JP6715064B2 - Metal nanoparticle generator and metal nanoparticle gas deposition apparatus - Google Patents

Description

Some aspects according to the present invention relate to a metal nanoparticle generator and a metal nanoparticle gas deposition device.

A technique for injecting and depositing nano metal particles by a method called a gas deposition method is known (for example, Patent Documents 1 to 6).

U.S. Pat. No. 7,767,574 Japanese Patent No. 5062763 Japanese Patent No. 4826924 Japanese Patent No. 5311503 Patent No. 5522662 Japanese Patent No. 5678612

However, in order to make a metal such as gold, silver, copper, or nickel into nanometal particles, it is necessary to give a temperature higher than at least the melting point of the metal. There was a problem that the electric power also became extremely large.

Some aspects of the present invention have been made in view of the above problems, and a metal nanoparticle generation apparatus and a metal nanoparticle gas deposition apparatus capable of suppressing an increase in size and power consumption of the apparatus. One of the purposes is to provide.

The apparatus for producing metal nanoparticles according to the present invention, a crucible for containing a film forming material, a graphite heater for heating the crucible by supplying power to a graphite resistor, and an inert gas supplied from the outside to heat the crucible. A nanoparticle generation chamber in which metal nanoparticles of the film forming material are generated by cooling the film forming material vaporized by the above in the inert gas, and a transfer pipe for transferring the metal nanoparticles to the outside. ..

The metal nanoparticle gas deposition apparatus according to the present invention is a metal nanoparticle generation apparatus that generates metal nanoparticles of a film forming material, and by depositing the metal nanoparticles supplied from the metal nanoparticle generation apparatus, A film forming apparatus for forming a metal deposition film. The metal nanoparticle generator is a crucible for containing the film forming material, a graphite heater for heating the crucible by supplying power to a graphite resistor, and an inert gas supplied from the outside to evaporate by heating the crucible. The nanoparticle production chamber in which the metal nanoparticles are produced by cooling the film forming material in the inert gas, and a delivery pipe for delivering the metal nanoparticles to the film deposition apparatus are provided.

In the present invention, “part”, “means”, “apparatus”, and “system” do not simply mean physical means, but “part”, “means”, “apparatus”, and “system”. It also includes the case where the function of “” is realized by software. Further, even if the function of one “unit” or “means”, “device”, or “system” is realized by two or more physical means or devices, two or more “units” or “means”, The functions of “apparatus” and “system” may be realized by one physical means or apparatus.

It is a figure which shows the specific example of schematic structure of a metal nanoparticle gas deposition apparatus. It is a figure which shows the specific example of schematic structure of the metal nanoparticle production|generation apparatus which concerns on this embodiment. It is a figure which shows the photograph which observed generation|occurrence|production of a giant metal particle in a metal nanoparticle production|generation apparatus. It is a figure showing a microscope picture of a metal deposition film formed at the time of generation of a giant metal particle. It is a figure which shows the microscope picture of the metal deposition film formed when a giant metal particle did not generate|occur|produce. It is a figure which shows the schematic diagram of the cross section when it puts in the crucible made from boron nitride, and heated the film-forming material. It is a figure which shows the schematic diagram of a cross section when it puts in the crucible made from tungsten, and heated the film-forming material. It is a figure which shows the relationship between the pressure in a nanoparticle production chamber, and the evaporation amount and film-forming amount of the film-forming material per unit time. It is a figure which shows the schematic diagram of the cross section of the crucible which concerns on a modification. It is a figure which shows the schematic diagram of the cross section of the crucible and the graphite heater which concern on a modification.

Embodiments of the present invention will be described below. In the following description and the description of the drawings to be referred to, the same or similar configurations are denoted by the same or similar reference numerals.

1 Outline A metal nanoparticle gas deposition apparatus is known, which deposits a metal nanoparticle film by generating a nanoparticle metal by using a gas deposition method and then spraying the metal nanoparticle together with an inert gas flow. There is. For example, if metal nanoparticles are sprayed for a certain period of time with a metal nanoparticle gas deposition device on a substrate with appropriate openings formed by photoresist, it is possible to form conical or pyramidal connection bumps on the substrate. Is. In addition to the above, the formation of a metal film using metal nanoparticles can be performed by using a device such as a sensor, an actuator, or an electronic circuit, which uses MEMS (Micro Electro Mechanical Systems), integrated on one silicon substrate, a glass substrate, an organic material, or the like. It can be applied to the field of fine semiconductor packaging technology.

FIG. 1 shows a specific example of the schematic configuration of the metal nanoparticle gas deposition apparatus. The metal nanoparticle gas deposition device 100 includes a metal nanoparticle generation device 110, a film forming device 130, and a carrier pipe 150. The metal nanoparticles generated in the metal nanoparticle generation device 110 are supplied to the film formation chamber 131 of the film formation device 130 through the transport pipe 150, and the metal film is formed by the metal nanoparticles in the film formation chamber 131. The details will be described below.

The metal nanoparticle generator 110 includes a carrier gas supply port 111, a nanoparticle generation chamber 113, a crucible 115, a high frequency dielectric heating coil 117, and an extra particle discharge pipe 119.

The carrier gas supply port 111 allows a carrier gas, which is an inert gas such as helium (He) gas, supplied from the outside to flow into the nanoparticle generation chamber 113. The nanoparticle generating chamber 113 is connected to the film forming chamber 131 of the film forming apparatus 130 through the transfer pipe 150, and the film forming chamber 131 is evacuated. Therefore, the carrier gas supplied to the nanoparticle generation chamber 113 is jetted into the film formation chamber 131 having a low atmospheric pressure through the carrier pipe 150 together with the metal nanoparticles generated in a mist state on the crucible 115. Further, a part of the carrier gas supplied into the nanoparticle generation chamber 113 is discharged to the outside from the extra particle discharge pipe 119.

In the crucible 115, a film forming material M which is a metal such as gold (Au), silver, copper, nickel (hereinafter, the case of gold will be mainly described) is put in advance. The crucible 115 containing the film-forming material M is heated to a high temperature by the high-frequency dielectric heating coil 117, and the film-forming material M is also heated to a high temperature and evaporates. The evaporated film forming material M is cooled by the carrier gas in the nanoparticle generation chamber 113 to be atomized metal nanoparticles. As described above, the metal nanoparticles together with the carrier gas flow into the film forming chamber 131 through the carrier pipe 150, and a part of the metal nanoparticles is discharged to the outside from the extra particle discharge pipe 119.
Next, the film forming apparatus 130 will be described. The film forming apparatus 130 includes a film forming chamber 131, a stage 133, and a stage driving device 135.

The metal nanoparticles generated by the metal nanoparticle generator 110 are sprayed from the nozzle 151 of the carrier pipe 150 onto the sample S such as a substrate mounted on the stage 133. Thereby, the metal nanoparticles are deposited on the sample S. The stage 133 is appropriately scanned in the X direction and the Y direction by the stage driving device 135, so that the metal nanoparticles form, for example, a metal deposition film on the sample S.

In such a metal nanoparticle gas deposition apparatus 100, in order to evaporate the film forming material M such as a metal in the carrier gas, it is necessary to heat the crucible 115 to a temperature higher than at least the melting point of the film forming material M. For example, when the film forming material M is gold, the melting point reaches 1064° C. and the evaporation temperature reaches about 1600° C.

As a method for heating the crucible 115 to such a high temperature, the high frequency dielectric heating coil 117 is used in the metal nanoparticle gas deposition apparatus 100 shown in FIG. In this method, for example, the crucible 115 made of graphite or the like is heated by a high-frequency dielectric heating coil 117 to generate electromagnetic waves by a high-frequency dielectric heating method, so that the crucible 115 is easily heated to a high temperature of 1500° C. or higher without contact. be able to.

However, in this method, since it is necessary to install a large water-cooled high-frequency dielectric heating coil 117 around the crucible 115, the metal nanoparticle gas deposition apparatus 100 including the metal nanoparticle generation apparatus 110 can be downsized. Is difficult. Further, since the metal portion cannot be brought close to the periphery of the high frequency induction heating coil 117, the chamber surrounding the high frequency induction heating coil 117 cannot be downsized. Further, there is a problem that the power consumption of the high frequency generator for generating electromagnetic waves in the high frequency induction heating coil 117 is extremely large. If the crucible 115 is upsized, the frequency to be supplied to the high-frequency induction heating coil 117 can be lowered, and the power consumption can be suppressed accordingly. However, with such a method, the metal nanoparticle generator 110 is upsized. I will end up.

Therefore, in order to downsize the metal nanoparticle generator 110, it is necessary to heat it by a heating means other than the high frequency dielectric heating method. Therefore, in the present embodiment, the heater is used to heat the crucible.

Generally, a heat resistant metal is often used as a resistor in a heater that can be used in an inert gas of 1600° C. necessary for generation of nano metal particles. However, since metal generally has a small resistance value, a low voltage-a large current is required to obtain a desired heating condition. Therefore, the current introduction terminal to the heater becomes large, and a large transformer is required for such a low-voltage/large-current power source, so that the device becomes large.

In order to solve such a problem, for example, a method of using a switching power supply, a method of using a resistor having a high resistance value in a heater, or the like can be considered. However, when a switching power supply is used, pulsed electric power is supplied to the heater. Therefore, when such a heater is used in an inert gas, glow discharge occurs. As a result, leakage of electric power, unstable operation, failure such as contamination in the chamber and the electrode portion, and the like are likely to occur, so that application of the switching power supply is not practical. Although a low-voltage and large-current DC power supply can be configured by using a switching power supply and a large-capacity capacitor, it is also difficult to reduce the size of such a configuration.

Therefore, in the metal nanoparticle generator according to the present embodiment, as a method of increasing the heater power, graphite is used as a resistor having a high specific resistance value to reduce the current. Since the power is calculated by the following formula, if the required power is the same, the current can be reduced by increasing the resistance value.

2 Configuration of Metal Nanoparticle Generation Device 200 According to this Embodiment 2.1 Overall Configuration FIG. 2 shows the configuration of the metal nanoparticle generation device 200 according to this embodiment. In addition, as the film forming apparatus used in combination with the metal nanoparticle generating apparatus 200 to configure the metal nanoparticle gas deposition apparatus 100, the same one as described above with reference to FIG. 1 should be used. You can That is, in the metal nanoparticle gas deposition apparatus 100 shown in FIG. 1, the metal nanoparticle generation apparatus 110 may be replaced with the metal nanoparticle generation apparatus 200.

The metal nanoparticle production apparatus 200 includes a carrier gas supply port 211, a nanoparticle production chamber 213, a crucible 215, and a graphite heater 217. The metal nanoparticles generated in the metal nanoparticle generator 200 are supplied to a film forming chamber of a film forming apparatus (not shown) through the transport pipe 250, and a metal film is formed by the metal nanoparticles in the film forming chamber.

The carrier gas supply port 211 allows a carrier gas, which is an inert gas such as helium gas, supplied from the outside to flow into the nanoparticle generation chamber 213 of the metal nanoparticle generation device 200. The nanoparticle generation chamber 213 is connected to the film formation chamber of the film formation apparatus through the transfer pipe 250, and the atmospheric pressure of the film formation chamber can be kept low by evacuation. As a result, the carrier gas supplied to the nanoparticle generation chamber 213 flows into the film formation chamber having a low atmospheric pressure through the transfer pipe 250 together with the metal nanoparticles generated in a mist state on the crucible 215.

The film forming material M, which is a metal such as gold, is put into the crucible 215 in advance. The crucible 215 containing the film forming material M is heated to a high temperature by the graphite heater 217, and the film forming material M having a high temperature is evaporated. The evaporated film forming material M is cooled by a carrier gas to be atomized metal nanoparticles. As described above, the metal nanoparticles flow into the film forming chamber through the carrier pipe 250 together with the carrier gas.

As shown in FIG. 1, the metal nanoparticles ejected from the nozzle 251 of the carrier pipe 250 are sprayed onto the sample placed on the stage in the film forming chamber to form a metal deposition film.

2.2 Graphite heater 217
In such a metal nanoparticle generator 200, when a graphite resistor having a large specific resistance value of 11000 nΩm is applied to the resistor in the graphite heater 217, a circular graphite heater 217 having a diameter of 20 mm and a height of 40 mm is used and the helium gas is 90 MPa. A high temperature of 1600° C. or higher can be obtained with an electric power of 1 kW or lower.

Here, a tungsten heater is typically used as the heat-resistant metal heater used when heating the crucible 215 to a high temperature. The specific resistance of the resistor made of tungsten is 53 nΩm. If the tungsten heater using the resistor and the graphite heater 217 are operated under the same voltage/power condition, a current of a square root of the specific resistance ratio is required. It is necessary to pass a current about 15 times that of the graphite heater 217. That is, when the tungsten heater is used, it is necessary to design the current introducing electrode and the like larger than the graphite heater 217, and thus it is difficult to downsize the metal nanoparticle generation device 200. In other words, it is preferable to use the graphite heater 217 having the direct current heating mechanism by the graphite resistor in order to downsize the metal nanoparticle generation device 200.

Further, in the example shown in FIG. 1, the high frequency dielectric heating coil 117 is used when heating the crucible 115. When a high frequency induction heating coil 117 having a diameter of 100 mm and a height of 70 mm is used, electric power of 5 kW is required to obtain a high temperature of 1600° C. or higher. On the other hand, when the above-mentioned graphite heater 217 is used, since the required electric power is 1 kW or less, the electric power required to heat the crucible 215 is much lower in the graphite heater 217. That is, by using the graphite heater 217, the metal nanoparticle generation device 200 can be downsized.
2.3 Crucible 215

As described above, when the graphite heater 217 using the graphite resistor is used, the size can be reduced and the power consumption can be reduced. However, if the crucible 215 is simply made smaller along with the miniaturization, a large amount of huge metal particles of several μm to several hundreds of μm are generated when the metal nanoparticles are generated in the carrier gas.

FIG. 3 shows a photograph of giant metal particles generated on the crucible 215 when the crucible 215 is simply made small, as observed from the same direction as in FIG. In the photograph of FIG. 3, the metal nanoparticles are not shown, and the white spots are all giant metal particles. Since the plurality of giant metal particles are reflected in the photograph of FIG. 3, it can be seen that the plurality of giant metal particles are generated at the same time. If the crucible 215 is continuously heated for a certain period of time until the metal film is formed, the huge metal particles continue to be generated during that time, so that a large number of huge metal particles are cumulatively generated.

Such huge metal particles cause the nozzle 251 for ejecting the metal nanoparticles to be clogged. In addition, when giant metal particles are generated, particles having a large size are mixed with the metal nanoparticles, which leads to deterioration of the quality of the metal deposition film formed by the injection of the metal nanoparticles. FIG. 4 shows a micrograph of a metal deposition film formed when giant metal particles were generated. In the example of FIG. 4, the giant metal particles sprayed on the metal deposition film appear as black dots. On the other hand, when the giant metal particles are not generated, a smooth metal deposition film is formed as shown in FIG. Therefore, in the downsizing of the metal nanoparticle generation device 200, it is necessary to suppress the generation of giant metal particles.

Therefore, when various materials and dimensions of the crucible 215 are changed and existence of giant metal particles is verified, it is considered that giant metal particles are generated by bumping (splash) of the film-forming material M in the crucible 215. .. There are two possible causes of such bumping.

(A) In the production of metal nanoparticles by the gas deposition method as in this embodiment, the temperature of the crucible 215 is less stable than that of vacuum vapor deposition or the like because the heating is performed in an inert gas that produces an air flow. thing.
(B) The temperature of the crucible 215 is likely to be unstable particularly at the interface with the film forming material M due to the heat of vaporization of the film forming material M.

Therefore, (1) improving the wettability between the crucible 215 and the film-forming material M, and (2) increasing the heat capacity by increasing the wall thickness of the crucible 215 when the crucible 215 is downsized. 2 are effective for suppressing bumping and significantly suppressing generation of giant metal particles. Hereinafter, these points will be described in detail.

A large capacity crucible 115 made of graphite used for high frequency heating in the metal nanoparticle generator 200 shown in FIG. 1 and a small crucible 215 for the graphite heater 217 shown in FIG. The same was done and heated to the same temperature. Table 1 shows the results of spray deposition of nano metal particles using the metal nano particle generator 200 under such conditions. As shown in Table 1, as compared with the large crucible 115, the small crucible 215 generates a large number of giant metal particles.

Therefore, a material and a structure in which giant metal particles are not generated even when the crucible 215 is downsized was examined. Table 2 shows the results of generation of giant metal particles in the crucible 215 of each material when the crucible 215 for the graphite heater 217 having substantially the same size is made of various materials. As can be seen from Table 2, when the crucible 215 having the same size is heated by the graphite heater 217, the use of the refractory metal crucible 215 suppresses the generation of huge metal particles as compared with the non-metal crucible 215. be able to.

6 and 7 are schematic views of a cross section when gold, which is the film forming material M, is heated in the crucible 215 made of boron nitride and tungsten. As shown in FIG. 6, since the crucible 215 made of boron nitride, graphite, or the like has low wettability with the film forming material M that is gold, the film forming material M in the molten state has a surface tension that causes the crucible 215 to melt. It is spherically deformed so that the contact area with the side wall 215a becomes small. As a result, a gap G is formed between the side wall 215a of the crucible 215 and the film forming material M, and the inert gas enters there. At this time, since the heat source of the film-forming material M that is a molten metal is only the crucible 215, the heat transfer between the film-forming material M and the crucible 215 greatly changes depending on how the gas enters. When the wettability between the crucible 215 and the film-forming material M is poor, the film-forming material M fluctuates by rotation or the like, so that an inert gas is taken in near the side wall 215a of the crucible 215. As a result, heating of the film forming material M becomes non-uniform, and as a result, bumping occurs and giant metal particles are generated.

In fact, when observing the generation locations of the giant metal particles, a large number of giant metal particles are generated near the boundary between the film-forming material M and the side wall 215a of the crucible 215. Further, once bumping starts, bumping occurs continuously. It is considered that this is because at the interface between the side wall 215a of the crucible 215 and the film forming material M, the temperature becomes unstable due to the occurrence of bumping, so that further bumping is induced. Some of the generated giant metal particles adhere to the side wall 215a of the crucible 215, as shown in FIG.

On the other hand, in the crucible 215 made of metal such as tungsten, as shown in FIG. 7, the film forming material M, which is gold, wets and spreads on the side wall 215 a of the crucible 215. That is, the film forming material M is deformed so that the contact area between the film forming material M and the side wall 215 a of the crucible 215 becomes large. As a result, the area where heat flows into the film-forming material M becomes large, so that the film-forming material M is heated almost uniformly. As a result, bumping of the film forming material M is less likely to occur, and generation of giant metal particles is also suppressed.

Therefore, as the material of the crucible 215, it is conceivable to use molybdenum or tungsten which is a heat-resistant metal having a high melting point capable of heating gold to 1500° C. or higher and having high wettability with gold. However, among these, molybdenum has extremely high wettability with gold, and therefore, gold is leaked to the outside through the grain boundary of molybdenum at 1500° C. or more, and thus it is difficult to use it as the crucible 215. Therefore, the crucible 215 according to this embodiment is made of tungsten.

Further, the instability of the inflow of heat into the molten metal that is the film forming material M that causes the generation of giant metal particles is related to not only the material of the crucible 215 but also the thickness of the inner wall of the crucible 215. Table 3 shows the results of observing the number of generated giant particles when the wall thickness was 0.3 mm, 0.5 mm, and 1.0 mm with the same internal volume.

As can be seen from Table 3, when the inner wall thickness of the crucible 215 is less than 0.5 mm, giant metal particles are generated, but when the wall thickness is 0.5 mm or more, giant metal particles of the film forming material M are generated. Suppressed. This is because when the wall thickness of the crucible 215 is thin, the heat capacity of the crucible 215 at the interface between the side wall 215a and the film-forming material M is small, so the temperature instability near the interface increases and bumping occurs. It is thought to be because it is easier to do. On the other hand, if the wall thickness of the crucible 215 is increased, the heat capacity near the interface between the film-forming material M, which is a molten metal, and the crucible 215 increases, and as a result, the temperature stability near the interface increases, so that bumping occurs. Suppressed. As a result, generation of giant metal particles caused by bumping can also be suppressed.

3 Operation and Effect of Metal Nanoparticle Generating Device 200 According to this Embodiment As described above, by using the graphite heater 217 instead of the high frequency induction heating coil 117 for heating the crucible 215, the metal nanoparticle generating device 200 Can be miniaturized.

Further, by using tungsten or molybdenum instead of graphite for the material of the crucible 215, it is possible to prevent bumping of the film forming material M and consequently reduce generation of giant metal particles. Above all, if tungsten is used, it is possible to suppress the film forming material M from leaking out.

Further, by setting the wall thickness of the crucible 215 to 0.5 mm or more, the heat capacity of the crucible 215 increases, so that bumping of the film-forming material M can be prevented and, as a result, generation of giant metal particles can be suppressed.

By doing so, it is possible to prevent the deterioration of the quality of the metal deposited film due to the generation of the giant metal particles while achieving downsizing of the metal nanoparticle production apparatus 200, and it is possible to produce a high quality metal deposited film. It will be possible.

4 Modifications The configurations of the above-described embodiments may be combined or some of the components may be replaced. Further, the configuration of the present invention is not limited to the above-described embodiments, and various changes may be made without departing from the scope of the invention. Hereinafter, an example in which the above embodiment is modified will be described.

4.1 Pressure in Nanoparticle Generation Chamber 113 Generally, when the pressure in the nanoparticle generation chamber 113 decreases, the film forming material M in the crucible 215 easily evaporates. It is considered that when the evaporation amount of the film-forming material M increases, the number of metal nanoparticles generated increases, and the film-forming rate of the metal deposition film formed by spraying the metal nanoparticles also increases.

FIG. 8 shows the pressure (kPa) in the nanoparticle generation chamber 113, the evaporation rate (mg/h) of gold that is the film forming material M, and the film forming rate (mg/h) of the metal deposition film that is generated. It is a graph which shows a relationship. As shown in FIG. 8, as the pressure inside the nanoparticle generation chamber 113 decreases up to 80 kPa, the evaporation rate of the film forming material M increases, and the film forming rate of the metal deposition film also increases accordingly. For example, if a film formation amount of 3.0 mg/h or more per unit time is required, the pressure in the nanoparticle generation chamber 113 may be set to 90 kPa or less.

Even if the pressure in the nanoparticle generation chamber 113 is lowered, it does not particularly affect the generation of the giant metal particles. Further, the film quality of the metal deposited film generated by the film forming apparatus 130, particularly the particle size, is not particularly affected by the pressure in the nanoparticle generation chamber 113.

On the other hand, when the pressure in the nanoparticle generation chamber 113 decreases, the flow rate of the carrier gas decreases, so that the generated nanometal particles are less likely to collide with the carrier gas and thus can easily go straight. As a result, the velocity of the nanoparticle metal sprayed toward the stage 133 in the film forming apparatus 130 is increased, and the range over which the nanoparticle metal is sprayed can be narrowed.

4.2. Structure of crucible 215 As described in "2.3 Crucible 215" above, when the wettability between the crucible 215 and the film forming material M is increased and the contact area between the film forming material M and the crucible 215 is increased, the film forming material M is formed. It becomes difficult for the bumping of the metal to occur, and generation of giant metal particles can be suppressed.

Therefore, in order to increase the surface area of the film forming material M, it is conceivable to provide, for example, plate-like fins 216 made of a material having high wettability with the film forming material M in a lattice shape in the crucible 215. In this case, for example, the fin 216 may be formed using a material having high wettability with the film forming material M, for example, molybdenum or tungsten.

FIG. 9 shows a specific example of a cross-sectional view when the fins 216 are put in the crucible 215. In the example of FIG. 9, two plate-shaped fins 216a and 216b (hereinafter collectively referred to as fins 216) are provided in the depth direction of the drawing. Although not shown in FIG. 9, another plate-shaped fin 216 can be provided in the lateral direction of the drawing.

By inserting the fin 216 into the crucible 215, the surface area of the contact surface MS of the film forming material M with the carrier gas is significantly increased as compared with the case where the fin 216 is not provided in FIG. 7. Thereby, the evaporation rate of the film forming material M can be increased.

4.3. Structure of Graphite Heater 217 In the example of the metal nanoparticle generator 200 shown in FIG. 2, the crucible 215 is arranged inside the cylindrical graphite heater 217. The graphite heater 217 and the crucible 215 are not in contact with each other and there is a gap.

However, if there is a gap between the graphite heater 217 and the crucible 215, the carrier gas moves through the gap, so that the crucible 215 is cooled and heat generation efficiency is reduced. Therefore, if the shapes of the graphite heater 217 and the crucible 215 are determined so as to prevent the flow of the carrier gas between the graphite heater 217 and the crucible 215, the heat generation efficiency can be improved.

FIG. 10 shows a sectional view of a graphite heater 217 and a crucible 215 according to a modification. The crucible 215 does not necessarily have to be made of a single material. For example, after forming the crucible 215 shown in FIG. 10 with a material having a large heat capacity, the crucible 215 shown in FIG. 10 is mounted so that the crucible 215 made of, for example, tungsten shown in FIGS. 6 and 9 can be inserted into the opening. You can also

In the example of FIG. 10, unlike the example shown in FIG. 2, the graphite heater 217 is not a simple cylindrical shape. Specifically, graphite heater 217 accommodates crucible 215 in a cylindrical shape, and upper end 217a is curved toward opening 215b of crucible 215, and upper end 215c of crucible 215 and upper end 217a of graphite heater 217 are formed. Are in contact.

As a result, the flow of carrier gas between crucible 215 and graphite heater 217 is blocked, and crucible 215 is less likely to be cooled. In addition, heat from graphite heater 217 is easily transferred to crucible 215. As a result, the heat generation efficiency is improved.

Further, in the example of FIG. 10, a cylindrical shield plate 219 is installed around the graphite heater 217. The shield plate 219 has an effect of confining radiant heat from the graphite heater 217. This makes it possible to suppress the cooling effect due to heat radiation from the graphite heater 217 to the outside.

100: Metal nanoparticle gas deposition apparatus 110: Metal nanoparticle generation apparatus 111: Carrier gas supply port 113: Nanoparticle generation chamber 115: Crucible 117: High frequency dielectric heating coil 119: Extra particle discharge tube 130: Film formation apparatus 131: Film forming chamber 133: Stage 135: Stage driving device 150: Conveying pipe 151: Nozzle 200: Metal nanoparticle generating device 211: Carrier gas supply port 213: Nanoparticle generating chamber 215: Crucible 215a: Side wall 216: Fin 217: Graphite heater 219: Shield plate 250: Conveying pipe 251: Nozzle M: Film forming material S: Sample G: Gap

Claims (9)

A crucible containing a film-forming material that is gold ,
A graphite heater for heating the crucible by supplying power to the graphite resistor,
An inert gas is supplied from the outside, and by cooling in the inert gas of the film forming material evaporated by heating the crucible, a nanoparticle generation chamber in which metal nanoparticles of the film forming material are generated,
An apparatus for producing metal nanoparticles, comprising: a transport pipe that transports the metal nanoparticles to the outside. The crucible is made of tungsten or molybdenum,
The metal nanoparticle generator according to claim 1. The crucible is made of tungsten,
The metal nanoparticle generator according to claim 1. The wall thickness of the crucible is 0.5 mm or more,
The metal nanoparticle production apparatus according to any one of claims 1 to 3. The pressure of the nanoparticle generation chamber is 90 kPa or less,
The metal nanoparticle production apparatus according to any one of claims 1 to 4 . The metal nanoparticle production apparatus according to any one of claims 1 to 5 , further comprising a plate-like member provided in the crucible for expanding a surface area of the film forming material. At least a part of the graphite heater and the crucible are in contact with each other,
The metal nanoparticle production|generation apparatus of any one of Claim 1 thru|or 6 . The graphite heater accommodates the crucible in a cylindrical shape, and contacts at the upper end of the crucible,
The apparatus for producing metal nanoparticles according to claim 7 . A metal nanoparticle generator for generating metal nanoparticles of a film-forming material that is gold ;
By depositing the metal nanoparticles supplied from the metal nanoparticle generator,
A metal nanoparticle gas deposition apparatus comprising: a film forming apparatus for forming a metal deposited film, wherein the metal nanoparticle generation apparatus comprises:
A crucible for containing the film forming material,
A graphite heater for heating the crucible by supplying power to the graphite resistor,
An inert gas is supplied from the outside, and by cooling in the inert gas of the film forming material evaporated by heating the crucible, a nanoparticle generation chamber in which the metal nanoparticles are generated,
A metal nanoparticle gas deposition apparatus, comprising: a transport pipe that transports the metal nanoparticles to the film forming apparatus.