WO2005058756A1

WO2005058756A1 - Device for producing endohedral fullerene and method for procuring endohedral fullerene

Info

Publication number: WO2005058756A1
Application number: PCT/JP2004/018934
Authority: WO
Inventors: Yasuhiko Kasama; Kenji Omote; Noriaki Takahashi; Yoshimi Endoh
Original assignee: Ideal Star Inc.
Priority date: 2003-12-17
Filing date: 2004-12-17
Publication date: 2005-06-30
Also published as: JP2005179090A

Abstract

In order to optimize the deposition condition of an endohedral fullerene producing device, it is necessary to perform deposition experiments using deposition substrates having various shapes under various deposition conditions. However, conventional endohedral fullerene producing devices are of the type where a single substrate is loaded and deposition is performed. Therefore it takes much time for evacuation, purging, and start and stop of plasma, thereby degrading the experimental efficiency. According to the invention, a rotary disk on which substrates can be mounted is used and replacement of substrate can be performed in a vacuum chamber. Without taking out a substrate into the air, a film of endohedral fullerene can be continuously formed. Optimum deposition substrates and optimum deposition conditions for high efficiency of production of endohedral fullerene can be found out in a short period of time.

Description

Specification

Device for producing endohedral fullerene and method for producing endohedral fullerene

Technical field

The present invention relates to an internal fullerene producing apparatus for introducing fullerene into a plasma flow of atoms to be included in a vacuum vessel and depositing the internal fullerene on a deposition substrate disposed downstream of the plasma flow, In particular, the present invention relates to an endohedral fullerene manufacturing apparatus provided with a multiloader capable of exchanging deposition substrates in a vacuum vessel.

Background art

[0002] Non-Patent Document 1: Plasma 'Journal of the Fusion Society of Japan, Vol.75, No.8, 1999, 8 p.927— 933

"Properties and applications of fullerene plasma"

[0003] Encapsulated fullerenes are used in electronic and medical applications in which spherical carbon molecules such as C, C, C, C, C, C, and C, which are known as fullerenes, include atoms to be included such as alkali metals. It is a material that is expected to be applied. As a method of producing endohedral fullerenes, plasma is generated by injecting metal vapor onto a hot plate heated in a vacuum chamber, and then the generated metal plasma stream is injected with fullerene vapor and placed downstream of the plasma stream. A method for depositing an endohedral fullerene on a deposited substrate is known.

As shown in FIG. 6, a conventional apparatus for producing fullerenes includes a main chamber 101, a unit for forming a plasma flow of atoms to be included, and a unit for introducing fullerenes into the plasma flow. And a deposition substrate 115 disposed downstream of the plasma flow.

[0005] The means for forming the alkali metal plasma flow includes a hot plate 107, an alkali metal evaporation oven 108, and an alkali metal introduction tube 109. When the alkali metal vapor generated in the evaporating oven 108 is sprayed onto the hot plate 107 from the alkali metal introduction tube 109, plasma consisting of alkali metal ions and electrons is generated by contact ionization. The generated plasma is confined in the axial direction in the main chamber 101 along the uniform magnetic field (B = 2 to 7 kG) formed by the electromagnetic coil 104, and becomes a plasma flow flowing from the hot plate 107 to the deposition substrate 115. .

[0006] The means for introducing fullerenes is a fullerene sublimation oven 110 and a sublimation circle. And a tube 111. In the resublimation cylinder 111, when fullerene vapor such as C sublimated from the fullerene sublimation oven 110 is jetted into the plasma flow, electrons constituting the plasma flow adhere to C having a high electron affinity to generate C negative ions. As a result, for example, when sodium is used as the alkali metal,

Na → Na + + e—

C + e— → C

60 60

Due to the reaction, the plasma flow becomes a plasma flow in which alkali metal ions, fullerene ions, and residual electrons are mixed.

[0007] When the deposition substrate 115 is arranged downstream of such a plasma flow and a positive bias voltage is applied to the deposition substrate 115, the alkali metal ions having a small mass are decelerated, and the fullerene ions having a large mass are accelerated. As a result, the interaction between the alkali metal ion and the fullerene ion is increased, and the encapsulation is likely to occur. Further, the bias voltage can be controlled by the noise voltage control device 118 to improve the inclusion rate. (Non-Patent Document 1)

[0008] (Loading and unloading of deposited substrate)

In the conventional endohedral fullerene manufacturing apparatus, one deposition substrate 115 attached to the tip of the deposition substrate insertion rod 116 is inserted into the main chamber 101 to perform deposition. In addition, when the depositing substrate 115 is taken in and out, the depositing substrate is moved from the atmosphere to the load lock chamber-102 and the load lock chamber-102 force main chamber-101 by manually operating the insertion rod 116. I was going by moving. FIGS. 7 (a) to 7 (f) are cross-sectional views illustrating a procedure for loading and unloading a deposition substrate using a conventional endohedral fullerene manufacturing apparatus.

In FIG. 7A, the main chamber 121 is connected to a load lock chamber 123 via a gate valve 122. The main chamber 121 and the load lock chamber 123 are evacuated by vacuum pumps 124 and 125, respectively.

[0010] When introducing a deposition substrate into the load lock chamber from the atmosphere, first, the main chamber 121 is evacuated, the gate valve 122 is closed, and the load lock chamber 123 is supplied with nitrogen. Purge with nitrogen gas introduced from line 126. A deposition substrate 128 is attached to the tip of the deposition substrate introduction rod 129. [0011] Next, the deposition substrate 128 is inserted into the load lock chamber 123, and the gate valve 127 is closed. The introduction of nitrogen gas is stopped, and the load lock chamber is evacuated (Fig. 7 (b)).

When the evacuation of the load lock chamber 123 is completed, the gate valve 122 is opened, and the deposition substrate 128 is introduced into the main chamber 121 (FIG. 7C).

Next, the gate valve 122 is closed, plasma 130 is generated, and the endohedral fullerene film is deposited on the deposition substrate 128 (FIG. 7 (d)). After the deposition is completed, the plasma 130 is stopped, the gate vane lever 122 is opened, and the deposition substrate 128 is moved to the load lock chamber 123 (FIG. 7 (e)).

[0014] Next, the gate valve 122 is closed, the evacuation of the load lock chamber 123 is stopped, and the load lock chamber 123 is purged with nitrogen gas. Then, the gate valve 127 is opened and the deposition substrate 128 is exposed to air. And perform work such as replacing the board (Fig. 7 (f)).

[0015] (Ion density distribution and deposition substrate)

When the ion density distribution in the radial direction of the plasma flow is measured near the deposition substrate, the density distributions of alkali metal ions and fullerene ions do not always match. FIG. 4A is a diagram showing the ion density distribution in the radial direction when no bias voltage is applied to the deposition substrate.

[0016] The Na ion density has a peak at the center of the plasma flow, and the ion density becomes lower toward the periphery. On the other hand, the density of fullerene ions has a peak on the circumference outside the center of the plasma flow.

[0017] How many alkali metals are likely to be included in one fullerene molecule depends on the types of fullerene and alkali metal, production conditions, and the like. For example, in the case of Na-containing C, there is a high probability that one C molecular force contains Na atoms. In this case, the portion of the deposition substrate where the density of the alkali metal ion and the fullerene ion do not match each other does not contribute to the generation of endohedral fullerene, and the number of ions increases, which lowers the generation efficiency of the endohedral fullerene. Become. In addition, even when two or more atoms are included in one fullerene, the generation efficiency will still be low unless the ion density distribution is appropriate for the number of included atoms.

As a method for solving this problem, a deposition substrate divided into a plurality of plates along the radial direction of the plasma flow as shown in FIG. 4 (c) is used, and each plate is controlled independently. Methods for applying possible bias voltages are known.

FIG. 4C shows an example in which the deposition substrate is divided into three divided plates 43, 44, and 45. The bias voltage applied to the split plate is controlled as shown in Fig. 4 (d). For example, when the split plates 44 and 45 are set to the floating potential (the same potential as the plasma) and a bias voltage of +1 V is applied to the central plate 43 with respect to the floating potential, as shown in FIG. The distribution of Na ions as ions spreads outside the plasma flow, and the distribution of C ions as negative ions changes to a shape with a peak at the center of the plasma flow, which can improve the efficiency of generating endohedral fullerenes .

[0020] As the shape of the deposition substrate, a shape divided into three plates is not always optimal. Depending on the shape and size of the endohedral fullerene manufacturing equipment, the deposition conditions, the type of endogenous atoms, and the type of fullerene, the substrate is divided into two, as shown in Fig. 4 (e), or into five, as shown in Fig. 4 (f). As shown in the example of the deposited substrate, there is a possibility that a substrate other than the three-divided substrate can perform superior deposition of fullerenes. Also, as shown in Fig. 4 (g) and (h), grid electrodes are provided on the front surface of the plate, and a bias voltage different from that of the plate is applied, for example, to control the ion velocity in the plasma, It is also possible to improve the efficiency of the generation.

Disclosure of the invention

Problems to be solved by the invention

[0021] In order to optimize the generation efficiency of endohedral fullerene deposited on a substrate by controlling the ion density distribution in plasma, deposition substrates of various shapes are required depending on the type of endohedral fullerene, structural factors of a manufacturing apparatus, and the like. In addition, it is necessary to perform a deposition experiment in which deposition conditions are changed.

However, in a conventional endohedral fullerene manufacturing apparatus, one substrate is loaded, a thin film is deposited after evacuation, and after the deposition is completed, the load lock chamber is purged and the substrate is taken out into the atmosphere. Since the work of replacing with another substrate is repeated, it takes a long time to evacuate and purge, and to stop and start the plasma, so that there is a problem that the experimental efficiency is poor.

Means for solving the problem

[0023] A disk-shaped member called a pallet on which a plurality of deposition substrates can be mounted is arranged in a housing. The chiller is connected to the vacuum chamber of the endohedral fullerene manufacturing equipment via a gate valve, and the pallet is rotated in the evacuated housing to change the deposition substrate, thereby continuously depositing the endohedral fullerene film on a plurality of substrates. Decided to do.

In addition, a nitrogen purge box was placed at the position where the substrate was taken out of the multiloader. Furthermore, in order to minimize the contamination of the vacuum chamber by the plasma and the raw material of the plasma, a shielding member is arranged in the multiloader and a shielding shutter is arranged in the main chamber.

The invention's effect

[0024] (1) Deposition for a plurality of conditions using different types of deposition substrates or changing deposition conditions such as bias voltage is performed in a vacuum chamber in which the substrates are not taken out to the atmosphere for each deposition. It became possible to perform continuously. The optimal deposition substrate and deposition conditions with high efficiency of endohedral fullerene generation can be found in a short time. It can also reduce the working time of engineers and operators who work on conditions.

[0025] (2) When producing endohedral fullerenes that are liable to be degraded by reacting with the atmosphere, use a nitrogen purge box to analyze the solvent or analyze the solvent for solvents without exposing the deposited endohedral fullerenes to the atmosphere. It is possible to carry the film to a processing chamber where the deposition is performed, and to evaluate the deposited film with higher accuracy.

(3) When a highly reactive and corrosive material such as Na is used, disposing a shielding member in the multiloader is highly effective in preventing contamination in the multiloader. In addition, when a shielding shutter is arranged in the main chamber, it is possible to load and unload the substrate without stopping the plasma, not only to prevent contamination of the vacuum chamber, but also to reduce the work time. Can be shortened.

Brief Description of Drawings

[FIG. 1] (a) and (b) are cross-sectional views of a multiloader according to the endohedral fullerene manufacturing apparatus of the present invention.

FIG. 2 (a) is a side view of a multiloader according to the present invention, and FIG. 2 (b) is a front view of the multiloader according to the present invention.

FIG. 3 is a cross-sectional view according to a first embodiment of the endohedral fullerene manufacturing apparatus of the present invention. [FIG. 4_1] (a) and (b) are diagrams showing a radial ion density distribution in a plasma flow.

(c), (d) is a diagram for explaining a first embodiment of the deposition substrate,

[FIG. 4_2] (e) to (h) are diagrams for explaining another embodiment of the deposition substrate.

[FIG. 5_1] (a), (c), and (e) are cross-sectional views for explaining a loading / unloading procedure of a deposition substrate using the endohedral fullerene manufacturing apparatus of the present invention. (D) and (f) are (a), (c),

It is a front view of the pallet corresponding to (e).

[FIG. 5-2] (g), (i), and (k) are cross-sectional views for explaining a loading / unloading procedure of a deposition substrate using the endohedral fullerene manufacturing apparatus of the present invention. ), (J) and (1) are front views of pallets corresponding to (g), (i) and (k), respectively.

FIG. 6 is a cross-sectional view of a conventional endohedral fullerene manufacturing apparatus.

[FIG. 7_l] (a), (b), and (c) are cross-sectional views illustrating a loading / unloading procedure using a conventional endohedral fullerene manufacturing apparatus.

[FIG. 7_2] (d), (e), and (f) are cross-sectional views for explaining a loading / unloading procedure using a conventional endohedral fullerene manufacturing apparatus.

FIG. 8 is a cross-sectional view according to a second embodiment of the endohedral fullerene manufacturing apparatus of the present invention.

9] (a) and (b) are cross-sectional views of a purge box according to the endohedral fullerene manufacturing apparatus of the present invention. [FIG.

[FIG. 10] (a), (b), (c) are diagrams for explaining a shielding member for preventing contamination of an apparatus for producing an endohedral fullerene according to the present invention.

FIG. 11 is a cross-sectional view according to a third embodiment of the endohedral fullerene manufacturing apparatus of the present invention.

Explanation of symbols

1 housing

2 No. Let

3 Deposition substrate

4 props

5 Pallet rotation axis

6 Pallet rotation motor

7, 12 flange Main chamber one

Magnetic field coil

Ma / reticle loader

Vacuum pump

Pallet rotation motor

Board mounting / dismounting motor

Board insertion rod moving motor

Multi loader opening / closing lid

Substrate input rod input section

, 101, 121, 201, 301 Main channel

, 31 1 Manolechi loader

2, 123, 202 Road Rock channel

, 103, 122, 127, 203, 312 Gate / Knoref,

, 104, 204, 205, 302 Magnetic field

, 26, 105, 106, 124, 125, 206, 207, 208, 308, 309 Vacuum pump 6 Nitrogen inlet tube

, 107, 209 hot plate

, 108, 210 Alkali metal evaporation oven

, 109, 211 Alkali metal vapor introduction pipe

, 110, 212, 305 Fullerene sublimation oven

, 111, 213, 306 Resublimation cylinder

, 112, 214 alkali metal plasma

, 113, 216 Langmuir 'probe

, 114, 217 probe current measuring device

, 115, 128, 215, 307 Deposition substrate

, 116, 129, 220, 315 Deposition substrate loading rod

, 117, 221 Wiring for bias voltage supply

, 118, 222 bias voltage controller 223 Alkali metal fullerene plasma

130 Plasma

40, 218, 313 no. Let

41, 219, 314 no. Let rotation axis

43, 44, 45, 46, 47, 48, 49, 50, 51 Harmful 'J plate

52 mesh electrode

53 Electrode support

303 Incorporated atom introduction tube

304 high frequency induction coil

310 grid electrode

1 Main chamber

2 Gate vanolev

3 housing

4 No. Let

5 Deposition substrate

6 Deposition substrate support

7 Deposition substrate insertion rod

8 Plasma

31, 243 message box

32, 251, 261 Main chamber

33, 255, 265

34, 256, 266 Manolet loader

35, 244 Multi-loader opening / closing lid

39, 247 Board handling gloves

36, 237, 238, 246 Substrate handling opening 40 Purge box opening / closing lid

41, 242 Nitrogen inlet tube

45 desiccator 252, 262 Plasma flow

253, 263 Deposition substrate

254 Raw material gas

257, 267 notes

258, 268 Rotating shaft

259, 269 Deposition substrate loading rod

260 shielding material

264 Shutter for shielding

BEST MODE FOR CARRYING OUT THE INVENTION

FIG. 3 is a cross-sectional view according to a first embodiment of the endohedral fullerene manufacturing apparatus of the present invention. A multiloader 22 is connected to a main chamber 21 via a gate vanoleb 23. Means for forming a plasma flow of an alkali metal such as Na as an encapsulating atom is constituted by a hot plate 27, an alkali metal evaporation oven 28, and an alkali metal introduction pipe 29. When the alkali metal vapor generated in the evaporating oven 28 is jetted from the alkali metal introduction pipe 29 onto the hot plate 27, plasma consisting of alkali metal ions and electrons is generated by contact ionization. The generated plasma is confined in the axial direction in the main chamber 21 along a uniform magnetic field (B = 2 to 7 kG) formed by the electromagnetic coil 24, and the hot plate 27 forces a plasma flow 32 flowing toward the deposition substrate 35. Become. The means for introducing fullerenes includes a fullerene sublimation oven 30 and a sublimation cylinder 31. In the sublimation cylinder 31, when fullerene vapor such as C sublimated from the fullerene sublimation oven 30 is jetted into the plasma flow, electrons constituting the plasma flow adhere to C having a high electron affinity to generate C negative ions. . as a result,

Na → Na + e—

C + e— → C —

60 60

Due to this reaction, the plasma flow 32 becomes a plasma flow 39 in which alkali metal ions, fullerene ions, and residual electrons are mixed.

[0030] By the plasma irradiation, the encapsulated fullerene film is deposited on the deposition substrate 35 disposed downstream of the plasma flow 39. The via controlled by the bias voltage controller 38 on the deposition substrate 35 A voltage is applied to optimize the generation efficiency of endohedral fullerenes.

The pallet 40 stored in the multiloader 22 can mount a plurality of deposition substrates and can rotate about a rotation axis 41. The transfer of the deposition substrate 35 between the pallet 40 and the main chamber 21 is performed by the substrate introduction rod 36. The pallet 40 and the substrate loading rod 36 are driven by a motor, and the loading and unloading operations can be automatically performed by computer control. By using a multiloader, deposition of endohedral fullerene films on multiple deposition substrates and substrate exchange can be performed continuously in a vacuum chamber. Example

[0032] (Structure of multi loader)

FIGS. L (a) and (b) are cross-sectional views of a multiloader according to the endohedral fullerene manufacturing apparatus of the present invention. The multiloader includes a disk-shaped pallet 2 on which a deposition substrate 3 is mounted, and a housing 1 for storing the pallet.

The pallet 2 and the housing 1 are made of a material such as stainless steel, and are connected via a flange 7 to the main chamber 1 of the endohedral fullerene manufacturing apparatus. At the bottom of the housing 1, there is an exhaust flange (not shown) for connecting to a vacuum pump. In the embodiment, ten pallets can be mounted on the pallet 2. The pallet 2 has a rotating shaft 5 mounted at the center, and is driven to rotate via a bevel gear by a pallet rotating motor 6 mounted outside the housing.

FIG. 2 (a) is a side view of a multiloader according to the endohedral fullerene manufacturing apparatus of the present invention.

The multiloader 13 is attached to the main chamber 10 via a flange 12 arranged on the side. A magnetic field coil 11 is arranged around the main chamber 10. The multi loader 13 performs evacuation by a vacuum pump 14 attached to a lower part. The driving device of the multi-header includes a motor 17 for moving the board insertion rod and a motor 16 for attaching and detaching the board, in addition to the motor 15 for rotating the pallet.

The substrate insertion rod is horizontally moved by the substrate insertion rod moving motor 17 to move the substrate from the pallet to the main chamber. In addition, by rotating the substrate on the pallet by the substrate attaching / detaching motor 16, an operation of fixing the substrate to the substrate supporting portion on the pallet or removing the substrate from the substrate supporting portion is performed. FIG. 2 (b) is a front view of the multiloader on the side where the deposition substrate is taken out of the multiloader into the atmosphere. An openable / closable lid 18 is provided on the housing of the multi-loader. The lid 18 can be opened to take out the substrate from the pallet.

[0037] (Load / Unload procedure)

FIGS. 5 (a), (c), (e), (g), (i), and (k) show the loading and unloading procedures of a deposition substrate using the endohedral fullerene manufacturing apparatus of the present invention. 5 (b), (d), (f), (h), (j), and (1) are cross-sectional views, respectively, of FIGS. 5 (a), (c), (e), and (g). FIG. 3 is a front view of a pallet corresponding to (i) and (k). The work of mounting the deposition substrate on the pallet from the outside of the manufacturing apparatus is performed by purging the multi-loader housing 63 with nitrogen gas while the gate chamber 16 is closed and the main chamber 61 is evacuated. Open the lid, for example, by hand.

In the embodiment shown in FIG. 5B, up to ten deposition substrates can be mounted on the pallet. After the mounting of the deposition substrate is completed, the lid of the case is closed, the introduction of nitrogen gas is stopped, and the case is evacuated.

First, an endohedral fullerene film is deposited on the deposition substrate A (FIG. 5 (a)). First, the substrate insertion rod 67 is protruded, and after fixing the substrate insertion rod 67 to the deposition substrate, the insertion rod 67 is rotated by a set angle. At the same time, the deposition substrate 65 rotates by the same angle, and the pallet 64 can be detached. The gate valve 62 is opened (FIG. 5 (c)), and the insertion rod 67 is further protruded to transfer the deposition substrate 65 to the main chamber 61 (FIG. 5 (e)). In a state where the deposition substrate is transported to a predetermined position, plasma 68 is irradiated to the deposition substrate 65, and an endohedral fullerene film is deposited on the deposition substrate 65 (FIG. 5 (g)).

Next, the plasma 68 is stopped, and the insertion rod 67 is moved to the position of the pallet. At the pallet position, the insertion rod 67 is rotated by the set angle to fix the deposition substrate 65 to the pallet 64 (FIG. 5 (i)).

Next, the pallet 64 is rotated to move the deposition substrate B to the transfer position by the insertion rod 67 (FIG. 5 (k)). The same procedure described above for substrate A is performed for the deposition substrates on other pallets, including substrate B, and when the set deposition on the deposition substrates on the pallets is completed, the gate Close 62.

Next, after stopping the evacuation of the housing 63 and performing a nitrogen purge, the lid of the housing is opened. Then, the deposition substrate is taken out of the manufacturing apparatus.

The work of mounting the deposition substrate on the pallet from the outside of the manufacturing apparatus can be performed while rotating the pallet by step driving with the pallet rotation motor. Also, the cross-sectional view showing the loading / unloading procedure of the deposited substrate shown in Fig. 5 describes the case where the plasma is stopped except during the deposition of the endohedral fullerene shown in Fig. 5 (g). It is also possible to change the deposited substrate as it is, and in this case, there is an effect that the time required to start or stop the plasma can be reduced.

(Second embodiment of endohedral fullerene manufacturing apparatus)

In the first embodiment of the endohedral fullerene manufacturing apparatus of the present invention shown in FIG. 3, since the magnetic field generated by the magnetic field coil 24 does not act at the position of the multiloader 22 and the plasma spreads, it is not possible to deposit the endohedral fullerene film. I can't do it. Therefore, it is necessary to transport the deposition substrate 35 from the position of the pallet 40 to the position where the magnetic field acts by using the substrate insertion rod 36 and irradiate the plasma to deposit the film. Time was a factor in reducing the efficiency of the deposition experiment.

In the second embodiment of the endohedral fullerene manufacturing apparatus of the present invention shown in FIG. 8, the pallet 218 is disposed between the magnetic field coil 204 and the magnetic field coil 205. In addition, non-magnetic materials such as stainless steel (non-magnetic) and molybdenum are used as materials for the pallets and peripheral device members. Therefore, the plasma is irradiated onto the deposition substrate also on the pallet 218, and the deposition of the endohedral fullerene film on the pallet is possible. The mounting of the substrate on the pallet is performed through the mouthpiece chamber 202 and the gate valve 203.

[0046] (Purge box)

In the first embodiment of the endohedral fullerene manufacturing apparatus of the present invention shown in FIG. 3, the lid attached to the case of the multiloader is opened, and the deposition substrate is directly attached to and detached from the pallet from outside the apparatus. However, some of the endohedral fullerene films are extremely reactive, and may react with moisture or oxygen in the air to deteriorate.

FIGS. 9A and 9B are cross-sectional views of the purge box according to the endohedral fullerene manufacturing apparatus of the present invention. The purge box 231 is a box attached to the multiloader 234, and supplies and supplies nitrogen from the introduction pipe 241. The purge box allows external work Work bags 239, 247 protruding into the purge box from the openings 236, 237, 238, 246 are attached. The operator can insert the desiccator 245 into the purge box 231 through the purge box opening / closing lid 240, operate the external force of the purge box, and attach and remove the deposition substrate to and from the pallet.

[0048] (Shielding member for preventing device contamination)

Among the encapsulating atoms that make up the endohedral fullerene, there are highly reactive materials and highly corrosive materials. For example, when Na is used as an encapsulated atom, it must be handled with great care when handling Na adhering to the inside of a vacuum vessel because Na reacts violently with explosion to water.

[0049] FIGS. 10 (a), (b) and (c) are diagrams for explaining a shielding member for preventing contamination of the apparatus according to the present invention.

In the embodiment shown in FIG. 10A, a shielding member is arranged in the multiloader 256. The shielding member 260 is attached to the side of the inner wall of the multiloader 256 adjacent to the gate valve 255, and is arranged so as to shield the gap between the pallet 257 and the inner wall of the housing. There is a gap of about 3 mm to 10 mm between the shielding member 260 and the pallet 257, and the pallet can rotate freely. By arranging the shielding member 260, it is possible to minimize the gas composed of Na or the like or the plasma from diffusing into the housing of the multiloader 256, thereby improving work safety, This is effective in simplifying the cleaning of the device.

In the embodiment shown in FIGS. 10B and 10C, a shielding member is arranged in the main chamber 261.

The shielding shutter 264 is attached to the vicinity of the fullerene film forming position in the main chamber so that it can be taken in and out by an operation from the outside.

As shown in FIG. 10 (b), when irradiating the deposition substrate with the plasma 262 to generate the encapsulated fullerene film, the plasma 262 is stored in the storage unit so that the shutter 264 does not hinder the flow of the plasma 262. Keep it. As shown in FIG. 10 (c), when the deposition substrate is pulled out by the insertion rod 269 and the deposition substrate is exchanged, the plasma 262 is shielded by exposing the shutter 264 inside the main chamber 1. Deposition substrates can be replaced without stopping plasma, and contamination of the multiloader can be prevented. Therefore, there is no need to stop and restart the plasma, which is effective in shortening the working time and improving the efficiency of the experiment. (Third Embodiment of Encapsulated Fullerene Production Apparatus)

When the atoms contained in the fullerene are gases, for example, as a method for producing a fullerene containing fluorine, a raw material gas such as CF is introduced into a vacuum chamber and distributed around the vacuum chamber.

Four

An alternating current is passed through the placed high-frequency induction coil 304 to excite the particles constituting the source gas and generate a high-frequency plasma comprising ions and electrons such as CF ⁺ and F—.

Three

A plasma conducting method is known.

[0054] The generated plasma is confined in the axial direction in the main chamber 301 along a uniform magnetic field (B = 2 to 7 kG) formed by the magnetic field coil 302, and the plasma flowing from the plasma generation part toward the deposition substrate 307. It becomes a flow. By applying a positive bias voltage to the grid electrode 310 through which the plasma flow passes, only negative charges such as electrons and fluorine ions are selectively passed. The electrons accelerated by the grid electrode have an energy of 10 eV or more, and collide with the fullerene molecules ejected from the fullerene sublimation oven 305, thereby depriving the fullerene molecules of the electrons, thereby causing the fullerene positive ions C Generate ⁺ . Plastic

60

The C ⁺ and F— constituents of the zuma react to form fluorine-containing fullerene and deposit on the deposition substrate 307.

60

Blame ^.

A multi-loader 311 is attached to the main chamber 301 via a gate valve 312. A pallet 313 on which a plurality of deposition substrates can be mounted is disposed in the multiloader, and the rotation of the pallet and the operation of the substrate insertion rod 315 allow the exchange of the deposition substrates.

In the generation of endohedral fullerenes by high-frequency induction plasma as shown in FIG. 11, since the ion density distribution in the plasma is uniform in the radial direction of the plasma flow, the deposition substrate is divided and the in-plane bias voltage is reduced. There is no need to control the distribution. Therefore, a single continuous disk-shaped deposition substrate is used, and a uniform bias voltage is applied to the deposition substrate to generate endohedral fullerenes.

[0057] In the generation of endohedral fullerenes by such a high-frequency induction plasma, it is necessary to carry out experiments for optimizing the deposition conditions by changing the deposition conditions in various ways, and by exchanging the deposition substrates using a multiloader. , It is possible to improve the efficiency of deposition experiments

Claims

The scope of the claims

[1] In the first vacuum vessel, fullerene is introduced from a fullerene introduction part into a plasma flow generated by a plasma generation part of atoms to be included, and the fullerene is deposited on a deposition substrate arranged downstream of the plasma flow. In a fullerene manufacturing apparatus, a substrate mounting member capable of mounting a plurality of deposition substrates is disposed in a second vacuum container connected to the first vacuum container via a gate valve, and the substrate mounting member is mounted on the first vacuum container. An apparatus for manufacturing an endohedral fullerene, wherein the deposition substrate is exchanged in a vacuum chamber by rotating.

[2] In the first vacuum vessel, fullerene is introduced from the fullerene introduction part into the plasma flow generated by the plasma generation part of the atom to be included, and the fullerene is deposited on the deposition substrate disposed downstream of the plasma flow. In the fullerene manufacturing apparatus, a substrate mounting member capable of mounting a plurality of deposition substrates is disposed in the first vacuum vessel, and the substrate mounting member is rotated to exchange the deposition substrate in a vacuum chamber. An apparatus for producing endohedral fullerenes.

3. The apparatus for producing an endohedral fullerene according to claim 1, wherein the fullerene is Cn (n = 60-84).

4. The apparatus for producing an endohedral fullerene according to claim 1, wherein the atom to be included is an alkali metal.

[5] The apparatus for producing an endohedral fullerene according to any one of [1] to [3], wherein the atom to be included is a halogen element.

6. The apparatus for producing an endohedral fullerene according to claim 1, wherein the substrate mounting member is a disk-shaped member.

[7] A purge box in which an inert gas is introduced is connected to the take-out portion of the deposition substrate.

3. The apparatus for producing an endohedral fullerene according to claim 1, wherein an operation of taking out or mounting the deposition substrate is performed in the purge box.

[8] A shielding member arranged between the inner wall of the second vacuum vessel and the substrate mounting member for preventing diffusion of plasma or gas comprising the contained atoms. Item 1. An apparatus for producing an endohedral fullerene according to item 1.

[9] A shutter for blocking a plasma flow at the time of protrusion and a storage part of the shutter are arranged in the first vacuum vessel, and the storage part is stored when the endohedral fullerene film is deposited on the deposition substrate. The apparatus for producing an endohedral fullerene according to any one of claims 1 to 2, wherein the shutter is protruded to replace a plasma flow when the deposition substrate is replaced in a storage chamber.

[10] In a vacuum vessel, a fullerene is introduced from a fullerene introduction section into a plasma flow generated by a plasma generation section of atoms to be included, and the fullerene is deposited on a deposition substrate disposed downstream of the plasma flow. A method for producing an endohedral fullerene, comprising exchanging the deposition substrate in a vacuum chamber.

11. The method for producing an endohedral fullerene according to claim 10, wherein the fullerene force is Cn (n = 60-84).

12. The method for producing an encapsulated fullerene according to any one of claims 10 to 11, wherein the atom to be included is an alkali metal.

13. The method for producing an encapsulated fullerene according to any one of claims 10 to 11, wherein the atom to be included is a halogen element.