JP5245499B2 - Method for producing carbon nanotube - Google Patents

Description

  The present invention relates to a method for producing carbon nanotubes, and more specifically, to a method for producing carbon nanotubes by vapor growth of carbon nanotubes on a substrate.

  Carbon nanotube production methods can be broadly divided into three methods: arc discharge, laser evaporation, and chemical vapor deposition. Among these, in the production of carbon nanotubes by chemical vapor deposition, a carbon nanotube is produced by reacting a gas containing carbon atoms as a raw material in the presence of a transition metal catalyst. The transition metal catalyst may be disposed on a substrate or the like.

  For example, a method for producing carbon nanotubes by chemical vapor deposition using alcohol gas as a raw material is known (see Non-Patent Documents 1 to 3). In any document, a substrate on which a metal catalyst (iron-based) is placed is placed in a quartz tube; the inside of the quartz tube is decompressed and heated to about 600 ° C. to 900 ° C .; alcohol is introduced into the quartz tube. Thus, carbon nanotubes are generated on the substrate.

On the other hand, a technique for producing a carbon nanotube array by vapor growth of carbon nanotubes on a wafer has been reported (see Patent Document 1).
JP 2007-161576 A Chemical Physics Letters 360 (2002) 229-334 J. Phys. Chem. B 2004, 108, 16451-16456 Surface Science Vol. 25, No6, pp318-325 (2004)

  The chemical vapor deposition method is generally considered to be suitable for mass production because the raw material is a gas. If a material gas that is liquid at room temperature is used as a raw material, it is easier to apply to industrial production. However, the production of carbon nanotubes by the conventional chemical vapor deposition method is, so to speak, production at a laboratory level, and it has been difficult to apply to an industrial scale. Accordingly, an object of the present invention is to produce high-quality carbon nanotubes on an industrial scale.

  In the semiconductor manufacturing process, a low pressure chemical vapor deposition (low pressure CVD) apparatus is widely used. Examples of the low pressure CVD apparatus include a batch type apparatus and a single wafer type apparatus. The present inventor studied the application of the low pressure CVD apparatus to the production of carbon nanotubes by vapor phase growth, and completed the present invention.

That is, the first of the present invention relates to a method for producing carbon nanotubes using a batch type low-pressure CVD apparatus described below.
[1] A tube-shaped chamber having a processing chamber for processing a substrate, gas introducing means for introducing a gas for processing the substrate into the processing chamber, and exhausting the gas in the processing chamber An exhaust means, a substrate carry-in / out means for carrying in and out a jig charged with a plurality of substrates in the processing chamber, and a heater provided around the chamber for adjusting the temperature of the substrate in the processing chamber. A method for producing carbon nanotubes on the plurality of substrates using a chemical vapor deposition apparatus comprising:
1) preparing a plurality of substrates on which a catalyst for vapor deposition of carbon nanotubes is arranged on the plane of a substrate having a plane; 2) charging the jig by separating the plurality of substrates from each other. A step of bringing the jig into the processing chamber; 3) a step of exhausting the gas in the processing chamber through the exhaust means to bring the processing chamber to an atmospheric pressure lower than atmospheric pressure; 4) in the processing chamber; Introducing a reducing gas and an inert gas, and raising the temperature of the substrate to a carbon nanotube production temperature with the heater; 5) introducing a raw material gas for producing carbon nanotubes into the processing chamber; A step of generating carbon nanotubes on a plane of the substrate; 6) after the generation of the carbon nanotubes, the temperature of the substrate is controlled by the carbon nanotubes; A step of lowering the temperature of the processing chamber to an atmospheric pressure, and a step of unloading the jig charged with the plurality of substrates from the processing chamber. A method for producing carbon nanotubes.
[2] A tube-shaped chamber having a processing chamber for processing a substrate, a gas introducing means for introducing a gas for processing the substrate into the processing chamber, and exhausting the gas in the processing chamber An exhaust means, a substrate carry-in / out means for carrying in and out a jig charged with a plurality of substrates in the processing chamber, and a heater provided around the chamber for adjusting the temperature of the substrate in the processing chamber. A method for producing carbon nanotubes on the plurality of substrates using a chemical vapor deposition apparatus comprising:
1) A substantially circular substrate having an orientation flat or notch, and having a plurality of regions partitioned in a lattice pattern on the plane, each of the plurality of regions for vapor phase growth of carbon nanotubes A step of preparing a plurality of substrates on which a catalyst is arranged; and 2) a step of charging the jig with the plurality of substrates spaced apart from each other and with the planes parallel to each other, and carrying the jig into the processing chamber. 3) exhausting the gas in the processing chamber through the exhaust means to bring the processing chamber to a pressure lower than atmospheric pressure, and 4) introducing a reducing gas and an inert gas into the processing chamber. , A step of raising the temperature of the substrate to a carbon nanotube generation temperature with the heater, 5) introducing a raw material gas for generating carbon nanotubes into the processing chamber Generating carbon nanotubes on the plane of the substrate, 6) lowering the temperature of the substrate to a temperature at which the carbon nanotubes are not oxidized by oxygen in the air after the generation of the carbon nanotubes, 7) in the processing chamber A method of producing carbon nanotubes, comprising: bringing the pressure to atmospheric pressure; and 8) carrying out a jig charged with the plurality of substrates from the processing chamber.

The second aspect of the present invention relates to a method for producing carbon nanotubes using a single wafer type low pressure CVD apparatus described below.
[3] A chamber having a processing chamber for processing a substrate, a gas introducing means for introducing a gas for processing the substrate into the processing chamber, and an exhausting means for exhausting the gas in the processing chamber. A chemical vapor phase having substrate loading / unloading means for loading and unloading a plurality of substrates charged in the jig one by one into the processing chamber, and a heater disposed in the processing chamber for adjusting the temperature of the substrate. A method of producing carbon nanotubes on the substrate using a growth apparatus,
1) A substantially circular substrate having an orientation flat or notch, and having a plurality of regions partitioned in a lattice pattern on the plane, each of the plurality of regions for vapor phase growth of carbon nanotubes Preparing a plurality of substrates on which a catalyst is disposed, 2) exhausting the gas in the processing chamber through the exhaust means to bring the processing chamber to a pressure lower than atmospheric pressure, and 3) 1 of the substrate A step of carrying a sheet into the processing chamber, 4) a step of raising the temperature of the substrate carried into the processing chamber to a carbon nanotube generation temperature, and 5) introducing a raw material gas for generating the carbon nanotube into the processing chamber. 6) generating carbon nanotubes on the plane of the substrate; 6) after generating the carbon nanotubes, the temperature of the substrate is set to the carbon Step nanotubes lowers in temperature that are not oxidized in the oxygen in the air, and 7) from the processing chamber, comprising the step of unloading the substrate, method of manufacturing the carbon nanotube.

  According to the present invention, carbon nanotubes can be mass-produced by diverting a semiconductor mass production line. In addition, since the carbon nanotube produced by the present invention is a single wall carbon nanotube having semiconducting properties, mass production of a field effect transistor (CNT-FET) using the carbon nanotube as a channel is realized.

  The carbon nanotube production method of the present invention is characterized in that carbon nanotubes are vapor-phase grown on a substrate on which a catalyst is disposed using a low-pressure CVD apparatus. That is, the carbon nanotube of the present invention is formed on a substrate on which a catalyst for vapor-phase growth of the carbon nanotube is disposed. The substrate is not particularly limited, but is preferably a semiconductor wafer when a low pressure CVD apparatus used in a semiconductor manufacturing process is applied. A semiconductor wafer is a substantially circular disk produced by slicing an ingot obtained by crystal growth of a semiconductor material into a columnar shape having a diameter of about 120 mm to about 200 mm to about 0.5 mm to 1.5 mm. Examples of semiconductor materials include silicon.

  A catalyst for vapor growth of carbon nanotubes from a source gas containing carbon atoms is disposed on the plane of the substrate. Although the catalyst arrange | positioned is not specifically limited, What is necessary is just the particle | grains of iron, cobalt, nickel, or those alloys. The catalyst may be arranged by patterning on the substrate by sputtering.

  Further, the plane of the substrate may be divided into a plurality of regions by being partitioned in a lattice shape. By providing a catalyst in each of the plurality of regions, it is possible to obtain a plurality of carbon nanotube device (such as carbon nanotube FET) chips from one substrate.

  The substrate of the present invention preferably has an orientation flat or notch as in the case of a general semiconductor wafer. The orientation of the semiconductor crystal is known by the orientation flat or notch.

  The source gas for vapor growth of the carbon nanotubes may be a gas containing carbon atoms, and may be a saturated hydrocarbon gas such as methane, ethane or propane, or an unsaturated hydrocarbon gas such as ethylene or acetylene. However, it is preferably a substance that is liquid at normal temperature (about 25 ° C.) and is a gas at 0.1 Torr to 0.6 Torr. If it is liquid at room temperature, a highly pure raw material can be easily obtained. In addition, safety is high. An example of a preferred source gas includes ethanol.

  As will be described later, the reducing gas is introduced into the processing chamber in which the substrate on which the catalyst is formed is disposed before introducing the carbon nanotube raw material gas. The reducing gas can activate the catalyst formed on the plane of the substrate. Examples of the reducing gas include hydrogen gas. Further, an inert gas may be introduced together with the reducing gas. This is for diluting the reducing gas. Examples of the inert gas include nitrogen gas and argon gas.

  The carbon nanotube production method of the present invention can be performed using a low-pressure CVD apparatus widely used in a semiconductor production process. The low-pressure CVD apparatus can be roughly classified into a batch type (see FIGS. 1 and 2) and a single wafer type (see FIG. 3). The batch type can be classified into a horizontal type (see FIG. 1) and a vertical type (see FIG. 2) depending on the arrangement of the chambers.

  The batch type low-pressure CVD apparatus has a chamber. The chamber is a tubular member generally made of quartz. A processing chamber for processing a substrate (including forming carbon nanotubes on the substrate) is disposed inside the chamber. The chamber of the batch type low-pressure CVD apparatus may be placed horizontally (the axial direction of the tube is horizontal) or vertically (the axial direction of the tube is vertical).

  The batch type low-pressure CVD apparatus has gas introduction means for introducing gas into the processing chamber of the chamber. The gas introduced into the processing chamber is a reducing gas or an inert gas in addition to the carbon nanotube raw material gas. The source gas is ethanol or the like.

Further, the batch type low-pressure CVD apparatus has an exhaust means for exhausting the gas in the processing chamber of the chamber. By exhausting the gas, the processing chamber can be depressurized, for example, 0.1 Torr to 0.6 Torr. By reducing the pressure to 0.1 Torr to 0.6 Torr, the atmosphere in the chamber (oxygen and other impurities in the atmosphere) can be discharged more reliably, the cause of the outside air can be eliminated, and the CNT can be removed in a more clean state. It can be purified.
On the other hand, if the pressure reduction is not sufficient (for example, 5 to 10 Torr), the volatilization amount of the raw material gas (ethanol or the like) at the time of vapor phase growth becomes high, which may cause the CNT crosslinking rate to increase too much. Then, it is considered that there is a high possibility that a plurality of CNTs including metallic CNTs are cross-linked, and the yield of FETs is reduced due to the cross-linking of one target SW-CNT.

  A heater is preferably provided around the chamber of the batch type low-pressure CVD apparatus. With the heater, the temperature of the substrate placed in the processing chamber can be adjusted. The substrate temperature in the processing chamber when the carbon nanotube source gas is introduced is preferably 700 ° C. or higher and 900 ° C. or lower. This is to form carbon nanotubes efficiently. Further, the processing chamber into which the substrate is loaded is decompressed to a pressure lower than the atmospheric pressure.

  When a batch type low-pressure CVD apparatus is used, a jig for charging a plurality of substrates is carried into the processing chamber. It is preferable that the plurality of substrates arranged on the jig are separated from each other, and the substrate surfaces on which the catalyst is arranged are arranged in parallel to each other. More specifically, it is preferable that the substrates have an interval of about 6 mm.

  Furthermore, it is preferable that the plurality of substrates charged in the jig are arranged in the processing chamber so that the plane thereof is orthogonal to the axial direction of the chamber tube. That is, since the axis of the batch tube of the batch type horizontal low pressure CVD apparatus is horizontal, the substrate plane is preferably arranged in the vertical direction. On the other hand, since the axis of the tube of the batch of the batch type vertical low pressure CVD apparatus is vertical, the substrate plane is preferably arranged in the horizontal direction.

  On the other hand, the chamber of the single-wafer type low-pressure CVD apparatus may be tubular like the batch type, but the shape is not particularly limited. Inside the chamber, there is a processing chamber for processing the substrate, and the substrates are carried into the processing chamber one by one. It is preferable that a heater for adjusting the temperature of the substrate is provided at a position where the substrate is disposed in the processing chamber.

  The chamber of the single wafer type low pressure CVD apparatus has a gas introduction means for introducing gas into the processing chamber and an exhaust means for exhausting the gas in the processing chamber, as in the batch type low pressure CVD apparatus.

  A chamber of a single wafer type low pressure CVD apparatus has a jig charged with a plurality of substrates. A plurality of substrates placed on the jig are carried one by one into a processing chamber in the chamber. A spare chamber may be provided between the jig and the chamber. The preliminary chamber and the processing chamber are adjacent to each other through a partition that can be opened and closed. When there is a spare chamber, first, the substrates are loaded one by one into the spare chamber, and further, the substrates are loaded into the processing chamber. When the substrate is loaded into the reserve chamber, the reserve chamber is set to a pressure lower than the atmospheric pressure, and then the substrate in the reserve chamber is loaded into the processing chamber whose pressure is reduced.

  Hereinafter, a method for producing a carbon nanotube of the present invention will be described with reference to the drawings.

1. Production of CNTs by vapor phase growth using a batch type horizontal low pressure CVD apparatus FIG. 1 shows a batch type low pressure CVD apparatus in which a quartz tube 1-1 constituting a chamber 1 is placed horizontally. (The axis of the quartz tube 1-1 of the chamber is horizontal). A plurality of substrates 6 are arranged in the processing chamber 1-2 inside the quartz tube 1-1. A heater 2 is disposed around the chamber 1.

  The chamber 1 is connected with gas introduction means 3 for introducing gas into the processing chamber 1-2. The gas introduction means 3 communicates with a gas introduction port 3-1 which is a connection port with the chamber 1 and the gas introduction port 3-1, 1) a source gas (ethanol in the figure) supply source 3-2, 2) reduction A gas source (3-3), and 3) an inert gas (nitrogen gas) source 3-4, 4) a carrier gas source 3-5. The carrier gas is a gas introduced into the processing chamber 1-2 together with the raw material gas. In the gas flow path of the gas introduction means 3, mass flow controllers MFC1 to MFC1, filters F, a gas flow meter MFM, a pressure reducing valve R, a gas sensor G, and the like are provided as appropriate.

  The chamber 1 is connected to an exhaust means 4 for exhausting the gas in the processing chamber 1-2. The exhaust unit 4 includes an exhaust port 4-1 that is a connection port with the chamber 1, a main valve M, an Auto Pressure Controller (APC), a turbo molecular pump TMP, and a diffusion pump DP.

  The chamber 1 is provided with substrate loading / unloading means 5 for loading the substrate 6 into the processing chamber 1-2 and unloading the substrate 6 in the processing chamber 1-2. The substrate loading / unloading means 5 loads the substrate loading / unloading port 5-1 which is the loading / unloading port to the chamber 1, the boat (jig) 5-2 for charging a plurality of substrates 6, and the boat 5-2 into the processing chamber 1-2. Or a fork 5-3 for carrying out from the processing chamber 1-2. That is, only the boat 5-2 charged with the substrate 6 is disposed in the processing chamber 1-2, and processing of the substrate 6 (formation of CNT, etc.) is performed.

  FIG. 4 is a graph showing the relationship between the carbon nanotube manufacturing process using the low-pressure CVD apparatus shown in FIG. 1 and the substrate temperature. First, the boat 5-2 that charges the substrate 6 is loaded into the processing chamber 1-2, and the atmospheric pressure inside the processing chamber 1-2 into which the substrate 6 is loaded is lowered (step 1). In step 1, it is sufficient that the temperature of the substrate is not higher than the temperature at which the catalyst is not easily oxidized (about 500 ° C. or lower), and is not necessarily room temperature. The pressure in the processing chamber after the pressure reduction is preferably in the range of 0.1 Torr to 0.6 Torr.

  When the atmospheric pressure inside the processing chamber 1-2 decreases to a predetermined value, the heater 2 disposed around the chamber 1 is heated to raise the temperature of the substrate 6 to the carbon nanotube generation temperature (step 2). The carbon nanotube generation temperature is, for example, 700 ° C. to 900 ° C. In step 2, reducing gas (such as hydrogen gas) and inert gas (such as nitrogen gas) are introduced into the processing chamber 1-2 while heating the substrate 6.

  When the temperature of the substrate 6 in the processing chamber 1-2 rises to the carbon nanotube generation temperature, a raw material gas (such as ethanol) is introduced into the processing chamber 1-2 (step 3). The temperature of the substrate 6 is preferably maintained at 700 ° C. to 900 ° C., and the atmospheric pressure inside the processing chamber 1-2 is preferably maintained at 0.1 to 0.6 Torr. The time of step 3 may be longer than the time required for the carbon nanotubes to grow on the substrate, but is usually about 1 hour.

  When carbon nanotubes grow on the substrate 6, the temperature of the substrate 6 is lowered (step 4). The temperature after the substrate 6 is lowered may be equal to or lower than the temperature at which the formed carbon nanotubes are not oxidized by oxygen in the air. The temperature after the lowering may be about 600 ° C. or less, and it is not always necessary to lower the temperature to about room temperature. In addition, after the substrate on which the carbon nanotubes are formed is unloaded, when another substrate is loaded and the carbon nanotube is repeatedly manufactured, if the temperature of the substrate is lowered to about room temperature, the temperature of the other substrate is reduced to carbon. A large amount of heat is required and time is required to raise the nanotube formation temperature. Therefore, the temperature of the substrate after the lowering is preferably about 600 ° C. or less and more than room temperature.

  After the temperature of the substrate is lowered, an inert gas is introduced into the processing chamber 1-2 so that the atmospheric pressure is the same as the atmospheric pressure. Thereafter, the boat 5-2 that charges the substrate 6 on which the carbon nanotubes are formed is unloaded from the processing chamber 1-2 (step 5).

2. Production of CNTs by vapor phase growth method using a batch type vertical low-pressure CVD apparatus FIG. 2 shows a batch type low-pressure CVD apparatus in which a quartz tube 1-1 constituting a chamber 1 is placed vertically. Is shown (the axis of the quartz tube 1-1 of the chamber is vertical). Similar to the batch type low-pressure CVD apparatus shown in FIG.

  As shown in FIG. 2, the substrate 6 is carried into the processing chamber 1-2 with the plane thereof being horizontal, but otherwise, the carbon nanotubes are made in the same manner as in the method using the apparatus shown in FIG. 1. Can be manufactured.

3. Production of CNTs by vapor phase growth method using single-wafer type low-pressure CVD apparatus FIG. 3 shows a single-wafer type low-pressure CVD apparatus. The single-wafer type low-pressure CVD apparatus has a chamber 1 having a processing chamber 1-2 for performing processing on the substrate 6 as in the batch-type low-pressure CVD (FIG. 1 or FIG. 2), but is adjacent to the chamber 1. A spare chamber 7 is further provided. In addition, an exhaust unit 4 for exhausting the gas inside the processing chamber 1-2 and an exhaust unit 4 ′ for exhausting the gas inside the preliminary chamber 7 are provided. The inside of the processing chamber 1-2 and the inside of the auxiliary chamber 7 are separated by a partition 8 that can be opened and closed, and the pressure inside each can be controlled independently. A heater 2 for heating the substrate 6 is disposed inside the processing chamber 1-2.

  A gas introducing means 3 for supplying gas to the processing chamber 1-2 is connected to the chamber 1 of the single-wafer type low-pressure CVD apparatus. The configuration of the gas introduction means 3 may be the same as that of the gas introduction means 3 of the batch type low pressure CVD described above.

  The single-wafer type low-pressure CVD apparatus has a substrate carry-in / out means 5, and the substrate carry-in / out means 5 carries a jig 5-1 for charging a plurality of substrates 6 and the substrates 6 one by one into a spare chamber. Means, means for moving the substrate carried into the preliminary chamber to the processing chamber, and means for carrying out the substrate carried into the processing chamber (each means is not shown).

  First, one piece of the substrate 6 fixed to the jig 5-1 is carried into the spare chamber 7, and the air pressure inside the spare chamber 7 is lowered by the exhaust means (pump) 4 '. On the other hand, the pressure inside the processing chamber 1-2 of the chamber 1 is also reduced by the exhaust means (pump) 4.

  The partition 8 between the inside of the processing chamber 1-2 and the inside of the preliminary chamber 7 is opened, and the substrate 6 in the preliminary chamber 7 is moved to the processing chamber 1-2. The temperature of the substrate 6 moved to the processing chamber 1-2 is raised to the carbon nanotube generation temperature (about 700 to 900 ° C.) by the heater 2. At this time, the reducing gas and the inert gas are introduced into the processing chamber 1-2 by the gas introduction means 3. After raising the temperature of the substrate 6 in the processing chamber 1-2, the carbon nanotube raw material gas is introduced into the processing chamber 1-2 by the gas introducing means 3 to grow the carbon nanotubes on the substrate 6. After the growth of the carbon nanotubes, the temperature of the substrate 6 is lowered to a temperature at which the carbon nanotubes are not oxidized by oxygen in the air. The substrate 6 whose temperature has dropped is unloaded from the processing chamber 1-2.

  On the other hand, while one substrate is being processed in the processing chamber 1-2, another substrate 6 is loaded into the spare chamber 7, and the pressure inside the spare chamber 7 is lowered. When the substrate 6 in the processing chamber 1-2 is unloaded, the substrate 6 that has been loaded into the preliminary chamber 7 moves to the processing chamber 1-2, and the same process is repeated.

  The present invention enables mass production of high quality single wall carbon nanotubes. Thereby, industrial production of carbon nanotube devices, such as carbon nanotube FETs, is realized.

It is a schematic diagram of a batch type horizontal low-pressure CVD apparatus for carrying out the manufacturing method of the present invention. It is a schematic diagram of a batch type vertical low-pressure CVD apparatus for carrying out the production method of the present invention. It is a schematic diagram of a single wafer type low-pressure CVD apparatus for carrying out the manufacturing method of the present invention. It is a graph which shows the relationship between the process of the manufacturing method of this invention, and substrate temperature.

Claims (17)

A tubular chamber having a processing chamber for processing the substrate, a gas introduction means for introducing a gas for processing the substrate into the processing chamber, and an exhaust means for exhausting the gas in the processing chamber; A chemical loading / unloading means for loading / unloading a jig charged with a plurality of substrates to / from the processing chamber, and a heater provided around the chamber for adjusting the temperature of the substrate in the processing chamber. Using phase growth equipment
A method of producing carbon nanotubes on the plurality of substrates,
1) preparing a plurality of substrates on which a catalyst for vapor deposition of carbon nanotubes is disposed on the plane of a substrate having a plane;
2) charging the jig with the plurality of substrates spaced apart from each other, and carrying the jig into a processing chamber set so that the temperature of the substrate is 500 ° C. or lower ;
3) exhausting the gas in the processing chamber through the exhaust means to bring the processing chamber to a pressure lower than atmospheric pressure;
4) introducing a reducing gas and an inert gas into the processing chamber and raising the temperature of the substrate to 700 ° C. or more and 900 ° C. or less with the heater;
5) introducing a raw material gas for producing carbon nanotubes into the processing chamber to produce carbon nanotubes on the plane of the substrate;
6) lowering the temperature of the substrate after the carbon nanotubes are generated to a temperature at which the carbon nanotubes are not oxidized by oxygen in the air;
7) setting the pressure in the processing chamber to atmospheric pressure ;
8) from the processing chamber, the step of unloading the jig was charged with the plurality of substrates, and
9) Among the plurality of substrates prepared in the step 1), a substrate different from the substrate carried out from the processing chamber in the step 8) is used, and the steps 2) to 8) are performed. Repeatedly generating carbon nanotubes on the plane of the substrate;
The manufacturing method of a carbon nanotube containing this.   The manufacturing method according to claim 1, wherein the substrate is a substantially circular semiconductor substrate having an orientation flat or a notch.   The manufacturing method according to claim 1, wherein the temperature at which the carbon nanotubes are not oxidized by oxygen in the air is 600 ° C. or less.   The manufacturing method according to claim 1, wherein the atmospheric pressure lower than the atmospheric pressure in the step 3) is between 0.1 Torr and 0.6 Torr.   The manufacturing method according to claim 1, wherein the source gas is a vaporized substance that is liquid at room temperature.   The manufacturing method according to claim 1, wherein the source gas is ethanol. A tubular chamber having a processing chamber for processing the substrate, a gas introduction means for introducing a gas for processing the substrate into the processing chamber, and an exhaust means for exhausting the gas in the processing chamber; A chemical loading / unloading means for loading / unloading a jig charged with a plurality of substrates to / from the processing chamber, and a heater provided around the chamber for adjusting the temperature of the substrate in the processing chamber. Using phase growth equipment
A method of producing carbon nanotubes on the plurality of substrates,
1) A substantially circular substrate having an orientation flat or notch, and having a plurality of regions partitioned in a lattice pattern on the plane, each of the plurality of regions for vapor phase growth of carbon nanotubes Providing a plurality of substrates on which a catalyst is disposed;
2) Charge the jig with the plurality of substrates spaced apart from each other and with the planes parallel to each other, and carry the jig into a processing chamber set so that the temperature of the substrate is 500 ° C. or less. Step to do,
3) exhausting the gas in the processing chamber through the exhaust means to bring the processing chamber to a pressure lower than atmospheric pressure;
4) introducing a reducing gas and an inert gas into the processing chamber and raising the temperature of the substrate to 700 ° C. or more and 900 ° C. or less with the heater;
5) introducing a raw material gas for producing carbon nanotubes into the processing chamber to produce carbon nanotubes on the plane of the substrate;
6) lowering the temperature of the substrate after the carbon nanotubes are generated to a temperature at which the carbon nanotubes are not oxidized by oxygen in the air;
7) setting the pressure in the processing chamber to atmospheric pressure ;
8) from the processing chamber, the step of unloading the jig was charged with the plurality of substrates, and
9) Among the plurality of substrates prepared in the step 1), a substrate different from the substrate carried out from the processing chamber in the step 8) is used, and the steps 2) to 8) are performed. Repeatedly generating carbon nanotubes on the plane of the substrate;
The manufacturing method of a carbon nanotube containing this. The manufacturing method according to claim 7 , wherein the substrate is a semiconductor substrate. The manufacturing method according to claim 7 , wherein the temperature at which the carbon nanotubes are not oxidized by oxygen in the air is 600 ° C. or less. The manufacturing method according to claim 7 , wherein the atmospheric pressure lower than the atmospheric pressure in the step 3) is between 0.1 Torr and 0.6 Torr. The manufacturing method according to claim 7 , wherein the source gas is a vaporized substance that is liquid at room temperature. The manufacturing method according to claim 7 , wherein the source gas is ethanol. A chamber having a processing chamber for performing a process on a substrate, and the preliminary chamber adjacent to the chamber, a gas introducing means for introducing into the processing chamber gas for performing processing on the substrate, wherein the preliminary chamber and the Arranged in the processing chamber for exhausting the gas in the processing chamber, substrate loading / unloading means for loading and unloading a plurality of substrates charged in the jig one by one into the spare chamber, and adjusting the temperature of the substrate And using a chemical vapor deposition apparatus having a heater,
A method of producing carbon nanotubes on the substrate,
1) A substantially circular substrate having an orientation flat or notch, and having a plurality of regions partitioned in a lattice pattern on the plane, each of the plurality of regions for vapor phase growth of carbon nanotubes Providing a plurality of substrates on which a catalyst is disposed;
2) carrying one of the substrates into a spare chamber;
3 ) exhausting the gas in the preliminary chamber and the processing chamber through the exhaust means to bring the preliminary chamber and the processing chamber to an atmospheric pressure lower than the atmospheric pressure;
4 ) carrying the substrate in the preliminary chamber into a processing chamber set so that the temperature of the substrate is 500 ° C. or lower ;
5 ) increasing the temperature of the substrate carried into the processing chamber to 700 ° C. or higher and 900 ° C. or lower ;
6 ) introducing a raw material gas for producing carbon nanotubes into the processing chamber to produce carbon nanotubes on the plane of the substrate;
7 ) After generating the carbon nanotubes, lowering the temperature of the substrate to a temperature at which the carbon nanotubes are not oxidized by oxygen in the air ;
8 ) unloading the substrate from the processing chamber; and
9) Among the plurality of substrates prepared in the step 1), a substrate different from the substrate carried out from the processing chamber in the step 8) is used, and the steps 2) to 8) are performed. Repeatedly producing carbon nanotubes on the plane of the substrate,
The manufacturing method of a carbon nanotube containing this. The manufacturing method according to claim 13 , wherein the substrate is a semiconductor substrate. The manufacturing method according to claim 13 , wherein the atmospheric pressure lower than the atmospheric pressure in the step 3) is between 0.1 Torr and 0.6 Torr. The manufacturing method according to claim 13 , wherein the source gas is a vaporized substance that is liquid at room temperature. The manufacturing method according to claim 13 , wherein the source gas is ethanol.

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