JP2002105646A - Gasifier - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a gasifier capable of effectively atomizing a liquid material and reducing generation of a non-gasified residual dross and a particle. SOLUTION: An orifice member 212 is arranged at a tip of a double tube constituting of an inside piping 200a where a liquid material flows and an outside piping 200b where a gas for atomization flows, the gas for atomization is jetted from a clearance between the orifice member 212 and the inside piping 200a As a result, atomization of the liquid material is effectively conducted, generation of the non-gasified residual dross and generation of the particle are reduced.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vaporizer for vaporizing a liquid material such as a liquid organic metal or an organic metal solution, which is used for CVD film formation.

[0002]

2. Description of the Related Art MOCVD (Metal Organic Chemic) is one of the methods for forming a thin film in a semiconductor device manufacturing process.
al Vapor Deposition method, which has been widely used in recent years due to its superior film quality, film forming speed, step coverage, etc. as compared with sputtering or the like. As a CVD gas supply method used in the MOCVD apparatus, there is a bubbling method, a sublimation method, or the like, but a method in which a liquid material obtained by dissolving a liquid organic metal or an organic metal in an organic solvent is vaporized and supplied immediately before a CVD reactor, It is attracting attention as a better method in terms of controllability and stability.

[0003]

However, in the conventional vaporizer, when the liquid material is vaporized, an unvaporized residue is apt to be generated, and the vaporizer may be clogged or particles due to the residue may not be deposited. There was a problem in the stability and reproducibility of the film formation due to the influence. In addition, there has been a problem that the vaporization amount cannot be so large, and a margin in the process cannot be obtained.

SUMMARY OF THE INVENTION An object of the present invention is to provide a vaporizer for vaporizing a liquid organic metal, an organic metal solution, or the like, to more effectively atomize the liquid material and reduce the generation of unvaporized residues and particles. It is to provide a vaporizer.

[0005]

An embodiment of the invention will be described with reference to FIGS. 2, 4, 5, and 10. FIG. (1) Explaining in association with FIG. 2, FIG. 4, and FIG.
The first aspect of the present invention is a spraying unit 20 for spraying a gas-liquid mixed material obtained by mixing a liquid material composed of a liquid organic metal or an organic metal solution and a carrier gas from the distal end of the transfer pipe 200.
And a vaporizer 21 for vaporizing the sprayed liquid material, which is applied to the vaporizer 2 that supplies the vaporized liquid material to the CVD film forming apparatus. An inner pipe 200a through which the liquid material is transferred, and an inner pipe 2
00a is inserted through the gap, and the outer pipe 200b transfers the atomizing gas. The outer pipe 200b has a double pipe structure in which the inner pipe 200a is inserted through the gap. The above-described object is achieved by providing an orifice member 212 at the tip end of the inner pipe 200a for ejecting the atomizing gas transferred by the nozzle 200b from the gap to the vaporizer 21. (2) Explaining in connection with FIG. 5, the invention according to claim 2 is the vaporizer according to claim 1, wherein a vaporization surface 211a for preventing the vaporized liquid material from being recondensed is formed. A nozzle ring 211 is provided at the tip of the spray unit 20 in the vicinity of the tip of the pipe 200a, and the orifice member 212 is formed of PEEK (polyether ether ketone) so that the orifice member 212 is formed between the nozzle ring 211 and the tip of the outer pipe 200b. PTFE (polytetrafluid) between the orifice member 212 and the tip of the outer pipe 200b.
The seal member 213 made of oroethylene is provided. (3) Explaining with reference to FIG. 10, the invention according to claim 3 is the vaporizer according to claim 2, wherein the nozzle ring 2
14 is a first member 214a screwed to the tip of the spraying section 20
And a second member 214 formed separately from the first member 214a and sandwiched between the orifice member 212 and the first member 214a.
And a member 214b. (4) The invention according to claim 4 is the vaporizer according to claim 1, wherein a vaporizing surface 215a for preventing the vaporized liquid material from being recondensed is formed, and the inner pipe 200a is formed.
A nozzle ring 215 fixed to the vaporizing section 21 in close proximity to the tip of the orifice member.
nozzle ring 215 formed from lyether ether ketone)
And between the end of the outer pipe 200b and
A seal member 213 made of PTFE (polytetrafluoroethylene) is provided between the orifice member 212 and the tip of the outer pipe 200b. (5) Explaining in association with FIGS. 3 and 5, the invention of claim 5 is a joint for fixing the inner pipe 200 a to the spray section 20 in the vaporizer according to any one of claims 1 to 4. A gasket-type seal joint 22 having a metal gasket 233 and a pair of joint members 220a, 220b provided to sandwich the metal gasket 223, and a pair of joint members 220a, 220b.
Is fixed to the spraying section 20, and the other 220a of the pair of joint members 220a, 220b is fixed to the inner pipe 200a. By adjusting the amount of axial tightening of the gasket-type seal joint, the tip of the inner pipe is adjusted. The amount h of protrusion of the orifice member 212 from the orifice member 212 can be adjusted. (6) Explained in connection with FIG. 2, the invention of claim 6 is to provide a gas-liquid mixed material obtained by mixing a liquid material composed of a liquid organic metal or an organic metal solution and a carrier gas from a distal end portion of a transfer pipe 200. A spraying unit 20 for spraying and a vaporizing unit 21 for vaporizing the sprayed liquid material are applied to the vaporizer 2 for supplying the vaporized liquid material to the CVD film forming apparatus. The material is supplied in a state of an annular spray flow.

In the section of the means for solving the above-mentioned problems, which explains the configuration of the present invention, the drawings of the embodiments of the present invention are used to make the present invention easier to understand. However, the present invention is not limited to the embodiment.

[0007]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to FIGS. FIG. 1 is a diagram showing a schematic configuration of the entire vaporizer. Reference numeral 1 denotes a liquid organic metal, an organic metal solution, or the like (hereinafter, these are referred to as liquid materials).
And a liquid material supply device for supplying the liquid material. The supplied liquid material is vaporized by the vaporizer 2 and provided to the CV provided in the CDV device.
It is supplied to the D reactor. For example, there is an organic metal such as Cu or Ta as a liquid organic metal, and an organic metal solution in which an organic metal such as Ba, Sr, Ti, Pb, or Zr is dissolved in an organic solvent.

The material containers 3A, 3B, 3C provided in the liquid material supply device 1 are filled with liquid materials 4A, 4B, 4C used for MOCVD. For example, BST
When a film (BaSrTi oxide film) is formed, the raw material B
a, Sr, Ti are converted to organic solvent THF (tetrahydrofuran)
Are used as the liquid materials 4A, 4B and 4C. The solvent container 3D is filled with THF as a solvent 4D. The containers 3A to 3D are provided in accordance with the number of the raw materials, and are not necessarily limited to four.

A charge gas line 5 and transfer lines 6A to 6D are connected to each of the containers 3A to 3D. When the charge gas is supplied into each of the containers 3A to 3D via the charge gas line 5, gas pressure is applied to the liquid surfaces of the liquid materials 4A to 4C and the solvent 4D filled in each of the containers 3A to 3D, Materials 4A-4C and solvent 4D are extruded into respective transfer lines 6A-6D, respectively. The liquid materials 4A to 4C and the solvent 4D that have been pushed out to the transfer lines 6A to 6D are further transferred to the transfer line 6E by gas pressure, and are mixed in the transfer line 6E.

The carrier gas line 7 is connected to the transfer line 6E.
The carrier gas, the liquid materials 4A to 4C and the solvent 4D are supplied from the gas-liquid 2
It is supplied to the vaporizer 2 in a phase flow state. A carrier gas is supplied to the vaporizer 2 via a carrier gas line 7, and the vaporized material is subjected to CV by the carrier gas.
It is sent to the D reactor.

An inert gas such as a nitrogen gas or an argon gas is used as the charge gas and the carrier gas. Further, the liquid material 4A in the transfer lines 6A to 6E.
It is preferable to reduce the amount of 〜4C and the solvent 4D as much as possible. In the present embodiment, 移送 inch piping is used for the transfer lines 6A to 6C.

Each of the transfer lines 6A to 6D has a mass flow meter 8A to 8D and a flow control valve 9 with a shutoff function.
A to 9D are provided. Mass flow meter 8A-8
D monitors the flow rates of the liquid materials 4A to 4C and the solvent 4D while controlling the flow control valves 9A to 9D so that the flow rates of the liquid materials 4A to 4C and the solvent 4D become appropriate. Note that a mixer may be provided immediately before the vaporizer in the transfer line 6E to further improve the mixing state of the liquid material. Further, instead of the flow control valves 9A to 9D for controlling the flow rates of the respective liquid materials 4A to 4C, the flow rate may be controlled using a pump such as a plunger pump.

FIG. 2 is a sectional view of the vaporizer 2 as viewed from the front. The vaporizer 2 includes a nozzle unit 20 that sprays the liquid materials 4A to 4C to form a mist, and a vaporization chamber 21 that further vaporizes the liquid material sprayed from the nozzle unit 20.
The nozzle section 20 is provided with a double pipe 200, and the mixed liquid of the liquid materials 4A to 4C introduced from the transfer line 6E and the carrier gas introduced from the carrier gas line 7 are guided to the double pipe 200. I will This carrier gas is used for atomizing the liquid materials 4A to 4C, and will be referred to as atomizing gas below.

A heater h1 for heating is provided in the vaporization chamber 21.
To h6, and the vaporization chamber 21 is maintained at a temperature higher than the vaporization temperature of the liquid materials 4A to 4C.
The liquid materials 4A to 4C which are sprayed vertically downward from the nozzle unit 20 as shown by a two-dot chain line 23
After being vaporized in the CV (not shown) through the outlet 24
It is sent to the D reactor.

Reference numeral 22 denotes a joint for connecting the transfer line 6E to the nozzle 20 of the vaporizer. FIG. 3 is an enlarged view of the joint 22. The joint 22 includes a pair of sleeves 220.
a, 220b, a nut 221, a plug 222, and a metal gasket 223. The pipe 224 of the transfer line 6E is disposed so as to penetrate the sleeve 220a in the axial direction, and the pipe 224 is fixed to the sleeve 220a by welding or the like. Sleeve 220a, 220
b, sealing surfaces S1 and S2 projecting in a ring shape are formed on the surfaces facing each other.
By disposing the metal gasket 223 between 1 and S2 and screwing the plug 222 into the nut 221, the pipe 224 is fixed to the nozzle unit 20. The pipe 224 is a 1/16 inch SUS pipe, and is processed into a thin tube having an outer diameter of 1 mm or less by swaging at a portion indicated by reference numeral C. In addition,
The dimensions of the thin tube portion are set to an optimum thickness in consideration of the flow rate and the like. Hereinafter, the thin tube portion below the reference sign C will be referred to as the inner tube 200a.

FIG. 4 is an enlarged view of a portion A in FIG. 2. The above-described double pipe 200 includes an inner pipe 200a and an outer pipe 200b. The gas-liquid fluid of the liquid materials 4A to 4C and the carrier gas flows in the inner pipe 200a, and the atomizing gas flows in the annular space between the inner pipe 200a and the outer pipe 200b. The outer pipe 200b is a water-cooled block 2 by welding or the like.
01, and the inner pipe 200a is fixed to the above-described sleeve 220a (see FIG. 3). A cooling rod 202 is provided around the double pipe 200 in contact with the outer pipe 200b. The cooling rod 202 extends to the lower end of the double pipe 200 as shown in FIG.

A male screw portion 203 is formed at the upper part of the outer periphery of the cooling rod 202 and the concave portion 2 of the water cooling block 201 is formed.
The male screw part 203 formed on the female screw part 205
, The cooling rod 202 is fixed to the water-cooling block 201. As shown in FIG. 2, a cooling water channel 206 is formed in the water cooling block 201, and cooling water supplied from the outside via a cooling water pipe 207 circulates through the cooling water channel 206, whereby the water cooling block 201 is formed.
Is cooled. The cooling rod 202 is a water cooling block 201
, And the cooling rod 202 cools the double pipe 200.

A casing 208 covering the periphery of the cooling block 202 is provided below the water cooling block 201 shown in FIG. 2, and a fixing flange 20 is provided below the casing.
8a are formed. By fixing the flange 208a to the vaporization chamber 21, the nozzle unit 20 is attached to the vaporization chamber 21. In this embodiment, the water-cooling block 201 and the cooling rod 202 are formed separately and fastened with screws, but they may be formed integrally. The cooling rod 202 is made of a material having good heat conductivity such as copper.

Next, the structure of the tip portion of the nozzle portion 20 will be described with reference to an enlarged view of a portion B in FIG. The distal end portion 208b of the casing 208 is formed to be thin, and is joined to the distal end portion of the outer pipe 200b by welding or the like.
Therefore, the internal space 209 of the casing 208 and the vaporization chamber space 210 are isolated, and the cooling rod 20
2 is protected from corrosion by the vaporized gas. As shown in FIG. 2, the internal space 209 has a structure that can be evacuated through a pipe 211. By evacuating the internal space 209, heat can be prevented from entering the cooling rod 202 from the casing 208 by convection. ing.

The inner pipe 200a protrudes downward in the drawing from the outer pipe 200b, and further projects through a hole formed in the center of the orifice member 212. The atomizing gas flowing downward between the inner pipe 200a and the outer pipe 200b is vaporized through a gap formed between the orifice member 212 and the outer pipe 200b, for example, a minute gap of 1 mm or less. It is ejected to the chamber space 210. The liquid materials 4A to 4C are atomized by the atomizing gas when they are discharged from the inner pipe 200a, and the atomized liquid materials 4A to 4C are sprayed into the vaporization chamber space 210.

In the vaporizer of the present embodiment, it is preferable that the inner pipe 200a is used with its tip slightly projecting below the orifice member 212. This protrusion amount h
Is adjusted by changing the tightening force of the joint 22 shown in FIG. Specifically, when the joint 22 is tightened with a tightening force required for the metal seal, the axial dimension of the inner pipe 200a is set such that the tip of the inner pipe 200a is substantially the same as the lower surface of the orifice member 212, Fine adjustment of the protrusion amount h is performed by retightening the joint 22.

The orifice member 212 includes the nozzle ring 2
11 is fixed to the casing front end portion 208b so as to sandwich the sealing material 213. Nozzle ring 211 attached to the tip of casing 208 in the form of a cap nut
Is formed with a conical vaporizing surface 211a. The nozzle ring 211 is for preventing the liquid materials 4A to 4C sprayed from the nozzle unit 20 from recondensing at the tip of the nozzle unit 20 and via a flange 208a (see FIG. 2) fixed to the vaporization chamber 21. And is kept at a high temperature by the heat flowing in. As a result, the atomized liquid material 4
Even if A to 4C adhere to the vaporized surface 211a, no unvaporized residue is generated.

The above-described casing 208, nozzle ring 211, pipes 200a and 200b are formed of SUS or the like in consideration of corrosion and the like. On the other hand, the orifice member 21
2. As the sealing material 213, a resin or the like having good heat insulating properties is used so that the heat penetration from the nozzle ring 211 to the cooling rod 202 is reduced. In particular, since the orifice member 212 and the sealing material 213 are required to have corrosion resistance to the liquid materials 4A to 4C, P having excellent heat insulation, heat resistance, and chemical resistance is used.
It is desirable to form with TFE (polytetrafluoroethylene). Further, in order to prevent deformation of the orifice member 212 due to high temperature environment or tightening of the nozzle ring 211,
It may be formed of PEEK (polyether ether ketone) having higher hardness.

As described above, the orifice member 212 and the sealing material 213 made of a heat insulating material prevent the temperature of the cooling rod 202 from rising due to the reduction of the heat penetration from the nozzle ring 211 to the cooling rod 202. In addition, the temperature of the nozzle ring 211 is prevented from lowering due to the cooling of the nozzle ring 211 by the cooling rod 202.

<< Description of Cooling Effect by Cooling Rod 202 >> When the liquid materials 4A to 4C are vaporized by the vaporizer,
In order to prevent the generation of unvaporized residues and the deterioration of the liquid materials 4A to 4C due to the heat history, it is necessary to decompress and heat the liquid materials 4A to 4C almost simultaneously and instantaneously. In the present embodiment, cooling rod 202 extending in the axial direction of double pipe 200 is provided so as to cover the periphery of double pipe 200, and cooling rod 202 is extended to the vicinity of the ejection part of double pipe 200. Provided. Thus, the liquid materials 4A to 4C flowing through the inner pipe 200a are sufficiently cooled until immediately before being ejected into the vaporization chamber space 210.

Here, the cooling rod 202 and the casing 2
08, a heat insulating space 209 is formed, and only the thin end portion 208b of the cooling rod 202 and the casing 208 are in contact with each other. In addition, the hot nozzle ring 211
Since the orifice member 212 and the sealing material 213 having excellent heat insulating properties are interposed therebetween, it is possible to reduce heat from entering the cooling rod 202 from the high-temperature vaporization chamber 21 or the nozzle ring 211.

FIG. 6 is a view for explaining the cooling effect of the cooling rod 202, and shows axial temperature distribution data in the inner pipe 200a when the vaporization chamber 21 is heated to 250 ° C. The temperature of the cooling water was 8 ° C., and the pressure of the space 209 was 1333 Pa (= 10 Torr). 6, the vertical axis represents the temperature of the inner pipe 200a, the horizontal axis represents the distance measured upward from the tip of the cooling rod 202, and the negative distance represents the portion protruding downward from the tip of the cooling rod 202. Represents. As shown in FIG.
Even in a high temperature environment of 250 ° C., the cooling rod 20
Due to the cooling effect of 2, the temperature of the inner pipe 200a is kept sufficiently low, for example, about 50 ° C. at a position 10 mm from the rod tip.

FIG. 7 qualitatively shows changes in temperature and pressure of the liquid material before and after vaporization.
Is related to the vaporizer of the present embodiment, and (b) and (c) are related to a conventional vaporizer. In FIG. 7, the vertical axis represents temperature and pressure, the horizontal axis represents time, the left region of the diagram represents temperature and pressure in a liquid state, and the right region of the diagram represents temperature and pressure after vaporization. I have.

FIG. 7 (b) shows the configuration of Japanese Unexamined Patent Application Publication No. 5-253402.
FIG. 1 shows changes in temperature and pressure when the apparatus described in Japanese Patent Application Laid-Open Publication No. H10-15064 is used. In the apparatus described in JP-A-5-253402, the liquid material pumped to the vaporizer is heated after being brought into contact with a high-temperature disk provided in the vaporizer and then decompressed to vaporize. The process has been adopted. FIG. 7 (c) is a table shown in FIG.
8 shows changes in temperature and pressure when the apparatus described in JP-A-8315 is used. Tokuhyo Hei 8-50831
In the device described in Japanese Patent Publication No. 5 (1995), after a pressurized liquid material is heated, it is permeated into a mesh placed under reduced pressure and vaporized.

In both cases (b) and (c) of FIG. 7, the intermediate state D until the liquid material changes from the room temperature and high pressure state to the high temperature and reduced pressure state is relatively long. In this intermediate state, the liquid material is apt to deteriorate due to heat history,
Unevaporated residues and clogging of the vaporizer are likely to occur. On the other hand, in the vaporizer according to the present embodiment, the liquid material 4A to 4C is cooled by the cooling rod 2 until immediately before being ejected from the inner pipe 200a.
02, the intermediate state D corresponds to FIG.
(A) As shown in FIG.
4C alteration, unvaporized residue, clogging of the vaporizer, and the like can be reduced.

<< Description of Spray Performance >> As described above, the inner pipe 200a is a thin pipe having an outer diameter of 1 mm or less. As described below, the gas-liquid two-phase flow in the pipe becomes an annular spray flow. Then, the flow rates of the liquid materials 4A to 4C and the carrier gas flowing through the inner pipe 200a are adjusted. Here, the annular spray flow means that the gas flow rate is larger than the liquid phase flow rate of the gas-liquid two-phase flow, there is a liquid film on the pipe wall, and a large number of droplets are formed at the center of the gas phase pipe cross section This is the accompanying flow. The flow conditions for performing stable spraying will be described later.

Further, the spraying performance of the above-mentioned liquid material 4A-
As well as the flow rate and pipe size of 4C and carrier gas,
It also depends on the flow rate of the atomizing gas flowing through the outer pipe 200b. FIG. 8 is a diagram illustrating the relationship between the liquid flow rate and the gas flow rate in the inner pipe 200a, the gas flow rate in the outer pipe 200b, and the spray stability. In the measurement shown in FIG.
THF was used as the liquid flowing through the inner pipe 200a, and nitrogen gas was used as the carrier gas and the gas for atomization.

In FIG. 8, the vertical axis represents the flow rate of carrier gas (SCCM), and the horizontal axis represents the flow rate of THF (cc / mi).
n). In this measurement, experiments were conducted by distinguishing the spray state into "stable spray" in which continuous spray was observed and "unstable spray" in which the pressure in the vaporization chamber fluctuated greatly due to discontinuous droplet bumping. Was. In FIG. 8, data of stable spraying is represented by a circle, and unstable spraying is represented by a cross. In addition, about 1333 Pa (= 10
Torr) to 6666 Pa (= 50 Torr) and flow rate 5
0 SCCM and the primary pressure of THF was 1.7 MPa. The temperature of the vaporization chamber was set at 250 ° C.

As shown in FIG. 8, the spray becomes more unstable as the THF flow rate increases, and the spray tends to be more stable as the carrier gas increases. Further, in a state where the amount of the carrier gas is large, the THF flow rate has an upper limit, and the line L1 indicates the limit. For example, carrier gas flow rate = 400 SCCM
At the intersection of the line L1 and the THF flow is about 1.7 (c
c / min), the carrier gas flow rate is 400 S
In the case of CCM, THF cannot flow at more than 1.7 (cc / min). And spraying can be performed stably in the area F1 below the line L1 and on the left side of the line L2, and below the line L1 and
It can be seen from FIG. 8 that the spray becomes unstable in the area F2 on the right side of the line L2.

For example, the flow rate of the mixture of the liquid metal material and the solvent THF flowing through the inner pipe 200a is set to 0.8 (cc / cc).
min), the carrier gas flow rate 150 (S
CCM), a spray gas flow rate of 50 (SCCM) is preferred,
When the mixed solution flow rate is 1.2 (cc / min),
Carrier gas flow rate 250 (SCCM), spray gas flow rate 5
0 (SCCM) is preferred.

By adjusting the hole diameter e of the orifice member 212 with respect to the outer diameter of the inner pipe 200a in FIG. 4, the flow rate of the atomizing gas flowing through the gap between the orifice member 212 and the inner pipe 200a can be adjusted appropriately. Set to a value. Further, the atomizing gas flowing through this gap causes the inner pipe 2
00a is centered with respect to the hole of the orifice member 212.

<< Modification of Cooling Rod >> FIG. 9 is a view showing a modification of the cooling rod 202, and FIG.
02B is a cross-sectional view of the cooling rod 202C. FIG. 9A shows a structure in which the cooling rod 202 and the water cooling block 201 of FIG.
51 and a rod portion 252, and are formed of a material having high thermal conductivity such as copper. In the cooling rod 202B having such an integrated structure, the cooling efficiency of the rod portion 252 is improved as compared with the case where the cooling rod 202 and the water cooling block 201 are integrated by a screw structure.

The cooling rod 202C shown in FIG.
The heat pipe structure is further added to the cooling rod 202B of FIG. In the cooling rod 202C, an annular cavity 255 is formed from a portion adjacent to the cooling water passage 206 provided in the water cooling section 253 to a tip of the rod section 254, and a coolant such as alcohol is sealed in the cavity 255. . The refrigerant sealed in the cavity 255 evaporates below the cavity 255 which is a high temperature part, and liquefies above the cavity 255 which is a low temperature part. Therefore, in addition to the heat conduction of the rod part 254, the heat transfer from the rod part 254 to the water cooling part 253 via the refrigerant can improve the cooling efficiency as compared with the cooling rod 202B. Although the cooling rod 202C has a heat pipe structure by forming a cavity 255 in the member, the cooling rod 202B shown in FIG.
Alternatively, a commercially available heat pipe may be embedded.

Although the water cooling block 201 and the cooling rod 202 shown in FIGS. 2 and 3 are fixed to each other by a screw structure, they may be integrated by pressing. When the pressure contact structure is adopted, for example, even when the water cooling block 201 is formed of SUS which is a dissimilar metal with respect to the copper cooling block 202, the contact transfer efficiency at the dissimilar metal interface can be improved.

<< Modification of Nozzle Ring >> FIG. 10 is a view showing a modification of the nozzle ring 211 shown in FIG. FIG. 10A shows a nozzle ring 214 having a two-part structure, and the nozzle ring 214 has a cap nut portion 214.
a and a holding ring 214b. In the nozzle ring 211 shown in FIG. 5, when the nozzle ring 211 is tightened and fixed to the casing, there occurs a problem that the orifice member 212 also rotates together.
However, in the case of the nozzle ring 214 having a two-part structure shown in FIG. 10A, even if the cap nut 214a is tightened, the orifice member 212 is pressed by the press ring 214b and rotates together with the cap nut 214a. Can be prevented.

FIG. 10B shows another modification of the nozzle ring 211. Nozzle ring 215 has flange 216
The flange 216 is fixed to the inner wall surface of the vaporization chamber 21 by bolts 217. As a result, the heat transfer from the vaporization chamber 21 to the nozzle ring 215 becomes larger, and the nozzle ring 21
5 can be kept at substantially the same temperature as the vaporization chamber 21, and the generation of unvaporized residues on the vaporization surface 215a can be prevented. The axial position of the nozzle ring 215 is
Adjust by screwing nozzle ring 215 into flange 216. Although the nozzle ring 215 and the flange 216 are separate here, they may be formed integrally.

By the way, the nozzle rings 211, 214,
215 so that the atomized liquid metal material hardly adheres
Those surfaces may be coated with PTFE. Thereby, the generation of unvaporized residues is further reduced. Also,
By forming a corrosion-resistant black film such as an oxide film on the surfaces of the nozzle rings 211, 214, and 215, the radiant heat from the vaporization chamber 21 can be easily absorbed, and the nozzle rings 211, 214, and 215 can be further moved to the vaporization chamber 21. The temperature may be kept close.

<< Description of Connection Between Transfer Line 6E and Inner Pipe 200a >> Next, the transfer line 6E and inner pipe 2
00a will be described. In the above-described embodiment, as shown in FIG.
24 was narrowed down by swaging and processed into a thin tube having an outer diameter of 1 mm or less, and the thin tube was used as the inner pipe 200a. As a result, the flow of the gas-liquid fluid in which the liquid metal material and the carrier gas are mixed is smoothed, and a dead volume that causes clogging of the liquid metal material and deterioration of the material is eliminated.

FIG. 11 is a diagram showing another example of the connection method. FIG. 11A shows an inner pipe 200 in a pipe 224.
(a) is obtained by inserting the upper end portion of the inner pipe 200a and welding the inner pipe 200a.
Is crimped from the outer periphery. Each is characterized by low cost. Also, in the case shown in FIG. 11C, the sleeve 220 to which the pipe 224 is fixed is provided.
A cylindrical hole 232 having a screw portion 231 is formed at a. Then, the inner pipe 200a with the PTFE ring-shaped sealing material 233 attached to the outer periphery of the tip is inserted into the cylindrical hole 232, and the set screw 234 externally inserted into the inner pipe 200a is screwed into the screw portion 231 of the cylindrical hole 232. As a result, the outer peripheral surface of the inner pipe 200a and the inner peripheral surface of the cylindrical hole 232 are sealed by the sealant 233. In this case, the inner pipe 200a which is relatively inexpensive and is easily clogged
Only can be easily replaced.

In the above-described embodiment, the liquid materials 4A to 4A
4C, for example, pipes 200a, 200
Although the b, 224 and the joint 22 are made of SUS, Ti or a Ti alloy (TiN or the like) which is a material having higher corrosion resistance may be used.

In the correspondence between the embodiment described above and the elements of the claims, the double pipe 200 connects the transfer pipe with
The nozzle section 20 is a spray section, the vaporization chamber 21 is a vaporization section, the cap nut section 214a is a first member, and the holding ring 2
14b constitutes each of the second members.

[0047]

As described above, according to the first to fifth aspects of the present invention, the liquid material of the gas-liquid two-phase flow is ejected from the inner pipe, and the mist is sprayed from the gap between the inner pipe and the orifice member. By ejecting the forming gas, atomization of the liquid material can be performed more effectively. As a result, generation of unvaporized residues and generation of particles can be reduced. According to the second to fourth aspects of the present invention, by disposing a heat insulating orifice member and a seal member between the nozzle ring and the outer pipe constituting the transfer pipe, heat from the nozzle ring to the transfer pipe is provided. Penetration can be reduced. According to the fifth aspect of the invention, the amount of protrusion of the inner pipe tip from the orifice member can be easily adjusted, and it is easy to adjust the spraying conditions to the optimum. According to the invention of claim 6, the atomization performance of the spray section can be improved by making the liquid material in the transfer pipe into an annular spray flow.

[Brief description of the drawings]

FIG. 1 is a diagram showing a schematic configuration of an entire vaporizer.

FIG. 2 is a sectional view showing the vaporizer 2 in detail.

FIG. 3 is an enlarged view of a joint 22.

FIG. 4 is an enlarged view of a portion A in FIG. 2;

FIG. 5 is an enlarged view of a portion B in FIG. 2;

FIG. 6 is a diagram illustrating a cooling effect of a cooling rod 202.

FIGS. 7A and 7B are diagrams qualitatively showing changes in the temperature and pressure of the liquid material before and after vaporization, wherein FIG. 7A relates to the vaporizer of the present embodiment, and FIGS. It is about a vessel.

FIG. 8 is a diagram illustrating spray stability.

FIG. 9 is a view showing a modification of the cooling rod 202;
(A) shows a first modification, and (b) shows a second modification.

FIGS. 10A and 10B are diagrams showing a modification of the nozzle ring 211, wherein FIG. 10A shows a first modification and FIG. 10B shows a second modification.

11A and 11B are diagrams illustrating another connection method of the pipe 224 and the inner pipe 200a, wherein FIG. 11A illustrates a first example, FIG. 11B illustrates a second example, and FIG. 11C illustrates a third example. .

[Explanation of symbols]

 2 vaporizer 20 nozzle part 21 vaporization chamber 200 double pipe 200a inner pipe 200b outer pipe 201 water cooling block 202, 202B, 202C cooling rod 208 casing 211, 214, 215 nozzle ring 212 orifice member

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Tatsushi Kawamoto 1 Nishinokyo Kuwaharacho, Nakagyo-ku, Kyoto-shi, Kyoto Prefecture Inside Shimadzu Corporation (72) Inventor Masashi Kawano 1 Nishi-no-Kyowaharacho, Nakagyo-ku, Kyoto-shi, Kyoto Inside Shimadzu Corporation (72) Inventor Shigeru Matsuno 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsubishi Electric Corporation (72) Inventor Akira Yamada 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsubishi Electric Corporation (72) Inventor Shoji Miyashita 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsubishi Electric Corporation (72) Inventor Hideko Uchikawa 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsubishi Electric Corporation F term (reference) 4K030 AA11 EA01 KA46 5F045 AA04 AC07 AC16 BB15 EE02 EE04 EE14 GB04 GB06

Claims (6)

[Claims] 1. A spray section for spraying a gas-liquid mixed material obtained by mixing a liquid material composed of a liquid organic metal or an organic metal solution and a carrier gas from a tip end of a transfer pipe, and vaporizing the sprayed liquid material. A vaporizer for supplying the vaporized liquid material to a CVD film forming apparatus, wherein the transfer pipe comprises: an inner pipe through which the liquid material is transferred in a gas-liquid two-phase flow; A double pipe structure comprising a pipe inserted through a gap and an outer pipe for transferring atomizing gas, wherein a hole is formed through which the inner pipe is inserted through the gap, and the outer pipe is formed. An orifice member for ejecting the atomizing gas transferred by the nozzle from the gap to the vaporizing section is provided at a tip end of the inner pipe. 2. The vaporizer according to claim 1, wherein a vaporizing surface is formed to prevent the vaporized liquid material from being re-condensed, and a tip of the spray unit is provided near a tip of the inner pipe. The orifice member is provided with a PEEK (polyether ether keto
ne) and sandwiched between the nozzle ring and the tip of the outer pipe, and PTFE (polytetrafluoroethene) between the orifice member and the tip of the outer pipe.
A vaporizer comprising a sealing material made of ylene). 3. The vaporizer according to claim 2, wherein the nozzle ring is screwed to a tip of the spray unit.
A vaporizer comprising: a member; and a second member formed separately from the first member and sandwiched between the orifice member and the first member. 4. The vaporizer according to claim 1, wherein a vaporizing surface is formed to prevent the vaporized liquid material from being re-condensed, and the vaporizing section is located near a tip of the inner pipe. The orifice member is provided with a PEEK (polyether ether keto
ne) and sandwiched between the nozzle ring and the tip of the outer pipe, and PTFE (polytetrafluoroethene) between the orifice member and the tip of the outer pipe.
A vaporizer comprising a sealing material made of ylene). 5. The vaporizer according to claim 1, wherein a metal gasket and a pair of metal gaskets are provided as joints for fixing the inner pipe to the spraying portion. A gasket-type seal joint comprising a gasket-type seal joint having a joint member, wherein one of the pair of joint members is fixed to the spray portion, and the other of the pair of joint members is fixed to the inner pipe. The amount of protrusion of the tip end of the inner pipe from the orifice member can be adjusted by adjusting the amount of tightening in the axial direction. 6. A spray section for spraying a gas-liquid mixed material obtained by mixing a liquid material composed of a liquid organic metal or an organic metal solution and a carrier gas from a tip end of a transfer pipe, and vaporizing the sprayed liquid material. A vaporizer for supplying the vaporized liquid material to a CVD film forming apparatus, wherein the liquid material is supplied in an annular spray flow state in the transfer conduit. .