KR20100050124A - Vacuum deposition apparatus with temperature control units and method of vacuum fixing solid powder on substrates and bodies - Google Patents

Abstract

PURPOSE: A vacuum deposition device with a temperature controller for solid powder and a method using the same are provided to use compressed air as transferred gas without using inert gas, and to eliminate noise. CONSTITUTION: A vacuum deposition device for solid powder is composed of an air supply unit, an air pressing unit, an air processing unit, a solid powder supply unit, a vacuum deposition chamber(26), an adiabatic carrier(22), a transfer gas heating temperature controller(102), a spraying nozzle(25), and a system controller(H). Solid powder is deposited in a base material. The base material is located inside the vacuum deposition chamber. The adiabatic carrier transfers an aerosol to the vacuum deposition chamber. The transfer gas heating temperature controller pre-heats transferred air, and controls the temperature of the air.

Description

Vacuum deposition apparatus with temperature control units and method of vacuum fixing solid powder on substrates and bodies}

The present invention controls the temperature of the solid phase powder according to the transport gas and the particle size injected from the injection nozzle outlet end in the subsonic and supersonic state to minimize the thermal shock (bow shock) to the substrate to be deposited on the substrate It relates to a solid-phase powder vacuum deposition apparatus equipped with a temperature control device that can be, and a deposition method thereof.

The inventors of the present invention uniformly disperse the aerosol mixed with the carrier gas and the solid powder regardless of the particle size, shape, specific gravity of the solid powder, uniformly and continuously deposited regardless of the material and size of the substrate to form a uniform thin film It has been applied for a device and a method which can be formed. (Korean Patent Application No. 2008-0072119 "Solid-Powder Continuous Deposition Apparatus and Solid-Powder Continuous Deposition Method")

The present invention is a continuous invention of the patent application No. 2008-0072119, the overall device configuration of 1) air supply and pressurization unit, 2) air processing unit, 3) transfer gas heating temperature control unit, 4) solid powder supply unit, 5) Solid powder cooling temperature control unit, 6) Insulation transport pipe, 7) Injection nozzle, 8) Vacuum deposition chamber, 9) Vacuum pump and vacuum chuck, 10) Solid powder dust collection and recovery processing unit, 11) System control unit By controlling the temperature of the solid powder according to the transport gas and the particle size, the transport gas and the solid powder at the nozzle outlet are controlled in the same temperature range, so that the deposition efficiency is reduced without damaging the substrate due to thermal shock and reducing the injection speed due to the reflux. It provides a solid powder deposition method that can increase the deposition efficiency.

Meanwhile, the conventional solid powder deposition method is as follows.

1) Thermal spray deposition method

The thermal spray deposition method is a method of dissolving a solid powder by a plasma, accelerated by a flame, and sprayed onto a substrate. In this process, the temperature applied to the powder varies depending on the type of the thermal spraying process, but a high temperature of 3,000K to 15,000K is applied. The cooling rate after reaching the substrate may reach 10 ⁶ K per second. At this time, the temperature of the powder is hot and sprayed at a high speed at a supersonic speed, so that the particle size of the powder is used for several tens of micrometers or more. Since particles are melted and deposited on a substrate, the bonding strength between particles is excellent. However, dimples are often present in the deposition layer, and the particles may be exposed to high temperature to cause evaporation or change in chemical composition. As a result, there is a disadvantage in that an amorphous phase is formed, cracks are easily generated, and bonding strength with the substrate is reduced, and a thick deposition layer can be formed at a high speed, but the thickness of the deposition layer is difficult to control and the surface is rough.

2) Cold Spray Deposition (Cold Spray Deposition) Method

The cold spray deposition method is similar to the spraying process, but sprays and deposits metal particles of several to several tens of micrometers on the surface of a substrate using a gas of several hundred degrees Celsius without using a high temperature gas or plasma, such as a spray deposition method. . The velocity of the gas injected by this method is supersonic, which is plastically deformed when the particles collide with the substrate by the kinetic energy and heat of the gas, and the deposition is performed in such a way that the particles are fused to the substrate by the temperature rise of the surface. The thickness can be from several mm to several cm. However, particles having a low specific gravity or fine particles have a disadvantage in that the deposition efficiency decreases due to a decrease in the velocity of the particle flow due to aerodynamic drag (flow returning after the gas collides with the substrate).

U.S. Patent No. 5,302,414 ("Gas-dynamic spraying method for applying a coating", 1994; PCT / SU90 / 00126) is a patented technology that aided in cold spraying, and has a size of 1 to 50 micrometers for transport gases at 40 to 400 ° C. The metal, alloy, and polymer powders are sprayed and deposited at 300 ~ 1,200m / s. Melting point of powders used in conventional spraying, plasma deposition and explosion deposition. It is a technology that can relatively reduce the thermal shock on the substrate because it is deposited at a temperature lower than the high temperature above the point, except that the ceramic is deposited by crushing the particles, unlike the metal which causes plastic deformation during deposition. Deposition of powders is difficult, and deposition efficiency is very low, and the deposition of nanometer powder particles of sub-micrometer size, whether metallic or ceramic powders, is sprayed by the return gas of the transfer gas. The injection speed of the powder at the exit of the blade is very low, and it is difficult to deposit on the substrate, and the deposition efficiency is very low.Therefore, it is difficult to deposit sub-micrometer-sized powder and low specific gravity powder by this low temperature injection method, The deposition efficiency of the ceramic powder to be deposited also has a very low problem.

Republic of Korea Patent Registration 10-0691161 ("Method for producing field emission emitter electrode") discloses a method for producing a field emission emitter electrode by spraying carbon nanotube powder at a supersonic speed to the substrate using the cold spray method. . This method has a disadvantage in that the gas is injected at supersonic speed in the air as described above, so that severe noise is generated. In particular, when carbon nanotubes, which are small particles and nanometer-sized particles, are injected rather than metal particles, the transfer gas is applied to the substrate. There is a problem in that it is difficult to deposit on the substrate due to the reflux phenomenon of the high-speed gas during the collision.

Korean Patent Registration 10-0515608 ("Low Temperature Spray Apparatus with Powder Preheating Device"; US Patent Publication US2007 / 0137560 A1, "Cold spray apparatus having powder preheating device"; PCT / KR04 / 03395) preheats the coating powder before coating. To provide a low temperature spray device equipped with a powder preheating device to obtain a high lamination rate and an excellent coating layer under the same low temperature spray process conditions. As described in this patent, low ductility ceramic materials, alloys, Since it is difficult to deposit the powder of cermat such as WC-Co by the existing low temperature spraying process, it is described as a technique to increase the deposition rate by preheating the powder rather than increasing the speed by preheating the main gas. It is. This method is shown in Fig. 5,302,414. As shown in Fig. 4, the compressed gas is transferred to the powder supply device, and the gas and powder are preheated in the heater and then transferred to the nozzle and sprayed onto the substrate. As shown in Fig. 5, it is similar to the method of mixing and spraying the unheated powder and the compressed gas preheated in the heater in the premix chamber located before the nozzle inlet. However, as shown in FIG. 1 of Patent Registration 10-0515608, the main gas passing through the gas supply amount control unit is heated through a heater, mixed with the preheated powder in the mixing chamber, and sprayed to the nozzle. As a result, the main gas temperature and the powder temperature in the mixing chamber are the same. As shown in FIG. 2 of the present invention, the temperature of the conveying gas and the solid powder which has passed through the supersonic nozzle throat is drastically lowered, and the temperature drop change is different depending on the particle size of the solid powder. Therefore, considering the temperature drop change according to the temperature of the transfer gas and the solid powder passing through the supersonic nozzle neck and the particle size of the solid powder as described above, if the temperature of the conveying gas and the solid powder is not adjusted at all stages of the nozzle neck, The large difference in temperature (ΔT _m ) between the conveying gas and the solid powder passing through the nozzle neck causes a greater thermal shock to the substrate. In particular, there is a limit that this method can not be applied to a substrate that is susceptible to thermal shock, such as plastic.

Republic of Korea Patent Registration 10-0575139 ("Low Temperature Spray Coating Device with Gas Cooling Device") is added to the Republic of Korea Patent Registration 10-0515608 ("Low Temperature Spray Device with Powder Preheating Device") in front of the main gas preheating device. By installing a cooling device to cool the gas at a low temperature and supplying it, the gas density per unit volume is increased, and the gas having a higher density is expanded by a preheating heater so that a higher gas velocity can be exhibited. It is described as a low temperature spray coating device technology equipped with a gas cooling device to obtain a rate and an excellent coating layer. That is, in the case of powders having reduced toughness, the critical speed at which the coating is increased increases, so increasing the gas pressure in order to increase the gas velocity for accelerating the powder increases the consumption of gas in proportion to the gas. In the injection method, the increase in the gas supply amount due to the use of nitrogen and helium gas may be a problem in economics. Thus, in order to reduce the gas supply amount and increase the speed, a device for increasing the density of gas through the cooling device is provided. As shown in FIG. 3 of the patent specification, the device cools the gas transferred from the compressed gas storage unit to a cryogenic temperature in a cooling device to a main gas preheater and a powder feeder, and the preheated main gas and preheated powder are mixed in a mixing chamber. It is intended to be mixed and sprayed. Therefore, this device is focused on high gas velocity by increasing the density of gas through the cooling device to reduce the use of inert gas (nitrogen, helium), but Korea Patent Registration 10-0515608 ("Powder preheating device is provided Like the low temperature spraying device "), the temperature of the transfer gas and the solid powder is adjusted at all stages of the nozzle neck by considering the temperature drop of the transfer gas and the solid powder passing through the supersonic nozzle neck and the particle size of the solid powder. Otherwise, a large temperature difference ΔT _m between the transfer gas passing through the supersonic nozzle and the solid phase powder is generated, and a greater thermal shock is applied to the substrate. In addition, when spraying the substrate with excessive gas velocity above the critical velocity of each powder, it is not a good idea to increase the spraying speed only by erosion of the deposition coating layer, and the deposition velocity and the erosion velocity of each powder are not excellent. ) By spray deposition.

As described above, problems commonly encountered in the conventional thermal spray deposition method and low temperature spray deposition method are; 1) Compressed expensive inert gas (e.g. nitrogen, helium, etc.) is difficult to recycle, and 2) pores are formed in the coated section due to thermal shock applied to the substrate, and 3) noise is injected into the air under atmospheric pressure. 4) It is impossible to use a substrate that is weak to thermal shock, such as plastic, due to high temperature gas and powder temperature, and 5) below the critical velocity of deposition of any powder by aerodynamic drag (bow shock). Decreased speed reduces deposition efficiency significantly, 6) it is difficult to deposit powders of low specific gravity or sub-micrometer size, and 7) the same temperature when the carrier gas and solid powder are sprayed onto the substrate after passing through the nozzle outlet Temperature control of the range is difficult.

In order to solve the above problems, the present invention is provided with a carrier gas heating temperature control device and a solid powder cooling temperature control device, the carrier gas and particles when spraying the aerosol mixed with the carrier gas and the solid powder at subsonic or supersonic speed By controlling the temperature of the solid powder according to the size, the temperature of the transfer gas and the solid powder is controlled in the same range, and the solid powder is spray deposited on the substrate located in the vacuum deposition chamber to reduce the spray rate due to the damage and backflow of the substrate by thermal shock. It is an object of the present invention to provide a solid-phase powder vacuum deposition apparatus having a temperature control device capable of increasing deposition efficiency without a reduction, and a deposition method thereof.

In order to solve the above problems, the solid-phase powder vacuum deposition apparatus with a temperature control apparatus according to the present invention comprises an air supply unit consisting of an air pump and an air storage tank; An air pressurizing unit for adding pressure to air supplied from the air supply unit; An air processor for filtering and drying the pressurized air provided from the air supply unit and the air pressurizing unit to discharge the filtered air; Solid powder supply unit for supplying a solid powder in a predetermined amount to the air discharged through the air processing unit; A vacuum deposition chamber in which a substrate is located inside and discharging the air through a vacuum pump connected by a vacuum connection tube to maintain the interior in a vacuum state; An insulating transport pipe for connecting the air processing unit and the vacuum deposition chamber, the aerosol formed by mixing the solid powder supplied from the solid powder supply unit with the air discharged from the air processing unit to the vacuum deposition chamber; Located between the air processing unit and the solid powder supply unit is placed in the adiabatic transport pipe and the transfer gas heating to control the temperature of the air by heating before the solid powder is mixed to form the aerosol mixed with the air discharged from the air processing unit Temperature control unit; An injection nozzle provided at the end of the adiabatic transport pipe and configured to single or slit to inject the aerosol to a substrate positioned inside the vacuum deposition chamber; And a system control unit connected to each of the above components and controlling the conditions such as pressure, speed, flow rate, temperature, etc. of the transfer gas and the solid powder to each component.

In this case, the air pump and the air storage tank, and between the air storage tank and the air processing unit is further configured to include a flow control valve, respectively installed between the air processing unit and the adiabatic transport pipe, filtered and dried air It is another feature of the present invention to be configured to further include a flow rate regulator for controlling the discharge of the flow rate constant. On the other hand, the air processing unit is characterized in that the primary filter, the primary dryer, the secondary filter and the secondary dryer are sequentially configured to perform the filtering and drying treatment of the introduced air repeatedly, the secondary filter Is preferably composed of a water filter, an oil filter and a dust filter. In addition, the water filter is installed between the secondary dryer and the flow regulator and the flow control valve between the primary filter and the primary dryer, and between the water filter and the flow regulator may be further configured to include.

On the other hand, the solid powder supply unit is connected to the front of the discharge port of the solid powder supply device and the solid powder supply device to uniformly regulate the amount of solid powder supplied per unit time and to distribute the solid powder evenly, the upper air flows into the inside The opening is formed so that the solid phase powder provided to the insulated transport pipe through the pressure difference is composed of a block chamber, the solid powder supply unit, one side is in communication with the lower portion of the block chamber The other side further comprises a block chamber lower connection pipe in communication with the insulated transport pipe.

On the other hand, the solid-phase powder vacuum deposition apparatus equipped with a temperature control apparatus according to the present invention, is installed in the opening located in the upper portion of the block chamber and a pre-treatment apparatus for removing moisture and impurities in the air introduced into the block chamber It is characterized by being configured to further include.

In addition, the present invention further comprises a flow rate meter, a pressure gauge and a temperature meter respectively installed in the insulation transport pipe to check whether the flow rate, speed and temperature of the aerosol transported through the insulation transport pipe is further In another aspect, it is preferable to further include a length adjusting device installed in the insulation transport pipe and to adjust the length of the insulation transport pipe to adjust the distance between the injection nozzle and the substrate.

On the other hand, when the elbow is formed in the middle of the adiabatic transport pipe is installed on the entry portion of the elbow is preferably configured to further include a flow regulator for maintaining a constant feed rate of the transfer gas, the adiabatic transport pipe If the diameter of the middle portion of the expansion is installed on the inner wall of the insulated transport pipe further comprises a flow regulator for maintaining a uniform flow distribution over the front end surface of the transport pipe to maintain a constant flow rate and flow rate of air It is preferable at the point which can adjust.

In addition, the injection nozzle of the components of the present invention is characterized in that the subsonic nozzle or supersonic nozzle, the subsonic nozzle is configured in the form of a tube narrowing the cross-sectional area from the nozzle inlet to the nozzle outlet. On the other hand, the ratio of the absolute pressure of the nozzle inlet and the absolute pressure of the nozzle outlet is distributed in the range of 0.001 to 1.0, and the ratio of the absolute pressure of the nozzle inlet and the absolute pressure of the nozzle outlet is 0.528 can achieve the fastest subsonic speed. Therefore, it is preferable to adjust the absolute pressure ratio in consideration of the critical speed and the erosion speed of each solid powder.

On the other hand, the supersonic nozzle is characterized in that the cross-sectional area is reduced from the nozzle inlet to the nozzle neck, the cross-sectional area is larger from the nozzle neck to the nozzle outlet, which is characterized in that the aerosol is supplied into the vacuum deposition chamber to be injected into the substrate When it is to be injected at supersonic speed.

In the case of using the supersonic nozzle in the above configuration, the solid powder supplied from the solid powder supply unit is directly supplied between the nozzle neck of the supersonic injection nozzle and the nozzle outlet without passing through the adiabatic transport pipe, and the nozzle neck of the supersonic nozzle The solid powder mixed with the conveying gas having a supersonic velocity passing through can be injected onto the substrate. A solid powder supply path is formed between the nozzle neck of the supersonic nozzle and the nozzle outlet through the one side of the nozzle body from the outside of the nozzle to the inside, and the other side of the block chamber lower connection pipe communicates with the solid powder supply path. It can be supplied directly into the nozzle through the solid powder supply path.

On the other hand, the present invention is connected to the vacuum deposition chamber through a substrate temperature control insulation tube and is characterized in that it further comprises a substrate temperature control device for controlling the temperature of the substrate in conjunction with the system control unit, which This is to increase the deposition efficiency of the solid phase powder by adjusting the temperature of the substrate located inside the vacuum deposition chamber to be lower than the temperature of the injection nozzle outlet through the substrate temperature control device. In addition, the vacuum deposition chamber is installed in the chamber, characterized in that it further comprises a transfer device for moving the substrate.

The present invention is characterized in that it further comprises a pressure control valve which is installed between the vacuum deposition chamber and the vacuum pump to efficiently maintain and control the vacuum state of the vacuum deposition chamber.

The present invention collects and recovers a small amount of solid powder remaining after being deposited on a substrate in the vacuum deposition chamber recovered through a solid powder dust collection connector and a solid powder dust collection connector connected to the vacuum pump. It is another feature that it further comprises a solid powder dust collection recovery portion consisting of a solid powder dust collection recovery processor and an air exhaust device.

In addition, the present invention is located between the solid powder supply unit and the adiabatic transport pipe, the solid powder cooling temperature control device and the cooled solid powder cooling temperature of the solid powder supplied from the block chamber lower connection pipe cooled temperature It is characterized in that it further comprises a solid-phase powder cooling temperature control unit consisting of a heat-insulating cooling tube in the form of a pipe that is passed through the heat-insulated transport pipe while maintaining the outlet. At this time, the adiabatic cooling tube is preferably in communication with the adiabatic transport tube located on the inlet side of the vacuum deposition chamber.

In another aspect, a solid powder vacuum deposition method of the present invention comprises the steps of: (a) sucking and storing air; (b) pressurizing air; (c) filtering and drying the sucked air to transfer a predetermined amount; (d) heating the air that has undergone the step (c); (e) supplying a solid powder to the air which has undergone the step (d) to form aerosol mixed and dispersed at a constant mixing density, and transferring the solid powder to the injection nozzle; And (f) spraying the aerosol at a subsonic or supersonic speed on a substrate provided in the vacuum deposition chamber in a vacuum state through a spray nozzle.

At this time, the step (e) is a step of supplying a solid powder to the heated air conveyed through the adiabatic transport pipe when spraying to the substrate at subsonic or supersonic speed to form a mixed aerosol to be transferred to the injection nozzle You may. In the case of supplying the solid powder to the adiabatic transport pipe, it is preferable that the aerosol is continuously controlled to have a constant speed, flow rate, and mixing density in order to increase the deposition efficiency, and transported to the injection nozzle.

The solid powder vacuum deposition method according to the present invention further comprises a step of cooling the solid powder before supplying the solid powder to the heated air conveyed through the adiabatic transport pipe in the step (e). do. .

On the other hand, in the solid-phase powder vacuum deposition method according to the present invention, when the aerosol is sprayed at a supersonic speed to deposit on the substrate, the step (e) is carried out in the supersonic transfer gas that has passed through the nozzle neck of the supersonic nozzle. It can also be configured to supply a direct injection to form aerosol dispersed between the nozzle neck and the nozzle outlet to the injection nozzle. In this case, the aerosol is injected at a supersonic speed to the substrate provided inside the vacuum deposition chamber in a vacuum state through the injection nozzle.

In addition, the solid powder vacuum deposition method according to the present invention is characterized in that after the step (f) further comprises a step of collecting and recovering a small amount of solid powder remaining in the vacuum deposition chamber after deposition.

Hereinafter, the configuration of the present invention will be described in more detail.

In the present invention, the following means are applied to solve the above problems.

First, in order to increase the deposition efficiency of the solid phase powder, the injection speed from subsonic to supersonic speed is required, and the transfer gas at this time must maintain a high flow rate and high pressure. For this purpose, it is difficult to solve by the performance of the high pressure pump (eg, 7 ~ 14bar) that is generally used, and expensive high pressure pump (eg ~ 40bar) or high pressure nitrogen gas should be used. In particular, the use of high pressure nitrogen gas has a problem in that an expensive nitrogen gas generator is used for the continuous process. In order to solve the above problems, by installing an air pressurizing unit capable of increasing the capacity of the air supply unit and the pressure of the transfer gas, it is possible to replace expensive high-pressure inert gas (eg, nitrogen, helium gas).

Second, to remove the dust, oil, moisture, etc. of the gas transporting the solid powder is configured to perform a filtering treatment and drying treatment to supply in a quantitative manner.

Third, the solid powder is dispersed so that the nozzle is sprayed at a constant amount and at a constant speed at the nozzle exit in the aerosol state.

Fourth, to configure a transfer gas heating temperature control device capable of raising the temperature of the transfer gas; In the case of a subsonic nozzle, the temperature of the conveying gas is lowered when passing through the nozzle, so that it is not heated to a predetermined level or is not heated within a range without thermal shock; In the case of a supersonic nozzle, since the temperature drops sharply when passing through the nozzle throat, the transfer gas is heated before the nozzle inlet so that the thermal shock is not applied to the substrate in the vacuum deposition chamber due to the temperature of the transfer gas injected from the nozzle outlet. For example, in the case of a plastic substrate, the temperature of the conveying gas injected from the nozzle outlet should be controlled within minus 40 ° C to 80 ° C.

Fifth, to constitute a solid powder cooling temperature control apparatus capable of lowering the solid powder temperature; As the heat transfer rate varies depending on the size of the solid powder supplied to the heated conveying gas, the temperature of the solid powder may directly affect the damage and thermal shock of the substrate when sprayed through the nozzle outlet; 1) If the supplied solid powder is micrometer size, it is higher than the temperature of the conveying gas when passing through the supersonic nozzle, so that the temperature of the solid powder supplied by the temperature difference between the conveying gas temperature and the solid powder is lowered so as not to apply thermal shock to the substrate. 2) If the supplied solid powder is in nanometer size, the temperature of the transfer gas and the temperature of the solid powder are almost in the same range when passing through the supersonic nozzle, so that the temperature of the supplied transfer gas is not applied to the substrate. The conveying gas temperature can be adjusted in the conveying gas heating temperature control unit within the range.

Sixth, 1) construct an orifice-type spray nozzle to express the subsonic critical deposition rate of the solid powder; Spraying speed subsonic an air supply and an air pressurizing portion of absolute pressure (P ₁₎ and the absolute pressure (P ₂₎ ratio (P ₂ / P ₁₎ a speed of about 340m / s or less by keeping it close to the 0.528 of the vacuum chamber ( V), and the flow rate Q = AV can be determined by the cross-sectional area A of the nozzle; Single or slit subsonic nozzles are constructed for two- and three-dimensional substrate coating. 2) construct a supersonic de Laval nozzle to express the supersonic critical deposition rate of the solid powder; The conveying gas and the solid powder are expressed at supersonic speed due to the adiabatic expansion of the conveying gas as they pass through the nozzle throat at subsonic velocity at the inlet of the nozzle cross section, and the temperature and pressure of the conveying gas and the solid powder passing through the nozzle throat rapidly become Reduced; Single or slit nozzles are constructed for two- and three-dimensional substrate coating.

Seventh, to provide a vacuum pump connected to the deposition chamber, to improve the chemical properties of the coating layer by reducing 1) chemical reactions (e.g., reaction with oxygen, etc.) in the deposition chamber through the vacuum state, 2) high-speed gas generated during deposition It is possible to prevent the injection speed from being reduced by the reflux (flow back after the gas collides with the substrate), 3) to remove the noise generated during deposition, and to adsorb and fix the substrate located in the deposition chamber. The vacuum chuck which can be provided is comprised, and it is comprised so that the function which suppresses the fluctuation | variation of the base material by injection can be performed.

According to the solid-state powder vacuum deposition apparatus having a temperature control device according to the present invention and the vacuum deposition method thereof, various problems posed by the conventional deposition method can be solved.

Specifically, first, the transfer gas can be used as compressed air by suctioning and pressurizing the air without using expensive inert gas, and the transfer gas can be used as compressed air. 1) Metals deposited by plastic deformation and ceramics deposited by fracture. (Oxides, nitrides, borides, etc.), special materials with intermediate deposition properties (carbon nanotubes, fullerenes, graphenes, dissimilar materials (e.g. metals + ceramics, metals (or ceramics) + specials) Solid powders, such as materials, etc.) and compounds that are combinations of the above elements; Quantum wells of structure, quantum wires of one-dimensional structure with two directions limited to nanometer size, quantum dots of zero-dimensional structure with three directions limited to nanometer size, and specific gravity Low solid powder, 3) the particles form a tubular, plate-shaped, spherical, linear (such as solid powder, which has a shape such as a rod, wire); a can be deposited on the substrate at a high deposition efficiency.

Second, since the transfer gas and the solid powder can be deposited on the substrate without thermal shock, phase transformation and porosity by controlling the temperature of the same temperature range when the substrate is sprayed on the substrate after passing through the nozzle outlet, Dense, high quality coatings can be made that are not seen in the deposition results.

Third, it is possible to maximize the deposition efficiency by eliminating the backflow of the high-speed gas and solid powder generated in the deposition method using the vacuum deposition chamber, to remove the noise generated during the injection, and to reduce the chemical reaction have.

Fourth, by controlling the temperature of the substrate (T _s ) lower than the temperature (T _e ) of the aerosol using a temperature control device connected to the vacuum deposition chamber, it is possible to minimize the reflux generated during deposition.

Fifth, using a subsonic nozzle and a supersonic nozzle, it is possible to realize a high deposition efficiency above the deposition critical speed according to the type of solid phase powder.

Sixth, it is possible to form a coating layer having a high density, uniformity and crack-free structure on the substrate (metal, ceramic, polymer plastic, polymer, etc.) of various materials. In particular, it has high applicability to polymer plastics and polymer materials which are weak to thermal shock.

Seventh, it is possible to form a high-speed coating layer, it is easy to control the thickness (submicrometer ~ hundreds of micrometer) of a wide range of coating layer.

Products which can be produced by the solid-phase powder deposition apparatus and deposition method according to the present invention include electrical and electronic related coating; Conductive (semi) transparent electrode, field emission device for FED (field emission display), field emission device for BLU (back light unit), lighting device, solar cell, semiconductor, electronic shielding material, heating element, sensor, flexible display, Electrostatic dispersions, dielectrics, magnetically conducting materials, and the like; Examples include antifriction materials, corrosion-resistance materials, surface hardening materials, and the like.

I. Solid Powder Deposition Equipment

The present invention air supply and pressurization; An air processing unit for filtering and drying the air provided from the air supply unit and discharging the air; A transfer gas temperature adjusting unit for heating the air discharged through the air processing unit; A solid powder supply unit supplying a solid powder to the heated transfer gas in a predetermined amount; Solid-phase powder cooling temperature control unit for cooling the solid-phase powder; A vacuum deposition chamber provided with a substrate therein; A tube for connecting the air processing unit and the vacuum deposition chamber, the adiabatic transport pipe for transporting the aerosol formed by mixing the solid powder into the air discharged from the air processing unit to the vacuum deposition chamber; An injection nozzle provided at an end of the adiabatic transport pipe to inject the aerosol to a substrate in the vacuum deposition chamber; And a vacuum chuck capable of adsorbing a vacuum pump and a substrate provided to maintain the vacuum deposition chamber in a vacuum state. A solid powder dust collection unit for collecting and recovering a small amount of solid powder remaining after deposition; It provides a solid-phase powder vacuum deposition apparatus equipped with a temperature control device configured to include a system control unit that can control the entire module.

Hereinafter, the present invention will be described with reference to the accompanying drawings.

1. Air supply and pressurization part

In the conventional deposition method, an inert gas such as argon (Ar), nitrogen (N ₂ ), helium (He), etc. was used as a transfer gas, and the transfer gas was introduced into a transport tube or an aerosol chamber to generate an aerosol. However, the inert gas is a very expensive gas to be used in a continuous process for mass production of a commercialized product, and even when used as a storage container, there is a disadvantage in that the continuous process cannot be performed due to the capacity limitation of the container. The present invention is configured not to use an inert gas, the general air is introduced to utilize from the outside, the air supply is responsible for providing the air processing unit to be introduced later, by introducing the external general air. Therefore, the present invention is suitable for a continuous process for mass-producing a commercialized product, it is possible to significantly reduce the manufacturing cost of the product produced using the present invention.

As shown in FIG. 1, the air supply and pressurizing unit is provided with an air pressurizing unit consisting of a pressurizing device 100 and a pressurizing tube 101, and a subsonic injection speed or a supersonic injection speed at the nozzle outlet (V _e ; Equation 1). It includes a device for increasing the pressure (P) of the transfer gas at the nozzle inlet, the air supply unit comprises an air pump 10 and the air storage tank 11, the air pump 10 is provided on one side The air sucked at the air inlet may be pumped to be introduced into the air storage tank 11, and the air storage tank 11 may be provided to the air processor B after storing the air introduced therein. The air storage tank 11 can prevent the irregularity and delay of the air discharge amount to be transported to the next step, it is possible to carry out a stable and continuous mass production. In addition, a flow control valve 34 is provided between the air pump 10 and the air storage tank 11 and between the air storage tank 11 and the air processor B, respectively, so that the amount of inlet-exhaust air in each stage is increased. Can be controlled quantitatively.

(식 1)

(Equation 1)

Where V _e = injection speed at the supersonic nozzle outlet (m / s)

T = absolute gas temperature at the nozzle inlet (K)

R = universal gas law constant, 8,314.5 J / (kmolK)

M = molecular mass of the carrier gas (kg / kmol)

k = c _p / c _v = isentropic expansion factor

c _p = conveying gas at constant pressure

Specific heat

c _v = specific heat of the carrier gas at constant volume

P _e = Absolute pressure of conveying gas at the supersonic nozzle outlet (Pa)

P = absolute pressure of the conveying gas at the supersonic nozzle inlet (Pa)

2. Air treatment unit

The air processing unit (B) is configured to discharge the filtered and dried treatment of the air provided from the air supply and pressurizing unit (A). In addition, the air processing unit may be further equipped with a flow controller 18 for constantly controlling the discharge of the filtered and dried air flow rate.

The air treatment unit removes impurities from a transfer gas (ie, air supplied from the air supply unit), and the flow regulator 18 supplies the filtered and dried air amount supplied from the air supply and pressurization unit A to a predetermined amount. In this case, the aerosol formed by the mixing of the solid powder and the air is controlled to be supplied at a predetermined amount (liter / min) per unit time in the vacuum deposition chamber 26.

Meanwhile, the air treatment unit includes a primary filter 12, a primary dryer 13, a secondary filter 13-1, and a secondary dryer 17 in order to filter and dry the introduced air. It can be configured to be repeated. In addition, the secondary filter 13-1 may be formed of a water filter 14, an oil filter 15, and a dust filter 16 to remove impurities in the air. Furthermore, after the secondary dryer 17, the air passes through the water filter 14 once again, so that the air may be discharged in a dry state.

A flow control valve 34 is also provided between the primary filter 12 and the primary dryer 13 and between the moisture filter 14 and the flow regulator 18 to quantify the inflow / exhaust air volume at each stage. Can be adjusted.

3. Transfer gas heating temperature control unit

As shown in Figure 1, the transfer gas heating temperature control unit is located between the air processing unit (B) and the solid powder supply unit (D), the device can heat the transfer gas to raise the temperature, Figures 2 and 7c As shown in 1) in the supersonic nozzle; The heated conveying gas increases in speed as it passes through the nozzle throat at the nozzle inlet, thereby generating a supersonic injection speed at the nozzle outlet, and the temperature of the conveying gas (T in Equation 1) and the pressure P drop rapidly. Therefore, the temperature of the transfer gas can be adjusted so as not to apply thermal shock to the substrate located in the vacuum deposition chamber.

For example, if the feed gas at room temperature (20 ℃) is not heated to give a supersonic injection speed of 650m / s, and it passes through the nozzle neck as it is, the temperature of the feed gas at the nozzle outlet is about minus 120 ℃. Thermal shock may be applied to the located substrate. Therefore, when the temperature of the transfer gas is heated to 160 ° C. and passed through the nozzle, the temperature of the transfer gas is 20 ° C., thereby avoiding thermal shock. 2) at subsonic nozzles; As shown in FIGS. 7A and 7B, the subsonic nozzle is used to produce less than 340 m / s injection speed, and the temperature drop due to the injection is relatively small compared to the supersonic nozzle because the injection speed is relatively slow. Therefore, in the subsonic nozzle, it is possible to control the temperature of the conveying gas at a temperature lower than the high heating temperature applied to the supersonic nozzle at a temperature that does not sufficiently apply thermal shock to the substrate. Therefore, by controlling the temperature of the transfer gas in accordance with the injection speed of the supersonic and subsonic speed it can be controlled to the thermal shock tolerance of the substrate.

In addition, through the substrate temperature control device 405 connected to the vacuum deposition chamber 26 as shown in FIG. As can be seen from the graph shown in FIG. 9, if the temperature T _s of the substrate located inside the vacuum deposition chamber is controlled to be higher than the aerosol temperature T _e at the nozzle outlet, the deposition efficiency of the solid phase powder is not reduced. Can be further improved. In other words, when the substrate temperature (T _s ) is greater than the temperature (T _e ) of the aerosol (T _a <T _s ), a large temperature difference occurs between the contact surface of the substrate and the injected aerosol, so that the solid powder present in the aerosol is sprayed with the substrate. The impact speed is reduced by receiving a large pressure P in the vertical direction of the substrate due to the temperature difference between the aerosols, which means that the deposition efficiency is reduced.

4. Solid powder supply

The solid powder supply unit D passes through the solid powder cooling temperature controller 103 and the adiabatic cooling tube 109 and supplies solid powder to the air discharged through the air processing unit B as shown in FIG. 3. It is a component for. The solid powder supply unit includes a solid powder supply device 21 and a block chamber 111. In the solid powder supply apparatus 21, the amount of solid powder discharged per unit time is constantly adjusted, and the solid powder must be evenly distributed. The block chamber 111 is connected to the front surface of the discharge port of the solid powder supply device 21, and the solid powder discharged from the solid powder supply device 21 is provided through the lower block chamber connection pipe 20. It is to be transferred to the solid powder cooling temperature control device (103). In addition, an opening 104 is provided at the upper portion of the block chamber 111 to allow gas to flow therein, so that the speed (several to several tens of m / s) and the pressure (˜40 bar) of the transfer gas is maintained. The solid powder is suctioned to the transport pipe 22. The opening 104 located above the block chamber 111 may be provided with a filter for removing moisture and impurities of the gas introduced therein, or may be provided with a pretreatment apparatus for supplying a gas from which moisture and impurities have been removed. .

5. Solid powder cooling temperature controller

Solid powder cooling temperature control unit (E) is directly connected to the solid powder supply unit (D) as shown in Figure 3 is discharged from the solid powder supply device 21 is supplied through the block chamber 111 It is a device to cool down the temperature. Temperature (T) of Fig transferred gas is heated passing through the supersonic nozzle inlet 201 as shown in 2 is a sudden temperature drop (T _e) generated through the supersonic nozzle throat 202 as discussed above. However, it should be considered because it shows a different aspect according to the particle size of the solid phase powder, as shown in FIG. 2, the solid phase powder of nanoparticle size almost shows the behavior of the temperature range (ΔT _n ) of the carrier gas, Since the powder shows a large temperature difference (ΔT _m ) with the temperature of the transfer gas, if the temperature of the solid powder is not lowered before the nozzle entrance by this temperature difference (ΔT _m ), the substrate may be damaged separately from the transfer gas. The temperature of the powder should be controlled to behave like a conveying gas. Therefore, not only the temperature of the transfer gas of the supersonic nozzle outlet 203 but also the temperature of the solid phase powder must be controlled within an allowable range in which no thermal shock is applied to the substrate located in the vacuum deposition chamber. Therefore, the transfer gas heating temperature control unit (C) and the solid-phase powder cooling temperature control unit (E) can be configured to configure a vacuum deposition apparatus capable of temperature control through feedback.

The position where the adiabatic cooling pipe 109 and the adiabatic transport pipe 22 connected to the solid powder cooling temperature control unit E can be maintained at a constant temperature by heating the transfer gas, and the cooling temperature of the solid powder is It is desirable to install at a location that is less affected by the temperature of the transfer gas. In other words, it is preferable that the outlet portion of the adiabatic cooling tube 109 is provided close to the vacuum deposition chamber 26. In other words, the heated conveying gas and the cooled solid powder reach the nozzle neck at an arbitrary temperature difference, and are sprayed with little difference in temperature between the conveying gas and the solid powder after passing through the nozzle neck. However, since there must be a certain distance for the dispersion of the aerosol well, by lengthening the length of the adiabatic cooling tube 109 sufficiently can achieve the cooling and dispersing effect of the solid phase powder at the same time.

By doing so, it is easy to control the temperature of the transfer gas and the solid powder, and it is possible to control the temperature change generated at the nozzle outlet in the temperature range without thermal shock.

On the other hand, there is a case where a solid powder cooling temperature control unit for cooling the solid powder is not necessary. As shown in FIG. 8A, when the solid powder at room temperature is supplied through the solid powder supply path 41 formed near the supersonic nozzle neck 202 among the supersonic nozzle neck 202 and the supersonic nozzle outlet 203, FIG. As shown in 8b, the heated conveying gas 106 introduced into the supersonic nozzle inlet 201 is mixed with the supplied solid powder at the moment of passing through the supersonic nozzle neck 202 to form an aerosol, and the solid powder and the conveying gas are The mixed aerosol 107 behaves at the same speed as the conveying gas and exits the supersonic nozzle outlet 203, and may be sprayed and deposited on the substrate in the vacuum deposition chamber at a temperature without thermal shock effects. However, it should satisfy the condition that the transfer gas should be heated and transferred to a temperature that does not apply thermal shock to the substrate.

6. Insulation transport pipe

The adiabatic transport pipe 22 is a conduit for transporting the aerosol formed by mixing the solid powder into the air discharged from the air processing unit B to the vacuum deposition chamber 26, and is provided to connect the air processing unit and the vacuum deposition chamber. It is.

In order to constantly control the aerosol temperature at the nozzle outlet, the heat loss of the conveying gas heated in the conveying gas heating thermostat section (C) or the solid state powder cooled in the solid state powder cooling thermostat section (D) can be reduced as much as possible. Insulated transport pipe 22 is required.

In order for the aerosol passing through the insulation transport pipe 22 to maintain a constant flow rate and speed, the cross-sectional area of the insulation transport pipe should not increase or decrease due to external impact or internal pressure. If the insulation transport pipe is made of plastic, etc., the insulation transport pipe is vibrated or the cross-sectional area is reduced or increased due to factors such as external pressure, so that the cross-sectional velocity distribution of the aerosol transferred through the insulation transport pipe is irregular, This is because it may be difficult to deposit uniformly.

In order to check whether the flow rate, speed, and temperature of the aerosol transferred through the adiabatic transport pipe are constant, the adiabatic transport pipe may be further equipped with a flow meter, a pressure gauge 23 and a temperature meter. In addition, the adiabatic transport pipe further includes a length adjusting device 24, by adjusting the length of the adiabatic transport pipe can adjust the distance between the injection nozzle 25 and the substrate 27 mounted at the end of the adiabatic transport pipe.

On the other hand, the adiabatic transport pipe 22 may be an elbow (elbow) is formed in the middle of the pipeline arrangement. As such, when the elbow is formed in the adiabatic transport pipe 22, the flow regulator 19 should be mounted on the inlet portion of the elbow in the adiabatic transport pipe. The flow regulator 19 is a device that maintains a constant speed of the transfer gas 106 even though the adiabatic transport pipe 22 is deformed in the form of an elbow. As shown in FIG. If the pipe and spray nozzle are connected, no additional installation is required.

However, as shown in (d) of FIG. 4, when the elbow is formed in the heat insulation transport pipe 22, the flow rate of the transport gas passing outside the inner wall of the heat insulation transport pipe by centrifugal force when the transport gas transported passes through the curved portion. Since this increase occurs, in order to maintain a uniform speed in the adiabatic transport pipe as shown in (c) of FIG. 4, the flow regulator 19 must be installed at the inlet portion of the elbow as shown in FIG. 4 (b). do.

In addition, as shown in (e) of FIG. 4, when the diameter of the adiabatic transport tube is extended in the middle, as shown in FIG. 4 (f), the highest velocity distribution is shown in the central portion of the adiabatic transport pipe. In order to obtain a uniform velocity distribution over the front end surface of the adiabatic transport tube, a flow regulator may be installed on the inner wall of the adiabatic transport tube to obtain a uniform flow rate distribution as shown in FIG.

Of course, the adiabatic transport pipe is most preferably configured so that there is no bending change or cross-sectional change such as elbow so that no separate flow regulator is required.

7. Injection nozzle

The injection nozzle 25 is provided at the end of the adiabatic transport pipe 22 so as to inject the aerosol to the substrate 27 inside the vacuum deposition chamber 26.

The injection nozzle 25 is for maximizing deposition efficiency by injecting a solid powder at a deposition velocity above a critical velocity and below an erosion velocity, depending on the type and size of the solid powder. Subsonic nozzles or supersonic nozzles may be applied. For example, when spraying 25μm tin powder at subsonic speed of about 150m / s, it is deposited on the substrate, but when spraying at supersonic speed of 340m / s or more, the substrate and the deposition layer are chipped out due to this spraying speed. May occur. Therefore, the critical speed and the erosion speed are different depending on the type, size, and specific gravity of each solid powder. Therefore, a spray nozzle suitable for each solid powder should be selectively used.

Subsonic nozzle 300 is an absolute pressure (P ₂₎ of the absolute pressure (P ₁₎ and the subsonic nozzle outlet 302 of the subsonic nozzle inlet 301, as shown in Fig. 7a and 7b i.e., inside the vacuum deposition chamber, If the ratio (P ₂ / P ₁ ) of the absolute pressure (P ₂ ) is less than or equal to 0.528, the injection speed can be achieved at subsonic speeds of less than 340 m / s, and the required flow rate depends on the pressure of P ₁ . P ₁ can be adjusted so as not to become large, and the cross-sectional area of the orifice for exhibiting the maximum injection speed of less than 340 m / s can be calculated using the relationship between the flow rate and the injection speed. 5A and 5B illustrate a configuration and a cross section of a subsonic nozzle having a single shape, and as shown in FIG. 5D, solid powder may be deposited on a two-dimensional substrate and an object having a three-dimensional shape. ) And the subsonic nozzle 300 is controlled by a device capable of moving in three axes (x, y, z axes) through the nozzle position controller 400 connecting the subsonic nozzle 300. On the other hand, Figure 5c shows the shape of the subsonic nozzle 303 having a slit (slit) form for large-area deposition, Figure 5e is a solid powder to the substrate 27 having a two-dimensional and three-dimensional large area shape A subsonic nozzle 303 is shown having a slit shape located within a vacuum deposition chamber 26 that can be deposited.

The supersonic nozzle 200 has a shape in which the cross-sectional area decreases as it goes from the supersonic nozzle inlet 201 to the supersonic nozzle throat 202, and then crosses the supersonic nozzle neck 202 and toward the supersonic nozzle outlet 203 and has a larger cross-sectional area. This is commonly called a laval nozzle. This supersonic nozzle was developed by Gustaf de Laval in Sweden in 1897 and used in steam turbines, which was then applied to rocket engines by Robert Goddard.

The relational expression of this supersonic nozzle is the same as that of Formula (1) mentioned above, and the cross section is as shown in FIG. 6A and 6B. As shown in FIG. 7C, the aerosol 107 in which the solid powder and the conveying gas are mixed expands while passing through the supersonic nozzle neck 202, and the speed becomes supersonic speed, and the pressure and the temperature drop sharply. Because the mass flow rate of the supersonic nozzle inlet 201 and the supersonic nozzle outlet 203 must be the same, the rapid cross-sectional change of the supersonic nozzle neck 202 can act as a supersonic nozzle, thereby making the device supersonic for a long time. It has been used as. Figure 6c shows the shape of the supersonic nozzle 306 of the slit (slit) for large area deposition, Figure 6d is able to deposit the solid state powder on the object of the two-dimensional and three-dimensional shape, the heat insulation transport pipe 22 ) And a device capable of moving in three axes (x, y, z axes) through a nozzle position controller 400 connecting the supersonic nozzle 200. 6E shows a slit-type supersonic nozzle 306 located in the vacuum deposition chamber 26 capable of depositing a solid powder on a large-area substrate 27 having a two-dimensional and three-dimensional shape.

As shown in FIG. 8A, using an improved supersonic nozzle capable of supplying a solid powder directly near the supersonic nozzle neck 202 to form an aerosol inside the nozzle, at the supersonic nozzle inlet 201 as shown in FIG. 8B. At the moment when the heated conveying gas 106 passes through the supersonic nozzle neck 202, it is mixed with the solid powder supplied directly through the solid powder supply path 41 to be in an aerosol state inside the nozzle and exits to the supersonic nozzle outlet 203. Naga is sprayed on the substrate at supersonic speed. Therefore, the solid powder behaves at the same speed as the transfer gas in the aerosol state, and can be deposited on the substrate in the vacuum deposition chamber at a temperature without temperature and thermal shock effects. Here, the temperature of the conveying gas is a temperature in which the aerosol is mixed with a solid powder at room temperature through a supersonic nozzle heated to a temperature in the range of no thermal shock. 8C and 8D show an embodiment applied using an improved supersonic nozzle.

The injection nozzle 25 can be properly adjusted the separation distance with the substrate 27 by the length adjusting device 24 mounted to the insulated transport pipe 22, considering the critical speed and erosion speed of each solid powder Thus, a subsonic nozzle or a supersonic nozzle can be selectively applied and used, and the subsonic speed near the subsonic speed can be expressed as a supersonic nozzle. The injection nozzle 25 may be made of a material, such as stainless steel, titanium, aluminum alloy, or the like, resistant to pressure and temperature.

8. Vacuum deposition chamber

The vacuum deposition chamber 26 provides a space for depositing the solid powder on the substrate and the shape object. The material of the vacuum deposition chamber 26 may be sufficiently resistant to external pressure according to the vacuum state, and may be made of durable stainless steel or the like, and may be transparent to observe the inside of the deposition chamber from the outside. Can be produced by combining.

The vacuum deposition chamber 26 may further include a transfer device 28 for moving the substrate 27. Looking at the embodiment shown in Figure 1 with a transfer device 28 in more detail as follows. In the embodiment shown in FIG. 1, the spray nozzle 25 is located in the vacuum deposition chamber 26, and the substrate 27 is disposed on the transfer device 28. As shown in FIG. In addition, the vacuum deposition chamber is connected to the vacuum pump 31. In addition, one side of the vacuum deposition chamber is provided with a door for locating the substrate into the vacuum deposition chamber or to facilitate the cleaning of the inside of the chamber. In the vacuum deposition chamber, the solid powder may be deposited regardless of the type of the substrate. However, for the process of depositing a large amount of solid powder on a substrate of a hard material such as glass, metal, etc., the transfer apparatus 28 is a batch type (substrate having a predetermined area is carried out by the transfer apparatus to carry out the deposition process. And the transfer device may be replaced with a roll-to-roll type in-line device when a substrate of a flexible material such as a polymer film or a foil is used. (In FIG. 1, only a batch type transfer device is illustrated.) The transfer device 28 may be configured to be assembled, disassembled, and replaced according to the material of the substrate. As shown in FIGS. 5D and 6D, a holder for depositing a solid powder on a three-dimensional object (regular or irregular shape such as a sphere, a tetrahedron, a rod, a tube, etc.) may be installed, and the holder may be a three-dimensional object. It is possible to control the position of the object to coat the whole. In addition, as shown in Figures 5e and 6e the transfer apparatus can be configured to adjust the feed rate of the substrate. In addition, as shown in FIG. 9, in order to minimize the generation of pressure in the opposite direction of the injection direction due to the difference between the temperature (T _e ) of the injected aerosol and the temperature (T _s ) of the substrate (reflection in the substrate), The temperature T _s must be kept below the temperature T _e of the aerosol at the nozzle outlet. To this end, the substrate temperature adjusting device 405 connected to the vacuum deposition chamber 26 may be further configured, and the substrate temperature adjusting device 405 may adjust the temperature of the substrate in conjunction with the system control unit H. .

However, if the vacuum degree of the vacuum deposition chamber is increased, the reflux can be minimized even without operating the temperature control device 405 connected to the vacuum deposition chamber.

9. Vacuum pump and vacuum chuck

The vacuum pump 31 is a device for maintaining the vacuum deposition chamber 26 in a vacuum state. By maintaining the vacuum deposition chamber in a vacuum state, the chemical reaction in the vacuum deposition chamber is reduced, and the velocity of the particle flow is increased by the aerodynamic drag (flow returning after the gas collides with the substrate) generated during deposition. The reduction can be prevented, and the deposition noise can also be reduced. By mounting a pressure control valve 30 between the vacuum deposition chamber 26 and the vacuum pump 31, it is possible to efficiently maintain and control the vacuum state of the vacuum deposition chamber. 5E and 6E are provided with a vacuum chuck 403 capable of adsorbing and fixing the substrate, and is configured to perform a function of suppressing the fluctuation of the substrate by spraying.

Therefore, when the deposition is carried out by a batch spraying process that does not have a separate transport device in the vacuum deposition chamber, it is located between the bottom surface of the vacuum deposition chamber and the substrate, and the lower part of the substrate is vacuum-adsorbed and fixed, and then aerosol is sprayed onto the substrate. When the solid powder can be deposited on the substrate, and the deposition is carried out by a continuous spraying process in which the transfer apparatus 28 must be provided in the vacuum deposition chamber 26, a vacuum is formed between the upper surface of the transfer apparatus 28 and the substrate. The chuck 403 is fixed to the lower part of the substrate 27 by vacuum suction. Even when the transfer device 28 is operated by the vacuum chuck 403, the base 27 is not only stably fixed, but also the occurrence of shaking due to aerosol injection can be suppressed.

10. Solid-state powder collection recovery unit

The solid powder collection and recovery processing unit (G) is connected to the vacuum pump 31 and is provided to collect and recover a small amount of solid powder remaining in the vacuum deposition chamber 26 after deposition.

The solid powder collecting and recovering unit may collect and recover the remaining solid powder by depositing an aerosol formed by mixing the transfer gas and the solid powder through a spray nozzle. Since solid powder is heavier than air, air may be exhausted and solid powder may be collected at a lower floor.

11. System Control

The solid powder vacuum deposition apparatus is composed of the above 1) air supply unit and pressurization unit, 2) air processing unit, 3) conveying gas heating temperature control unit, 4) solid powder supply unit, 5) solid powder cooling temperature control unit, 6 A) Insulation transport pipe, 7) injection nozzle, 8) vacuum deposition chamber, 9) vacuum pump and vacuum chuck, 10) solid-phase powder dust collection unit and 11) system control unit for controlling the modules, system control unit ( H) is configured to control and control the pressure, speed, flow rate, temperature, etc. of the transfer gas and solid phase powder to each module of 1) to 10 in order to exhibit high deposition efficiency.

II. Solid Powder Vacuum Deposition

The present invention (a) a step of sucking and storing air; (b) pressurizing air; (c) filtering and drying the sucked air to transfer a predetermined amount; (d) heating the air that has undergone the step (c); (e) quantitative supply and cooling of solid powder; (f) quantitatively supplying the cooled solid powder to the air that has undergone the step (d) to form aerosols dispersed at a constant mixing density, and transferring the same to a spray nozzle; And (g) spraying the transported aerosol at a subsonic or supersonic speed on a substrate provided in the vacuum deposition chamber in a vacuum state through a spray nozzle; (h) collecting and recovering a small amount of solid powder remaining after deposition; And it provides a solid-phase powder vacuum deposition method for controlling the (a) ~ (h) process as a whole.

Only in the case where the solid powder is a submicrometer (nanometer size) in the process, the process of cooling the solid powder in the step (e) may be omitted. This is because, as shown in FIG. 2, the temperature difference between the conveying gas injected from the nozzle outlet and the solid powder behaves in a small temperature range.

The solid powder vacuum deposition method may be realized by operating the solid powder vacuum deposition apparatus described above, and details thereof will be described for each process below.

1. (a) Process

This step is a step of sucking and storing air. In this process, the air is sucked into the air pump and stored in the air storage tank, thereby preventing irregularities and delays in the air discharge amount, thereby enabling stable and continuous mass production.

2. (b) process

This step is a step of pressurizing the air, in this step by using a pressure booster (pressure booster) to further increase the pressure of the air pump, it is possible to express the injection speed of subsonic or supersonic at the nozzle outlet.

3. (c) process

This process is a process of filtering and drying the sucked air to discharge a certain amount. This process can be specifically performed by the following process.

Iii) primarily filtering impurities contained in the inhaled and stored air;

Ii) removing the moisture of the air through the primary filtered air through the primary dryer;

Iii) secondary filtering the impurities in the air transported through the primary air dryer with a water filter, an oil filter and a dust filter;

Iii) transporting the secondary filtered air to a secondary dryer to remove moisture from the air;

Iii) filtering to remove moisture;

Iii) discharging the air from which impurities are removed through each of the above steps to a flow controller;

Each of the above steps can be carried out by the air processing unit of the solid-phase powder vacuum deposition apparatus described above.

4. (d) process

This step is a step of heating the air that has passed through the step (c), and as described above, the range that does not give a thermal shock to the substrate and the object located in the vacuum deposition chamber (for example, the plastic substrate is minus 40 ℃ ~ image 80 ℃ ) Is the process of heating the transfer gas to produce the injection speed from subsonic to supersonic speed.

5. (e) Process

This process is a process to quantify and cool the solid powder. As described above, the micrometer particle size that passes through the supersonic nozzle neck takes into account the difference between the temperature of the transfer gas and the solid powder at the supersonic nozzle exit. After cooling the solid powder in advance before the inlet of the supersonic nozzle, it is transferred to the conveying gas that is heated and transported, and at the outlet of the supersonic nozzle, the carrier gas and the solid powder of the micrometer particle size are sprayed on the substrate in the same temperature range, In case of adopting a process that does not apply thermal shock to the substrate and using a solid-state powder of nanometer particle size, there is almost no temperature difference between the transfer gas and the solid-phase powder in the vacuum deposition chamber even when passing through the supersonic nozzle outlet. The step of cooling may be omitted.

Therefore, the temperature of the solid-state powder as well as the temperature of the conveying gas at the nozzle outlet must also be controlled at the temperature of the initial solid-phase powder within an allowable range in which no thermal shock is applied to the substrate located in the vacuum deposition chamber. Therefore, the apparatus for controlling temperature through feedback may be configured by interlocking the transfer gas heating temperature adjusting unit and the solid powder cooling temperature adjusting unit.

6. (f) Process

This process is a process of quantitatively supplying the cooled solid powder to the air that has passed through the step (d) to form aerosol dispersed in a constant mixing density to transfer to the injection nozzle.

This process can be carried out in the adiabatic transport pipe, it is possible to maintain a constant flow rate and flow rate of the aerosol transported in the transport pipe by controlling a certain amount of solid powder and air.

7. (g) Process

This step is a step of injecting the aerosol to the substrate provided in the vacuum deposition chamber in a vacuum state at a subsonic or supersonic speed. The vacuum deposition chamber may maintain a vacuum state by interlocking with a vacuum pump, minimize deposition rate reduction due to reflux, and remove deposition noise.

On the other hand, in addition to the method of minimizing the reflux during the deposition of the vacuum deposition chamber described above, as shown in Figure 1 through the temperature control device connected to the vacuum deposition chamber the temperature (T _s ) of the substrate located inside the vacuum deposition chamber nozzle When controlling the temperature of the aerosol jet (T _e) less than the temperature at the outlet, it is possible to further improve the deposition efficiency without reducing the impact velocity of the solid powder. That is, as shown in 9, a temperature of the substrate above the temperature of the aerosol (T _e) If (T _s) is large (T _e <T _s) larger in the vertical direction due to the temperature difference in the contact surface of the base material and spraying the aerosol Under the pressure P, the collision speed is reduced, thereby reducing the deposition efficiency.

Here, the substrate temperature control device connected to the vacuum deposition chamber controls the temperature to a range that does not apply a thermal shock to the substrate located in the vacuum deposition chamber.

8. (h) process

This is a step of collecting and recovering a small amount of solid powder which is not deposited among the solid powder injected by the step (g).

In order to achieve the maximum deposition efficiency, the steps (a) to (h) are performed in the following steps: 1) air supply unit and pressurization unit, 2) air processing unit, 3) transfer gas heating temperature control unit, 4) solid phase powder supply unit, 5) solid phase Powder Cooling Temperature Control Unit, 6) Insulation Transport Pipe, 7) Injection Nozzle, 8) Vacuum Deposition Chamber, 9) Vacuum Pump and Vacuum Chuck, 10) Solid Module Dust Collector Provided is a solid powder vacuum deposition method that can be controlled.

III. Result formed by solid powder vacuum deposition

The area to which the present invention described above is applicable is as follows.

1. Conductive (semi) transparent electrode formed by depositing with solid phase powder (carbon nanotube, ITO (indium tin oxide), etc.)

2. Field emission device for FED (field emission display) and BLU (back light unit) which is deposited by carbon nanotube powder

3. High-efficiency lighting device deposited by carbon nanotube powder

4. Solar Cells Deposited by Solid Powders

  -Silicon solar cell

  -Group III-V compound GaAs, InP solar cell

  -CIGS (CGS, CIS), CdTe Solar Cell

-Quantum dot solar cell

5. Quantum dot semiconductor diode deposited by solid powder

6. Semiconductor wiring deposited by solid powder (carbon nanotube, copper, etc.)

7. Electronic shield material deposited by solid powder

8. High efficiency heating element deposited by carbon nanotube powder

9. High-efficiency sensor deposited with carbon nanotube powder

10. Flexible Display Deposited by Solid-Powder

11. Electrostatic Dispersion Impregnated with Solid Powder

12. Polymer composite and ultra light, high strength composite with carbon nanotubes

13. Dielectric deposited by solid powder

14. Magnetically conducting material deposited by solid powder

15. Antifriction material deposited by solid powder

16. Corrosion-resistance material deposited by solid powder

17. Surface hardening materials, etc., deposited by solid powder.

1 is a schematic diagram of an apparatus of the present invention.

Figure 2 is a graph of the temperature change according to the particle size of the solid gas and the conveying gas in the supersonic nozzle.

3 is a schematic view showing that the solid powder cooled in the adiabatic transport pipe is mixed with a heated transport gas.

Figure 4 is a schematic diagram showing the velocity distribution of the transfer gas generated in the elbow cross-section or expansion cross-section of the transport pipe.

5A is a cross-sectional view of a subsonic nozzle.

5B is a cross-sectional view taken along the line A-A of FIG. 5A.

Figure 5c shows the structure of the subsonic nozzle in the slit form.

5D is a schematic diagram for coating a three-dimensional shape with a subsonic nozzle positioned in the deposition chamber.

5E is a schematic diagram for coating a large area substrate of a two-dimensional shape with a subsonic slit nozzle positioned in the deposition chamber.

6A is a cross-sectional view of the supersonic nozzle.

FIG. 6B is a cross-sectional view taken along the line B-B in FIG. 6A.

6C is a perspective view of the supersonic slit nozzle.

6D is a schematic diagram for coating a three-dimensional shape with a supersonic nozzle located in the deposition chamber.

6E is a schematic diagram for coating a large area substrate of a two-dimensional shape with a supersonic slit nozzle positioned in the deposition chamber.

7A is a graph of injection speed in a subsonic nozzle.

Figure 7b is a graph according to the injection rate change of absolute pressure of the nozzle inlet (P ₁₎ and the nozzle outlet absolute pressure (P ₂₎ ratio (P ₂ / P _1).

Figure 7c is a graph showing the distribution of the change in injection speed, pressure and temperature according to the cross-sectional position of the supersonic nozzle.

8A is a cross-sectional view of an improved supersonic nozzle capable of supplying a solid powder to the rear of the supersonic nozzle neck.

8B is a graph showing the temperature behavior and the speed change of the conveying gas and the solid powder generated when the solid powder at room temperature is supplied to the latter part of the supersonic nozzle neck.

8C is a schematic diagram for coating the three-dimensional shape by placing the supersonic nozzle of FIG. 8A in a vacuum deposition chamber.

FIG. 8D is a schematic diagram for coating a large area substrate having a two-dimensional shape by placing the slit-type supersonic nozzle of FIG. 8A in a vacuum deposition chamber.

9 is a graph showing the pressure (P) changes according to the nozzle exit transport gas and solid phase between powder is the temperature (T _s) of the substrate temperature (T _e) of an aerosol of a mixture formed and the nozzle and the substrate distance (D) in to be.

<Description of Codes for Main Parts of the Invention>

A: Air supply part and air pressurization part B: Air processing part

C: Transfer gas heating thermostat part D: Solid powder supply part

E: Solid powder cooling temperature controller

F: Aerosol injection deposition part G: Solid powder dust collection part

H: system control unit

10: air pump 11: air storage tank

12: 1st filter 13: 1st dryer

13-1: Secondary filter 14: Moisture filter

15 oil filter 16 dust filter

17: secondary dryer 18: flow controller

19: flow regulator 20: block chamber lower connection pipe

21: solid powder supply device 22: heat insulation transport pipe

23: pressure measuring instrument 24: length adjusting device

25: injection nozzle 26: vacuum deposition chamber

27: substrate 28: transfer device

29: vacuum connection pipe 30: pressure control valve

31: vacuum pump 34: flow control valve

35: insulated transport pipe and spray nozzle connection

40: air intake 41: solid powder supply path

100: pressure device 101: pressure tube

102: transfer gas heating temperature control device 103: solid powder cooling temperature control device

104: opening 105: solid powder

106: transfer gas 107: aerosol of solid powder and air

108: solid powder dust collection unit 109: adiabatic cooling tube

110: solid-state powder dust collection connector 111: block chamber

200: supersonic nozzle 201: supersonic nozzle inlet

202: Supersonic nozzle neck 203: Supersonic nozzle exit

205: square cross section of the supersonic nozzle 206: circular cross section of the supersonic nozzle

300: subsonic nozzle 301: subsonic nozzle inlet

302: subsonic nozzle outlet 303: slit type subsonic nozzle

304: square cross section of a subsonic nozzle 305: circular cross section of a subsonic nozzle

306: Slit-type supersonic nozzle 400: nozzle position controller

401: three-dimensional object position control table 402: three-dimensional object

403: vacuum chuck 404: substrate temperature control insulation tube

405: substrate temperature control device 500: system control device

Claims (32)

An air supply unit configured of an air pump and an air storage tank; An air pressurizing unit for adding pressure to air supplied from the air supply unit; An air processor for filtering and drying the pressurized air provided from the air supply unit and the air pressurizing unit to discharge the filtered air; Solid powder supply unit for supplying a solid powder in a predetermined amount to the air discharged through the air processing unit; A vacuum deposition chamber in which a substrate is located inside and discharging the air through a vacuum pump connected by a vacuum connection tube to maintain the interior in a vacuum state; An insulating transport pipe for connecting the air processing unit and the vacuum deposition chamber, the aerosol formed by mixing the solid powder supplied from the solid powder supply unit with the air discharged from the air processing unit to the vacuum deposition chamber; The transfer gas heating is installed in the adiabatic transport pipe located between the air processing unit and the solid powder supply unit and heats the air discharged and transferred from the air processing unit before the solid powder is mixed to form an aerosol to control the temperature of the air. Temperature control unit; An injection nozzle provided at an end of the adiabatic transport pipe and configured to inject the aerosol to a substrate positioned inside the vacuum deposition chamber; And Is connected to each of the components, the temperature control device characterized in that it comprises a system control unit for controlling the conditions, such as pressure, speed, flow rate, temperature, etc. of the transfer gas and solid state powder to each component Solid-phase powder vacuum deposition apparatus provided. In claim 1, And a flow control valve disposed between the air pump and the air storage tank, and between the air storage tank and the air processing unit, respectively. In claim 1, And a flow controller installed between the air processing unit and the adiabatic transport pipe and configured to discharge and regulate the flow rate of the filtered and dried air uniformly. 4. The method of claim 3, The air processing unit is a solid-state with a temperature control device, characterized in that the primary filter, the primary dryer, the secondary filter and the secondary dryer are sequentially configured to perform filtering and drying treatment of the incoming air repeatedly Powder vacuum deposition system. In claim 4, The secondary filter is a solid-phase powder vacuum deposition apparatus having a temperature control device, characterized in that consisting of a water filter, an oil filter, and a dust filter. In claim 5, A water filter installed between the secondary dryer and the flow controller; And a flow control valve disposed between the primary filter and the primary dryer and between the moisture filter and the flow regulator, respectively. In claim 1, The solid powder supply unit is connected to the front of the discharge port of the solid powder supply device and the solid powder supply device that uniformly regulates the amount of solid powder supplied per unit time and evenly distributes the solid powder, the air can be introduced into the upper portion The solid-state powder vacuum deposition apparatus with a temperature control device, characterized in that the opening is formed so that it consists of a block chamber to suck the solid powder provided to the insulation transport pipe through the pressure difference. In claim 7, The solid powder supply unit is a solid powder vacuum with a temperature control device, characterized in that the one side is further connected to the lower portion of the block chamber and the other side is connected to the lower chamber chamber connecting tube is in communication with the heat insulating transport pipe Vapor deposition apparatus. In claim 8, It is installed in the opening located in the upper portion of the block chamber and solid-phase powder vacuum deposition with a temperature control device characterized in that it further comprises a pre-treatment device for removing moisture and impurities in the air introduced into the block chamber Device. In claim 1, Temperature control device, characterized in that further comprises a flow rate meter, a pressure gauge and a temperature meter respectively installed in the insulation transport pipe to check whether the flow rate, speed and temperature of the aerosol transported through the insulation transport pipe Equipped with a solid powder vacuum deposition apparatus. In claim 10, The solid-phase powder vacuum deposition apparatus provided with the temperature control device is installed in the insulation transport pipe and further comprising a length adjusting device to adjust the distance between the injection nozzle and the substrate by adjusting the length of the insulation transport pipe. . In claim 1, When the elbow is formed in the middle of the adiabatic transport pipe is installed in the initial portion of the elbow is provided with a temperature control device characterized in that it further comprises a flow regulator for maintaining a constant feed rate of the transfer gas Solid powder vacuum deposition system. In claim 1, When the diameter of the middle portion of the insulation transport tube is expanded, the temperature control, characterized in that it is installed on the inner wall of the insulation transport pipe further comprises a flow regulator to maintain a uniform flow rate distribution over the front end surface of the transport pipe Solid powder vacuum deposition apparatus equipped with a device. In claim 1, The spray nozzle is a solid-phase powder vacuum deposition apparatus equipped with a temperature control device, characterized in that the subsonic nozzle or supersonic nozzle. The method of claim 14, The subsonic nozzle is a solid-phase powder vacuum deposition apparatus equipped with a temperature control device, characterized in that the cross-sectional area is narrowed toward the nozzle outlet from the nozzle inlet. The method of claim 14, The supersonic nozzle is a solid-phase powder vacuum deposition apparatus having a temperature control device, characterized in that the cross-sectional area is reduced from the nozzle inlet to the nozzle neck, the cross-sectional area is larger from the nozzle neck to the nozzle outlet. In claim 1, Is connected to the vacuum deposition chamber through a substrate temperature control heat insulating tube and the solid state powder with a temperature control device characterized in that it further comprises a substrate temperature control device for controlling the temperature of the substrate in conjunction with the system control unit Vacuum deposition equipment. The method of claim 17, The substrate temperature control device is a solid-phase powder vacuum deposition apparatus having a temperature control device, characterized in that for controlling the temperature of the substrate located inside the vacuum deposition chamber lower than the temperature of the injection nozzle outlet. In claim 1, Solid-phase powder vacuum deposition apparatus is installed in the vacuum deposition chamber and further comprising a transfer device for moving the substrate. In claim 1, It is installed under the substrate of the vacuum deposition chamber, the lower portion of the substrate by vacuum adsorption fixed to the vacuum chuck to suppress the generation of shaking of the substrate by aerosol injection is provided with a temperature control device Solid powder vacuum deposition system. In claim 1, It is installed between the vacuum deposition chamber and the vacuum pump and the solid-state powder vacuum deposition apparatus provided with a temperature control device further comprises a pressure control valve for efficiently maintaining and controlling the vacuum state of the vacuum deposition chamber . In claim 1, Solid powder which is capable of collecting and recovering a small amount of solid powder remaining after being deposited on a substrate in the vacuum deposition chamber recovered through the solid powder dust collection and recovery pipe connected to the vacuum pump and the solid powder dust collection and recovery pipe Solid-phase powder vacuum deposition apparatus having a temperature control device, characterized in that further comprises a solid-state powder dust collection recovery portion consisting of a dust collection and the air exhauster. The method according to any one of claims 1 to 22, Located between the solid powder supply unit and the insulated transport pipe, the solid powder cooling temperature control device and the cooled solid powder to cool the temperature of the solid powder supplied through the block chamber lower connection pipe while maintaining the cooled temperature Solid powder vacuum equipped with a temperature control device characterized in that it further comprises a solid powder cooling temperature control unit consisting of a heat insulation cooling tube in the form of a pipe passing through the insulation transport pipe so that the outlet is supplied to the insulation transport pipe. Vapor deposition apparatus. The method of claim 23, And the adiabatic cooling tube is in communication with the adiabatic transport tube located at the inlet side of the vacuum deposition chamber. The method of claim 16, A solid powder supply path is formed between the nozzle neck of the supersonic nozzle and the nozzle outlet through one side of the nozzle body from the outside to the inside of the nozzle, and the other side of the block chamber lower connection pipe communicates with the solid powder supply path. The solid state powder supplied directly into the nozzle through the supply passage is mixed with the air accelerated at supersonic speed through the nozzle neck to form an aerosol and then sprayed on the substrate at supersonic speed. Solid powder vacuum deposition system. (a) inhaling and storing air; (b) pressurizing air; (c) filtering and drying the sucked air to transfer a predetermined amount; (d) heating the air that has undergone the step (c); (e) supplying a solid powder to the air which has undergone the step (d) to form aerosol mixed and dispersed at a constant mixing density, and transferring the solid powder to the injection nozzle; And (f) solid-phase powder vacuum deposition method comprising the step of injecting the aerosol to the substrate provided in the vacuum deposition chamber in a vacuum state at a subsonic or supersonic speed through a spray nozzle. The method of claim 26, Wherein (e) is a solid powder vacuum deposition method characterized in that the step of supplying the solid powder to the heated air conveyed through the adiabatic transport pipe to form a mixed aerosol dispersed and transported to the injection nozzle. The method of claim 27, The step (e) is a solid-phase powder vacuum deposition method characterized in that the aerosol is continuously controlled to have a constant speed, flow rate, mixing density and conveyed to the injection nozzle. The method of claim 27, Wherein (e) is a solid powder vacuum deposition method further comprises the step of cooling the solid powder before supplying the solid powder to the heated air conveyed through the adiabatic transport pipe. The method of claim 26, The step (e) is a process of forming aerosol dispersed between the nozzle neck and the nozzle outlet by directly supplying and mixing the solid powder into the nozzle in the air transferred to the supersonic speed toward the nozzle outlet through the nozzle neck of the supersonic nozzle. Solid-phase powder vacuum deposition method characterized in that. The method of claim 30, The step (f) is a solid-phase powder vacuum deposition method, characterized in that for spraying the aerosol to the substrate provided in the vacuum deposition chamber in a vacuum state at a supersonic speed through the injection nozzle. The method of any one of claims 26 to 31, After the step (f) is a solid-phase powder vacuum deposition method characterized in that it further comprises the step of collecting and recovering a small amount of solid powder remaining in the vacuum deposition chamber after deposition.

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