JP2948791B2 - How to change the liquid storage container - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid storage container for storing a liquid used in a semiconductor manufacturing process, that is, a so-called ampule.

[0002]

2. Description of the Related Art For example, when a TiN film or a Ti film is formed by a CVD process, TDMAT (Tetrak) is used as a Ti source.
is Dimethylamino Titanium) is generally used. Since TDMAT is a liquid at room temperature, it is necessary to heat it to a predetermined temperature and supply saturated vapor obtained by bubbling it to the CVD chamber as a material gas. For this purpose, the ampule storing the TDMAT is provided with a heating device.

A conventional ampule is composed of a stainless steel cylindrical container body and an electric resistance type silicon rubber heater wound on the outer peripheral surface thereof, and the internal liquid is heated by heat from the silicon rubber heater. Is heated and bubbled to obtain saturated steam.

[0004]

However, in the conventional ampoule as described above, the silicon rubber heater is simply wound around the outer peripheral surface of the container main body with a metal band or the like. An air film is formed between the two. Further, silicon rubber is used as a material of the heater, but this material has low thermal conductivity and poor heat resistance. Therefore, in the conventional ampoule,
The heat transfer was poor and the liquid could not be heated rapidly. In addition, since heat is not sufficiently transmitted, convection of the liquid is small, and it takes a long time for the temperature distribution of the liquid to be uniform. Further, the conventional ampule has not been provided with a means for lowering the temperature of the liquid inside.

For this reason, the time required for the actual ampule replacement work has been considerably long. That is, when replacing the ampoule, first, the temperature of the ampoule itself and the liquid such as TDMAT remaining in the used ampule is returned to room temperature by cooling in the air, which requires about 3 hours. After replacing the ampoule with a new ampoule filled with sufficient liquid, it took about 3 hours to raise the liquid temperature in the ampoule from room temperature to the supply temperature, for example, 50 ° C.

Accordingly, it is an object of the present invention to provide a method for replacing an ampoule or a liquid storage container in a short time.

[0007]

To achieve the above object, the present invention provides a liquid storage container for heating a stored liquid to a predetermined temperature to supply saturated vapor of the liquid to a predetermined supply destination. A method of replacing a used liquid container with a new liquid storage container comprising a container main body for storing the liquid and an enclosure arranged to form an annular space around the container main body. A first step of flowing the cooling water through the annular space in the used liquid storage container to lower the temperature of the liquid remaining inside the container body; and, if the temperature of the liquid remaining in the container body has dropped. For example, a second step of replacing a used liquid storage container with a new liquid storage container, and a third step of flowing hot water through an annular space in the new liquid storage container to heat the liquid in the container body to a predetermined temperature It is characterized in exchange method comprising.

In this method, when heating the liquid,
Hot water flows into the annular space between the enclosure and the container body, and cooling water flows when cooling. Since the warm water or the cooling water is in direct contact with the outer peripheral surface of the container body, heat transfer is efficiently performed, and the time required for adjusting the liquid temperature, which has conventionally taken a long time, can be reduced.

[0009]

1 shows an ampoule (liquid storage container) 10 suitable for carrying out the replacement method according to the invention. Hereinafter, this ampoule 10 is a TDM used for forming a TiN film or a Ti film in a CVD process.
Although the description will be made assuming that the AT 12 is stored, the stored liquid is not limited to this, and the supply destination of the saturated vapor is not limited to the CVD chamber.

As shown, the ampoule 10 has a TDM
It has a double structure including a cylindrical container body 14 in which the AT 12 is stored, and a cylindrical enclosure 16 disposed coaxially outside the main body. The container body 14 and the enclosure 16 are
It is preferable to be manufactured from a material such as stainless steel that has good thermal conductivity, high strength, and is chemically stable.

An annular space 18 is formed between the container body 14 and the enclosure 16, and the enclosure 16 has an inlet port 20 and an outlet port 22 for flowing cooling water or hot water through the annular space 18. Is provided.

Further, the two conduits 24 and 26 are connected to the container body 1.
4 extends through the upper plate 28 into the container body 14. One end of the conduit 24 extends to near the bottom plate 30 of the container body 14. The other conduit 26 terminates near the top plate 28. The conduit 24 is connected to a supply source (not shown) of a helium gas as a carrier gas,
Conduit 26 is connected to a gas distribution plate (not shown) in the CVD chamber.

In such a configuration, when the temperature of the TDMAT 12 contained in the container body 14 is raised from room temperature to about 50 ° C., 50 ° C. hot water is introduced from the inlet port 20. The hot water flows through the annular space 18 between the container body 14 and the surrounding body 16, but has a very high heat transfer coefficient because it contacts the outer peripheral surface of the container body 14 without any gap. Therefore, the internal T
The DMAT 12 is rapidly heated to the target temperature.

The hot water supplied into the annular space 18 is TD
After performing heat exchange with the MAT 12, the heat is finally discharged from the outlet port 22.

The temperature of the TDMAT 12 can be estimated by measuring the temperature of the hot water discharged from the outlet port 22. That is, when the temperature of the hot water at the outlet port 22 is stabilized at about 50 ° C., the hot water and the TDMAT
12 is completed, and TDMAT 12
It can be determined that the temperature has reached 0 ° C. Of course, TDMA
In order to directly measure the temperature of T12, a temperature sensor such as a thermocouple may be arranged on the lower surface of the bottom plate 30 of the container body 14.

Helium gas is supplied through conduit 24 while the hot water is flowing. The TDMAT 12 is agitated by bubbling helium gas from the conduit 24, thereby quickly uniformizing the temperature distribution of the TDMAT 12.

When the temperature of the TDMAT 12 reaches 50 ° C., when the valve 32 of the conduit 26 is opened, the saturated vapor of the TDMAT 12 at 50 ° C. is sent to the CVD chamber using helium gas as a carrier gas. In addition, CVD
During the execution of the process, the supply of hot water and helium gas is continued.

On the other hand, when the remaining amount of the TDMAT 12 in the ampoule 10 becomes equal to or less than a predetermined value, it is necessary to lower the temperature of the TDMAT 12 in the ampoule 10 to room temperature in order to replace the ampoule 10. In this case, the inlet port 22
Cooling water below room temperature may be supplied. In the same manner as described above, since the cooling water contacts the outer peripheral surface of the container body 14 without any gap, the heat of the TDMAT 12 is efficiently transmitted to the cooling water,
The TDMAT 12 cools down quickly.

As described above, since the heating and cooling of the TDMAT 12 are performed at a high speed, the time required to replace the ampoule 10 is 6 hours or more in the conventional method.
With an ampoule 10 of the same capacity, it can be reduced to about one hour.

Although the preferred embodiments of the present invention have been described in detail, it goes without saying that the present invention is not limited to the above embodiments. For example, fins or coolant paths may be provided on the outer peripheral surface of the container body 14 to promote heat transfer. Further, the bubbling gas is not limited to the helium gas.

[0021]

As described above, according to the method of the present invention, the temperature of the stored liquid can be quickly adjusted and the temperature distribution can be made uniform. Therefore, as described above, the replacement time of the liquid storage container can be shortened, and the start-up time of the entire equipment to which the liquid storage container is connected is shortened, and the working efficiency is improved.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view schematically showing one embodiment of a liquid storage container to which the method according to the present invention can be applied.

[Explanation of symbols]

10: ampoule (liquid storage container), 12: TDMAT
(Liquid), 14: Container body, 16: Enclosure, 18: Annular space, 20: Inlet port, 22: Exit port, 24: Bubbling gas conduit, 26: Conduit, 28: Upper plate, 30
... bottom plate, 32 ... valve.

────────────────────────────────────────────────── (5) References JP-A-9-315900 (JP, A) JP-A-9-186147 (JP, A) JP-A-10-85581 (JP, A) (58) Field (Int.Cl. ⁶ , DB name) H01L 21/205 H01L 21/28-21/288 H01L 21/31 H01L 21/365 H01L 21/44-21/445 H01L 21/469 H01L 21/86 C23C 16 / 00-16/56

Claims (2)

(57) [Claims] 1. A liquid storage container for heating a stored liquid to a predetermined temperature and supplying a saturated vapor of the liquid to a predetermined supply destination, a container main body for storing the liquid, and a container main body for storing the liquid. A method of replacing a used liquid storage container with a new one comprising a surrounding body arranged to form an annular space around the cooling container, wherein the cooling water flows through the annular space in the used liquid storage container. A first step of lowering the temperature of the liquid remaining inside the container body, and when the temperature of the liquid remaining in the container body has dropped, the used liquid storage container is replaced with a new liquid storage container. A second step of exchanging; and a third step of circulating hot water in the annular space of the new liquid storage container to heat the liquid in the container body to a predetermined temperature. 2. The liquid storage container according to claim 1, wherein the bubbling gas is introduced into the container body to agitate the liquid while the liquid in the container body is being heated in the third step. method of exchange.