JP2719282B2 - Knudsen cell for low temperature - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an improvement of a Knudsen cell used in a molecular beam epitaxy apparatus. This may be a molecular beam cell or simply a K cell. The name of the inventor is sometimes called Knudsen. In any case, put the ingredients in a crucible and
The material is heated by a heater to evaporate or sublimate the material into a molecular beam.

[0002] Since a molecular beam epitaxy apparatus heats a material in an ultra-high vacuum, what is evaporated or sublimated becomes a molecular beam. Materials for molecular beam epitaxy are various such as metals and nonmetals. Here, low temperature means that a substance having a high vapor pressure even at a low temperature, such as an organic material, sulfur S, selenium Se, or chlorine Cl, is targeted.

[0003]

2. Description of the Related Art FIG. 2 shows a sectional view of a Knudsen cell according to a conventional example. This is not for low temperatures but for materials with relatively low vapor pressure, such as metals. There is currently no suitable Knudsen cell for low temperature, low vapor pressure materials. The cell shown here is provided in a part of a molecular beam epitaxy apparatus.

[0004] A crucible 1 containing a material and a heater 2 for heating the material are provided.
Are provided in the holes. All of them are inside the vacuum chamber 3. Since a Knudsen cell is required for each material, a plurality of such Knudsen cells are provided inside the vacuum chamber.

The Knudsen cell includes a crucible 1 and a heater 2 as well as a reflector 11 for shielding heat from the heater, and a support 12 for supporting the reflector 11, the crucible 1 and the heater 2.
Having. The column 12 is attached to an ultra-high vacuum flange 13 fixed to an opening of the vacuum chamber 3. The heater power line 14 for supplying the heater power, the terminals of the thermocouple, and the like are taken out through the ultrahigh vacuum flange. Crucible 1
For example, PBN is used. As the heater, a W or Ta coil or ribbon is used. Hee
The temperature of the heater is monitored by a thermocouple. The reflector is formed by stacking a number of thin Ta plates. The radiant heat is confined in the vicinity of the crucible without being released to the outside.
In addition, a shutter (not shown) is provided to open and close the opening of the crucible.

[0006] In addition to the above, a manipulator (not shown) is provided inside the vacuum chamber 3 and supports a substrate fixed to a holder. The manipulator has a heater for heating the substrate and often has a rotating mechanism. This is because epitaxial growth often does not occur unless the substrate is heated. The reason for rotating the substrate is to cause the epitaxial growth to occur uniformly on the substrate. Further, a transport mechanism (not shown) is provided so that the sample holder can be automatically transported to a sample preparation room, an analysis room, or the like in the preceding stage.

[0007] Such a molecular beam epitaxy apparatus is already well known. After filling the Knudsen cell with the material, the vacuum chamber is closed and a vacuum is drawn. The baking removes the gas on the inner wall and the inner structure of the chamber, and further evacuates to 10 ^-10.
An ultra-high vacuum of -10 ^-11 Torr is applied. Since the transfer of the substrate is performed through a different vacuum chamber, the ultra-high vacuum is maintained even when the substrate is replaced. When the epitaxial growth is repeated, the material put in the crucible is depleted. At this time, the vacuum in the vacuum chamber 3 must be broken, and the crucible 1 must be filled with the material. Once at atmospheric pressure, gas and impurities adhere to the wall surface, so it is necessary to repeat the operation of baking the whole and drawing a vacuum again. It takes time to make the original ultra-high vacuum. It takes 3 days to 1 week depending on the equipment and conditions.

The opening and closing of a chamber for material supplementation varies depending on the type of epitaxial growth.
Sometimes, once a month, or once a week. It is better not to open and close the chamber as much as possible, since it takes a long time to start the vacuum and causes a decrease in productivity.

In order to solve such a problem, a gas source is used.
Sussel has been proposed. In this method, a gas serving as a material is introduced into a chamber from a gas cylinder placed outside the chamber. Since the material is supplied from the outside, the material is not depleted, and the necessity of breaking the ultrahigh vacuum is reduced. In some cases, the molecular beam cell is moved away from the center of the chamber and the vacuum chamber is not opened, and the material is replenished. (JP-A-63-310792, JP-A-64-79095).

[0010]

In a conventional molecular beam epitaxy apparatus which fills a Knudsen cell inside a chamber with a material, it is necessary to break the vacuum in order to refill the material. It takes time to re-evacuate, which is undesirable. In particular, there is a further problem when using a substance having a high vapor pressure even at a low temperature. During the evacuation, the entire chamber is baked. At this time, a substance having a high vapor pressure is heated, evaporates and sublimates, and its weight is reduced. To avoid this, baking must be performed at a low temperature. This is not impossible, but the increase in vacuum is slow.

A gas source cell which supplies a material from the outside as a gas does not have such a disadvantage. However, materials that are gas at room temperature are limited. Since molecular beam epitaxy is made of a simple substance, a thin film having excellent purity can be grown. There are even fewer materials that are gases by themselves.
Since many of hydrides, chlorides, halides and organometallics are gaseous at around room temperature, materials of these compounds are also used. However, some substances do not always produce gaseous compounds.

Further, since it is a molecular beam of a compound, it is different from a single molecular beam. There is a drawback that impurities are easily contained in the thin film and the composition is difficult to control. The present invention relates to a Knudsen cell for handling a material having a high vapor pressure even at a low temperature. It is an object of the present invention to provide a Knudsen cell. As for the cracker cell, there is, for example, Japanese Utility Model Laid-Open No. 4-29664, but this is a large-scale apparatus, and it is not easy to manufacture and use it.

[0013]

The Knudsen cell of the present invention has an openable and closable reservoir for filling a material outside a vacuum chamber, and the reservoir and the inside of the vacuum chamber are separated from each other. Connected by an inlet pipe, the reservoir has its own heater and vacuum pump. The introduction pipe 5 also has its own heater in the middle and the opening at the end. Reservoir bar
The material is heated by the heater to produce steam, and the steam is introduced into the vacuum chamber through an introduction pipe to form a molecular beam. The reservoir has an evacuation device and can evacuate only the reservoir. A partition valve is provided between the reservoir and the vacuum chamber. When the gate valve is closed, the reservoir and the vacuum chamber are shut off. When the valve is opened, steam is introduced from the reservoir to the vacuum chamber.

[0014]

Since the reservoir is outside the vacuum chamber,
There is no need to open the vacuum chamber when filling the reservoir with material. With the sluice valve closed, the reservoir lid is opened and material is refilled into the reservoir. After this, the reservoir
Is closed and evacuated to a vacuum. When a sufficient degree of vacuum is reached, the gate valve is opened to connect the reservoir to the vacuum chamber. The vapor of the material generated from the reservoir enters the vacuum chamber and becomes a molecular beam. The temperature of these parts can be controlled independently by controlling the reservoir heater, the heater at the intermediate connection part of the introduction pipe, and the heater at the tip opening.

The connecting portion heater can prevent the material vapor from cooling and solidifying inside the introduction pipe 5 and adhering to the inner wall. Since the reservoir is provided outside, there is a possibility that the material vapor solidifies on the way. This is unnecessary in the conventional configuration shown in FIG. The opening heater has a cracking action in which when the vapor of the material is a mass of a large number of molecules and is not molecular, it is ignited to make it small.

Further, since the material is outside the vacuum chamber, when the vacuum chamber is baked, the heat for baking is not transferred to the material, and the material is evaporated and sublimated, so that the weight is not reduced. Particularly, a material having a low temperature and a high vapor pressure is preferable.

[0017]

FIG. 1 shows a schematic structure of a Knudsen cell according to an embodiment of the present invention. The Knudsen cell does not have a crucible-like container inside the vacuum chamber 3. The vacuum chamber 3 is merely inserted with an introduction pipe 5 for introducing the vapor of the material.
The introduction pipe 5 communicates with the outside of the vacuum chamber 3 and is connected to the reservoir 8 at the outside end. External reservoir
The bar 8 is a container that can be opened and closed, and can store materials. A liquid nitrogen shroud 4 is provided inside the vacuum chamber 3.
Is inserted.

An opening heater 6 is provided around the introduction pipe 5. This is at a position corresponding to the heater 2 around the crucible 1 in FIG. 2, but the function is slightly different. Opening heater 6
Is surrounded by a reflector 11. A column 12 erected on the ultra-high vacuum flange 13 supports the opening heater 6, the reflector 11, the power line of the heater, the thermocouple, and the like. The introduction pipe 5 extends through the ultra-high vacuum flange 13 to the outside. A partition valve 7 is provided on the way, and is connected to a reservoir 8 via this.

The reservoir 8 has a lid (not shown) that opens and closes.
Have their own. The lid can be opened to freely refill the material. The reservoir 8 also has its own reservoir heater 9 around the outer wall. This is to heat and evaporate and sublimate the material inside the reservoir 8.

A connecting portion heater 16 is provided at the connecting portion in the middle of the introducing pipe 5. The present invention is directed to a material having a low melting point, but some materials are still solid at room temperature. Some pipes may be cooled and solidified in the middle of the pipe 5. The connecting portion heater 16 is for preventing the material from being cooled here and adhering to the inner wall of the introduction pipe 5. The reservoir heater 9, the opening heater 6, and the connecting heater 16 can operate independently.
Therefore, the reservoir temperature T ₁ and the inlet pipe intermediate temperature T
_2, the opening temperature of the inlet pipe T ₃ can be controlled independently. These temperature parameters can be appropriately determined depending on the difference in materials. Further, the reservoir 8 is connected to a vacuum exhaust device (not shown) via an exhaust pipe 15, and the vacuum exhaust device can exhaust the vacuum independently of the vacuum chamber 3. An evacuation valve 10 is provided in the exhaust pipe 15.

When the partition valve 7 is closed, the evacuation device is operated, and the evacuation valve 10 is opened, only the reservoir 8 can be evacuated. Close the gate valve 7,
The material can be refilled into the reservoir 8 by also closing the evacuation valve 10 and introducing atmospheric pressure to the reservoir 8 and opening the lid. The gate valve 7 can be fully opened or fully closed. At an intermediate opening, the pressure difference before and after cannot be strictly controlled with good reproducibility.

The operation of the above configuration will be described.
It is not necessary to open the vacuum chamber 3 to fill the Knudsen cell with material. The gate valve 7 is closed and the evacuation valve 10 is also closed to guide the atmospheric pressure to break the vacuum state of the reservoir 8. Open the reservoir 8 lid. Fill the reservoir 8 with the required amount of material. During this time, the ultra-high vacuum in the vacuum chamber 3 is still maintained. The lid is closed and the evacuation valve 10 is opened to operate the evacuation device. The inside of the reservoir 8 is evacuated to a high vacuum. Heater for reservoir
The heater 8 is energized and heated. The material of the reservoir 8 is heated to start evaporation or sublimation. Open the gate valve 7. The vapor flows out from the tip of the introduction pipe 5 of the vacuum chamber 3 into the inside of the vacuum chamber 3 as a molecular beam through the introduction pipe 5.

When the melting point of the material is higher than room temperature, the connecting portion heater 16 has a function of cooling and solidifying inside the introduction pipe 5 to prevent the material from adhering to the inner wall. It is unnecessary if it is a gas at normal temperature.

The heater 6 in the chamber has the function of preventing the material from solidifying at the tip of the introduction pipe 5. Further, depending on the material, the reservoir heater 9 alone may not be sufficiently activated to be a mass of many molecules. Immediately before being introduced into the vacuum chamber 3, it can be heated and finely divided by the opening heater 6 to obtain molecules. That is, the cracking action can be performed by the opening heater 6. The opening heater 6 can be used not only for cracking but also for controlling the energy of the molecular beam. Since there is the liquid nitrogen shroud 4 in the vicinity of this, the opening of the leading end of the introduction pipe 5 can be controlled to an arbitrary temperature in parallel with this.

However, it is firstly the reservoir heater 9 that controls the molecular dose. Increasing its temperature will increase the molecular dose, and decreasing its temperature will decrease the molecular dose.
As described above, there is an advantage that the material can be supplemented while the vacuum chamber 3 is maintained at a high vacuum.

Another advantage is more critical. It is necessary to perform baking when the vacuum of the vacuum chamber 3 is started up.
In the dosencell, sufficient baking cannot be performed because the material is lost by baking. However, in the case of the present invention, the gate valve 7 is closed, the reservoir 8 and the vacuum chamber 3 are shut off, and then the vacuum chamber 3 is closed.
Baking can be performed. No baking heat is applied to the reservoir 8. Therefore, the baking temperature can be freely increased, and the purpose of baking can be achieved well.

A very advantageous Knudsen cell can be provided for materials having a high vapor pressure at low temperatures. For example, the present invention can be applied to S, Se, organic materials, and the like belonging to VI.

The leading end of the introduction pipe may be a simple opening as described above. However, if there is too much difference between the degree of vacuum inside the vacuum chamber and the degree of vacuum of the reservoir 8, a narrow neck or a perforated plate for increasing the flow path resistance is installed at the tip of the introduction pipe to maintain the pressure difference. You may be able to.

[0029]

According to the present invention, a reservoir for accommodating a material and converting it into vapor is provided outside the vacuum chamber, and both are connected by an introduction pipe, and the vapor generated by the reservoir is introduced into the vacuum chamber. I can guide you. A partition valve is provided in the middle of the introduction pipe so that the gas flow can be shut off. Further, a connecting portion heater 16 is provided at an intermediate portion of the introduction pipe 5 so as to prevent the vapor of the material from condensing on the inner wall surface.

When filling the reservoir with the material, the gate valve 7 can be closed and the lid can be opened to replenish the material. It has no effect on the ultra-high vacuum of the vacuum chamber. Once the vacuum chamber is brought to atmospheric pressure, it takes a long time and trouble of three days to one week to start up the next time, but the present invention can save such time and labor. The epitaxial growth can be performed continuously, and the productivity of molecular beam epitaxy can be enhanced.

When the vacuum chamber is opened to exchange the material, harmful substances may be scattered in the air and deteriorate the working environment. However, the present invention can avoid such dangers and improve working hygiene. Also excellent in point.

Furthermore, during baking of the vacuum chamber, since the reservoir is cut off from the vacuum chamber, the heat of the baking is not transferred to the material in the reservoir and does not evaporate. Do not lose weight. There is an advantage that baking can be performed freely, and loss of a material having a high vapor pressure at a low temperature can be prevented.

[Brief description of the drawings]

FIG. 1 is a schematic sectional view of a Knudsen cell according to an embodiment of the present invention.

FIG. 2 is a schematic cross-sectional view of a Knudsen cell according to a conventional example.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Crucible 2 Heater 3 Vacuum chamber 4 Liquid nitrogen shroud 5 Introducing pipe 6 Heater 7 Partition valve 8 Reservoir 9 Heater for reservoir 10 Vacuum evacuation valve 11 Reflector 12 Column 13 Ultra-high vacuum flange 14 Heater power line 15 Exhaust pipe 16 Connector heater

 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Shigeharu Ohashi 47-inch, Umezu Takaune-cho, Ukyo-ku, Kyoto-shi, Nichishin Electric Co., Ltd. (56) References JP-A-60-226493 (JP, A) JP-A-64 −56397 (JP, A) Real opening 4-29664 (JP, U)

Claims (1)

(57) [Claims] 1. A Knudsen cell of a molecular beam epitaxy apparatus in which a vacuum chamber is placed in an ultra-high vacuum and a material is heated and vaporized to irradiate a substrate in the ultra-high vacuum as a molecular beam to epitaxially grow on the substrate. A reservoir provided outside the vacuum chamber and having a lid that can be opened and closed, and capable of containing a material, a reservoir heater for heating the material of the reservoir, and a reservoir; Pipe that connects the vacuum chamber and the vacuum chamber to introduce a molecular beam into the vacuum chamber; an opening heater provided near the outlet of the pipe in the vacuum chamber; and a heater provided in the middle of the introduction pipe. A low-temperature knuckle having a partition valve, a connecting portion heater provided for heating an intermediate portion of the introduction pipe, and a vacuum exhaust device for evacuating the reservoir. Dosencell.