JP2002069650A - Method and apparatus for vapor phase deposition, and method and device for manufacturing semiconductor device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vapor phase deposition apparatus which forms wiring having stress and resistivity which are sufficiently controlled not to be increased, on a base substance, as well as sufficiently controls the generation of particles. SOLUTION: A CVD apparatus 1 comprises a chamber 2 having a susceptor 3 which supports a wafer 5 consisting of Si, and having a shower head 4 which is connected to a gas supplying system 30. This showerhead 4 consists of a body 41, a base plate 43, a face plate 45, and a blocker plate 47, and comprises space parts, Sa and Sb inside. A pore size ϕ of several through holes 47a provided on the blocker plate 47 has a predetermined value so that gas pressure in the space part Sa can be about the same as that in the upper part of the wafer 5.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vapor deposition method and apparatus, and a method and apparatus for manufacturing a semiconductor device.
More specifically, a vapor deposition method and apparatus for supplying a plurality of types of gases onto a substrate through at least one perforated plate having a plurality of through holes to deposit a predetermined compound on the substrate, and a semiconductor device And a device therefor.

[0002]

2. Description of the Related Art In recent years, with the miniaturization of semiconductor integrated circuits, a semiconductor integrated circuit is formed on a substrate such as a semiconductor wafer from the viewpoint of reducing wiring resistance, improving wiring reliability, and further improving flatness at a wiring level. A so-called tungsten plug (W-plug) has come to be used as all or a part of the metal wiring to be formed. In this method, holes provided in an insulating layer for forming interlayer connections (through contacts, vias, etc.) are filled with tungsten (W).

A conventional method of forming such a W-plug is chemical vapor deposition (CV) having a process gas supply such as a shower head having a perforated plate.
D) using a chamber, sequentially forming a barrier layer and a W layer,
After that, there is a method of removing W deposited on the portions other than the interlayer connection holes by chemical mechanical polishing (CMP).

At this time, prior to forming a W layer in the CVD method, usually, silane (SiH ₄ ) is supplied into a chamber together with WF ₆ which is a raw material of W, and tungsten silicide (W) is used as a seed layer. nucleation step of forming the _x Si _y) layer is performed.

[0005]

The inventors of the present invention have repeatedly studied a method for forming a wiring using a conventional CVD chamber, and have found the following problems. (1) The stress (internal stress (residual stress)) of the formed wiring layer tends to increase, and in some cases, various characteristics of the wiring may be deteriorated, and the shape of the upper layer portion of the W layer may be changed in a later process. was there. (2) The resistivity of the formed wiring layer becomes undesirably high, which may increase the sheet resistance or the wiring resistance. (3) In a so-called W-CVD process in which W is formed on a substrate by a CVD method, there is a problem that particles are easily generated. For this purpose, for example, there are conceivable countermeasures such as adjusting the amount of use of a plurality of source gases used for film formation or the timing of supply to the chamber, or reducing the temperature in the showerhead described above. However, even in this case, the above-mentioned (1) and (2) cannot be solved, and the reduction of particles may not be sufficient.

Accordingly, the present invention has been made in view of such circumstances, and it is possible to sufficiently suppress the generation of particles and to form a wiring on a substrate on which stress and an increase in resistivity are sufficiently suppressed. It is an object of the present invention to provide a vapor deposition method and apparatus which can be formed on a substrate. It is another object of the present invention to provide a method for manufacturing a semiconductor device having a wiring formed of a conductive layer in which an increase in stress and resistivity is sufficiently suppressed, and an apparatus therefor.

[0007]

Means for Solving the Problems In order to solve the above-mentioned problems, the present inventors have made intensive studies and, as a result, have obtained the following further findings. That is, from the viewpoint of the physical properties of the formed substrate (semiconductor device); (1) It is highly possible that the increase in stress depends on the change in the crystallinity of the compound (W or the like) forming the wiring layer (conductive layer). (2) This change in crystallinity is because a W _x Si _y layer having a desired composition ratio cannot be obtained, particularly in the nucleation step. It has been found that a change in crystallinity of a compound forming a layer is a main factor.

(4) In the W-CVD process, the supply amount of the SiH ₄ gas to the shower head was increased with respect to the WF ₆ gas in order to reduce particles in the W-CVD process. Nevertheless, WF ₆ may be enriched on the substrate, and the direct cause is considered to be that both gases are presumed to have reacted in the showerhead. Was. The present inventors have further studied based on these findings, and reached the present invention.

That is, the vapor deposition method according to the present invention comprises:
A method of supplying a plurality of types of gases onto a substrate through at least one perforated plate having a plurality of through holes and depositing a predetermined compound on the substrate, wherein the following formula (1): P1 / P2 ≦ 1.15 (1) or a plurality of gases are supplied onto the substrate so as to satisfy the relationship represented by the following formula (2): P1−P2 ≦ 0.7 (2) It is characterized by the following.

Here, in the formula, P1 indicates the total pressure (kPa) of the plurality of gases flowing into the porous plate located on the most upstream side in the flow path of the plurality of gases, and P2
Indicates the total pressure (kPa) of the plurality of gases flowing out of the perforated plate located at the most downstream side in the flow path of the plurality of gases. P1 / P2 is preferably 1.12 or less, more preferably 1.05 or less, and particularly preferably approximately 1 (that is, P1 ≒ P2).
(P1−P2) is preferably 0.5 kPa or less, more preferably 0.3 kPa or less, and particularly preferably about 0 kP.
a.

In such a vapor phase deposition method, a plurality of types of gases are sufficiently dispersed and mixed by at least one perforated plate and flow out to the substrate side through a plurality of through holes provided in the perforated plate. . Thereby, a plurality of mixed gases are supplied on the substrate at a sufficiently uniform concentration,
A predetermined compound is deposited, and a film having excellent uniformity is formed. In addition, from the viewpoint of sufficiently mixing a plurality of types of gases, as a supply unit to which those gases are supplied, a gas distribution unit such as a so-called shower head having an internal space defined by a perforated plate and other members and defining an internal space is provided. It is desirable to supply those gases onto the substrate through a section.

At this time, the relationship represented by the equation (1) or (2) is satisfied, that is, the side on which a plurality of types of gas flows into the perforated plate and the gas flows out from the perforated plate. When the pressure difference on the side is substantially equal to that on the side, the reaction of these gases in the gas phase before flowing out of the perforated plate is sufficiently suppressed. Therefore, the ratio of at least one of the plurality of gases in the gas phase to the other gas is prevented from being different from the initially desired ratio.

When a reaction occurs on the upstream side of the perforated plate, the reaction product accumulates on the perforated plate, so that the through-holes in the perforated plate tend to gradually close. In this case, the pressure difference before and after the perforated plate increases, and the reaction tends to be further promoted on the upstream side of the perforated plate. On the other hand, in the present invention, as described above, the reaction of the gas in the gas phase before flowing out of the perforated plate is sufficiently suppressed, so that the reaction on the upstream side of such a perforated plate is promoted. Can be suppressed.

More specifically, in the vapor deposition method according to the present invention, the following formulas (3) and (4) are used as at least one of the perforated plates: 0.01 ≦ φ ≦ 0 .10 (3), 1 ≦ K ≦ 40 (4) It is preferable to use a material that satisfies the following relationship. Here, in the formula, φ indicates the hole diameter (mm) of the through hole provided in the at least one perforated plate, and K indicates the aperture ratio (%) of the through hole in the at least one perforated plate. .

More preferably, the relationship represented by the following formulas (5) and (6): 0.02 ≦ φ ≦ 0.05 (5), 5 ≦ K ≦ 30 (6) Use those satisfying, particularly preferably,
It is preferable to use those satisfying the following expressions (7) and (8): 0.02 ≦ φ ≦ 0.035 (7), 10 ≦ K ≦ 25 (8) .

The "opening ratio of through-holes" in the present invention.
The term "percentage" means a value representing the ratio of the total area of the through holes to the area of one surface of the perforated plate in percentage. It has been confirmed that the relationship represented by the formula (1) or the formula (2) is suitably achieved by using the porous plate configured as described above.

Further, in the vapor deposition method of the present invention, a plurality of types of gases are supplied to the lid portion of the perforated plate, which is opposed to the most upstream perforated plate in the flow path of the plurality of gases. It is desirable to allow the gas to flow into the perforated plate from the provided gas supply port, and to use a lid whose surface facing the perforated plate forms a substantially smooth surface.

As described above, when a plurality of types of gases are introduced into a gas distribution unit such as a shower head, a pressure loss of the gas may occur immediately after the gas is introduced, depending on the internal shape of the gas supply unit. . For example, the lid constituting the upper part of the gas supply unit may be provided with a concave / convex portion for positioning, a step, or the like in manufacturing the gas supply unit. In particular, if the projection is configured to protrude into the internal space of the gas supply unit, pressure loss in the space tends to occur easily. Therefore, if the surface facing the perforated plate forms a substantially smooth surface as the lid, a plurality of types of gases can be supplied from the gas supply port of the lid disposed opposite to the perforated plate located on the most upstream side. Since there is no barrier when flowing into the perforated plate, it is possible to sufficiently prevent pressure loss of gas.

More specifically, a compound containing a tungsten atom (for example, WF ₆
A gas comprising a compound containing a silicon atom (for example, silanes, alkylsilanes, etc.);
May be supplied on the substrate.

The above-mentioned "silanes" are not limited to monosilane, but have a molecular form in which silicon hydride having at least one silicon atom in the molecule, that is, a carbon in which methane series hydrocarbon is substituted with silicon. And a hydrogen atom may be replaced by a halogen atom. Among these, monosilane, disilane, dichlorosilane and the like are preferable from the viewpoint of industrial utility. Examples of the “alkylsilanes” include at least one of methylsilane, dimethylsilane, trimethylsilane, tetramethylsilane, 1,1,1-trimethyldisilane, and hexamethyldisilane.

When a plurality of such gases are used, a tungsten silicide (W _x Si _y ) layer serving as a seed layer can be formed as a nucleation step as described above. In the vapor deposition method according to the present invention, the reaction of gas on the upstream side of the perforated plate is suppressed, so that a tungsten silicide layer having a desired composition ratio can be surely formed. Then, a tungsten layer having conductivity is formed on such a seed layer.

The vapor deposition apparatus according to the present invention is an apparatus for effectively implementing the vapor deposition method of the present invention.
Depositing a predetermined compound on a substrate,
(A) a chamber provided with a gas supply port to which a plurality of types of gases are supplied, and provided with a substrate supporting portion for supporting a substrate; and (b) at least one space communicating with the gas supply port. A gas distributor having at least one perforated plate disposed opposite to the base support so that a portion is defined;
And (c) the gas distribution unit is provided so as to satisfy the relationship represented by the above formula (1) or the above formula (2).

Further, it is preferable that at least one of the perforated plates (d) is provided so as to satisfy the relationship represented by the above formulas (3) and (4). .

Further, (e) the gas distribution portion is disposed so as to face a perforated plate located on the most upstream side in a flow path of a plurality of types of gas among the perforated plates, and is provided with the gas supply port. (F) It is more preferable that the surface of the lid facing the perforated plate forms a substantially smooth surface.

Furthermore, (g) a first gas supply source connected to the gas distribution unit and supplying a gas comprising a compound containing tungsten atoms, and (h) a first gas supply source connected to the gas distribution unit and containing silicon atoms. And a second gas supply source for supplying a gas composed of a compound having the following characteristics.

Further, a method of manufacturing a semiconductor device according to the present invention is a method of manufacturing a semiconductor device having a conductive layer, wherein a predetermined compound is formed on a semiconductor substrate as a base by using the vapor deposition method of the present invention. A compound having conductivity is formed.

Alternatively, in the method of manufacturing a semiconductor device according to the present invention, a plurality of types of gases are supplied to a semiconductor substrate through at least one perforated plate having a plurality of through holes, and the semiconductor substrate has conductivity. A method for forming a conductive layer made of a compound, wherein a plurality of types of gases are supplied onto a semiconductor substrate so as to satisfy the relationship represented by the above formula (1) or the above formula (2). Is also good.

A semiconductor device manufacturing apparatus according to the present invention is suitable for carrying out the semiconductor device manufacturing method of the present invention, and is an apparatus for manufacturing a semiconductor device having a conductive layer. A phase deposition apparatus is provided, and a chamber constituting the vapor deposition apparatus accommodates a semiconductor substrate as a base.

Alternatively, a semiconductor device manufacturing apparatus according to the present invention is an apparatus for manufacturing a semiconductor device having a conductive layer, having a gas supply port through which a plurality of types of gases are supplied, and a semiconductor substrate. A chamber provided with a base supporting portion, and at least one perforated plate disposed opposite to the base supporting portion so as to define at least one space communicating with the gas supply port, and , The above equation (1)
Or a gas distribution unit provided so as to satisfy the relationship represented by the above equation (2).

[0030]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described in detail. Note that the same components are denoted by the same reference numerals, and redundant description will be omitted. Unless otherwise specified, the positional relationship such as up, down, left, and right is based on the positional relationship shown in the drawings. Further, the dimensional ratios in the drawings are not limited to the illustrated ratios.

FIG. 1 is a schematic view (partly in section) schematically showing a preferred embodiment of a semiconductor device manufacturing apparatus according to the present invention which also serves as a vapor deposition apparatus according to the present invention. The CVD apparatus 1 (a vapor deposition apparatus and a semiconductor device manufacturing apparatus) includes Si
A gas supply system 30 is connected to a chamber 2 in which a wafer 5 (substrate, semiconductor substrate) formed of is housed.

The chamber 2 has a susceptor 3 (substrate support) on which a wafer 5 is placed. Above the susceptor 3, a shower head 4 having a hollow disk shape is provided.
(Gas distribution unit) is provided. The susceptor 3 is hermetically provided in the chamber 2 by an O-ring, a metal seal, or the like, and is provided so as to be vertically movable by a movable mechanism (not shown). Thereby, the distance between the wafer 5 and the shower head 4 is adjusted. Further, a heater 3a is provided inside the susceptor 3, and the wafer 3 is heated to a desired temperature by the heater 3a.

The shower head 4 has a base plate 43 having a substantially cylindrical body 41 at the upper end and the lower end with a gas supply port 9 through which a gas to be described later is supplied at the center. (Lid) and a face plate 45 (perforated plate). A blocker plate 47 (perforated plate) is provided inside the shower head 4 substantially in parallel with the face plate 45. A space Sa is defined by the body 41, the base plate 43, and the blocker plate 47.
1. Face plate 45 and blocker plate 47
Defines a space Sb. The base plate 43 has a substantially smooth surface facing the blocker plate 47, that is, a surface shape having substantially no irregularities.

Further, an opening 4 is provided in the lower part of the chamber 2.
0, and the opening 40 is provided with the chamber 2
A vacuum pump (not shown) for decompressing the inside of the device is connected via a pipe (not shown).

On the other hand, the gas supply system 30 includes a WF ₆ gas supply source 31 (first gas supply source), a SiH ₄ gas supply source 32
(Second gas supply source), Ar (argon) gas supply source 3
3 and an H ₂ (hydrogen) gas supply source 34. These gas supply sources 31 to 34 are provided with MFCs (mass flow controllers) 31a to 34a for controlling the mass flow rate of each gas.
Is connected to a gas supply port 9 provided in a base plate 43 of the shower head 4 via a pipe 10 provided with a gas supply port. Thereby, each gas (WF ₆ gas, SiH ₄ gas, Ar gas, H ₂ gas) is introduced into the shower head 4 from the gas supply system 30 and supplied into the chamber 2 via the blocker plate 47 and the face plate 45. You.

Here, the face plate 45 and the blocker plate 47 constituting the shower head 4 are provided with a plurality of through holes 45a and 47a, respectively.
The spaces Sa and Sb communicate with each other so that gas can flow. The shower head 4 is represented by the following equation (1): P1 / P2 ≦ 1.15 (1) or the following equation (2): P1−P2 ≦ 0.7 (2) It is provided to satisfy the relationship.

In these equations (1) and (2), P1
Is a total pressure value (kPa) in the space Sa of a plurality of types of gases (hereinafter, exemplified as “WF ₆ gas and SiH ₄ gas”) supplied into the shower head 4, that is, flows into the blocker plate 47. The total pressure value of a plurality of types of gases (WF ₆ gas and SiH ₄ gas) is shown.
P2 is the face plate 4 of the shower head 4.
5 gases (WF ₆ gas and SiH ₄ gas)
Gas), that is, the total pressure of a plurality of types of gases (WF ₆ gas and SiH ₄ gas) in the space between the susceptor 3 and the shower head 4 in the chamber 2.

The showerhead 4 preferably has P1 / P2 in the formula (1) of 1.12 or less, more preferably 1.05 or less, and particularly preferably about 1 (that is, P1 ≒).
P2), or (P1-P2) in Formula (2) is preferably 0.5 kPa or less, more preferably 0.3 kPa or less, and particularly preferably approximately 0 kPa.
It is configured to be Pa.

When P1 / P2 exceeds 1.15, or (P1-P2) becomes 0.7 kPa (5.3 Torr).
Exceeds WF in the space Sa or the space Sb.
₆ gas and SiH ₄ gas tend to react easily. Usually, the supply amount of the SiH ₄ gas with respect to the WF ₆ gas is appropriately determined according to the film forming conditions and the like. For example, the supply amount of the SiH ₄ gas may be larger than that of the WF ₆ gas. At this time, if both gases react in the spaces Sa and Sb,
The concentration ratio between the WF ₆ gas and the SiH ₄ gas supplied into the chamber 2 may be different from the concentration ratio between the WF ₆ gas and the SiH ₄ gas that has actually reached the wafer 5 placed on the susceptor 3. There is.

The size and shape of the shower head 4, the chamber 2, the wafer 5 to be processed, etc.
Although the optimum value differs depending on the gas supply flow rate to
At least one of the through hole 47a of the blocker plate 47 and the through hole 45a of the face plate 45 satisfies the relationship of the expression (1) or the expression (2).
More preferably, the following expressions (3) and (4) are satisfied: 0.01 ≦ φ ≦ 0.10 (3), 1 ≦ K ≦ 40 (4) Is particularly preferably so as to satisfy the following expressions (5) and (6): 0.02 ≦ φ ≦ 0.05 (5), 5 ≦ K ≦ 30 (6) Is provided so as to satisfy the relationship represented by the following formulas (7) and (8): 0.02 ≦ φ ≦ 0.035 (7), 10 ≦ K ≦ 25 (8) It is suitable.

Where φ is the through hole 47a and / or
Or, indicates the hole diameter (mm) of the through hole 45a, and K indicates the opening ratio (%) of the through hole 47a in the blocker plate 47 and / or the opening ratio (%) of the through hole 45a in the face plate 45. .

If the hole diameter φ of these through holes 47a, 45a is less than 0.01 mm, or if the through holes 47a, 45a
If the opening ratio K of a is less than 1%, the blocker plate 47 and the blocker plate 47 and (P1−P2) are set to the extent that the above-mentioned P1 / P2 or (P1-P2) exceeds the upper limit shown by the equations (1) and (2), respectively. And / or the face plate 45 tends to increase the pressure loss.

On the other hand, if the hole diameter φ exceeds 0.10 mm, or the opening ratio K of the through holes 47a and 45a is 40%
Is exceeded, the WF ₆ gas and the SiH ₄ gas introduced into the space Sa from the gas supply port 9 are supplied to the blocker plate 47.
Therefore, there is a tendency that the water is not sufficiently diffused and moves to the outside of the space portion Sb and thus the shower head 4.

The through holes 4 of the blocker plate 47
The hole diameter φ and aperture ratio K of 7a are calculated by the above equations (3) and (4).
When the relationship is satisfied, the hole diameter φ and the aperture ratio K of the through hole 45a of the face plate 45 may not be particularly limited, that is, a shape that satisfies the relationship of Expressions (3) and (4). However, the present invention is not limited to this.

Hereinafter, the CVD apparatus 1 configured as described above will be described.
An example of a method for manufacturing a semiconductor device which also serves as a vapor deposition method according to the present invention using a semiconductor device will be described. Each operation of the CVD apparatus 1 described below is controlled by a control device (system) (not shown) based on an operation by an automatic or operator.

First, the pressure in the chamber 2 is reduced by a vacuum pump. Under this reduced pressure, titanium (Ti) and titanium nitride (TiN) were deposited in this order on a wafer 5 (in this case, a concave portion such as a hole, a trench, or the like was formed or not formed). Is transported into the chamber 2 from a predetermined location such as a load lock chamber, another chamber, another wafer preparation chamber, etc., and is placed on the susceptor 3 and accommodated therein. Next, the Ar gas and the H ₂ gas are supplied from the respective supply sources 33 and 34 into the chamber 2 through the pipe 10, and the pressure is adjusted so that the inside of the chamber 2 has a predetermined pressure.

After the pressure in the chamber 2 is stabilized at a predetermined value, WF ₆ gas and SiH ₄ gas are supplied as source gases for film formation from the respective supply sources 31 and 32 to the shower head 4 through the pipe 10. Both gases introduced into the space Sa from the gas supply port 9 are dispersed and sufficiently mixed by the blocker plate 47, and flow out to the space Sb through the plurality of through holes 47a. At this time, since the blocker plate 47 satisfies the relations shown in the above formulas (3) and (4), the dispersibility and mixing properties of both gases are sufficiently enhanced, and the space portion Sa is changed from the space portion Sa to the space portion Sb. An increase in pressure loss during the transition can be sufficiently suppressed.

WF ₆ gas and S introduced into the space Sb
The mixed gas of the iH ₄ gas flows out below the shower head 4 through the through hole 45 a of the face plate 45, and is supplied onto the wafer 5. At this time, face plate 4
Depending on the hole diameter or the opening ratio of the through-hole 45a of No. 5, both gases can be further dispersed and mixed in the space Sb. At this time, the WF ₆ gas and Si in the space Sa are
The relationship expressed by the formula (1) or (2) between the total pressure value P1 of the H ₄ gas and the total pressure value P2 of the WF ₆ gas and the SiH ₄ gas supplied onto the wafer 5. Holds.

On the other hand, WF ₆ gas and SiH ₄ gas are supplied into the chamber 2, and electric power is supplied to the heater 3 a of the susceptor 3 to heat the wafer 5 via the susceptor 3 to a predetermined temperature. Thereby, the WF ₆ gas reaching the wafer 5 reacts with the SiH ₄ gas (nucleation),
Tungsten silicide (W _x Si _y ) (predetermined compound) is deposited on the wafer 5. After performing the formation of the W _x Si _y film for a predetermined time, for example, about several seconds to about ten seconds,
The supply of the SiH ₄ gas is stopped, and the flow rate of the WF ₆ gas is adjusted. As a result, tungsten (W) is deposited on the W _x Si _y film on the wafer 5.

After the formation (film formation) of the W layer is continued for a predetermined time, the supply of the WF ₆ gas and the SiH ₄ gas is stopped, and the film formation is completed. Next, if necessary, the WF ₆ gas and the SiH ₄ gas remaining in the chamber 2 are purged with an Ar gas, and then the wafer 5 on which the W _x Si _y layer and the W layer are formed is formed.
The (semiconductor device) is carried out of the chamber 2.

According to the CVD apparatus 1 configured as described above and the method of manufacturing a semiconductor device using the same, the through hole 47 a of the blocker plate 47 and the face plate 45
At least one of the through holes 45a of the formula (3)
And the relationship represented by the formula (4) is satisfied, whereby the WF ₆ gas and the SiH ₄ gas from the gas supply system 30 satisfy the relationship represented by the formula (1) or the formula (2). Since the two gases are supplied into the chamber 2, the two gases are sufficiently dispersed and mixed, and the reaction of the two gases in the shower head 4 is sufficiently suppressed.

Accordingly, it is possible to prevent the concentration ratio of the two gases reaching the wafer 5 from changing to an inconvenient extent as compared with the concentration ratio of the two gases supplied from the gas supply system 30. In other words, the balance between the concentration ratios of the two gases can be suitably maintained. Therefore, the composition ratio of tungsten silicide (W _x Si _y ) generated during nucleation is expressed as W
It can be ensured that the desired composition ratio is suitable for forming the layer. As a result, the crystal structure of W _x Si _y layer can occupy not desired suitable construction, it is sufficiently possible to reduce the residual stress of the W _x Si _y layer and W layer. Thereby, W
_x Si _y layer and W degradation or the film properties of the formed wiring layers from layer can sufficiently suppress the deterioration, it is possible to suppress the increase of stress and resistivity of the wiring layer.

Further, since the reaction between the WF ₆ gas and the SiH ₄ gas in the space portions Sa and Sb in the shower head 4 can be sufficiently suppressed, the generation of particles such as crystalline particles due to the reaction products of the two. Can also be prevented sufficiently. In order to prevent the generation of particles, WF
It is not necessary to adjust the ratio of the supply amounts of the ₆ gas and the SiH ₄ gas, or to adjust the timing of supplying them into the chamber 2 or to cool the shower head 4 to lower the temperature. Therefore, the labor involved in such an operation can be saved, so that the operability and the controllability of the apparatus, and further, the processing efficiency can be improved.

Further, since the reaction between the two gases in the showerhead 4 is sufficiently suppressed, the reaction products are deposited on the blocker plate 47 and the like in the showerhead 4 and the through holes 47a are easily blocked. Can be sufficiently prevented. As a result, an increase in pressure loss due to the blocker plate 47 or the like is extremely unlikely to be promoted. Therefore, deterioration or deterioration of the film characteristics of the wiring layer formed of the W _x Si _y layer and the W layer formed on the wafer 5 can be further suppressed, and the stress and the resistivity of the wiring layer can be further suppressed from increasing. Moreover, since the through holes 47a are hard to be closed, the blocker plate 4
The frequency of replacing members such as 7 can be reduced.

Further, since the surface (that is, the inner surface) of the base plate 43 facing the blocker plate 47 is substantially a smooth surface, the gas supply port 9 can be provided as compared with the case where, for example, an uneven portion or the like is provided. There is an advantage that the pressure loss in the space Sa of the WF ₆ gas and the SiH ₄ gas introduced from the air can be reduced. Therefore, the reaction between the two gases in the space Sa can be further suppressed. Therefore, particles can be further reduced and the wafer 5
Deterioration or deterioration of the film characteristics of the wiring layer composed of the W _x Si _y layer and the W layer formed thereon can be further suppressed.

[0056]

EXAMPLES Hereinafter, specific examples according to the present invention will be described, but the present invention is not limited to these examples.

<Embodiment 1> A structure similar to that of the CVD apparatus 1 shown in FIG.
And the gap between the lower surface of the face plate 45 and the upper surface of the susceptor 3 is 400 mm.
Mils (approximately 10.2 mm) CVD equipment (Applie
d Materials manufactured by CENTURA (registered trademark) Main Frame, Wx
(Based on Z + chamber). This CVD
While the pressure in the chamber 2 of the apparatus was reduced, an 8-inch Si wafer having a via and a 60-nm-thick TiN layer formed thereon was housed in the chamber 2.

In this state, WF ₆ gas,
A nucleation step was performed by supplying SiH ₄ gas, Ar gas, and H ₂ gas to form a 50 nm thick W _x Si _y layer on the wafer. The film forming conditions at this time are shown below.・ WF ₆ gas flow rate: 20 sccm (cm ³ / min; the same applies hereinafter) ・ SiH ₄ gas flow rate: 5, 10, 15, 20, 30 sc
cm · Ar gas flow rate: 2800 sccm · H ₂ Gas flow rate: 1000 sccm · film formation temperature: 440 ° C.

At this time, the space Sa of the shower head 4 is
When the gas pressure (corresponding to P1) inside the chamber and the gas pressure (P2) inside the chamber 2 and outside the shower head 4 were measured, both were 30 Torr (4 kPa).

Next, the supply of the SiH ₄ gas is stopped, and W _x S
On the i _y layer, a W layer having a thickness of 350 nm was formed (Via fill) under the following film forming conditions to obtain a semiconductor device in which a wiring layer composed of the W layer was formed.・ WF ₆ gas flow rate: 150 sccm ・ Ar gas flow rate: 1200 sccm ・ H ₂ gas flow rate: 500 sccm ・ Film forming temperature: 440 ° C.

<Embodiment 2> In the CVD apparatus, the distance between the lower surface of the face plate 45 and the upper surface of the susceptor 3 is 700 m.
A semiconductor device having a wiring layer formed of a W layer was obtained in the same manner as in Example 1 except that the ils (17.8 mm) was used. In the nucleation step, the gas pressure (corresponding to P1) in the space Sa of the shower head 4 and the gas pressure (P2) in the chamber 2 and outside the shower head 4 were measured.
Torr (4 kPa).

<Comparative Example 1> A blocker plate having a through hole having a hole diameter φ of 0.014 mm or 0.016 mm (half the hole diameter of Example 1) was used, and a base plate around a gas supply port was used. A semiconductor device having a wiring layer formed of a W layer was obtained in the same manner as in Example 1 except that a CVD device having a convex shape (convex with respect to the space portion Sa) was used. In the nucleation step, the gas pressure (corresponding to P1) in the space Sa of the shower head and the gas pressure (P2) in the chamber and outside the shower head were measured.
6 Torr (4.8 kPa) and P2 is 30 Torr
r (4 kPa).

<Residual Stress Measurement Test> Examples 1 and 2
In addition, with respect to the semiconductor device obtained in Comparative Example 1, the residual stress (internal stress) of the W layer was measured. FIG. 2 is a graph showing the measurement results of the residual stress of the W layer of the semiconductor devices obtained in Examples 1 and 2 and Comparative Example 1. In the figure, curve L
0, L1, and L2 are reference lines indicating the results of Comparative Example 1, Example 1, and Example 2, respectively.

FIG. 2 shows that the CVD apparatus 1 according to the present invention and the W formed in Examples 1 and 2 using the method according to the present invention.
It was found that the residual stress of the layer was significantly smaller than that of the W layer formed in Comparative Example 1 under the same SiH ₄ gas flow rate. In Comparative Example 1, the residual stress exceeded 500 MPa irrespective of the flow rate of the SiH ₄ gas, whereas in Example 1, the residual stress was 0 (depending on the flow rate ratio between the WF ₆ gas and the SiH ₄ gas). Zero). From these, it is understood that the present invention can sufficiently reduce the residual stress of the W layer.

<Resistance Measurement Test> With respect to the semiconductor devices obtained in Examples 1 and 2 and Comparative Example 1, the resistivity of the W layer was measured. FIG. 3 is a graph showing the measurement results of the resistivity of the W layer of the semiconductor devices obtained in Examples 1 and 2 and Comparative Example 1. In the figure, curves L10, L11, L12 are reference lines connecting the results (data) of Comparative Example 1, Example 1, and Example 2, respectively.

FIG. 3 shows that the CVD apparatus 1 according to the present invention and the W formed in Examples 1 and 2 using the method according to the present invention.
No significant difference in the resistivity of the layer from that of Comparative Example 1 was observed until the flow rate of the SiH ₄ gas was 20 sccm (the fluctuation range of the resistivity was 5 μΩ · cm or less). In contrast, SiH
_{(4) When the} gas flow rate is 30 sccm, the resistivity of the W layer formed in Examples 1 and 2 is significantly reduced as compared with Comparative Example 1; In the example, it was found that the resistivity was reduced by about 200 to 500 μΩ · cm (note the vertical scale in the figure).

From these results, according to the present invention, WF
It has been found that the resistivity of the W layer is significantly reduced under a predetermined flow ratio condition between the ₆ gas flow rate and the SiH ₄ gas flow rate. Further, the resistivity greatly depends on the crystallinity of the W layer, and considering that the crystallinity greatly depends on the quality of the W _x Si _y layer as the underlayer, according to the present invention,
It is understood that a high quality W _x Si _y layer can be obtained as compared with the related art.

<Evaluation Test of Particle Generation> Example 1
And 2 and each wafer processing according to Comparative Example 1,
The measurement was continuously performed on a plurality of and the same number of wafers, and the weight of the blocker plate before and after the measurement was measured.
FIG. 4 is a graph showing the weight increase before and after the treatment of the blocker plate of the CVD apparatus used in Examples 1 and 2 and Comparative Example 1, respectively. In the figure, graphs R0, R1, R2
Indicates the results of Comparative Example 1, Examples 1 and 2, respectively.

FIG. 4 shows that the weight of the blocker plate after the treatment of Comparative Example 1 was increased by 0.9 mg as compared with that before the treatment. This is probably because the WF ₆ gas and the SiH ₄ gas undergo a gas phase reaction in the shower head, and the reaction product adheres or accumulates on the blocker plate. In contrast, the blocker plate 47 after the treatment of Examples 1 and 2 had a weight increase of 0.6 mg and only 0.2 mg, respectively.

From these results, according to the present invention, WF
It has been confirmed that the gas phase reaction between the ₆ gas and the SiH ₄ gas in the shower head 4 can be sufficiently suppressed. In addition, since reaction products adhering or accumulating on the blocker plate 47 are reduced, particles generated by such adhering substances or deposits as a particle source can be sufficiently reduced.

[0071]

As described above, according to the vapor deposition method and apparatus of the present invention and the method of manufacturing a semiconductor device and the apparatus of the present invention, it is possible to sufficiently suppress the generation of particles when forming a wiring layer on a substrate. In addition to the above, it is possible to form a wiring on the substrate in which stress and an increase in resistivity are sufficiently suppressed.

[Brief description of the drawings]

FIG. 1 is a configuration diagram (partial cross section) schematically showing a preferred embodiment of a semiconductor device manufacturing apparatus according to the present invention which also serves as a vapor deposition apparatus according to the present invention.

FIG. 2 is a graph showing measurement results of residual stress in a W layer of the semiconductor devices obtained in Examples 1 and 2 and Comparative Example 1.

FIG. 3 is a graph showing the measurement results of the resistivity of the W layer of the semiconductor devices obtained in Examples 1 and 2 and Comparative Example 1.

FIG. 4 is a graph showing an increase in weight of a blocker plate of a CVD apparatus used in Examples 1 and 2 and Comparative Example 1 before and after processing.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... CVD apparatus (vapor deposition apparatus, semiconductor device manufacturing apparatus), 2 ... chamber, 30 ... gas supply system, 3 ... susceptor (substrate support part), 4 ... shower head (gas distribution part),
5 wafer (substrate, semiconductor substrate), 9 gas supply port, 3
1 ... WF ₆ gas supply source (first gas supply source), 32 ... S
iH ₄ gas supply source (second gas supply source), 43: base plate (cover), 45: face plate (perforated plate), 45a, 47a: through hole, 47: blocker plate (perforated plate), Sa, Sb ... space.

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Masahiro Morimoto 14-3 Shinizumi, Narita-shi, Chiba Applied Materials Japan Co., Ltd. (72) Inventor Toshihiko Nishiyama 14-3 Shinizumi, Narita-shi, Chiba Nogedaira Industrial Park Applied Materials Japan Co., Ltd. (72) Inventor Mamiko Miyanaga 14-3 Shinsen, Narita-shi, Chiba Applied Materials Japan Co., Ltd. (72) Inventor Hiroyuki Makizaki Narita-shi, Chiba 14-3 Shinizumi Nogedaira Industrial Park Applied Materials Japan Co., Ltd. F-term (reference) 4K030 AA04 AA05 AA06 AA17 BA20 BA35 BA38 BB12 CA04 EA04 FA10 JA01 JA07 JA09 KA08 LA15 4M104 BB18 BB30 DD44 DD45 HH16 HH20

Claims (12)

[Claims] 1. A gas phase deposition method comprising: supplying a plurality of types of gases onto a substrate through at least one perforated plate having a plurality of through holes to deposit a predetermined compound on the substrate; (1); P1 / P2 ≦ 1.15 (1), or the following equation (2): P1-P2 ≦ 0.7 (2), P1: the most upstream gas in the flow path of the plurality of types of gases Pressure value (kPa) of the plurality of types of gases flowing into the perforated plate located on the side of the side, P2: the plurality of types of gases flowing out of the perforated plate positioned at the most downstream side in the flow paths of the plurality of types of gases. A gas phase deposition method comprising: supplying the plurality of types of gases onto the substrate so as to satisfy a relationship represented by a total pressure value of a gas (kPa). 2. The vapor-phase deposition method according to claim 1, wherein at least one of the perforated plates has the following formula (3); 0.01 ≦ φ ≦ 0.10 (3), φ: the at least one perforated plate. And the following formula (4): 1 ≦ K ≦ 40 (4), K: aperture ratio of the through hole in the at least one perforated plate ( %), Those that satisfy the relationship represented by
The method of claim 1, wherein: 3. The vapor-phase deposition method according to claim 1, wherein the plurality of types of gases are provided on a lid portion of the perforated plate facing the most upstream side of the perforated plate in the flow path of the plurality of types of gases. 3. The gas according to claim 1, wherein the gas flows into the perforated plate from a gas supply port provided, and the lid has a surface facing the perforated plate forming a substantially smooth surface. 4. Phase deposition method. 4. The method according to claim 1, wherein a gas composed of a compound containing a tungsten atom and a gas composed of a compound containing a silicon atom are supplied to the substrate as the plurality of types of gases. The vapor phase deposition method according to any one of claims 1 to 3. 5. A vapor-phase deposition apparatus for depositing a predetermined compound on a substrate, comprising: a gas supply port through which a plurality of types of gases are supplied;
A chamber provided with a substrate supporter on which the substrate is supported; and at least one space disposed opposite to the substrate supporter so as to define at least one space communicating with the gas supply port. A gas distribution unit having a perforated plate, wherein the gas distribution unit is provided so as to satisfy the relationship represented by the above formula (1) or the above formula (2). Vapor deposition equipment. 6. The method according to claim 1, wherein at least one of the perforated plates is provided so as to satisfy a relationship represented by the above formulas (3) and (4). Item 6. A vapor deposition apparatus according to Item 5. 7. The gas distribution unit is disposed to face a perforated plate located on the most upstream side in the flow path of the plurality of types of gas among the perforated plates, and is provided with the gas supply port. The vapor phase deposition apparatus according to claim 5, further comprising a cover, wherein the surface of the cover facing the perforated plate forms a substantially smooth surface. 8. A first gas supply means for supplying a gas comprising a compound containing a tungsten atom and connected to the gas distribution section.
And a second gas supply source connected to the gas distribution unit and configured to supply a gas made of a compound containing a silicon atom. A vapor deposition apparatus according to claim 1. 9. A method for manufacturing a semiconductor device having a conductive layer, wherein the predetermined compound is formed on a semiconductor substrate as the base by using the vapor deposition method according to claim 1. Forming a compound having conductivity as a semiconductor device. 10. A semiconductor device in which a plurality of gases are supplied onto a semiconductor substrate through at least one perforated plate having a plurality of through holes, and a conductive layer made of a conductive compound is formed on the semiconductor substrate. Wherein the plurality of types of gases are supplied onto the semiconductor substrate so as to satisfy the relationship represented by the above formula (1) or the above formula (2). Manufacturing method. 11. A manufacturing apparatus for a semiconductor device having a conductive layer, comprising: the vapor deposition apparatus according to claim 5; and the chamber forming the vapor deposition apparatus. Is a device for manufacturing a semiconductor device, wherein a semiconductor substrate is accommodated as the base. 12. An apparatus for manufacturing a semiconductor device having a conductive layer, comprising: a gas supply port through which a plurality of types of gases are supplied;
A chamber provided with a base support for supporting the semiconductor substrate; and at least one porous member opposed to the base support so as to define at least one space communicating with the gas supply port. An apparatus for manufacturing a semiconductor device, comprising: a plate; and a gas distribution unit provided so as to satisfy a relationship represented by the above formula (1) or the above formula (2).