include various plasma materials as glass powder, thereby forming a glass coating structure having excellent plasma resistance and corrosion resistance on the surface of a semiconductor or display processing apparatus on which plasma etching is performed and its formation To provide a method.

Glass coating structure according to the present invention to achieve the above object is a base material; And a transparent coating layer having no grain boundary formed by heat-treating an opaque coating layer having grain boundaries formed by mechanical impact of glass powder on the base material.

The base material is glass, tempered glass, quartz glass, quartz, epoxy, alumina (Al ₂ O ₃ ), zirconia (ZrO ₂ ), zinc oxide (ZnO), aluminum nitride (AlN), aluminum (Al), copper (Cu) , Tungsten (W), stainless steel (SUS), PC (Polycarbonate), PET (Polyethylene terephthalate), PI (Polyamide), PMMA (Polymethyl Methacrylat), PBT (Polybutylene terephthalate), PU (Polyurethane), PVA (Polyvinyl alcohol) Or polyvinyl butyral (PVB).

The glass powder is Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ O, ZnO-B ₂ O ₃ -P ₂ O ₅ , PbO- It may be at least one selected from B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO and PbO-SiO ₂ -B ₂ O ₃ .

The glass powder may comprise a plasma resistant material.

The plasma material is Al ₂ O ₃ , TiO ₂ , AlN, ZrO ₂ , CaO, SiC, SiO ₂ , Si ₃ N ₄ , B ₂ C, BN, TiN, Y ₂ O ₃ , Y ₂ O ₃ -Al _{2 O 3, YOF, Y 5 O} 4 F 7, Y 6 O 5 F 8, Y 7 O 6 F 9, Y 17 O 14 F 23, YF 3, YCl 3, YBr 3, LaF 3, LaCl 3, LaBr 3 , YOCl, YOBr, YOFCl, YOBrCl, rare earth series (element series from 57 to 71 including Y and Sc) oxide, rare earth series (element series from 57 to 71 including Y and Sc) fluoride , Rare earth series (element series from 57 to 71 including Y and Sc) chloride, MgF ₃ , AlF ₃ , CaF ₃ , BaF ₃ , YAG (Y ₃ Al ₅ O ₁₂ ) and Yttria stabilized Zirconia (YSG) It may be at least one selected from.

The transparent coating layer may be an X-ray peak does not appear when X-Ray Diffrectometer (XRD) measurement.

Glass coating structure according to the present invention to achieve the above object is a base material; And the glass powder on the base material may include a transparent coating layer without a grain boundary formed by mechanical impact.

In order to achieve the above object, a method of manufacturing a glass coating structure according to the present invention includes providing a base material; Mechanically impacting the glass powder on the base material to form an opaque coating layer having grain boundaries; And annealing the opaque coating layer having the grain boundary to amorphize the transparent coating layer without the grain boundary.

The glass powder may have a particle size range of 1 nm to 50 μm.

Mechanically impacting the glass powder to form an opaque coating layer having grain boundaries may be made by impacting the base material at a speed of 100 m / s to 1500 m / s by making the glass powder in an aerosol state.

Amorphizing the transparent coating layer without grain boundary by heat treatment may include laser beam heat treatment apparatus, rapid thermal annealing system, electric heat treatment apparatus, induction heating apparatus, steam heat treatment apparatus, plasma heat treatment apparatus, and flash lamp heat treatment apparatus. It may be carried out by one or two selected.

The light transmittance of the opaque coating layer may be 0.1% to 60%, and the light transmittance of the transparent coating layer may be 30% to 95%.

The present invention provides a glass coating structure having a high light transmittance without grain boundaries and a method of forming the same by coating the glass powder on a base material by a vacuum injection method at room temperature, and then performing a heat treatment process.

That is, the present invention forms a opaque coating layer having a plurality of grains and grain boundaries by making the glass powder in an aerosol state and then impacting the base material by a normal temperature vacuum injection method, and then heat treating or annealing the opaque coating layer in various ways, The opaque coating layer having grains and grain boundaries of is made to be amorphous with a transparent coating layer having no grains and grain boundaries.

In this way, the present invention is because the coating layer does not have grain and grain boundaries, the coating layer expresses the inherent characteristics of materials such as bulk, and the coating layer has a high light transmittance, thereby realizing the color of the base material.

In addition, the present invention further comprises a variety of plasma materials as the glass powder, the glass coating structure having a plasma resistance excellent in corrosion resistance and plasma etching characteristics on the surface of the semiconductor or display processing apparatus is subjected to plasma etching and a method of forming the same To provide. In one embodiment, the present invention provides a film of rare earth-based (element-based atomic number 57 to 71, including Y and Sc) oxides, fluorides, or chlorides as a corrosion resistant coating layer of a semiconductor or display processing apparatus, thereby improving plasma characteristics. It provides a coating structure and a method of forming the same.

1 is a flowchart illustrating a method of forming a glass coating structure according to an embodiment of the present invention.

2A and 2B are schematic views illustrating a room temperature spraying apparatus and a heat treatment apparatus, respectively, for forming a glass coating structure according to an embodiment of the present invention.

3A to 3C are schematic views illustrating a method of forming a glass coating structure according to an embodiment of the present invention.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. The embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art, and the following examples can be modified in various other forms, and the scope of the present invention is It is not limited to an Example. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the inventive concept to those skilled in the art.

In addition, in the following drawings, the thickness or size of each layer is exaggerated for convenience and clarity of description, the same reference numerals in the drawings refer to the same elements. As used herein, the term "and / or" includes any and all combinations of one or more of the listed items.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a", "an" and "the" may include the plural forms as well, unless the context clearly indicates otherwise. Also, as used herein, "comprise" and / or "comprising" refers to the presence of the mentioned shapes, numbers, steps, actions, members, elements and / or groups. It is not intended to exclude the presence or the addition of one or more other shapes, numbers, acts, members, elements and / or groups.

Although the terms first, second, etc. are used herein to describe various members, parts, regions, layers, and / or parts, these members, parts, regions, layers, and / or parts are defined by these terms. It is obvious that not. These terms are only used to distinguish one member, part, region, layer or portion from another region, layer or portion. Thus, the first member, component, region, layer or portion described below may refer to the second member, component, region, layer or portion without departing from the teachings of the present invention.

1 is a flowchart illustrating a method of forming a glass coating structure according to an embodiment of the present invention.

As shown in FIG. 1, the method of forming the glass coating structure according to the embodiment of the present invention does not have a base material providing step S1, an opaque coating layer forming step having grain boundaries S2, and a grain boundary (that is, having no grain boundaries). Amorphous transparent coating layer conversion step (S3) is included.

In the base material providing step S1, a base material having a predetermined thickness and a predetermined width is provided. Here, the base material may be, for example, but not limited to, a flat plate form, or may be in various forms in two or three dimensions. In addition, a base material is, for example, but not limited to, glass, tempered glass, quartz glass, quartz, epoxy, alumina (Al ₂ O ₃ ), zirconia (ZrO ₂ ), zinc oxide (ZnO), aluminum nitride (AlN). ), Aluminum (Al), Copper (Cu), Tungsten (W), Stainless Steel (SUS), PC (Polycarbonate), PET (Polyethylene terephthalate), PI (Polyamide), PMMA (Polymethyl Methacrylat), PBT (Polybutylene terephthalate) It may be at least one selected from polyurethane (PU), polyvinyl alcohol (PVA), polyvinyl butyral (PVB), and equivalents thereof.

In the step of forming an opaque coating layer having grain boundaries (S2), the glass powder is mechanically impacted on the base material to form an opaque coating layer having grains and grain boundaries.

Here, the step of forming an opaque coating layer having grains and grain boundaries may be achieved by impacting the base metal at a speed of approximately 100 m / s to 1500 m / s in an aerosol glass powder. That is, the present invention can form an opaque coating layer having a grain boundary by impacting the glass substrate in the aerosol state by the normal temperature vacuum injection method.

Glass powders include, but are not limited to, Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ O, ZnO-B ₂ O _{At least one selected from 3} -P ₂ O ₅ , PbO-B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ , and equivalents thereof.

In addition, the glass powder may further include a plasma resistant material. Plasma-resistant materials are, for example, but not limited to Al ₂ O ₃ , TiO ₂ , AlN, ZrO ₂ , CaO, SiC, SiO ₂ , Si ₃ N ₄ , B ₂ C, BN, TiN, Y ₂ O ₃ , Y ₂ O ₃ -Al ₂ O ₃ , YOF, Y ₅ O ₄ F ₇ , Y ₆ O ₅ F ₈ , Y ₇ O ₆ F ₉ , Y ₁₇ O ₁₄ F ₂₃ , YF ₃ , YCl ₃ , YBr ₃ , LaF ₃ , LaCl ₃ , LaBr ₃ , YOCl, YOBr, YOFCl, YOBrCl, rare earth series (element series from atomic number 57 to 71 including Y and Sc) oxide, rare earth series (atomic number including Y and Sc) Elemental compounds from 57 to 71) fluoride, rare earths (elements from 57 to 71 including Y and Sc) chloride, MgF ₃ , AlF ₃ , CaF ₃ , BaF ₃ , YAG (Y ₃ Al ₅ O ₁₂ ), at least one selected from Yttria stabilized Zirconia (YSG) and equivalents thereof.

Here, the above-mentioned plasma-resistant material is used alone or the above-mentioned Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ O, ZnO- Mixed with one or two selected from B ₂ O ₃ -P ₂ O ₅ , PbO-B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO and PbO-SiO ₂ -B ₂ O ₃ Can be used.

As such, by including various plasma materials as the glass powder, a glass coating structure having plasma characteristics excellent in corrosion resistance and plasma etching characteristics on a surface of a semiconductor or display processing apparatus on which plasma etching is performed, and a method of forming the same may be provided. Can be. In one embodiment, the present invention provides a coating having improved plasma resistance by forming a rare earth (oxide based element number from 57 to 71 including Y and Sc) oxide, fluoride or chloride coating layers as a corrosion resistant coating layer of a semiconductor or display processing apparatus. It provides a structure and a method of forming the same.

In addition, the glass powder may have a particle size range of approximately 1 nm to 50 μm. When the particle size range of the glass powder is less than about 1 nm, a substantially opaque coating layer may not be formed. In addition, when the particle size range of the glass powder exceeds approximately 50 μm, the base material may be etched, and the porosity of the opaque layer may be too large.

On the other hand, by this process, the light transmittance of the opaque coating layer may be approximately 0.1% to 60%. Such light transmittance is considered to be a phenomenon due to the formation of many pores inside the opaque coating layer.

In the step of converting the transparent coating layer having no grain boundary (S3), the opaque coating layer having grains and grain boundaries is heat-treated to form an amorphous transparent coating layer having no grains or grain boundaries. That is, the opaque coating layer having grains and grain boundaries is converted to an amorphous transparent coating layer having no grains or grain boundaries.

Here, the transparent coating layer shows an amorphous property when measured by using X-Ray Diffrectometer (XRD) and / or Transmission Electro Microscopy (TEM).

For example, the measuring method using XRD is a method of measuring the intensity of X-rays reflected from the transparent coating layer by radiating X-rays (X-ray) to the transparent coating layer. Specifically, when radiating X-rays from X-ray sources and irradiating the transparent coating layer to be measured at various angles, some of the radiated X-rays are transmitted and some are reflected. The intensity of the double reflected X-rays may be measured to determine whether the transparent coating layer is amorphous. When the X-rays irradiated on the transparent coating layer are reflected from any crystal plane, the intensity of the reflected X-rays is reinforced or canceled according to Bragg's law. The reflected X-rays can be analyzed to determine the direction of the crystal plane. However, when the X-rays encounter an amorphous portion, the reflected X-rays do not show a peak or show a peak in a broad range different from that reflected by meeting the crystal plane (i.e., no characteristic peaks appear at all). Moreover, the method of using a TEM is a method of cutting a transparent coating layer and observing the image of the cross section, Even with this method, a transparent coating layer is considered amorphous.

Here, the heat treatment is, for example, but not limited to one selected from a laser beam heat treatment apparatus, a rapid heat treatment apparatus, an electric heat treatment apparatus, an induction heating apparatus, a steam heat treatment apparatus, a plasma heat treatment apparatus and / or a flash lamp heat treatment apparatus, or It can be performed by two species.

By this heat treatment, a transparent coating layer is obtained which is substantially free of grain or grain boundaries and has little air porosity (less than about 0.01%). By way of example, but not limitation, the light transmittance of the transparent coating layer may range from approximately 30% to 95%.

In this way, the present invention is to provide a glass coating structure having a high light transmittance without grain boundary by coating the glass powder on the base material by the vacuum injection method at room temperature, and then performing a heat treatment process, and a method of forming the same. In particular, in the present invention, since the opaque coating layer is formed by the vacuum injection at room temperature, the thickness control is easy, and the internal structure of the opaque coating layer and / or the transparent coating layer can be controlled as desired by controlling the particle size range and heat treatment temperature of the glass powder. It becomes possible.

2A and 2B are schematic views illustrating a room temperature spraying apparatus and a heat treatment apparatus, respectively, for forming a glass coating structure according to an embodiment of the present invention.

As shown in FIG. 2A, the room temperature injection apparatus 100 transfers the glass powder from the transport gas supply unit 110, a powder supply unit 120 storing and supplying glass powder, and a powder supply unit 120. Transfer tube 122 to transfer at a high speed by using, a nozzle 132 for coating / laminating or spraying the glass powder from the transfer tube 122 to the base material 310, the glass powder from the nozzle 132 By mechanically impinging and crushing the surface of the 310, it may include a process chamber 130 to form an opaque coating layer having a certain thickness, grains and grain boundaries.

A process of forming an opaque coating layer having grains and grain boundaries on the base material 310 by the room temperature spraying device 100 will be described.

First, the transport gas stored in the transport gas supply unit 110 may be, for example, but not limited to, one or two mixtures selected from the group consisting of oxygen, helium, nitrogen, argon, carbon dioxide, hydrogen, and equivalents thereof. Can be. The transfer gas is directly supplied from the transfer gas supply unit 110 to the powder supply unit 120 through the pipe 111, and the flow rate and pressure may be adjusted by the flow controller 150.

The powder supply unit 120 stores and supplies a large amount of glass powder, wherein the particle diameter range of the glass powder is about 1 nm to 50 μm, preferably about 1 nm to 30 μm, more preferably about 1 nm to 10 μm. When the thickness is about 1 nm to 100 nm, and more preferably, about 1 nm to 100 nm, an opaque coating layer having a relatively low porosity (porosity or porosity) (relatively high density) and easy control of the glass powder can be obtained.

When the particle size range of the glass powder is smaller than about 1 nm, an opaque coating layer may not be formed, and due to the aggregation phenomenon during storage and feeding of the glass powder, the powder may be smaller than 1 nm when spraying, colliding, crushing and / or grinding The green compact, which is a form in which particles are agglomerated, is not only easily formed, but also has a disadvantage in that a large area opaque coating layer is difficult to form.

In addition, when the particle size range of the glass powder is greater than about 50 μm, sand blasting may be easily generated to shave the base material during the injection, impact crushing, and / or pulverization of the powder.

Moreover, the above-mentioned glass powder may be in the form of granules that maintain the state of aggregation with each other. In one example, the glass powder may agglomerate and become approximately 10 to 200 times larger than the powder size, which may be redried to obtain glass granules. By this granulation, the glass granules become a porous structure, and thus the formation of an opaque coating layer can be made easier. Such glass granules may have a particle size ranging from approximately 10 nm to 50 μm.

The process chamber 130 maintains a vacuum while forming the opaque coating layer, and may be connected to the vacuum unit 140 for this purpose. More specifically, the pressure of the process chamber 130 by driving the vacuum unit 140 is approximately 1 Pascal to 800 Pascals, and the pressure of the glass powder conveyed by the high speed feed tube 122 is approximately 1500 Pascals to 2000 It may be Pascal. However, in any case, the pressure of the high speed transfer pipe 122 should be higher than that of the process chamber 130.

In addition, the internal temperature range of the process chamber 130 is maintained at room temperature, that is, approximately 0 ° C. to 30 ° C., and thus, there may be no member for increasing or decreasing the internal temperature of the process chamber 130 separately. That is, the conveying gas and / or the base material can be maintained at a temperature of 0 ° C to 30 ° C without being heated separately. Therefore, in the present invention, the base material is not thermally impacted.

However, in some cases, in order to improve deposition efficiency and density of the opaque coating layer, the transport gas or / and the base material may be heated to a temperature of approximately 30 ° C to 1000 ° C. That is, the transfer gas in the transfer gas supply unit 110 may be heated by a separate not shown heater, or the base material 310 in the process chamber 130 may be heated by a separate not shown heater. The stress applied to the glass powder in the formation of the opaque coating layer by heating of the carrier gas and / or the base material is reduced, thereby obtaining a small porosity and a dense opaque coating layer. Here, when the transport gas or / and the base material is higher than the temperature of approximately 1000 ℃, the glass powder melts causing a sharp phase transition, thereby increasing the porosity of the opaque coating layer (lower filling) and the internal structure of the opaque coating layer It may become unstable.

However, the present invention is not limited to this temperature range, and the internal temperature range of the transfer gas, the base material and / or the process chamber may be adjusted between 0 ° C and 1000 ° C, depending on the characteristics of the base material on which the opaque coating layer is to be formed. For example, a process temperature of approximately 0 ° C. to 30 ° C. may be provided to coat a window of the display device, and a process temperature of approximately 0 ° C. to 1000 ° C. may be provided to coat a semiconductor / display processing equipment. .

Meanwhile, the pressure difference between the process chamber 130 and the high speed transfer pipe 122 (or the transfer gas supply unit 110 or the powder supply unit 120) may be approximately 1.5 times to 2000 times. If the pressure difference is less than approximately 1.5 times, the high speed conveyance of the powder may be difficult, and if the pressure difference is greater than approximately 2000 times, the surface of the base material may be excessively etched by the powder.

According to the pressure difference between the process chamber 130 and the transfer tube 122, the powder from the powder supply unit 120 is sprayed through the transfer tube 122 and simultaneously transferred to the process chamber 130 at high speed.

In addition, the process chamber 130 is provided with a nozzle 132 connected to the transfer pipe 122, by impinging the glass powder on the surface of the base material 310 at a speed of approximately 100 to 1500m / s, to form an opaque coating layer do. That is, the glass powder through the nozzle 132 is crushed by the kinetic energy obtained during the transfer and the collision energy generated during the high-speed collision to form an opaque coating layer of a predetermined thickness on the surface of the base material 310.

Here, the opaque coating layer may have nano or micro pores therein and may also be stacked by mechanical impact, and thus, a plurality of grains and grain boundaries may be observed when viewed in the normal direction or the planar direction of the base material.

Since the glass powder is sprayed through the nozzle and crushed while colliding with the base material 310 to form an opaque coating layer, the particle size of the particles forming the opaque coating layer has a smaller size than the particle size of the glass powder for forming the opaque coating layer. .

The base material 310 may be made of at least one selected from ceramic, glass, tempered glass, quartz glass, quartz, plastic, metal, epoxy, and equivalents thereof. That is, the base material 310 may be a single layer base material made of one material, or a multilayer base material in which two or more materials are stacked. For example, the base material 310 may be a single layer base material made of tempered glass or a multilayer base material in which ceramics are laminated on the glass. In particular, the base material 310 may have a surface roughness of 0.1 μm or more, or an organic material or a plastic material.

The ceramic may be at least one of alumina (Al ₂ O ₃ ), zirconia (ZrO ₂ ), zinc oxide (ZnO), and aluminum nitride (AlN). The metal may be any one of aluminum (Al), copper (Cu), tungsten (W), and stainless steel (SUS). Plastics include PC (Polycarbonate), PET (Polyethylene terephthalate), PI (Polyamide), PMMA (Polymethyl Methacrylat), PBT (Polybutylene terephthalate), PU (Polyurethane), PVA (Polyvinyl alcohol), PVB (Polyvinyl butyral) and It may be any one of the equivalents.

Glass powder for forming the opaque coating layer, for example, but not limited to, Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ At least selected from O, ZnO-B ₂ O ₃ -P ₂ O ₅ , PbO-B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O _3, and their equivalents It may be one kind.

In addition, the glass powder may further include a plasma resistant material. Plasma-resistant materials are, for example, but not limited to Al ₂ O ₃ , TiO ₂ , AlN, ZrO ₂ , CaO, SiC, SiO ₂ , Si ₃ N ₄ , B ₂ C, BN, TiN, Y ₂ O ₃ , Y ₂ O ₃ -Al ₂ O ₃ , YOF, Y ₅ O ₄ F ₇ , Y ₆ O ₅ F ₈ , Y ₇ O ₆ F ₉ , Y ₁₇ O ₁₄ F ₂₃ , YF ₃ , YCl ₃ , YBr ₃ , LaF ₃ , LaCl ₃ , LaBr ₃ , YOCl, YOBr, YOFCl, YOBrCl, rare earth series (element series from atomic number 57 to 71 including Y and Sc) oxide, rare earth series (atomic number including Y and Sc) Elemental compounds from 57 to 71) fluoride, rare earths (elements from 57 to 71 including Y and Sc) chloride, MgF ₃ , AlF ₃ , CaF ₃ , BaF ₃ , YAG (Y ₃ Al ₅ O ₁₂ ), at least one selected from Yttria stabilized Zirconia (YSG) and equivalents thereof. This plasma resistant material may be used in combination with the material of the glass powder described above.

Meanwhile, as illustrated in FIG. 2B, the heat treatment apparatus 200 may include a process chamber 210, a heater 220 located inside the process chamber 210, and at least one flash located above the heater 220. The lamp 230 may include a reflector 240 positioned above the flash lamp 230.

Here, the heat treatment apparatus 200 is only an example for understanding the present invention, and the present invention should not be limited to such a heat treatment apparatus. In addition, the heater 220 may be omitted in some cases.

As described above, the base material 310 having an opaque layer (not shown) having grain boundaries may be positioned on the heater 220 of the chamber 210, and may be preheated to a predetermined temperature. Subsequently, the flash lamp 230 operates to transmit high energy only to the opaque layer formed on the base material 310. For example, the opaque layer may be heat treated or annealed by flash lamp 230 after preheating for approximately 0.1 to 10 minutes at each temperature between approximately 0 ° C. and 400 ° C. In addition, the preheating temperature can be increased to approximately 1500 ° C. when the energy density of the flash lamp being scanned is low or the power is low. In addition, the preheating may be performed in an inert nitrogen (N ₂ ) atmosphere.

The flash lamp 230 may be irradiated at least once in a shot. When the number of times of irradiation of the flash lamp 230 is one or more times, the conversion efficiency of the opaque layer having grain boundaries to the transparent coating layer having no grain boundaries is increased. The one shot irradiated from the flash lamp 230 preferably has an energy density of approximately 1 to 50 J / cm 2. If the energy density of the one shot irradiated from the flash lamp 230 is too low, the conversion efficiency (opacity-> transparent) becomes too low. In addition, if the energy density of the light irradiated from the flash lamp 230 is too high, the opaque coating layer may only partially melt. In addition, the one-shot shot irradiated from the flash lamp 230 may have a full width at half maximum of about 1 msec to 20 msec when applied as a sine wave.

One shot irradiated from such a flash lamp may have a pulse width of approximately 1 ms to 50 msec regardless of the waveform. One shot irradiated from the flash lamp may have a pulse width of approximately 1 msec. The full width at half maximum or pulse width of a single shot affects the conversion efficiency from the opaque coating layer to the transparent coating layer. If it is too short, the conversion efficiency is low, and if it is too long, the characteristics of the transparent coating layer may be affected.

In one example, heat treatment / annealing with such a flash lamp resulted in a light transmittance of approximately 0.1% to 60% of the opaque coating layer and a light transmission of 30% to 95% of the transparent coating layer.

In other words, the opaque coating layer is converted into a transparent coating layer having no grains or grain boundaries, so that the transparent coating layer not only has excellent light transmittance, but also has excellent magnetic properties, corrosion resistance, wear resistance, high strength, hardness and toughness, and high specific resistance. .

3A to 3C are schematic views illustrating a method of forming a glass coating structure according to an embodiment of the present invention.

As shown in FIG. 3A, for example, but not by way of limitation, a substrate 310 in the form of a substantially flat plate is provided. Subsequently, as shown in FIG. 3B, the glass powder in an aerosol state is sprayed onto the base material 310 through a room temperature spraying process, thereby forming an opaque coating layer 320 having grain boundaries. Finally, as shown in FIG. 3C, the heat treatment process is performed to convert the opaque coating layer 320 having the grain boundary into the transparent coating layer 330 having no grain boundary.

As described above, the present invention provides a glass coating structure 300 having a high light transmittance without grain boundary and a method of forming the same by coating the glass powder on a base material by a normal temperature vacuum spraying method, and then performing a heat treatment process.

What has been described above is just one embodiment for carrying out the glass coating structure and the method for forming the same according to the present invention, the present invention is not limited to the above-described embodiment, as claimed in the following claims Without departing from the gist of the invention, anyone of ordinary skill in the art to which the present invention will have the technical spirit of the present invention to the extent that various modifications can be made.

Claims (17)

1. Base material; And

   The glass coating structure, characterized in that the glass coating on the base material comprises a transparent coating layer without grain boundary formed by the heat treatment of the opaque coating layer having a grain boundary formed by mechanical impact.
2. The method of claim 1,

   The base material is glass, tempered glass, quartz glass, quartz, epoxy, alumina (Al ₂ O ₃ ), zirconia (ZrO ₂ ), zinc oxide (ZnO), aluminum nitride (AlN), aluminum (Al), copper (Cu) , Tungsten (W), stainless steel (SUS), PC (Polycarbonate), PET (Polyethylene terephthalate), PI (Polyamide), PMMA (Polymethyl Methacrylat), PBT (Polybutylene terephthalate), PU (Polyurethane), PVA (Polyvinyl alcohol) Or glass-coated structure comprising a PVB (Polyvinyl butyral).
3. The method of claim 1,

   The glass powder is Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ O, ZnO-B ₂ O ₃ -P ₂ O ₅ , PbO- Glass coating structure, characterized in that at least one selected from B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO and PbO-SiO ₂ -B ₂ O ₃ .
4. The method of claim 1,

   The glass powder structure, characterized in that the glass containing a plasma material.
5. The method of claim 4, wherein

   The plasma material is Al ₂ O ₃ , TiO ₂ , AlN, ZrO ₂ , CaO, SiC, SiO ₂ , Si ₃ N ₄ , B ₂ C, BN, TiN, Y ₂ O ₃ , Y ₂ O ₃ -Al _{2 O 3, YOF, Y 5 O} 4 F 7, Y 6 O 5 F 8, Y 7 O 6 F 9, Y 17 O 14 F 23, YF 3, YCl 3, YBr 3, LaF 3, LaCl 3, LaBr 3 , YOCl, YOBr, YOFCl, YOBrCl, rare earth series (element series from 57 to 71 including Y and Sc) oxide, rare earth series (element series from 57 to 71 including Y and Sc) fluoride , Rare earth series (element series from 57 to 71 including Y and Sc) chloride, MgF ₃ , AlF ₃ , CaF ₃ , BaF ₃ , YAG (Y ₃ Al ₅ O ₁₂ ) and Yttria stabilized Zirconia (YSG) Glass coating structure, characterized in that at least one selected from.
6. The method of claim 1,

   The transparent coating layer is a glass coating structure, characterized in that the X-ray peak does not appear when measured by XRD (X-Ray Diffrectometer).
7. Base material; And

   The glass coating structure, characterized in that the glass powder on the base material comprises a transparent coating layer without grain boundary formed by mechanical impact.
8. Providing a base material;

   Mechanically impacting the glass powder on the base material to form an opaque coating layer having grain boundaries; And

   And heat-treating the opaque coating layer having the grain boundary to amorphize the transparent coating layer without grain boundary.
9. The method of claim 8,

   The glass powder is a method of forming a glass coating structure, characterized in that having a particle size range of 1 nm to 50 ㎛.
10. The method of claim 8,

    Mechanically impacting the glass powder to form an opaque coating layer having grain boundaries, the glass powder is made into an aerosol state by impacting the base material at a speed of 100 m / s to 1500 m / s. Method of forming the coating structure.
11. The method of claim 8,

    Amorphizing the transparent coating layer without grain boundary by heat treatment may include laser beam heat treatment apparatus, rapid thermal annealing system, electric heat treatment apparatus, induction heating apparatus, steam heat treatment apparatus, plasma heat treatment apparatus, and flash lamp heat treatment apparatus. Method of forming a glass coating structure, characterized in that carried out by one or two selected.
12. The method of claim 8,

    The light transmittance of the opaque coating layer is 0.1% to 60%,

    The light transmittance of the transparent coating layer is a method of forming a glass coating structure, characterized in that 30% to 95%.
13. The method of claim 8,

    The base material is glass, tempered glass, quartz glass, quartz, epoxy, alumina (Al ₂ O ₃ ), zirconia (ZrO ₂ ), zinc oxide (ZnO), aluminum nitride (AlN), aluminum (Al), copper (Cu) , Tungsten (W), stainless steel (SUS), PC (Polycarbonate), PET (Polyethylene terephthalate), PI (Polyamide), PMMA (Polymethyl Methacrylat), PBT (Polybutylene terephthalate), PU (Polyurethane), PVA (Polyvinyl alcohol) Or polyvinyl butyral (PVB).
14. The method of claim 8,

    The glass powder is Bi ₂ O ₃ -B ₂ O ₃ -BaO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO-SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -ZnO, B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ , ZnO-B ₂ O ₃ -SiO ₂ , Bi ₂ O ₃ -B ₂ O ₃ -SiO ₂ -R ₂ O, ZnO-B ₂ O ₃ -P ₂ O ₅ , PbO- B ₂ O ₃ -ZnO, PbO-SiO ₂ -B ₂ O ₃ -ZnO and PbO-SiO ₂ -B ₂ O _{3 A} method for forming a glass coating structure, characterized in that at least one selected from.
15. The method of claim 8,

    The glass powder is a method of forming a glass coating structure, characterized in that it comprises a plasma-resistant material.
16. The method of claim 15,

    The plasma material is Al ₂ O ₃ , TiO ₂ , AlN, ZrO ₂ , CaO, SiC, SiO ₂ , Si ₃ N ₄ , B ₂ C, BN, TiN, Y ₂ O ₃ , Y ₂ O ₃ -Al _{2 O 3, YOF, Y 5 O} 4 F 7, Y 6 O 5 F 8, Y 7 O 6 F 9, Y 17 O 14 F 23, YF 3, YCl 3, YBr 3, LaF 3, LaCl 3, LaBr 3 , YOCl, YOBr, YOFCl, YOBrCl, rare earth series (element series from 57 to 71 including Y and Sc) oxide, rare earth series (element series from 57 to 71 including Y and Sc) fluoride , Rare earth series (element series from 57 to 71 including Y and Sc) chloride, MgF ₃ , AlF ₃ , CaF ₃ , BaF ₃ , YAG (Y ₃ Al ₅ O ₁₂ ) and Yttria stabilized Zirconia (YSG) Method of forming a glass coating structure, characterized in that at least one selected from.
17. The method of claim 8,

    The transparent coating layer is a glass coating structure, characterized in that the X-ray peak does not appear when measured by XRD (X-Ray Diffrectometer).

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