JP3296611B2 - Liquid material vaporizer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates, for example a gas such as silicon tetrachloride (SiCl ₄₎ is used in semiconductor manufacturing,
The present invention relates to a liquid material vaporizing supply device that supplies a liquid material by vaporizing the liquid material.

[0002]

2. Description of the Related Art As shown in FIG. 3, there is known a liquid material vaporizing and supplying apparatus in which a liquid material whose flow rate is controlled is introduced into a vaporizer provided with a heater and the entire amount is directly vaporized. ing. In FIG. 3, reference numeral 41 denotes a vaporizer provided with a heater inside, and a liquid material L provided with a liquid flow controller 42 and a stop valve 43 on the upstream side thereof.
The supply path 44 of S and the supply path 46 of the carrier gas CG provided with the mass flow controller 45 are connected in parallel with each other, and on the downstream side, the vaporized gas G generated in the vaporizer 41 is provided with the carrier gas. A heating pipe 47 flowing together with the CG is connected.

The construction of the vaporizer 41 is roughly as shown in FIG. That is, in this figure, reference numeral 48 denotes a housing having a heat insulating structure, in which a heater block 4 is provided.
9 and a carrier gas introduction pipe 50 are provided. The heater block 49 is made of a material having good heat conductivity, and a pipe 51 made of a material having good heat conductivity and corrosion resistance is inserted therein, and a heater 52 for heating the pipe 51 is provided. Built-in. Then, in the portion of the pipe 51 inside the heater block 49, powder 53 having good thermal conductivity and corrosion resistance is meshed with the mesh bodies 54 and 55.
It is filled so as to be sealed.

[0004] At the inlet side on the upstream side of the pipe 51, an inlet pipe 5 for the liquid material LS having a small diameter portion 56 at the tip end.
7 is inserted concentrically with the pipe 51, and the upstream side thereof is connected to the liquid material supply path 44. The carrier gas introduction pipe 50 is made of a material having good thermal conductivity, the upstream side of which is connected to the carrier gas supply passage 46, and the downstream side of which has thermal conductivity and corrosion resistance. Is connected to the upstream side of the pipe 51 via a block-shaped pipe joint 58 made of a good metal. Reference numeral 59 denotes an outlet for a mixed gas of the vaporized gas G and the carrier gas CG provided at the downstream end of the pipe 51, and the heating pipe 47 is connected downstream thereof.

The vaporizer 41 having the structure shown in FIG. 4 has been filed by the applicant of the present invention as Japanese Patent Application No. 2-151270 (Japanese Patent Application Laid-Open No. 4-45838). The vaporizer 41 has an excellent advantage that the pressure fluctuation due to the vaporization of the liquid supplied at a constant flow rate is extremely small, and the liquid material can be vaporized stably and supplied stably.

[0006]

Meanwhile, in an apparatus for directly vaporizing the liquid material LS, such as the above-described liquid material vaporization supply apparatus, a stop valve is provided inside the vaporizer 41 as shown in FIG. Therefore, when the generation of the vaporized gas G is stopped, it must be dealt with by closing the stop valve 43. In such a case, the piping 44 from the stop valve 43 to the vaporizer 41 is required.
The liquid material LS is filled in a.

As described above, the stop valve 4
In a state in which the liquid material LS is filled in the pipe 44a from 3 to the vaporizer 41, the vaporizer 41
A vacuum (vacuum) condition occurs in the line downstream of
In order to cope with this, a problem occurs in that the liquid material LS is gradually vaporized, and the generated vaporized gas G leaks to the downstream side of the vaporizer 41.

[0008] The present invention has been made in mind the above-described matters, and an object, in the liquid material vaporizing supply apparatus of a system for vaporizing the liquid material directly, carburetor parallel
And its surrounding structure are simplified, making it more compact.
In addition to making it possible to obtain a vessel, the inconvenience that occurs when the downstream side of the vaporizer is in a reduced pressure state is eliminated.

[0009]

In order to achieve the above object, a liquid material vaporizing and supplying apparatus according to the present invention vaporizes a liquid material introduced therein by heating, and separates a gas generated by the vaporizing into a gas inside. A flow control valve for adjusting the flow rate of the liquid material introduced into the vaporizer is provided as close as possible to the vaporizer led out by the introduced carrier gas, and the flow control valve is shut off. It has a function and cools it, and a carrier for introducing the carrier gas into one end of a vaporizing chamber of the vaporizer.
A gas introduction section is provided and the carrier gas introduction
The liquid material is introduced into the side of this vaporization chamber downstream of the section.
Liquid material introduction part is provided.

[0010]

In the liquid material vaporizing / supplying apparatus having the above structure,
Since the flow control valve for adjusting the flow rate of the liquid material and the vaporizer are provided as close as possible, accumulation of the liquid material on the upstream side of the vaporizer can be reduced as much as possible. In addition, since the flow control valve has a shut-off (fully closed) function, there is no need to separately provide a shutoff valve or the like, and the configuration is simplified. Since the flow control valve is configured to be cooled, it is possible to prevent the liquid material supplied to the vaporizer from being vaporized before being introduced into the vaporizer. It operates stably without being affected by temperature and can be used for a long time.
In addition, the carrier gas introduced into the vaporization chamber is
Sufficient heat exchange before the material reaches the site to be vaporized
Has been maintained at a predetermined temperature. Therefore, carry
Minimize temperature drop at the vaporization site by introducing Agas
Can be stopped. Also, from the carrier gas introduction section
The liquid that introduces the liquid material to the side of the vaporization chamber also on the downstream side
A material introduction section is provided. That is, as shown in FIGS.
The liquid material introduction pipe 57 is connected to the pipe 5 as in the conventional structure shown in FIG.
Unlike the one inserted concentrically into the
The inlet and the liquid material inlet are downstream of the latter,
A configuration that is provided independently in another part is adopted.

[0011]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a diagram schematically showing an example of a liquid material vaporization supply apparatus according to the present invention. In this figure, reference numeral 1 denotes a vaporizer, and reference numerals 2 and 3 denote a liquid material LS,
These pipes supply the carrier gas CG. The liquid material supply pipe 2 is provided with a flow control valve 4 provided as close as possible to the vaporizer 1 and a fluid flow meter 5 on the upstream side thereof. The flow control valve 4 is provided with a device 6 for cooling it. Further, a mass flow controller 7 is interposed in the carrier gas supply pipe 3.
Reference numeral 8 denotes a controller for controlling the entire liquid material vaporizing / supplying apparatus. The controller 8 controls the flow rate control valve 4 based on the flow rate of the liquid material LS detected by the fluid flow meter 5 and the carrier detected by the meter section of the mass flow controller 7. The control valve of the mass flow controller 7 is controlled based on the flow rate of the gas CG.

FIG. 2 shows a main part of the liquid material vaporizing and supplying apparatus.
In particular, FIG. 3 is a diagram showing the connection relationship between the vaporizer 1 and the flow control valve 4 in detail. The vaporizer 1 is configured as follows.
That is, in FIG. 2, reference numeral 9 denotes a pipe made of a metal having good heat conductivity and corrosion resistance such as stainless steel, for example, and is inserted into a through hole formed in a heater block 10 having good heat conductivity such as aluminum. It is provided as follows. The heater block 10 has a built-in heater 11 for heating the pipe 9 and the heater block 10.

A portion of the pipe 9 inside the heater block 10 has a powder 12 having good thermal conductivity and corrosion resistance.
Is filled in the mesh bodies 13 and 14 which also function as filters so as to be sealed, and is formed in the vaporization chamber 15. As the powder 12, for example, a powder obtained by forming a metal such as stainless steel or titanium or a ceramic such as SiC into a powder having a diameter of 100 μm or more, preferably about 120 μm is used. In addition, the mesh bodies 13, 1
The mesh 4 has a mesh size of, for example, about 20 μm in order to prevent the powder 12 from coming out of the vaporization chamber 15. The length of the vaporization chamber 15 (the length between the mesh bodies 13 and 14 in this example) is, for example, 100 mm, and the inner diameter of the vaporization chamber 15 is about 9.5 mm.

Reference numeral 16 denotes a carrier gas CG introduction portion formed at one end of the vaporization chamber 15, which is made of a metal having good heat conductivity and corrosion resistance (for example, stainless steel). The carrier gas supply pipe 3 is connected. As the carrier gas CG used here,
H ₂ , He, N ₂ and the like. 18 is the vaporization chamber 15
Is formed of a metal having good thermal conductivity and corrosion resistance, such as stainless steel, and a connecting portion 19 is provided with, for example, gas to a semiconductor manufacturing apparatus (not shown). A supply pipe (not shown) is connected.

Reference numeral 20 denotes an introduction portion for introducing the liquid material LS into the vaporization chamber 15, which is located at a downstream side of the carrier gas introduction portion 16 and, in the example shown in FIG. Slightly upstream (approximately 1 /
3). This liquid material introduction part 2
Numeral 0 is a capillary (for example, having an inner diameter of, for example, 0.2 mm) such as a capillary.
A small-diameter portion 21 having an inner diameter (for example, 0.1 mm) smaller than the diameter of the powder 12 is formed on the downstream side. The distal end of the liquid material introduction section 20 is inserted into a portion filled with the powder 12, for example, about 5 mm.

The flow control valve 4 is of a so-called normal open type, and can be shut off as required. That is, in FIG. 2, 22 is a main body block made of a metal having good corrosion resistance, 23 and 24 are a liquid introduction block and a liquid derivation block detachably attached to the main body block 22, and the liquid derivation block 24 is In order to make it difficult for the heat from the vaporization chamber 15 to be transmitted to the main body block 22, it is formed of metal, ceramic, or the like having poor heat conductivity. The liquid material introduction section 20 is inserted through the liquid outlet block 24. Reference numeral 25 denotes a liquid flow path formed in the main body block 22, and a control valve 26 as a flow control unit is provided in the middle thereof.

The control valve 26 is configured as follows. That is, an orifice block 27 has a valve port 28 facing the liquid flow path 25. Reference numeral 29 denotes a valve body for adjusting the opening degree of the valve port 28, and the valve head 30 and the plunger 31
The valve head 30 is provided in a state of being close to the valve port 28. The valve element 29 is connected to the main body block 2.
In a normal state, a metal diaphragm 33 provided in a lower space of a valve block 32 connected in series is held movably up and down such that a slight gap is formed between the orifice block 27 and the normal state. ing. Reference numeral 34 denotes a spring interposed between the diaphragm 33 and a spring receiver 35 fixed to the plunger portion 31.

Reference numeral 36 denotes a piezoelectric actuator which presses and drives the valve element 29 in a predetermined direction, and is housed in a cylindrical valve case 37 screwed to the valve block 32. The lower end of the piezoelectric actuator 36 is in contact with the upper surface of the plunger portion 31 of the valve body 29 via a sphere 38.

A cooling device 6 made of, for example, a Peltier element is provided on the side surface of the main body block 22 opposite to the side on which the piezoelectric actuator 36 protrudes. Reference numeral 39 denotes the support frame.

Next, the operation of the apparatus for vaporizing and supplying a liquid material having the above structure will be described. First, the heater 11 is heated to heat the powder 12 filled in the vaporizing chamber 15 to a predetermined temperature. In this state, the liquid material LS is introduced into the vaporization chamber 15 through the liquid material introduction unit 20 while the carrier gas CG is introduced into the pipe 9 via the carrier gas introduction unit 16.

The liquid material LS introduced through the liquid material introduction section 20 is introduced into the heated powder 12 through the small diameter section 21 and comes into contact with the powder. However, the contact area is large. The liquid material LS is vaporized in a short time to become a desired vaporized gas G. In this case, the liquid material LS flowing in the liquid material introduction portion 20 flows out to the powder 12 side through the small diameter portion 21 having a smaller diameter than the liquid material LS. Even if the pressure rises due to vaporization, the pressure is relieved by the small-diameter portion 21, so that the pressure rise pressure is not rapidly transmitted to the upstream side, so that there is no adverse effect on the line for supplying the liquid material LS. Disappears.

On the other hand, the carrier gas CG introduced from one end side of the vaporization chamber 15 into the interior of the powder material 12, that is, the tip of the liquid material introduction part 20 is inserted into the powder 12. Heat is sufficiently exchanged before reaching the vicinity of the portion to maintain a predetermined temperature. Therefore,
The introduction of the carrier gas CG can minimize the decrease in the temperature of the vaporized portion, so that the vaporization of the liquid material LS is not hindered, so that the vaporized gas G can be generated smoothly.

The vaporized gas G generated as described above is
The carrier gas CG promptly leads to the downstream side,
The vaporized gas G can be supplied to a downstream semiconductor manufacturing apparatus (not shown).

In the liquid material vaporizing / supplying apparatus according to the above embodiment, the flow rate control valve 4 for adjusting the flow rate of the liquid material LS and the vaporizer 1 are provided as close to each other as possible. The dead volume between the valve 4 and the vaporizer 1 is small, and the accumulation of the liquid material on the upstream side of the vaporizer 1 can be minimized. The flow control valve 4 has a shut-off (fully closed) function.

Therefore, for example, when the downstream side of the vaporizer 1 is in a depressurized state and the flow control valve 4 is closed to stop the generation of the vaporized gas G, the falling speed is fast and a conventional apparatus of this type is used. As described above, the problem that the generated vaporized gas G leaks out to the downstream side of the vaporizer 1 does not occur, and there is an advantage that the response in the pressure reduction process is quickly performed.

The flow control valve 4 is connected to the cooling device 6
Therefore, the thermal effect of the vaporizer 1 on the flow control valve 4 is greatly reduced, and the supplied liquid material LS is vaporized before being introduced into the vaporizer 1. In the flow control valve 4, the liquid material LS can be controlled in a liquid state. In addition, since the flow control valve 4 is cooled, the temperature of the vaporizer 1 can be set high, and therefore, the high-boiling liquid material LS can be easily vaporized.

Further, by appropriately selecting the inner diameter of the liquid material introduction section 20, foaming in the vicinity of the valve port 28 of the flow control valve 4 can be effectively suppressed.

Further, in the example shown in FIG. 4, the liquid material introduction pipe 57 is provided concentrically with the pipe 51, so that the structure is complicated. Since it is provided on the side of the vaporization chamber 15, the structure is simple and maintenance and inspection can be easily performed.

The present invention is not limited to the above embodiment. For example, the carrier gas introducing section 16 does not necessarily need to be provided at one end of the vaporizing chamber 15. Further, a plurality of liquid material introduction sections 20 may be provided. In that case, it goes without saying that the liquid material introduction section 20 is provided downstream of the carrier gas introduction section 16. Then, the liquid material introduction unit 20
May be provided on the downstream side of the carrier gas introduction unit 16, but in consideration of the temperature gradient in the vaporization chamber 15 and the like,
It may be provided at a position closer to the carrier gas inlet 16 and, conversely, farther from the carrier gas inlet 16. Further, the cooling device 6
May be water-cooled or air-cooled.

[0030]

As described above, according to the present invention,
The pressure fluctuation due to the vaporization of the liquid is extremely small, and the liquid material can be stably vaporized and supplied stably, so that the line for supplying the liquid material is not adversely affected. The structure around the vessel is simplified,
This type of vaporizer can be made more compact. At the same time, the introduction of the carrier gas
Temperature drop to a minimum
The vaporization of the material is not hindered and the vaporized gas
Can be generated. Also shown in FIGS.
The liquid material introduction pipe 57 has a pipe 51 as in the conventional structure shown in FIG.
Unlike the one inserted concentrically into the carrier gas
Section and the liquid material introduction section with the latter on the downstream side,
The configuration that is provided independently in the part of is adopted
The structure becomes extremely simple, and the structure around the vaporizer
It can be further simplified. As a result, maintenance and inspection work
Easy to do. In addition, production is easy and cost reduction
Can greatly contribute to Eun.

[Brief description of the drawings]

FIG. 1 is a diagram schematically illustrating an example of a liquid material vaporization supply device according to the present invention.

FIG. 2 is a diagram showing a connection relationship between a vaporizer and a flow control valve.

FIG. 3 is a diagram schematically showing a conventional liquid material vaporization supply device.

FIG. 4 is a diagram showing a configuration of a conventional vaporizer.

[Explanation of symbols]

Reference numeral 1 denotes a vaporizer, 4 denotes a flow control valve, 6 denotes a cooling device, LS denotes a liquid material, CG denotes a carrier gas, and G denotes a vaporized gas.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-4-45838 (JP, A) JP-A-63-91128 (JP, A) JP-A-57-165737 (JP, A) JP-A-60-1985 132639 (JP, A) JP-A-54-60224 (JP, A) JP-A 64-42 (JP, U) JP-A 56-59134 (JP, U) (58) Fields investigated (Int. Cl. ⁷ , DB name) G01N 1/22 B01J 4/00 102 B01J 7/02 H01L 21/31

Claims (1)

(57) [Claims] 1. A vaporizer for vaporizing a liquid material introduced therein by heating and introducing a gas generated by the vaporization to the outside by a carrier gas separately introduced into the vaporizer. A flow control valve for adjusting the flow rate of the liquid material is provided as close as possible, and the flow control valve has a shut-off function and cools it, and one end of a vaporization chamber of the vaporizer. Side
A carrier gas introduction section for introducing the rear gas is provided, and a side of the vaporization chamber downstream of the carrier gas introduction section.
A liquid material introduction unit for introducing the liquid material into the unit ;