U.S. patent application number 16/902382 was filed with the patent office on 2020-10-01 for master alloy for sputtering target and method for producing sputtering target.
The applicant listed for this patent is JX Nippon Mining & Metals Corporation. Invention is credited to Takayuki Asano, Kunihiro Oda.
Application Number | 20200308692 16/902382 |
Document ID | / |
Family ID | 1000004896964 |
Filed Date | 2020-10-01 |
United States Patent
Application |
20200308692 |
Kind Code |
A1 |
Asano; Takayuki ; et
al. |
October 1, 2020 |
Master Alloy for Sputtering Target and Method for Producing
Sputtering Target
Abstract
Provided is a master alloy for a sputtering target, wherein,
when elements constituting the master alloy are following X1, X2,
Y1, Y2, Y2, and Y3; specifically, where X1 is one or two types of
Ta or W; X2 is at least one type of Ru, Mo, Nb or Hf; Y1 is one or
two types of Cr or Mn; Y2 is one or two types of Co or Ni; and Y3
is one or two types of Ti or V, the master alloy comprises any one
combination of X1-Y1, X1-Y2, X1-Y3, X2-Y1, and X2-Y2 of the
foregoing constituent elements. This consequently yields superior
effects of being able to obtain a sintered sputtering target with
few defects and having a high-density and uniform alloy
composition, and, by using this target, to realize the deposition
of an alloy barrier film with uniform quality and few particles at
a high speed.
Inventors: |
Asano; Takayuki; (Ibaraki,
JP) ; Oda; Kunihiro; (Ibaraki, JP) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
JX Nippon Mining & Metals Corporation |
Tokyo |
|
JP |
|
|
Family ID: |
1000004896964 |
Appl. No.: |
16/902382 |
Filed: |
June 16, 2020 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
15515457 |
Mar 29, 2017 |
10704137 |
|
|
PCT/JP2015/077249 |
Sep 28, 2015 |
|
|
|
16902382 |
|
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|
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
C22C 14/00 20130101;
C22C 19/03 20130101; C22C 27/02 20130101; C22C 27/04 20130101; C22C
27/06 20130101; C22C 19/07 20130101; H01J 37/3426 20130101; C23C
14/3414 20130101; C22C 5/04 20130101; C23C 14/165 20130101; C22C
1/045 20130101; C22C 22/00 20130101; C22C 27/00 20130101 |
International
Class: |
C23C 14/34 20060101
C23C014/34; C22C 27/00 20060101 C22C027/00; C22C 27/02 20060101
C22C027/02; C22C 27/04 20060101 C22C027/04; C22C 27/06 20060101
C22C027/06; C22C 14/00 20060101 C22C014/00; C22C 22/00 20060101
C22C022/00; C22C 19/07 20060101 C22C019/07; C22C 5/04 20060101
C22C005/04; C22C 19/03 20060101 C22C019/03; C22C 1/04 20060101
C22C001/04; C23C 14/16 20060101 C23C014/16; H01J 37/34 20060101
H01J037/34 |
Foreign Application Data
Date |
Code |
Application Number |
Sep 30, 2014 |
JP |
2014-201063 |
Claims
1. A master alloy for a sputtering target, wherein, when elements
constituting the master alloy are following X1, Y1, Y2, and Y3;
specifically, where: X1 is Ta; Y1 is one or two types of Cr or Mn;
Y2 is one or two types of Co or Ni; and Y3 is one or two types of
Ti or V, the master alloy comprises any one combination of X1-Y1,
X1-Y2, and X1-Y3 of the foregoing constituent elements.
2. The master alloy for a sputtering target according to claim 1,
wherein a composition ratio of the Y1, Y2, or Y3 falls within a
range of 50.0 to 80.0 at % of an entire composition constituting
the master alloy.
3. The master alloy for a sputtering target according to claim 2,
wherein X1 as one constituent metal constituting the master alloy
and Y1, Y2, or Y3 as another constituent metal constituting the
master alloy form an intermetallic compound or a complete solid
solution.
4. The master alloy for a sputtering target according to claim 1,
wherein X1 as one constituent metal constituting the master alloy
and Y1, Y2, or Y3 as another constituent metal constituting the
master alloy form an intermetallic compound or a complete solid
solution.
5. A method of producing a sputtering target, wherein the master
alloy for a sputtering target according to claim 1 is pulverized,
and mixed with a powder composed of the X1, and the mixed powder is
sintered to obtain a sputtering target material for a barrier
metal.
6. The method of producing a sputtering target according to claim
5, wherein the mixing is performed so that a composition of Y1, Y2,
or Y3 constituting the master alloy falls within a range of 0.1 to
40.0 at %, and the mixed powder is sintered.
7. A sputtering target in which elements constituting the
sputtering target are selected from X1, Y1, Y2, and Y3, where X1 is
Ta, Y1 is one or two types of Cr or Mn, Y2 is one or two types of
Co or Ni, and Y3 is one or two types of Ti or V, wherein the
sputtering target comprises an alloy of X1-Y1, X1-Y2, or X1-Y3, and
wherein a variation in an in-plane metal composition of Y1, Y2, or
Y3 of the sputtering target is 30% or less.
8. The sputtering target according to claim 7, wherein the
variation in the in-plane metal composition of Y1, Y2, or Y3 of the
sputtering target is 20% or less.
9. The sputtering target according to claim 7, wherein the
variation in the in-plane metal composition of Y1, Y2, or Y3 of the
sputtering target is 15% or less.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of co-pending U.S.
application Ser. No. 15/515,457 which is a 371 National Stage of
International Application No. PCT/JP2015/077249, filed Sep. 28,
2015, which claims the benefit under 35 USC 119 of Japanese
Application No. 2014-201063, filed Sep. 30, 2014.
BACKGROUND
[0002] The present invention relates to a master alloy for a
sputtering target, which enables the deposition of a film with a
uniform quality by achieving uniformity of the composition of the
raw material powder and the internal texture through use of the
master alloy; and a method of producing the sputtering target.
[0003] As a next-generation barrier metal, a combination of alloy
elements comprising the characteristics as an alloy film considered
to be a candidate of a barrier film to be used as a "pair" with a
Cu seed layer, and a production method thereof are being
desired.
[0004] For example, in cases that the foregoing alloy is an alloy
containing X as the main component and further containing a Y
component, it is normally used as an alloy (XY alloy) in which the
Y component falls within a range of 0.1 to 40 at %. In the case of
this kind of alloy, in a combination of X having a high melting
point (for instance, Ta: melting point of 3017.degree. C.) and Y
having a low boiling point (for instance, Mn: boiling point of
2061.degree. C.), Y will become volatilized under the conditions of
melting X, and therefore it is impossible to control the
composition with the melting method.
[0005] When reviewing publications, JP 2003-064473 A describes a
sputtering target capable of depositing an antiferromagnetic
reinforced film having high compositional uniformity, an
antiferromagnetic film, a magnetoresistive sensor comprising said
film, a magnetic head, and a magnetoresistive effect-type random
access memory.
[0006] Specifically, J P 2003-064473 A describes a sputtering
target composed of at least one type of element selected from
nickel, palladium, platinum, cobalt, rhodium, iridium, vanadium,
niobium, tantalum, copper, silver, gold, ruthenium, osmium,
chromium, molybdenum, tungsten and rhenium, and manganese, wherein
the number of defects per a sputtered surface of 1 cm.sup.2 is 10
defects or less.
[0007] Furthermore, J P 2003-064473 A describes an
antiferromagnetic film which is deposited using the foregoing
sputtering target, a magnetoresistive sensor comprising the
foregoing antiferromagnetic film, a tunnel magnetoresistive sensor
comprising the foregoing antiferromagnetic film, a magnetic head
comprising the foregoing magnetoresistive sensor, and a
magnetoresistive effect-type random access memory comprising the
foregoing tunnel magnetoresistive sensor.
[0008] Furthermore, WO 98/22636 describes a sputtering target
composed of at least one type of R element selected from Ni, Pd,
Pt, Co, Rh, Ir, V, Nb, Ta, Cu, Ag, Au, Ru, Os, Cr, Mo, W and Re,
and Mn, wherein the sputtering target comprises, as at least a part
of the target texture, at least one type selected from an alloy
phase and a compound phase of the R element and Mn; and further
describes an antiferromagnetic film formed by using the foregoing
sputtering target, and a magnetoresistive sensor.
[0009] Furthermore, J P 2000-160332 A describes a sputtering target
composed of at least one type of R element selected from Ni, Pd,
Pt, Co, Rh, Ir, V, Nb, Ta, Cu, Ag, Au, Ru, Os, Cr, Mo, W and Re,
and Mn, wherein the oxygen content in the sputtering target is 1 wt
% or less (including 0). The antiferromagnetic film 3 is obtained
by subjecting this kind of sputtering target to sputter deposition.
Patent Document 3 describes that the antiferromagnetic film 3 is
used, for instance, as an exchange coupled film 2 by being
laminated with a ferromagnetic film 4, and that this kind of
exchange coupled film 2 is used in a magnetoresistive sensor or the
like.
[0010] Nevertheless, all of these Patent Documents encounter the
problem where, in cases where one of the alloy components has a
high melting point and the other component has a low boiling point,
one of the metal components become volatilized upon melting these
components, and the intended alloy composition will undergo a
change and become uncontrollable. But no solution for resolving the
foregoing problem is disclosed.
SUMMARY
[0011] Conventionally, in cases where one of the alloy components
has a high melting point and the other component has a low boiling
point, there is a problem in that one of the metal components
become volatilized when melting is performed to produce an alloy,
and the intended alloy composition will undergo a change and become
uncontrollable. The present invention provides a sputtering target
capable of resolving the foregoing problem and a method of
producing such a sputtering target. Thus, an object of the present
invention is to obtain a sintered sputtering target with few
defects and having a high-density and uniform alloy composition,
and, by using this target, to realize the deposition of an alloy
barrier film with uniform quality and few particles at a high
speed.
[0012] In order to achieve the foregoing object, as a result of
intense study, the present inventors discovered that, by using a
master alloy, it is possible to cause the composition of the raw
material powder and the internal texture to be uniform, and realize
the deposition of a film with a uniform quality.
[0013] Based on the foregoing discovery, the present invention
provides the following invention, namely, a master alloy for a
sputtering target, wherein, when elements constituting the master
alloy are following X1, X2, Y1, Y2, Y2, and Y3; specifically,
where: X1 is one or two types of Ta or W; X2 is at least one type
of Ru, Mo, Nb or Hf; Y1 is one or two types of Cr or Mn; Y2 is one
or two types of Co or Ni; and Y3 is one or two types of Ti or V,
the master alloy comprises any one combination of X1-Y1, X1-Y2,
X1-Y3, X2-Y1, and X2-Y2 of the foregoing constituent elements. A
composition ratio of the Y1, Y2, or Y3 in the master alloy for a
sputtering target as described above may fall within a range of
50.0 to 80.0 at % of an entire composition constituting the master
alloy. In addition, X1 or X2 as one constituent metal constituting
the master alloy and Y1, Y2, or Y3 as another constituent metal
constituting the master alloy may form an intermetallic compound or
a complete solid solution.
[0014] In addition, a method of producing a sputtering target is
provided, wherein the master alloy for a sputtering target as
described above is pulverized, and mixed with a powder composed of
the X1 or X2, and the mixed powder is sintered to obtain a
sputtering target material for a barrier metal. The method of
producing a sputtering target may include mixing such that a
composition of Y1, Y2, or Y3 constituting the master alloy falls
within a range of 0.1 to 40.0 at %, and the mixed powder is
sintered.
[0015] The sputtering target may have a variation in an in-plane
metal composition of Y1, Y2, or Y3 of the sputtering target of 30%
or less, a variation in an in-plane metal composition of Y1, Y2, or
Y3 of the sputtering target of 20% or less, or a variation in an
in-plane metal composition of Y1, Y2, or Y3 of the sputtering
target of 15% or less.
[0016] Accordingly, the present invention provides a master alloy
for a sputtering target, which enables the deposition of a film
with a uniform quality by achieving uniformity of the composition
of the raw material powder and the internal texture through use of
the master alloy; and a method of producing the sputtering target.
The present invention consequently yields superior effects of being
able to obtain a sintered sputtering target with few defects and
having a high-density and uniform alloy composition, and, by using
this target, to realize the deposition of an alloy barrier film
with uniform quality and few particles at a high speed.
DETAILED DESCRIPTION
[0017] As described above, the present invention provides a master
alloy for a sputtering target, wherein, when elements constituting
the master alloy are following X1, X2, Y1, Y2, Y2, and Y3;
specifically, where:
[0018] X1 is one or two types of Ta or W;
[0019] X2 is at least one type of Ru, Mo, Nb or Hf;
[0020] Y1 is one or two types of Cr or Mn;
[0021] Y2 is one or two types of Co or Ni; and
[0022] Y3 is one or two types of Ti or V,
[0023] the master alloy comprises any one combination of X1-Y1,
X1-Y2, X1-Y3, X2-Y1, and X2-Y2 of the foregoing constituent
elements. The master alloy having the foregoing composition can be
prepared with the melting method.
[0024] When providing the explanation by collectively referring to
X1 and X2 above as "X", and collectively referring to Y1, Y2, and
Y3 above as "Y", the boiling point will decrease as the composition
of Y increases, and therefore a master alloy having a composition
of a high Y content can be melted under conditions of suppressing
the volatilization of Y.
[0025] Furthermore, the melted master alloy can be pulverized; and,
by selecting a compositional range of 50.0 to 80.0 at % Y, in which
Y can exist as an intermetallic compound phase without including a
composition of Y itself, for minimizing the reaction during
sintering after mixing the pulverized powder with an X powder for
controlling the composition, it is possible to obtain a raw
material powder for controlling the composition.
[0026] Moreover, by mixing the pulverized master alloy and a metal
powder and sintering the mixed powder, it is possible to produce a
TG having a prescribed composition and in which the in-plane
composition is uniform.
[0027] It is thereby possible to obtain a target with few defects
and having a high-density and uniform alloy composition. By using
this target, it is possible to realize the deposition of an alloy
barrier film of an XY component with uniform quality and few
particles at a high speed. Moreover, it is also possible to produce
a target having a size of 300 mm.
[0028] The composition ratio of Y1, Y2, or Y3 above preferably
falls within a range of 50.0 to 80.0 at % of the entire composition
constituting the master alloy. This is based on the reason that as
the composition approaches X, the melting point will generally
increase and the Y alloy will become volatilized, and, as the
composition approaches Y, a Y monophase region will become
generated.
[0029] Preferably, X1 or X2 as one constituent metal constituting
the master alloy and Y1, Y2, or Y3 as another constituent metal
constituting the master alloy form an intermetallic compound or a
complete solid solution. This is effective and important for
causing the target texture to be uniform.
[0030] Upon producing a sputtering target, the master alloy for a
sputtering target is pulverized, and mixed with a powder composed
of the X1 or X2, and the mixed powder is sintered to obtain a
sputtering target material for a barrier metal. It is thereby
possible to obtain a target with few defects and having a
high-density and uniform alloy composition.
[0031] Preferably, the mixing is performed so that a composition of
Y1, Y2, or Y3 constituting the master alloy falls within a range of
0.1 to 40.0 at %, and the mixed powder is sintered.
[0032] The variation in an in-plane metal composition of Y1, Y2, or
Y3 of the sputtering target is 30% or less, preferably 20% or less,
and more preferably 15% or less.
[0033] Note that, upon measuring the variation, the composition
measurement is performed at arbitrary in-plane points of the target
(for instance, 9 locations on cross lines in a plane of the
target), and "the value of (maximum value-minimum value)/maximum
value.times.100%" may be defined as being the variation.
EXAMPLES
[0034] The Examples and Comparative Examples of the present
invention are now explained. Note that these Examples and
Comparative Examples are described for facilitating the
understanding of the present invention, and it should be understood
that the subject matter of this invention is not limited by these
Examples and Comparative Examples.
Example 1
[0035] In Example 1, a material having a composition of W-75 at % V
was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
V would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-26 at % V was prepared.
[0036] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (V
component) was 2.6%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are shown in Table 1.
TABLE-US-00001 TABLE 1 Intended composition Intended Actual of
Master composition composition master alloy Variation in X Y Press
Melting Production alloy melting target X Y (at %) (at %)
temperature temperature method (at %) temperature composition
Example 1 W V 26 26 1550.degree. C. -- Master alloying 75
2200.degree. C. 2.6% Example 2 W Ti 10 10.1 1550.degree. C. --
Master alloying 66 1800.degree. C. 2.4% Example 3 W Co 1 1.4
1350.degree. C. -- Master alloying 57 1600.degree. C. 4.9% Example
4 W Ni 19 19.2 1350.degree. C. -- Master alloying 58 1600.degree.
C. 8.5% Example 5 W Cr 21 21.4 1550.degree. C. -- Master alloying
73 2000.degree. C. 3.1% Example 6 W Mn 28 27.5 1150.degree. C. --
Master alloying 50 1400.degree. C. 1.5% Example 7 Ta V 6 6.3
1550.degree. C. -- Master alloying 71 2000.degree. C. 1.0% Example
8 Ta Ti 33 32.8 1550.degree. C. -- Master alloying 55 1800.degree.
C. 8.8% Example 9 Ta Co 37 37.4 1200.degree. C. -- Master alloying
60 1700.degree. C. 1.7% Example 10 Ta Ni 11 10.5 1250.degree. C. --
Master alloying 52 1600.degree. C. 7.6% Example 11 Ta Cr 3 2.9
1550.degree. C. -- Master alloying 63 1800.degree. C. 9.7% Example
12 Ta Mn 151 14.7 1100.degree. C. -- Master alloying 61
1400.degree. C. 9.9% Example 13 Mo Co 38 38.1 1250.degree. C. --
Master alloying 59 1500.degree. C. 5.5% Example 14 Mo Ni 30 30.2
1250.degree. C. -- Master alloying 72 1500.degree. C. 1.1% Example
15 Mo Cr 5 5.4 1550.degree. C. -- Master alloying 66 1900.degree.
C. 4.0% Example 16 Mo Mn 21 21.2 1100.degree. C. -- Master alloying
75 1400.degree. C. 4.9% Example 17 Nb Co 18 17.5 1150.degree. C. --
Master alloying 67 1500.degree. C. 5.8% Example 18 Nb Ni 3 3.2
1100.degree. C. -- Master alloying 57 1500.degree. C. 10.0% Example
19 Nb Cr 21 20.5 1550.degree. C. -- Master alloying 71 1700.degree.
C. 7.9% Example 20 Nb Mn 18 17.8 1100.degree. C. -- Master alloying
75 1300.degree. C. 2.2% Example 21 Ru Cr 13 12.6 1550.degree. C. --
Master alloying 65 1700.degree. C. 3.1% Example 22 Ru Mn 11 11.2
1200.degree. C. -- Master alloying 50 1400.degree. C. 4.4% Example
23 Hf Cr 14 13.8 1500.degree. C. -- Master alloying 53 1800.degree.
C. 9.3% Example 24 Hf Mn 8 8.2 1100.degree. C. -- Master alloying
56 1400.degree. C. 1.6% Comparative W V 26 -- -- Not Melting method
-- -- -- Example 1 producible Comparative W Ti 10 -- -- Not Melting
method -- -- -- Example 2 producible Comparative W Co 1 -- -- Not
Melting method -- -- -- Example 3 producible Comparative W Ni 19 --
-- Not Melting method -- -- -- Example 4 producible Comparative W
Cr 21 -- -- Not Melting method -- -- -- Example 5 producible
Comparative W Mn 28 -- -- Not Melting method -- -- -- Example 6
producible Comparative Ta V 6 3.2 -- 3100.degree. C. Melting method
-- -- 42.5% Example 7 Comparative Ta Ti 33 14.6 -- 3100.degree. C.
Melting method -- -- 39.7% Example 8 Comparative Ta Co 37 -- -- Not
Melting method -- -- -- Example 9 producible Comparative Ta Ni 11
-- -- Not Melting method -- -- -- Example 10 producible Comparative
Ta Cr 3 -- -- Not Melting method -- -- -- Example 11 producible
Comparative Ta Mn 15 -- -- Not Melting method -- -- -- Example 12
producible Comparative Mo Co 38 32.3 -- 2700.degree. C. Melting
method -- -- 16.2% Example 13 Comparative Mo Ni 30 21.1 --
2700.degree. C. Melting method -- -- 26.8% Example 14 Comparative
Mo Cr 5 -- -- Not Melting method -- -- -- Example 15 producible
Comparative Mo Mn 21 -- -- Not Melting method -- -- -- Example 16
producible Comparative Nb Co 18 14.1 -- 2500.degree. C. Melting
method -- -- 32.0% Example 17 Comparative Nb Ni 3 1.7 --
2500.degree. C. Melting method -- -- 41.5% Example 18 Comparative
Nb Cr 21 9.2 -- 2500.degree. C. Melting method -- -- 31.6% Example
19 Comparative Nb Mn 18 -- -- Not Melting method -- -- -- Example
20 producible Comparative Ru Cr 13 9.4 -- 2400.degree. C. Melting
method -- -- 28.3% Example 21 Comparative Ru Mn 11 -- -- Not
Melting method -- -- -- Example 22 producible Comparative Hf Cr 14
10 -- 2300.degree. C. Melting method -- -- 29.6% Example 23
Comparative Hf Mn 8 -- -- Not Melting method -- -- -- Example 24
producible
Example 2
[0037] In Example 2, a material having a composition of W-66 at %
Ti was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
Ti would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-10.1 at % Ti was prepared.
[0038] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Ti
component) was 2.4%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 3
[0039] In Example 3, a material having a composition of W-57 at %
Co was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
Co would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-1.4 at % Co was prepared.
[0040] The press temperature during sintering was set to
1350.degree. C. Variation of the master alloy composition (Co
component) was 4.9%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 4
[0041] In Example 4, a material having a composition of W-58 at %
Ni was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
Ni would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-19.2 at % Ni was prepared.
[0042] The press temperature during sintering was set to
1350.degree. C. Variation of the master alloy composition (Ni
component) was 8.5%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 5
[0043] In Example 5, a material having a composition of W-73 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
Cr would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-21.4 at % Cr was prepared.
[0044] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Cr
component) was 3.1%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 6
[0045] In Example 6, a material having a composition of W-50 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a W powder was further
added thereto to adjust the composition so that the total amount of
Mn would fall within a range of 0.1 to 40.0 at %, the obtained
powder was subject to vacuum sintering, and a target composed of a
material having a composition of W-27.5 at % Mn was prepared.
[0046] The press temperature during sintering was set to
1150.degree. C. Variation of the master alloy composition (Mn
component) was 1.5%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 7
[0047] In Example 7, a material having a composition of Ta-71 at %
V was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of V would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-6.3 at % V was
prepared.
[0048] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (V
component) was 1.0%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 8
[0049] In Example 8, a material having a composition of Ta-55 at %
Ti was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of Ti would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-32.8 at % Ti was
prepared.
[0050] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (V
component) was 8.8%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 9
[0051] In Example 9, a material having a composition of Ta-60 at %
Co was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of Co would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-37.4 at % Co was
prepared.
[0052] The press temperature during sintering was set to
1200.degree. C. Variation of the master alloy composition (Co
component) was 1.7%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 10
[0053] In Example 10, a material having a composition of Ta-52 at %
Ni was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of Ni would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-10.5 at % Ni was
prepared.
[0054] The press temperature during sintering was set to
1250.degree. C. Variation of the master alloy composition (Ni
component) was 7.6%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 11
[0055] In Example 11, a material having a composition of Ta-63 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of Cr would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-2.9 at % Cr was
prepared.
[0056] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Cr
component) was 9.7%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 12
[0057] In Example 12, a material having a composition of Ta-61 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ta powder was
further added thereto to adjust the composition so that the total
amount of Mn would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ta-14.7 at % Mn was
prepared.
[0058] The press temperature during sintering was set to
1100.degree. C. Variation of the master alloy composition (Mn
component) was 9.9%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 13
[0059] In Example 13, a material having a composition of Mo-59 at %
Co was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Mo powder was
further added thereto to adjust the composition so that the total
amount of Co would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Mo-38.1 at % Co was
prepared.
[0060] The press temperature during sintering was set to
1250.degree. C. Variation of the master alloy composition (Co
component) was 5.5%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 14
[0061] In Example 14, a material having a composition of Mo-72 at %
Ni was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Mo powder was
further added thereto to adjust the composition so that the total
amount of Ni would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Mo-30.2 at % Ni was
prepared.
[0062] The press temperature during sintering was set to
1250.degree. C. Variation of the master alloy composition (Ni
component) was 1.1%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 15
[0063] In Example 15, a material having a composition of Mo-66 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Mo powder was
further added thereto to adjust the composition so that the total
amount of Cr would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Mo-5.4 at % Cr was
prepared.
[0064] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Cr
component) was 4.0%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 16
[0065] In Example 16, a material having a composition of Mo-75 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Mo powder was
further added thereto to adjust the composition so that the total
amount of Mn would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Mo-21.2 at % Mn was
prepared.
[0066] The press temperature during sintering was set to
1100.degree. C. Variation of the master alloy composition (Mn
component) was 4.9%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 17
[0067] In Example 17, a material having a composition of Nb-67 at %
Co was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Nb powder was
further added thereto to adjust the composition so that the total
amount of Co would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Nb-17.5 at % Co was
prepared.
[0068] The press temperature during sintering was set to
1150.degree. C. Variation of the master alloy composition (Co
component) was 5.8%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 18
[0069] In Example 18, a material having a composition of Nb-57 at %
Ni was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Nb powder was
further added thereto to adjust the composition so that the total
amount of Ni would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Nb-3.2 at % Ni was
prepared.
[0070] The press temperature during sintering was set to
1100.degree. C. Variation of the master alloy composition (Ni
component) was 10.0%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 19
[0071] In Example 19, a material having a composition of Nb-71 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Nb powder was
further added thereto to adjust the composition so that the total
amount of Cr would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Nb-20.5 at % Cr was
prepared.
[0072] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Ni
component) was 7.9%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 20
[0073] In Example 20, a material having a composition of Nb-75 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Nb powder was
further added thereto to adjust the composition so that the total
amount of Mn would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Nb-17.8 at % Mn was
prepared.
[0074] The press temperature during sintering was set to
1100.degree. C. Variation of the master alloy composition (Mn
component) was 2.2%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 21
[0075] In Example 21, a material having a composition of Ru-65 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ru powder was
further added thereto to adjust the composition so that the total
amount of Cr would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ru-12.6 at % Cr was
prepared.
[0076] The press temperature during sintering was set to
1550.degree. C. Variation of the master alloy composition (Cr
component) was 3.1%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 22
[0077] In Example 22, a material having a composition of Ru-50 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Ru powder was
further added thereto to adjust the composition so that the total
amount of Mn would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Ru-11.2 at % Mn was
prepared.
[0078] The press temperature during sintering was set to
1200.degree. C. Variation of the master alloy composition (Mn
component) was 4.4%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 23
[0079] In Example 23, a material having a composition of Hf-53 at %
Cr was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Hf powder was
further added thereto to adjust the composition so that the total
amount of Cr would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Hf-13.8 at % Cr was
prepared.
[0080] The press temperature during sintering was set to
1500.degree. C. Variation of the master alloy composition (Cr
component) was 9.3%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Example 24
[0081] In Example 24, a material having a composition of Hf-56 at %
Mn was melted to prepare a master alloy, and this master alloy was
pulverized to obtain a powder. Subsequently, a Hf powder was
further added thereto to adjust the composition so that the total
amount of Mn would fall within a range of 0.1 to 40.0 at %, the
obtained powder was subject to vacuum sintering, and a target
composed of a material having a composition of Hf-8.2 at % Mn was
prepared.
[0082] The press temperature during sintering was set to
1100.degree. C. Variation of the master alloy composition (Mn
component) was 1.6%, and the compositional variation was small.
Moreover, the master alloy could be pulverized easily. The results
are similarly shown in Table 1.
Comparative Example 1
[0083] In Comparative Example 1, V was added to W in an amount of
26 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 2
[0084] In Comparative Example 2, Ti was added to W in an amount of
10 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 3
[0085] In Comparative Example 3, Co was added to W in an amount of
1 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 4
[0086] In Comparative Example 4, Ni was added to W in an amount of
19 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 5
[0087] In Comparative Example 5, Cr was added to W in an amount of
21 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 6
[0088] In Comparative Example 6, Mn was added to W in an amount of
28 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 7
[0089] In Comparative Example 7, V was added to Ta in an amount of
6 at %, and an attempt was made to melt the obtained product at
3100.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
42.5%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 8
[0090] In Comparative Example 8, Ti was added to Ta in an amount of
33 at %, and an attempt was made to melt the obtained product at
3100.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
39.7%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 9
[0091] In Comparative Example 9, Co was added to Ta in an amount of
37 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 10
[0092] In Comparative Example 10, Ni was added to Ta in an amount
of 11 at %, and an attempt was made to melt the obtained product
and produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 11
[0093] In Comparative Example 11, Cr was added to Ta in an amount
of 3 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 12
[0094] In Comparative Example 12, Mn was added to Ta in an amount
of 15 at %, and an attempt was made to melt the obtained product
and produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 13
[0095] In Comparative Example 13, Co was added to Mo in an amount
of 38 at %, and an attempt was made to melt the obtained product at
2700.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
16.2%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 14
[0096] In Comparative Example 14, Ni was added to Mo in an amount
of 30 at %, and an attempt was made to melt the obtained product at
2700.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
26.8%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 15
[0097] In Comparative Example 15, Cr was added to Mo in an amount
of 5 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 16
[0098] In Comparative Example 16, Mn was added to Mo in an amount
of 21 at %, and an attempt was made to melt the obtained product
and produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 17
[0099] In Comparative Example 17, Co was added to Nb in an amount
of 18 at %, and an attempt was made to melt the obtained product at
2550.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
32.0%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 18
[0100] In Comparative Example 18, Ni was added to Nb in an amount
of 3 at %, and an attempt was made to melt the obtained product at
2550.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
41.5%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 19
[0101] In Comparative Example 19, Cr was added to Nb in an amount
of 21 at %, and an attempt was made to melt the obtained product at
2550.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
31.6%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 20
[0102] In Comparative Example 20, Mn was added to Nb in an amount
of 18 at %, and an attempt was made to melt the obtained product
and produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 21
[0103] In Comparative Example 21, Cr was added to Ru in an amount
of 13 at %, and an attempt was made to melt the obtained product at
2400.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
28.3%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 22
[0104] In Comparative Example 22, Mn was added to Ru in an amount
of 11 at %, and an attempt was made to melt the obtained product
and produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
Comparative Example 23
[0105] In Comparative Example 23, Cr was added to Hf in an amount
of 14 at %, and an attempt was made to melt the obtained product at
2300.degree. C. and produce an alloy having the same component
composition. In this case, the compositional variation increased to
29.6%, and it was unfit for actual production. The results are
similarly shown in Table 1.
Comparative Example 24
[0106] In Comparative Example 22, Mn was added to Hf in an amount
of 8 at %, and an attempt was made to melt the obtained product and
produce an alloy having the same component composition.
Nevertheless, it was not possible to melt this alloy material and
produce the intended alloy. The results are similarly shown in
Table 1.
[0107] In foregoing Comparative Examples 1 to 24, the elements
shown in Table 1 were respectively added to W, Ta, Mo, Nb, Ru, and
Hf that are high melting point metals, and attempts were made to
melt the obtained product and produce an alloy. However, it is
evident that, in all of these cases, the intended alloy could not
be produced, or the compositional variation increased and it was
unfit for actual production.
[0108] The present invention provides a master alloy for a
sputtering target, which enables the deposition of a film with a
uniform quality by achieving uniformity of the composition of the
raw material powder and the internal texture through use of the
master alloy; and a method of producing the sputtering target. The
present invention consequently yields superior effects of being
able to obtain a sintered sputtering target with few defects and
having a high-density and uniform alloy composition, and, by using
this target, to realize the deposition of an alloy barrier film
with uniform quality and few particles at a high speed. The present
invention is particularly effective in producing a film in which
the compositional variation thereof needs to be suppressed, such as
with a gate film in a semiconductor device.
* * * * *