TWI698399B - Metal chloride generating device and method for manufacturing metal powder - Google Patents

Abstract

To provide a method to prevent damage or destruction of the manufacturing device and to stably manufacture metal powder, a metal chloride generating device capable of realizing this method, and a metal powder manufacturing system including the metal chloride generating device. The metal chloride generation device has: a chlorination furnace equipped with "a first heating furnace with a metal inlet for introducing metal" and a "second heating furnace connected to the first heating furnace", and heating the first heating furnace The first heater and the second heater that heats the second heating furnace. The second heating furnace has a discharge port for discharging metal chloride gas. The chlorination furnace has a first gas inlet for introducing chlorine-containing gas, and the first gas inlet is surrounded by either the first heater and the second heater.

Description

Metal chloride generating device and manufacturing method of metal powder

One of the embodiments of the present invention relates to a metal chloride generating device, a system for producing metal powder, and a method for producing metal powder using this system.

Fine metal particles (metal powders) have been used in various fields. For example, powders of metals exhibiting high conductivity such as copper, nickel, and silver have been widely used as internal electrodes for stacked ceramic capacitors (MLCC). The original material of the part. Although several methods of producing such metal powders are known, a gas phase method can be cited as an example. In this method, as disclosed in Patent Documents 1 and 2, for example, a metal chloride gas is brought into contact with a reducing gas such as hydrogen and reduced to form a metal powder.

『Patent Literature』 "Patent Document 1": Japanese Patent Publication No. H6-76609 "Patent Document 2": Japanese Patent Publication No. H10-219313

One of the problems of one of the embodiments of the present invention is to provide a method for preventing damage or destruction of the manufacturing device and stably manufacturing metal powder, a metal chloride generating device that can realize this method, and a metal chloride generating device containing The manufacturing system of the metal powder of the device.

One of the embodiments related to the present invention is a metal chloride generating device. This metal chloride generator has: a chlorination furnace equipped with "a first heating furnace with a metal introduction port for introducing metal" and a "second heating furnace connected to the first heating furnace", and a first heating furnace The first heater for heating and the second heater for heating the second furnace. The second heating furnace has a discharge port for discharging metal chloride gas. The chlorination furnace has a first gas inlet for introducing chlorine-containing gas, and the first gas inlet is surrounded by either the first heater and the second heater.

One of the embodiments related to the present invention is a metal chloride generating device. This metal chloride generating device has a first heating furnace that "has a metal introduction port for introducing metal and a gas introduction port for introducing nitrogen", connected to the first heating furnace, and has a chloride for metal The second heating furnace at the discharge outlet, the first heater for heating the first heating furnace, the second heater for heating the second heating furnace, and the third heater for heating nitrogen.

One of the related embodiments of the present invention is a method of manufacturing metal powder. This method includes: in a chlorination furnace constructed by heating by a first heater and a second heater, reacting metal with chlorine gas to generate chlorides of the metal, and self-installing in the chlorination furnace 1 The gas inlet introduces chlorine-containing gas and transports the chloride vapor to the reduction furnace. The first gas inlet is surrounded by either the first heater and the second heater.

One of the related embodiments of the present invention is a method of manufacturing metal powder. The method includes: introducing heated nitrogen into a chlorination furnace and simultaneously reacting metal and chlorine gas in the chlorination furnace to generate metal chloride, and using a chlorine-containing gas to transport the chloride vapor to the reduction furnace.

One of the embodiments related to the present invention is a metal chloride generating device. This metal chloride generating device has a chlorination furnace equipped with "a first heating furnace with a metal introduction port for introducing metal" and a "second heating furnace connected to the first heating furnace". The second heating furnace has a discharge port for discharging metal chloride gas and a first gas introduction port for introducing chlorine-containing gas.

One of the embodiments related to the present invention is a metal chloride generating device. This metal chloride generation device has a chlorination furnace equipped with a "first heating furnace" and a "second heating furnace connected to the first heating furnace". The first heating furnace has a metal introduction port for introducing metal and a first gas introduction port for introducing chlorine-containing gas. The second heating furnace has a discharge port for discharging metal chloride gas. The first gas introduction port is closer to the connection part of the first heating furnace and the second heating furnace than the metal introduction port for introducing metal. The metal chloride generating device may further have a first heater for heating the first heating furnace. In addition, the first gas inlet may be surrounded by the first heater.

Hereinafter, each embodiment of the present invention will be described with reference to the drawings. However, the present invention can be implemented in various forms within the scope not departing from the gist thereof, and is not limited to the explanation by the description of the following example implementation forms.

The drawing is to make the description clearer. Compared with the actual state, the drawings show schematic representations of the width, thickness, shape, etc. of each part, but it is an example after all and does not limit the interpreter of the present invention. In this specification and the figures, the same reference numerals are sometimes attached to elements that have the same functions as those described in the figures that have already appeared, and repeated descriptions are omitted.

In this specification and the scope of the patent application, when the state of "arranging other structures on or under a certain structure" is simply described as "up" or "down", unless otherwise noted, it is defined as Including: the case where other structures are arranged directly above or below by contacting a certain structure, and the case where other structures are arranged above or below a certain structure by interposing another structure. In addition, the arrangement of the above-mentioned structure is mainly explained based on the movement sequence of the metal chloride gas, and it also includes the case where the structure called the upper and the structure called the lower are positioned horizontally, for example.

(First implementation type)

The metal chloride generating device 110 and the metal powder manufacturing system (hereinafter referred to as the system) 100 including the metal chloride generating device 110 related to one of the embodiments of the present invention will be described.

1. Overall structure

The outline of the structure of the system 100 is shown in FIG. 1. The system 100 includes a metal chloride generator 110 and a reduction furnace 200 as main structures. Although not shown, the system 100 may further include a separation device 300 connected to the reduction furnace 200, or a recovery device such as a bag filter connected to the reduction furnace 200 or the separation device 300. The metal chloride generating device 110 and the reduction furnace 200 are connected by a first transfer pipe 112, and the reduction furnace 200 and the separation device 300 are connected by a second transfer pipe 202.

The metal chloride generating device 110 has a function of generating a metal chloride (hereinafter referred to as a chloride) by the reaction of a zero-valent metal and chlorine gas as one of the functions. The chloride exists as a gas (vapor) in the metal chloride generating device 110, and a part of it exists as a liquid depending on the type of metal or reaction conditions. The chloride vapor is introduced into the reduction furnace 200 through the first delivery pipe 112. As the metal, copper, silver, nickel, etc. can be used. The shape of the metal used is not limited, and metals in the form of particles, wires, and plates can be used, for example.

The reduction furnace 200 is connected to the first delivery pipe 112 and has a gas introduction port (fifth gas introduction port) 204 for introducing the chloride vapor delivered from the metal chloride generation device 110 into the reduction furnace 200. The reduction furnace 200 is further provided with a gas introduction port (sixth gas introduction port) 206 for introducing hydrogen, hydrazine, ammonia, methane, etc., which are reducing gases used for chloride reduction. In the reduction furnace 200, the chloride is reduced, thereby generating metal powder. In the reduction furnace 200, an inert gas such as nitrogen is introduced from an external intermediary gas inlet (not shown), and the produced metal powder is transported to the separation device 300 or the recovery device through the second transport pipe 202 while being cooled.

Although detailed description is omitted, the separation device 300 has a function of purifying the metal powder by removing the agglomerates contained in the metal powder or the sintered product of the metal by-produced in the reduction furnace 200. The recovery device is configured to separate the purified metal powder from nitrogen separately. Although not shown in detail in FIG. 1, as described later, the metal chloride generating device 110 is provided with a gas introduction port for introducing various gases.

2. Metal chloride generator

A schematic cross-sectional view of the metal chloride generating device 110 is shown in FIG. 2. The metal chloride generating device 110 has a chlorination furnace 120, and a first heater 160 and a second heater 162 provided to surround the chlorination furnace 120 and heat the chlorination furnace 120 as main structures. The first heater 160 and the second heater 162 can be independently controlled.

The chlorination furnace 120 includes a first heating furnace 122 and a second heating furnace 124. In the example shown in FIG. 2, although the second heating furnace 124 is located below the first heating furnace 122, the first heating furnace 122 and the second heating furnace 124 may be arranged horizontally. In addition, the reduction furnace 200 may also be installed under the first heating furnace 122 or the second heating furnace 124 (refer to FIG. 1), or may be arranged horizontally. In addition, in the example shown in FIG. 2, the inner diameter of the connecting portion 123 of the first heating furnace 122 and the second heating furnace 124 is smaller than the other parts, but as shown in FIG. 3, from the first heating furnace 122 to the second heating furnace The inner diameters of the heating furnace 124 and the chlorination furnace 120 are the same. Alternatively, the inner diameters of the first heating furnace 122 and the second heating furnace 124 may be different.

The chlorination furnace 120 may have the partition member 126 (refer FIG. 3) which distinguishes the 1st heating furnace 122 and the 2nd heating furnace 124 as an arbitrary structure. That is, the chlorination furnace 120 may include a first heating furnace 122 and a second heating furnace 124 connected to the first heating furnace 122 by the partition member 126. The partition member 126 is provided with at least one opening, whereby the gas introduced into the first heating furnace 122 or the second heating furnace 124 and the vapor of the chloride generated therefrom can pass through the partition member 126. Although detailed description is omitted, the number, size, arrangement, etc. of the openings may be appropriately designed in consideration of reaction conditions, the vapor pressure of the chloride, and the shape or size of the metal used. In addition, in the case of generating molten chloride, the partition member 126 may be designed such that the liquid chloride can pass through the partition member 126. In FIG. 3, a state where metal particles 114 are made and arranged on the partition member 126 in the first heating furnace 122 is shown.

As the material used in the chlorination furnace 120, quartz or ceramics can be used, and the melting point of the metal or its chloride can be considered. Examples of materials used for the partition member 126 include metal or semimetal oxides such as quartz, alumina, and zirconia, nitrides such as ceramics, and boron nitride, graphite, and the like.

As shown in FIG. 2, the first heating furnace 122 has a metal introduction port 128 for introducing metal into the first heating furnace 122. The chlorine-containing gas used for chlorination may be introduced into the first heating furnace 122 using the metal inlet 128. Alternatively, a gas introduction port (third gas introduction port) 130 may be provided as an arbitrary structure, and the valve 132 may be interposed to introduce chlorine-containing gas. The chlorine-containing gas may also include nitrogen or inert gases such as argon and helium for diluting chlorine. By using a gas containing inert gas and chlorine (hereinafter also referred to as mixed gas), the amount of chlorine can be easily and precisely controlled. In the example shown in FIG. 2, the third gas introduction port 130 is surrounded by the first heater 160, but the third gas introduction port 130 may be exposed from the first heater 160 instead of being surrounded by the first heater 160.

The first heating furnace 122 is heated by the first heater 160, and the metal arranged in the first heating furnace 122 reacts with the chlorine gas introduced from the metal inlet 128 and/or the third gas inlet 130 to produce metal chlorine化物. Depending on the type of metal, the chloride is a gas (vapor) in the chlorination furnace 120, or a state of equilibrium between gas and liquid is achieved. In the latter case, part of the chloride system is in a molten state, and part of it is present as vapor. The vapor of the molten chloride and the chloride generated in the first heating furnace 122 moves to the second heating furnace 124 by the intermediary connecting portion 123 (when the partition member 126 is provided, the hole is opened).

The second heating furnace 124 has the function of "transmitting the vapor of the chloride generated in the first heating furnace 122 to the reduction furnace 200" and "when generating molten chloride, it is vaporized to generate the vapor of chloride. The main function is to transport it to the reduction furnace 200". The second heating furnace 124 is surrounded and heated by the second heater 162. As described above, the first heater 160 and the second heater 162 are independently controlled, and the first heating furnace 122 and the second heating furnace 124 can be heated at different temperatures, respectively. The first heater 160 and the second heater 162 are driven so that the temperature of the second heating furnace 124 is higher than the temperature of the first heating furnace 122. For example, by controlling the temperature of the first heating furnace 122 and the second heating furnace 124 so that the temperature of the second heating furnace 124 is as high as 200-300°C, even when molten chloride is generated, the temperature of the first heating furnace When the furnace 122 moves to the second heating furnace 124, the chloride can still be rapidly vaporized in the second heating furnace 124.

In addition, in order to efficiently vaporize the molten chloride, the second heating furnace 124 may be filled with the vaporization auxiliary material 140. As the gasification auxiliary material 140, particles or particles containing metal or semi-metal oxides such as quartz, aluminum oxide, and zirconium oxide, ceramics, nitrides such as boron nitride, and graphite. With a large heating area to vaporize molten chloride.

The second heating furnace 124 has a discharge port 134 for conveying the chloride vapor generated in the first heating furnace 122 or the second heating furnace 124 to the reduction furnace 200. Furthermore, in the chlorination furnace 120, in more detail, at least any one of the first heating furnace 122 and the second heating furnace 124 is provided with a gas introduction port (first gas introduction port) for introducing chlorine-containing gas ) 136. The first gas introduction port 136 may be arranged so as to surround either the first heater 160 and the second heater 162. In the example shown in FIG. 2, the first gas inlet 136 is provided in the second heating furnace 124 and is surrounded by the second heater 162. The first gas inlet 136 further mediates the valve 138 and is connected to a chlorine gas source (gas cylinder, etc.) not shown. The chlorine-containing gas introduced through the first gas inlet 136 may also include an inert gas.

It is desirable that the discharge port 134 for transporting the chloride vapor to the reduction furnace 200 is arranged at a position higher than the bottom of the second heating furnace 124. This is to prevent the molten chloride from flowing into the reduction furnace 200 in an unvaporized state.

When the first gas introduction port 136 is provided in the second heating furnace 124, the first gas introduction port 136 may be arranged at a position lower than the discharge port 134 (a position farther from the first heating furnace 122). This is because the molten chloride tends to accumulate in the lower part of the second heating furnace 124, so by introducing the chlorine-containing gas from the lower part of the second heating furnace 124, the chloride gas can be efficiently sent to the discharge port 134 Because of the import.

The chlorine-containing gas introduced from the metal inlet 128 or the first gas inlet 136 and the third gas inlet 130 applies a positive pressure to the chlorination furnace 120. The function is that the chloride vapor generated in the chlorination furnace 120 is introduced into the first delivery pipe 112 through the positive pressure intermediate discharge port 134 and delivered to the reduction furnace 200. All or most of the chlorine introduced from the metal inlet 128 or the third gas inlet 130 is consumed by the reaction with the metal. However, the chlorine introduced from the first gas introduction port 136, if compared with the chlorine introduced from the metal introduction port 128 or the third gas introduction port 130, contributes less to the reaction with the metal and has a lower consumption rate. Therefore, the vapor of the chloride comes into contact with at least the chlorine added through the first gas inlet 136 and is sent to the reduction furnace 200 at the same time.

As described above, the chloride delivered to the reduction furnace 200 is reduced in the reduction furnace 200 to produce metal powder. The obtained metal powder is further transported to the separation device 300 and purified, and further separated separately by the recovery device.

3. The contribution of chlorine

In the metal chloride generating device 110 of the system 100 of this embodiment, the intermediary metal inlet 128 or the third gas inlet 130 introduces a gas containing chlorine. This gas system is introduced in order to provide positive pressure for chlorinating the metal and for transporting the vapor of the generated chloride to the second heating furnace 124.

On the other hand, in the metal chloride generating device 110, the gas containing chlorine is further introduced into the second heating furnace 124 through the first gas introduction port 136, and a positive pressure is applied to the chlorination furnace 120. Thereby, the vapor of chloride can be efficiently sent to the exhaust port 134, and the vapor of chloride can be quickly transported to the reduction furnace 200. As a result, it is possible to suppress defects such as the chloride remaining in the second heating furnace 124 or the solidification and precipitation of the chloride in the second heating furnace 124 or the first conveying pipe 112. In addition, it is also possible to prevent the reducing gas introduced into the reduction furnace 200 through the sixth gas inlet 206 from flowing back through the first delivery pipe 112 at the same time. The function is to prevent the defects in the first conveying pipe 112 that the chloride is reduced and the metal is deposited, which causes the first conveying pipe 112 to be blocked and damaged.

Here, the chlorine-containing gas introduced through the first gas inlet 136 not only functions as a physical means for imparting a positive pressure for simply introducing the chloride vapor intermediate outlet 134 into the reduction furnace 200 as described above, but also It functions as a chemical means to more effectively prevent defects in the system 100 as described below.

Metal and chloride exist in an equilibrium state shown by the following formula. "Hua 1"

For example, when the metal is copper, the following balance holds. "Hua 2"

Although it depends on the type or temperature of the metal, even if it is assumed that the metal is completely changed to chloride in the chlorination furnace 120, due to the existence of this equilibrium, part of the chloride will still be changed back to metal. The problem is that metal will precipitate in the second heating furnace 124 or the first conveying pipe 112, which is a major cause of clogging.

However, the inventor found that by introducing chlorine gas due to this equilibrium system, the equilibrium is shifted to the right side (chloride side) to prevent gaseous chlorides from being precipitated as metals. That is, the chlorine introduced through the first gas inlet 136 is almost not consumed by the chlorination of the metal that has been put in the first heating furnace 122, so it can be combined with the second heating furnace 124 or the first conveying pipe 112 Contact with chloride vapor. The role is that the chlorine introduced through the first gas inlet 136 contributes as a chemical means to shift the balance between the metal and the chloride to the chloride side. As a result, it is possible to more effectively suppress defects such as clogging or breakage of the first conveying pipe 112 due to metal precipitation from the chloride gas in the second heating furnace 124 or the first conveying pipe 112, and destruction of the second heating furnace 124.

By introducing chlorine-containing gas from the first gas inlet 136 not only by physical means, but also by chemical means, it is possible to provide a metal powder manufacturing system that can be driven stably for a long time without breakage or damage. By using this system, metal powder can be produced efficiently.

4. Modifications

The metal chloride generating device 110 is not limited to the structure shown in FIG. 2 or FIG. 3. For example, as shown in FIG. 4, the chlorination furnace 120 may have a plurality of gas inlets for "supplying a gas containing chlorine that functions as a chemical means". Chlorine gas can be supplied with inert gas. In the example shown in FIG. 4, the second heating furnace 124 is further provided with a gas introduction port (second gas introduction port) 142 for introducing chlorine-containing gas. The second gas introduction port 142 may be arranged above the discharge port 134. That is, the second gas introduction port 142 may be provided so that the distance from the first heating furnace 122 to the discharge port 134 is larger than the distance from the first heating furnace 122 to the second gas introduction port 142. The second gas inlet 142 is connected to a chlorine source not shown, and the supply of chlorine-containing gas is controlled by a valve 144.

By adopting this structure, the contribution as a chemical means can be increased, and the precipitation of metal in the second heating furnace 124 or the first conveying pipe 112 can be prevented more effectively.

Alternatively, as shown in FIG. 5, the metal chloride generating device 110 may have a gas introduction port (fourth gas introduction port) 146 and a third heater 164 for introducing the heated inert gas. The fourth gas introduction port 146 is provided in the first heating furnace 122, and the intermediate valve 148 is connected to the third heater 164. The third heater has a function of heating the inert gas.

By supplying the heated inert gas to the first heating furnace 122, a larger positive pressure can be applied in the chlorination furnace 120 without causing the temperature of the first heating furnace 122 to drop. The job is that all or most of the chloride generated in the first heating furnace 122 becomes able to maintain a gas state and is introduced from the second heating furnace 124 to the reduction furnace 200 via the first transfer pipe. When the boiling point of the chloride is high, the gasification in the second heating furnace 124 takes a relatively long time. Therefore, this structure is particularly effective when producing metal powders that produce chlorides with a high boiling point.

In addition, when the fourth gas introduction port 146 and the third heater 164 are provided, it is not necessary to provide the first gas introduction port 136 or the second gas introduction port 142 (see FIG. 6). In the case where the boiling point of the chloride is relatively low, by adopting this structure, the system 100 can be efficiently driven, and the manufacturing cost of the system 100 can be reduced, thereby, the metal powder can be provided at low cost.

(The second implementation type)

In this embodiment, a method of manufacturing metal powder using the system 100 is described. Here, the system 100 equipped with the metal chloride generating device 110 shown in FIG. 2 is used to illustrate the method of manufacturing metal powder as an example. The description of the structure that is the same as or similar to the structure described in the first embodiment is sometimes omitted.

First, the intermediary metal introduction port 128 puts metal into the first heating furnace 122. As mentioned above, as the metal, copper, silver, nickel, etc. can be used. The second heating furnace 124 may also be filled with the auxiliary gasification material 140 in advance.

Here, the first heater 160 and the second heater 162 are used to heat the first heating furnace 122 and the second heating furnace 124, respectively. Although the temperature of the first heating furnace 122 depends on the type of metal, it can be appropriately set in the range of, for example, 800°C or higher and 1000°C or lower. By setting the temperature of the first heating furnace 122 to a temperature lower than the melting point of the metal, it is possible to prevent the metal as the raw material (metal particles 114) from melting. In the first heating furnace 122, metal reacts with chlorine to produce chloride.

On the other hand, the temperature of the second heating furnace 124 may be set higher than the temperature of the first heating furnace 122. Although it depends on the type of metal, it can be appropriately set in the range of, for example, 900°C or higher and 1200°C or lower. By setting the temperature of the second heating furnace 124 to a temperature higher than the boiling point of the chloride, the chloride can be quickly vaporized.

Simultaneously with the heating of the first heating furnace 122 and the second heating furnace 124, a chlorine-containing gas is introduced into the second heating furnace 124 through the first gas introduction port 136. In addition, the intermediary metal inlet 128 and/or the third gas inlet 130 introduce chlorine-containing gas into the first heating furnace 122. When the chlorine-containing gas introduced into the second heating furnace 124 through the first gas inlet 136 is mixed with an inert gas, for example, the chlorine concentration in the mixed gas is adjusted to 0.001 wt% or more and 20 wt% or less, or 0.01 wt% or more and 10 wt% or less, or 0.1 wt% or more and 2 wt% or less. The flow rate of these gases can be adjusted appropriately according to the ratio. When the second gas inlet 142 (refer to FIG. 4) is used to introduce the chlorine-containing gas, the composition or total flow rate of the chlorine-containing gas introduced through the first gas inlet 136 and the second gas inlet 142 can be They are the same or different from each other. For example, the flow rate of the chlorine-containing gas introduced through the first gas introduction port 136 may be greater than the flow rate of the chlorine-containing gas introduced through the second gas introduction port 142. The amount of chlorine in the chlorine-containing gas introduced into the second heating furnace 124 via the first gas introduction port 136 or the second gas introduction port 142 is more than that of the intermediary metal introduction port 128 and/or the third gas introduction port 130. It is preferable that the amount of chlorine contained in the chlorine-containing gas of the first heating furnace 122 is small. Thereby, the chlorine content of the obtained metal powder can be reduced.

In addition, in the example shown in FIGS. 4 and 5, when the heated nitrogen gas is introduced into the first heating furnace 122, the temperature of the nitrogen gas may be adjusted to, for example, 800°C or more and 1000°C or less.

The vapor of the chloride generated in the chlorination furnace 120 is discharged from the discharge port 134 and is introduced into the reduction furnace 200 from the fifth gas inlet 204 through the first delivery pipe 112. A reducing gas system selected from hydrogen, hydrazine, ammonia, methane, etc. is supplied from the sixth gas inlet 206 (see FIG. 1), and the flow rate or concentration thereof may be adjusted so as to be at least the stoichiometric ratio of the reaction with chloride. The metal powder generated in the reduction furnace is physically separated by the nitrogen introduced into the reduction furnace 200 to a recovery device (not shown) such as a separator 300 or a bag filter. Through the above process, metal powder can be produced.

As described in the first embodiment, the chlorine-containing gas introduced into the second heating furnace 124 from the first gas introduction port 136 or the second gas introduction port 142 not only provides rapid and stable delivery of the chloride vapor to the reduction furnace 200 As a physical means, the transport function also has the function of preventing metal precipitation as a chemical means. The job is to provide a metal powder manufacturing system that can be stably driven and can efficiently manufacture metal powder by applying this embodiment.

(The third implementation type)

In this embodiment, the structure of the metal chloride generating device 116 having a structure different from that of the metal chloride generating device 110 will be described. The description of the structure that is the same as or similar to the structure described in the first embodiment is sometimes omitted.

The metal chloride generating device 116 differs in structure from the metal chloride generating device 110 at least in that the inner diameters of the first heating furnace 122 and the second heating furnace 124 are different, and the second heating furnace 124 has a tube shape.

More specifically, as shown in FIG. 7, the second heating furnace 124 has a tube shape, and its inner diameter is smaller than that of the first heating furnace 122. By making it into such a shape, the vapor of the chloride and the chlorine gas can be mixed more effectively, and the physical and chemical effects of the chlorine-containing gas introduced through the first gas introduction port 136 are increased.

The first gas inlet 136 is provided in the first heating furnace 122 and is surrounded by the first heater 160. The first gas inlet 136 is preferably arranged to be closer to the second heating furnace 124 than the metal inlet 128. This is because when molten chloride is generated, the chloride will accumulate in the lower part of the first heating furnace 122, and vaporization will occur preferentially in this part. Therefore, as shown in FIG. 7, it is preferable to arrange the vaporization auxiliary material 140 in the first heating furnace 122 so that the upper surface is located above the first gas introduction port 136. The particles 114 may be arranged on the gasification auxiliary material 140 in a manner in contact with the gasification auxiliary material 140.

In this structure, the first heater 160 and the second heater 162 are driven to heat the chlorination furnace 120, and chlorine-containing gas is introduced from the metal inlet 128 and/or the third gas inlet 130, whereby the metal and The reaction of chlorine gas takes place to produce chloride. The chloride present as vapor moves to the second heating furnace 124 through the gap of the gasification auxiliary material 140. On the other hand, the liquid chloride in the molten state absorbs the heat energy supplied from the first heater 160 while immersing the layer of the gas-permeable auxiliary material 140 to vaporize, and then moves to the second heating furnace 124. In this way, in the metal chloride generating device 116, the generation of chloride and the vaporization of the chloride in the molten state occur in the first heating furnace 122.

Like the metal chloride generating device 110, the chlorine-containing gas introduced from the first gas inlet 136 can not only physically introduce the chloride vapor into the second heating furnace 124, but also chemically prevent the chloride from depositing metal. The job is that in the tubular second heating furnace 124, the precipitation of metals or chlorides can also be effectively suppressed, the system 100 can be operated stably without causing damage or damage, and metal powder can be efficiently provided.

Furthermore, as shown in FIG. 7, by folding the second heating furnace 124 in a tubular shape, the total length can be increased without incurring an increase in the occupied area. When the boiling point of the chloride is high, the gasification in the second heating furnace 124 takes a relatively long time, so this structure is particularly effective when producing metal powders that produce chlorides with a high boiling point.

"Example"

(Example 1)

In this embodiment, an example of manufacturing copper powder using the system 100 "equipped with the metal chloride generating device 110 having the structure shown in FIG. 2 as a basic structure" is described. Specifically, copper pellets are placed in the first heating furnace 122, and quartz pellets are placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 are used, and heating is performed so that the first heating furnace 122 and the second heating furnace 124 become 900°C and 1150°C, respectively. The mixed gas containing nitrogen and chlorine is introduced from the metal inlet 128 and the first gas inlet 136, respectively. The chlorine concentration of the mixed gas is shown in Table 1. Table 1 also shows that when the flow rate of the mixed gas introduced from the first gas inlet 136 is adjusted to 1.0, the ratio of the flow rate of the mixed gas introduced from the metal inlet 128 (that is, the ratio of the mixed gas introduced from the metal inlet 128) The flow rate ratio of the mixed gas to the mixed gas introduced from the first gas inlet 136). The reaction time was set at 10 hours.

"Table 1"

After the completion of the reaction, the first heater 160 and the second heater 162 were removed, and the chlorination furnace 120 was observed. As a result, the accumulation of copper chloride was not observed in the lower part of the second heating furnace 124, and it was confirmed that the damage of the second heating furnace 124 did not occur.

(Example 2)

In this embodiment, an example of manufacturing copper powder using the system 100 "equipped with the metal chloride generating device 110 having the structure shown in FIG. 4 as a basic structure" is described. Specifically, copper pellets are placed in the first heating furnace 122, and quartz pellets are placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 are used, and heating is performed so that the first heating furnace 122 and the second heating furnace 124 become 900°C and 1150°C, respectively. A mixed gas containing nitrogen and chlorine is simultaneously introduced from the metal inlet 128, the first gas inlet 136, and the second gas inlet 142. The reaction is carried out in two stages. When the flow rate of the mixed gas introduced from the first gas inlet 136 is adjusted to 1.0, the flow rate of the mixed gas introduced from the second gas inlet 142 and the metal inlet 128 and the chlorine concentration in the respective mixed gas are as follows Table 2 shows. The first gas inlet 136 and the second gas inlet 142 are connected to the same mixed gas source, and the concentrations of the components of the mixed gas introduced from these gas inlets are the same. The reaction time of the first stage and the second stage are 9 hours and 8 hours respectively.

"Table 2"

After the reaction in each stage is completed, the first heater 160 and the second heater 162 are removed, and the chlorination furnace 120 is observed. As a result, compared with Example 1, it was confirmed that the precipitation of metallic copper inside the chlorination furnace 120 was significantly reduced. In addition, it was confirmed that the precipitation of copper inside the first transfer pipe 112 also decreased.

(Example 3)

In this embodiment, the results of investigating the influence of the chlorine concentration of the mixed gas introduced from the first gas inlet 136 using the system 100 is disclosed. The system 100 is equipped with a metal chloride generating device having the structure shown in FIG. 2 as a basic structure. 110. Specifically, copper pellets are placed in the first heating furnace 122, and quartz pellets are placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 are used to heat so that the first heating furnace 122 and the second heating furnace 124 become 900°C and 1150°C, respectively. A mixed gas containing nitrogen and chlorine is introduced from the metal inlet 128 together with the first gas inlet 136. When the flow rate of the mixed gas introduced from the first gas inlet 136 is adjusted to 1.0, the flow rate of the mixed gas introduced from the metal inlet 128 is fixed to 3.2, and the chlorine concentration of the mixed gas introduced from the metal inlet 128 is fixed to 43 wt%, the concentration of chlorine in the mixed gas introduced from the first gas inlet 136 is changed as shown in Table 3. Experiment 3 in Table 3 is a comparative example in which only nitrogen is introduced from the first gas inlet 136. The reaction time was set at 10 hours.

"table 3"

As shown in Table 3, it can be seen that by introducing the chlorine-containing gas from the first gas inlet 136, copper powder of almost the same amount as the calculated value (target reaction amount) can be obtained (Experiments 1, 2). In contrast, in the case where the chlorine gas was not introduced from the first gas introduction port 136 (Experiment 3), the recovery amount deviated from the target reaction amount, and the recovery rate was low compared to Experiment 1 and Experiment 2. This incident implies that copper precipitated in the chlorination furnace 120.

After the completion of the reaction, the first heater 160 and the second heater 162 were removed, and the chlorination furnace 120 was observed. As a result, when the chlorine-containing gas is introduced from the first gas introduction port 136, copper is not precipitated in the chlorination furnace 120, or even if it precipitates, the amount does not affect the driving of the system 100. On the other hand, when the chlorine gas was not introduced from the first gas introduction port 136 (Experiment 3), it was visually observed that copper was deposited in the chlorination furnace 120.

As can be understood from Examples 1, 2, and 3, it was confirmed that by applying the implementation mode of the present invention, defects such as accumulation of metals or chlorides in the chlorination furnace 120 or precipitation in the first delivery pipe 112 can be suppressed.

As the embodiment of the present invention, the various embodiments described above can be combined appropriately as long as they do not contradict each other. In addition, based on the devices of each implementation type, those with ordinary knowledge in the technical field who add, delete, or change the design of appropriate structural elements, or who perform the addition, omission, or condition change of the process, also have the requirements of the present invention. The gist is included in the scope of the present invention.

Even if it is other effects that are different from the effects brought about by the various implementation modes described above, those that can be clearly known from the description of this specification, or those with ordinary knowledge in the technical field can obtain Those who are easy to predict can of course also be understood as those facilitated by the present invention.

100‧‧‧Metal Powder Manufacturing System 110‧‧‧Metal Chloride Generator 112‧‧‧The first delivery pipe 114‧‧‧Particle 116‧‧‧Metal Chloride Generator 120‧‧‧Chlorination furnace 122‧‧‧The first heating furnace 123‧‧‧Connecting part 124‧‧‧The second heating furnace 126‧‧‧Partition 128‧‧‧Metal inlet 130‧‧‧3rd gas inlet 132‧‧‧valve 134‧‧‧Exhaust outlet 136‧‧‧The first gas inlet 138‧‧‧valve 140‧‧‧Auxiliary materials for gasification 142‧‧‧Second gas inlet 144‧‧‧valve 146‧‧‧4th gas inlet 148‧‧‧valve 160‧‧‧The first heater 162‧‧‧Second heater 164‧‧‧The third heater 200‧‧‧Reduction furnace 202‧‧‧Second delivery pipe 204‧‧‧The fifth gas inlet 206‧‧‧The 6th gas inlet 300‧‧‧Separation device

<Figure 1> A schematic configuration diagram of a metal powder manufacturing system related to one of the embodiments of the present invention. <Figure 2> A schematic cross-sectional view of a metal chloride generating device related to one embodiment of the present invention. <Figure 3> A schematic cross-sectional view of a metal chloride generating device related to one of the embodiments of the present invention. <Figure 4> A schematic cross-sectional view of a metal chloride generating device related to one of the embodiments of the present invention. <Figure 5> A schematic cross-sectional view of a metal chloride generating device related to one of the embodiments of the present invention. <Figure 6> A schematic cross-sectional view of a metal chloride generating device related to one embodiment of the present invention. <Figure 7> A schematic side view of a metal chloride generating device related to one embodiment of the present invention.

110‧‧‧Metal Chloride Generator

112‧‧‧The first delivery pipe

114‧‧‧Particle

120‧‧‧Chlorination furnace

122‧‧‧The first heating furnace

123‧‧‧Connecting part

124‧‧‧The second heating furnace

128‧‧‧Metal inlet

130‧‧‧3rd gas inlet

132‧‧‧valve

134‧‧‧Exhaust outlet

136‧‧‧The first gas inlet

138‧‧‧valve

140‧‧‧Auxiliary materials for gasification

160‧‧‧The first heater

162‧‧‧Second heater

Claims (14)

A metal chloride generating device, comprising: a chlorination furnace, a first heating furnace having a metal introduction port for introducing metal, and a second heating furnace connected to the first heating furnace; a first heater, The first heating furnace heats; and the second heater heats the second heating furnace; wherein the second heating furnace has a discharge port for discharging the gas of the metal chloride; the chlorination furnace has A first gas introduction port for introducing chlorine-containing gas; the first gas introduction port is surrounded by either the first heater and the second heater. The metal chloride generating device according to claim 1, wherein the first gas inlet is provided in the second heating furnace, and is arranged to be farther from the first heating furnace than the discharge port. The metal chloride generation device according to claim 1, wherein the first gas inlet is provided in the first heating furnace; the first gas inlet is closer to the first heating furnace and the second heating furnace than the metal inlet The connecting part of the heating furnace. The metal chloride generating device according to claim 2, wherein the second heating furnace further includes a second gas inlet for introducing chlorine-containing gas; The second gas introduction port is arranged closer to the first heating furnace than the discharge port. The metal chloride generating device according to claim 1, wherein the second heater is configured to heat the second heating furnace at a temperature higher than the temperature of the first heating furnace. The metal chloride generating device according to claim 1, wherein the first heating furnace further has a third gas introduction port for introducing chlorine-containing gas; the third gas introduction port is exposed from the first heater. The metal chloride generating device according to claim 1, wherein the first heating furnace has: a fourth gas introduction port for introducing chlorine-containing gas; and a third heater for heating the nitrogen. The metal chloride generating device according to claim 1, wherein the inner diameter of the second heating furnace is smaller than the inner diameter of the first heating furnace. A method of manufacturing metal powder, comprising: in the first heating furnace with a first heater and a second heating furnace with a second heater connected to the first heating furnace in the first chlorination furnace In the heating furnace, the metal is reacted with chlorine gas to produce the chloride of the metal; in the second heating furnace, the chloride is gasified; and by self-installing in the first heating furnace or the second heating furnace The first gas inlet introduces chlorine-containing gas, and conveys the aforementioned chloride vapor to the reduction furnace. The method according to claim 9, wherein the gasification of the chloride in the second heating furnace is performed at a temperature higher than the temperature at which the chloride is generated. The method according to claim 9, wherein the first gas inlet is provided in the first heating furnace. The method according to claim 9, wherein the first gas inlet is provided in the second heating furnace. The method according to claim 12, wherein the transportation of the vapor of the chloride to the reduction furnace is carried out by intermediary installation at the outlet of the second heating furnace; and the introduction of the chlorine-containing gas is performed using the first 1 gas inlet and the second gas inlet provided in the aforementioned second heating furnace. The method according to claim 9, which further comprises introducing heated nitrogen into the aforementioned first heating furnace.

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