JP4711614B2 - Method and apparatus for producing endohedral fullerene - Google Patents

Description

  The present invention relates to an endohedral fullerene production method and apparatus.

The Journal of Plasma and Fusion Research, Vol. 75, No. 8, issued in August 1999 Conventionally, as a technique for producing an endohedral fullerene, a technique shown in FIG. 6 has been proposed (see Non-patent 1).

  In this technique, an endohedral fullerene is produced by injecting fullerene into a plasma flow of atoms to be encapsulated in a vacuum vessel and depositing the endohedral fullerene on a plate disposed downstream of the plasma flow.

  According to such a technique, it is possible to produce an endohedral fullerene at a low temperature and with a high yield.

  However, such a technique has a problem that the inclusion rate is not good at the center of the plate. That is, there is a problem that the endohedral fullerene is almost deposited on the radially outer portion of the plasma flow, and the endohedral fullerene is hardly deposited on the radially inner side of the plasma flow.

On the other hand , recently, attention has been paid to various usefulness of endohedral fullerene, and a technique capable of producing endohedral fullerene with higher yield is desired.

  An object of this invention is to provide the manufacturing method and manufacturing apparatus of endohedral fullerene which can manufacture endohedral fullerene with more yield property.

The method for producing an endohedral fullerene according to the present invention includes forming a plasma flow of atoms to be encapsulated by introducing atoms to be encapsulated toward a hot plate in a vacuum vessel, introducing fullerene into the plasma flow, and In a method for producing an endohedral fullerene in which an endohedral fullerene is deposited while applying a bias voltage to a deposition plate disposed downstream of the flow, the deposition plate is composed of a plurality of division plates divided concentrically, and of the division plates The gist is to apply a bias voltage Δφ _ap of −2 V <Δφ _ap <+20 V to the central plate of the plate and introduce the fullerene along the outflow direction of the plasma flow.

Method for producing endohedral fullerenes of the present invention, the radius of the hot plate as R, the radius of the plate in the center of the split plate and gist that the following R + 5 mm.

Method for producing endohedral fullerenes of the present invention, the measuring means for measuring the distribution of fullerene ions contained target atom ions in the plasma stream into the deposition plate before provided, on the basis of the measurement signal from the measuring means and gist applying any bias voltage per plate divided plate.

  In the method for producing an endohedral fullerene according to the present invention, a radius of the hot plate is set as R, a cylinder having an inner diameter of R + 5 mm or more is provided in the middle of the plasma flow, and fullerene is disposed from the outer periphery of the cylinder along the plasma flow. The gist is to introduce.

  The method for producing an endohedral fullerene according to the present invention is summarized in that the encapsulating target atom is an alkali metal atom.

  The fullerene production apparatus of the present invention includes a vacuum vessel, a plasma flow forming means for forming a plasma flow of atoms to be included, and a fullerene introduced into the vacuum vessel along the outflow direction of the plasma flow. Introducing means, holding means for holding a plurality of divided plates arranged concentrically downstream of the fullerene introduction position downstream of the plasma flow, and an arbitrary bias voltage for each of the divided plates And a bias applying means for applying.

  A gist of the endohedral fullerene manufacturing apparatus of the present invention is that the bias applying means independently varies the voltage applied to each of the divided plates.

The apparatus for producing an endohedral fullerene according to the present invention is characterized in that the bias applying means applies a bias voltage Δφ _ap of −2 V <Δφ _ap <+20 V to the divided plate disposed in the center.

  The gist of the endohedral fullerene production apparatus of the present invention is that the radius of the plasma flow forming means is R, and the radius of the central part of the divided plate is R + 5 mm or less.

  In the endohedral fullerene production apparatus of the present invention, measuring means for measuring the distribution of fullerene ions and encapsulating target atomic ions in the plasma flow is arranged upstream of the dividing plate, and a signal from the measuring means is received. The gist of the invention is that the bias voltage applied to each of the divided plates applied by the bias applying means is independently controlled.

  In the endohedral fullerene production apparatus of the present invention, a tube having an inner diameter of R + 5 mm or more is disposed in the middle of the plasma flow, where R is the radius of the plasma flow forming means, and the tube is arranged so as to follow the plasma flow. The gist is that fullerene is introduced from the outer periphery.

  The gist of the endohedral fullerene manufacturing apparatus of the present invention is that the distance from the downstream end of the cylinder to the dividing plate is set to be twice or more the length of the cylinder.

  The gist of the endohedral fullerene production apparatus of the present invention is that the inclusion target atom is an alkali metal atom.

  The apparatus for producing endohedral fullerene according to the present invention is characterized in that the plasma flow forming means includes a hot plate and a nozzle for introducing the encapsulating target atoms toward the hot play.

Apparatus for producing endohedral fullerenes of the present invention, at least downstream of the downstream end of said tube, and gist in that a cooling means order to cool the wall of the vacuum vessel.

  According to the method for producing an endohedral fullerene of the present invention, by introducing encapsulating target atoms toward the hot plate, a plasma flow of the encapsulating target atoms is formed in the vacuum vessel, and the inside of the vacuum vessel is aligned along the outflow direction of the plasma flow. The fullerene is introduced into the plasma plate, and the inclusion fullerene is deposited by applying a bias voltage to the deposition plate disposed downstream of the plasma flow, so that it is possible to obtain the inclusion fullerene even at the center of the hot plate. Combined with the introduction of fullerene along the outflow direction, the yield of endohedral fullerene can be greatly improved, and the distance from the fullerene introduction position to the hot plate can be shortened. This can contribute to the miniaturization of the entire apparatus.

  FIG. 1 shows an endohedral fullerene production apparatus according to an embodiment of the present invention.

This apparatus includes a vacuum vessel 1, a hot plate 3 as a plasma flow forming means for forming a plasma flow 2 of inclusion target atoms, an inclusion target atom oven 4, and a concentric circle disposed downstream of the plasma flow 2. A holding means 6 for holding the endohedral fullerene deposition plate 5 composed of a plurality of divided plates 5a, 5b, 5c (see FIG. 2), and an arbitrary bias voltage is applied to each of the divided plates 5a, 5b, 5c. Bias applying means 7 a , 7 b, 7 c (see FIG. 2) and fullerene introducing means 8 for introducing fullerene upstream of the endohedral fullerene deposition plate 5.

  This apparatus will be described in detail below.

  In this example, the means for forming the plasma flow of the inclusion target atoms includes a hot plate 3 such as tungsten and an inclusion target atomic oven 4 as an evaporation oven for alkali metal (example of inclusion target atoms). . When alkali as an inclusion target atom is sprayed from the inclusion target atom oven 4 toward the hot plate 3 heated to about 2500 ° C., plasma is generated by contact ionization. The generated plasma is confined in the axial direction in the vacuum chamber 1 along a uniform magnetic field (B = 2 to 7 kG) formed by the electromagnetic coil 11. At this time, the diameter of the hot plate 3 is approximately the diameter of the plasma flow 2. Therefore, the diameter of the plasma flow 2 can be arbitrarily selected to an appropriate size according to the size of the apparatus by changing the diameter of the hot plate 3.

A cooling means (not shown) is provided on the outer periphery of the vacuum vessel 1. By this cooling means, the inner wall of the vacuum vessel 1 is cooled, and neutral gas molecules are trapped on the inner wall of the vacuum vessel 1. Plasma free of impurities by preparative wrap the neutral gas molecules in the inner wall allows generation, it is possible to obtain a high endohedral purity is over-encapsulated fullerene deposition plate 5. In particular, when the cylinder 13 is provided, it is preferable to cool at least the inner wall of the vacuum vessel 1 between the downstream end of the cylinder 13 and the internal fullerene deposition plate 5. The inner wall temperature of the vacuum vessel 1 is preferably room temperature or lower, more preferably 0 ° C. or lower. By setting such a temperature, it becomes easy to trap neutral molecules, and it is possible to obtain a higher-purity endohedral fullerene.

In this example, a copper tube 13 is provided in the middle of the plasma flow 2 so as to cover the plasma flow 2. The tube 13 is provided with a hole, and fullerene is introduced into the plasma flow 2 through the hole.
At that time, the cylinder 13 is heated to 400 to 450 ° C. Fullerene adhering to the inner surface after being introduced into the cylinder 13 without ionization in the plasma is re-sublimation.

The inner radius of the tube 13, the radius of the hot plate 3 when the R, it is preferable that the R + 5 mm or more. When the inner radius of the tube 13 is less than R + 5 mm, the interaction between the plasma flow 2 and the tube 13 is increased, the plasma retention is lowered, and the yield of the endohedral fullerene is decreased. In addition, when the inner radius of the cylinder 13 is too large, not only the entire apparatus becomes large, but also problems such as a reduced plasma confinement effect by the cylinder 13 occur.
Therefore, the inner radius of the cylinder 13 is preferably R + 5 cm or less. If the inner radius of the tube 13 is R + 5 cm or less, a plasma confinement effect can be obtained. The inner radius of the cylinder 13, and more preferably, the R + 5 cm or less. With R + 5 cm or less, the reaction of ions necessary for forming the endohedral fullerenes can be sufficiently high plasma density occurs at high probability.

In the apparatus shown in FIG. 6 , the yield was different for each apparatus. The present inventor is the radius of the cylinder is found to affect the yield. In particular, it was found that the relationship between the radius of the plasma flow. Further, as R + 5mm~R + 5cm, it was found that the yield is markedly properly increased in a limited range.

It is the divergence angle of the introduction angle of the fullerene at the time of introducing the fullerenes provided in the cylinder 13, preferably 90 to 120 °. The divergence angle of introducing higher efficiency of the fullerene into plasma by this range, the yield of endohedral fullerenes is enhanced. In order to change the spread angle degree may be changed the ratio between the diameter and the length of the inlet nozzle of the fullerene.

Further, fullerenes, as shown in FIG. 5, is ejected along the flow Re direction of the plasma stream 2.

  The introduction rate of fullerene may be controlled by the rate of temperature increase of the fullerene sublimation oven 4. The rate of temperature increase is preferably 100 ° C./min or more. The upper limit is the rate of temperature rise at which bumping does not occur.

Distance _{l u} between the upstream end and the hot plate 3 (the drawing left of FIG. 1) of the cylinder 13, to be set to be ^{_{1.0~2.0 × (πD H 2/4}} ) preferable. _DH is the outer diameter of the hot plate. Such l cylinder 13 by a _u, it is possible to achieve heat due can be avoided to undergo maintenance over time to a stable plasma than from the hot plate.

  In the vacuum container 1, an ion measurement probe 14 for measuring ion distribution is provided on the front side of the inclusion fullerene deposition plate 5. A signal from the probe 14 is sent to the probe circuit 15 and the computer 16, and the bias voltage applied to the endohedral fullerene deposition plate 5 is controlled based on the signal.

  The bias voltage control based on the measured ion density distribution is performed as follows, for example. The ion measurement probe 14 measures a current flowing through the ion measurement probe 14 by applying a bias voltage with respect to the plasma potential, and obtains the measured current force ion density by calculation. When a positive bias voltage is applied to the ion measurement probe 14, fullerene ions that are negative ions flow into the ion measurement probe 14, and the ion density of the fullerene can be measured. Conversely, when a negative bias voltage is applied to the ion measurement probe 14, the ion density of the inclusion target atoms such as Na, which is a positive ion, can be measured. In this way, by switching the polarity of the bias voltage applied to the ion measurement probe 14 and moving the ion measurement probe 14 in the radial direction of the plasma flow 2 to measure the probe current, fullerene ions and ions of inclusion target atoms are obtained. The bias voltage applied to the endohedral fullerene deposition plate 5 is controlled as follows according to the measured ion density distribution.

At the measurement position corresponding to each divided plate,
(1) Ion density of fullerene> Ion density of inclusion target atom → Decrease the bias voltage of the corresponding divided plate.
(2) Ion density of fullerene <Ion density of inclusion target atom → Increase the bias voltage of the corresponding divided plate.
(3) Ion density of fullerene ≒ Ion density of inclusion target atom → The bias voltage of the corresponding divided plate is not changed.

The degree to which the bias voltage is changed is controlled by the difference in ion density between fullerene and inclusion target atoms.

  As shown in FIG. 2, the endohedral fullerene deposition plate 5 is concentrically divided into three divided plates 5a, 5b, and 5c. That is, the central division plate 5a is circular, and ring-shaped division plates 5b and 5c are arranged on the outer periphery of the division plate 5a so as to be electrically insulated from the division plate 5a. In addition, the number of division | segmentation plates is not limited to three, Two may be sufficient and four or more may be sufficient. Each of the divided plates 5a, 5b, 5c is provided with bias applying means 7a, 7b, 7c so that a bias voltage can be applied independently. The shape of the divided plates 5a, 5b, and 5c is not limited to a circular or circular ring as long as the shape of the vacuum vessel is not limited, and may be, for example, a square or a square ring or other shapes.

The radius of the central split plate 5a is preferably R + 5 mm or less, where R is the radius of the hot plate 3. Be larger than the R + 5 mm, probability to be encapsulated fullerene gas formed in part of the outer is because low. From the viewpoint of improving the degree of background vacuum and shortening the evacuation time, it is preferable to downsize the manufacturing apparatus. Therefore, from the viewpoint of using the generated plasma without waste and reducing the size of the manufacturing apparatus, it is preferable that the radius of the divided plate 5a disposed at the center is R + 5 mm or less. However, even when the encapsulated fullerene deposition plate 5 is not divided and the same bias voltage is applied to the entire surface of the encapsulated fullerene, it is possible to form the encapsulated fullerene by optimizing the deposition conditions.

The radius of the plasma flow 2 confined by the magnetic field having the magnetic field strength B is larger than the radius of the hot plate 3 that generates plasma by the Larmor radius _{RL of} ions constituting the plasma. _RL is inversely proportional to the magnetic field strength B. For example, under the condition of B = 0.3T and the plasma temperature of 2500 ° C.,
Na of _{R L = 1.1mm, R L =} 4.0mm of _{C 60}
Can be estimated. Therefore, it is preferable to design the sizes of the divided plates 5a, 5b, and 5c on the basis of R + 5 mm in consideration of the application range of manufacturing conditions such as the magnetic field strength B and the plasma temperature.

  It is preferable to apply a positive bias voltage to the central divided plate 5a. Thereby, the interaction between the inclusion target atom ion and the fullerene ion is increased, and the inclusion target atom is easily included. However, it is possible to form the endohedral fullerene by optimizing the deposition conditions even in the case where the floating voltage state is applied without applying a bias voltage to the divided plate 5a in the central portion.

  Further, when a bias voltage is applied to the central divided plate 5a, the inclusion rate can be increased by controlling the bias voltage so that the fullerene ions have a distribution having the peak at the center of the plasma flow 2. it can. The optimum bias voltage varies depending on the atoms to be included, the type of fullerene, and other film forming conditions, but may be grasped in advance by experiments.

For example, when an alkali metal is used as the inclusion target atom and C ₆₀ is used as the fullerene, a bias voltage of −2 V <φ _{ap 1} <+20 V is applied to the central divided plate 5 a shown in FIG. Is preferred. Further, 0V ≦ φ _{ap 1} ≦ + 18V is particularly preferable.

  The divided plates 5b and 5c other than the central divided plate 5a may be in a floating potential state. Even in the floating state, the same amount of endohedral fullerene as in the prior art is deposited on the portion of the divided plate 5b. Accordingly, the overall yield is increased by the increase in the yield of the split plate 5a at the center.

Of course, when the density of the fullerene ions in the portion corresponding to the divided plate 5b is lowered due to fluctuations in the film forming conditions, a bias voltage may be applied to the divided plate 5b to increase the fullerene ion density. During deposition, the absolute pictorial distribution measured by the ion measuring probe 11 may be automatically controlled bias voltage to be applied dividing plate 5b, to 5c by a computer 16. The same applies to the automatic control of the application to the divided plate 5a.
The vacuum vessel 1 is provided with a pump 10 so that the inside of the vacuum vessel 1 can be evacuated.
Examples of the fullerene in the present invention include C _n (n = 60 , 70 , 74 , 82 , 84 , ...).

  When the distance from the downstream end of the cylinder 13 to the endohedral fullerene deposition plate 5 is set to be twice or more than the length of the cylinder 13, the concentration of neutral fullerene in the film deposited on the endohedral fullerene deposition plate 5 is It can be made even lower. That is, the concentration of the endohedral fullerene in the film can be further increased.

At this time, by setting the fullerene introduction direction along the plasma flow 2, the set shortest distance from the downstream end of the tube 13 to the inclusion fullerene deposition plate 5 can be shortened, and the apparatus main body can be downsized. be able to. At this time, the set shortest distance from the downstream end of the tube 13 to the endohedral fullerene deposition plate 5 is preferably twice the length of the tube 13.
Further, there may be a plurality of nozzles for introducing fullerene, or a shape having a mouth in an oblique direction.

Example 1
Sodium-encapsulated C ₆₀ (Na @ C ₆₀ ) fullerene was formed using the apparatus shown in FIG.

  In this example, the vacuum vessel 1 having a diameter of 100 mm and a length of 1200 mm was used.

In this example, a φ20 mm tungsten hot plate was used as the hot plate 3. The tungsten hot plate 3 was heated to 2500 ° C. Sodium vapor was introduced from the oven 4 toward the heated tungsten hot plate 3. The inside of the vacuum vessel 1 was set to 1 × 10 ⁻⁴ Pa, and the magnetic field strength B was set to B = 0.3T.

In the middle of the plasma flow 2, a copper cylinder 13 having holes was provided. Copper tube 13, the inner diameter D _c is used as a 55 mm. The cylinder 13 was heated to about 400 ° C.

It was then introduced fullerenes along the bore of the tube 13 in the flow Re direction of the plasma stream 2.

  On the other hand, a three-split type plate was used as the split plate. The central dividing plate 5a has a diameter of 14 mm, the outer dividing plate 5b has a diameter of 32 mm, and the outer dividing plate has a diameter of 50 mm.

Δφ _ap = 5V was applied as the bias voltage Δφ _ap (= φ _{ap 1} −φ _s ) to the central divided plate 5a. The divided plates 5b and 5c were in a floating potential state. Note that φ _ap is a DC voltage, and φ _s is a plasma space potential.

When the ion distribution in the middle of the film formation was measured by the ion measurement probe 14, the distribution was in the radius r direction as shown by the solid line in FIG. That is, a result was obtained in which C ₆₀ ⁻ ions were concentrated in the central region.

After film formation for 30 minutes, the endohedral fullerene (Na @ C _{60 in} this example) -containing thin film deposited on the divided plate was analyzed. The endohedral fullerene was formed with a high content on the divided plate 5a in the center. Moreover, the deposition film | membrane containing an endohedral fullerene was recognized on the division | segmentation plate 5b in the outer side of center part.

The mass spectrometry result is shown in FIG.
(Example 2)
In this example, the influence of the diameter of the cylinder 13 was examined.

  The inner diameter D of the cylinder 13 was set to 30 mm, 40 mm, 48 mm, 50 mm, 60 mm, 70 mm, 80 mm, and 100 mm, and film formation was performed in the same manner as in Example 1 to examine the yield of the endohedral fullerene.

In the case of Example 1 (in the case of D _c = 55 mm), when the yield on the split plate at the center was 1, the following yield was obtained. The values in parentheses are the ratio with the outer diameter of the hot plate.

30 mm (1.5) 0 . 6
40 mm (2.0) 0.7
48mm (2.4) 0.8
50mm (2.5) 0.95
55mm (2.8) 1
60mm (3.0) 0.95
70 mm (3.5) 0.7
80 mm (4.0) 0.5
100 mm (5.0) 0.5
It can be seen that when the ratio to the outer diameter of the hot plate is in the range of 2.5 to 3.0, the yield is very excellent as compared with the other ranges.
(Example 3)
In this example, the inclusion fullerene was deposited by changing the bias value to the central divided plate 5a in the range of -10V to 20V.

  The result is shown in FIG.

Excellent yields are shown in the range of −5 V <φ _{ap 1} <+20 V. 0V ≦ φ _{ap 1} ≦ + 1
A better yield is shown in the 8V range.

It is a conceptual diagram which shows the manufacturing apparatus of the endohedral fullerene which concerns on embodiment of this invention. It is a front view which shows the division | segmentation plate of FIG. 2 is a graph showing the distribution of fullerene ions in Example 1. 6 is a graph showing the distribution of fullerene ions in Example 3. It is a conceptual diagram which shows the manufacturing apparatus of the endohedral fullerene which concerns on embodiment of this invention. It is a conceptual diagram which shows the manufacturing technique of the conventional endohedral fullerene.

DESCRIPTION OF SYMBOLS 1 Vacuum container 2 Plasma flow 3 Hot plate 4 Inclusion object atomic oven 5, 5a, 5b, 5c Division | segmentation plate 6 Introduction means (support means)
7a, 7b, 7c Bias voltage applying means
8 Oven for fullerene sublimation 10 Exhaust pump 11 Electromagnetic coil (coil for external magnetic field application)
13 Tube 14 Probe for ion measurement 15 Probe circuit 16 Computer

Claims (19)

In a vacuum vessel, by introducing atoms to be included toward the hot plate, a plasma flow of the atoms to be included is formed, fullerene is introduced into the plasma flow, and a bias is applied to the deposition plate disposed downstream of the plasma flow. In the method for producing an endohedral fullerene in which the endohedral fullerene is deposited while applying a voltage,
The deposition plate is composed of a plurality of divided plates concentrically divided, and a bias voltage Δφ _ap of −2 V <Δφ _ap <+20 V is applied to a central plate of the divided plates ,
The method for producing an endohedral fullerene, wherein the fullerene is introduced along the outflow direction of the plasma flow. Wherein the radius of the hot plate as R, the manufacturing method of the endohedral fullerenes as claimed in claim 1 in which the radius of the plate in the center portion of the divided plates, characterized in that not more than R + 5 mm. Measuring means for measuring the distribution of fullerene ions contained target atom ions in the plasma stream into the deposition plate before provided, any bias voltage for each plate of the division plate based on the measurement signal from the measuring means The method for producing an endohedral fullerene according to claim 1 or 2, wherein: is applied. 2. A cylinder having an inner diameter of R + 5 mm or more is provided in the middle of the plasma flow with a radius of the hot plate as R, and fullerene is introduced from an outer periphery of the cylinder along the plasma flow. The method for producing an endohedral fullerene according to any one of claims 3 to 3 . The method for producing an endohedral fullerene according to any one of claims 1 to 4 , wherein the encapsulating target atom is an alkali metal atom. The method for producing endohedral fullerene according to any one of claims 1 to 5 , wherein the fullerene is introduced from a plurality of nozzles . The method for producing an endohedral fullerene according to any one of claims 1 to 5 , wherein the fullerene is introduced from a nozzle having a mouth in an oblique direction . A vacuum vessel, a plasma flow forming means for forming a plasma flow of atoms to be included, and an introducing means for introducing fullerene along the outflow direction of the plasma flow into the vacuum vessel;
Holding means for holding a plurality of divided plates arranged concentrically downstream of the fullerene introduction position downstream of the plasma flow; and for applying an arbitrary bias voltage to each of the divided plates An endohedral fullerene manufacturing apparatus, comprising: a bias applying unit. 9. The endohedral fullerene manufacturing apparatus according to claim 8 , wherein the bias applying unit varies the voltage applied to each of the divided plates independently. It said bias application means, -2V _{<Δφ ap <+} 20V apparatus for producing endohedral fullerenes as claimed in claim 8 or 9, characterized in that a bias voltage is applied [Delta] [phi _ap to split plates arranged in the central part. The radius of the plasma flow forming means as R, production of endohedral fullerenes of mounting any one of claims 8 to 1 0 the radius but arranged in the center of the division plate, characterized in that not more than R + 5 mm apparatus. Measuring means for measuring the distribution of fullerene ions and inclusion target atomic ions in the plasma flow is arranged upstream of the divided plate, and the bias applying means applies the measurement based on a signal from the measuring means. The apparatus for producing an endohedral fullerene according to any one of claims 8 to 11, wherein a bias voltage applied to each divided plate is controlled independently. A tube having a radius of not less than R + 5 mm is disposed in the middle of the plasma flow, where R is the radius of the plasma flow forming means, and fullerene is introduced from the outer periphery of the tube along the plasma flow. to claims 8 to 1 2 of an apparatus for manufacturing endohedral fullerenes according to any one. Apparatus for producing endohedral fullerenes according to claim 1 3, characterized in that the distance to the division plate from the downstream end of the tube was more than twice the length of the tube. The inclusion target atoms apparatus for producing endohedral fullerenes according to any one of claims 8 to 1 4, characterized in that an alkali metal atom. The plasma flow forming means comprises a hot plate and any one of claims 8 to 1 5, characterized in that it comprises a nozzle for introducing the encapsulated object atoms toward the hot plate A device for producing the endohedral fullerene described above. At least downstream of the downstream end of the tube, endohedral fullerenes according to any one of claims 8 to 1 6, characterized in that a cooling means order to cool the wall of the vacuum chamber Manufacturing equipment. The endohedral fullerene manufacturing apparatus according to any one of claims 8 to 17 , wherein the fullerene is introduced from a plurality of nozzles. The endohedral fullerene production apparatus according to any one of claims 8 to 17 , wherein the fullerene is introduced from a nozzle having a mouth in an oblique direction.

Images