U.S. patent application number 09/783377 was filed with the patent office on 2001-12-06 for methods of forming aluminum-comprising physical vapor deposition targets; sputtered films; and target constructions.
Invention is credited to Alford, Frank, Ferrasse, Stephane, Li, Jianxing, Segal, Vladimir M..
Application Number | 20010047838 09/783377 |
Document ID | / |
Family ID | 26888912 |
Filed Date | 2001-12-06 |
United States Patent
Application |
20010047838 |
Kind Code |
A1 |
Segal, Vladimir M. ; et
al. |
December 6, 2001 |
Methods of forming aluminum-comprising physical vapor deposition
targets; sputtered films; and target constructions
Abstract
The invention includes a method of forming an
aluminum-comprising physical vapor deposition target. An
aluminum-comprising mass is deformed by equal channel angular
extrusion. The mass is at least 99.99% aluminum and further
comprises less than or equal to about 1,000 ppm of one or more
dopant materials comprising elements selected from the group
consisting of Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu,
Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N,
Nb, Nd, Ni, O, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru,
S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb,
Zn and Zr. After the aluminum-comprising mass is deformed, the mass
is shaped into at least a portion of a sputtering target. The
invention also encompasses a physical vapor deposition target
consisting essentially of aluminum and less than or equal to 1,000
ppm of one or more dopant materials comprising elements selected
from the group consisting of Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd,
Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu,
Mg, Mn, Mo, N, Nb, Nd, Ni, O, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu,
Ra, Rf, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Ti,
Tm, V, W, Y, Yb, Zn and Zr. Additionally, the invention encompasses
thin films.
Inventors: |
Segal, Vladimir M.;
(Veradale, WA) ; Li, Jianxing; (Spokane, WA)
; Alford, Frank; (Veradale, WA) ; Ferrasse,
Stephane; (Veradale, WA) |
Correspondence
Address: |
Shannon Morris
Honeywell International Inc.
Box 2245
101 Columbia Road
Morristown
NJ
07962
US
|
Family ID: |
26888912 |
Appl. No.: |
09/783377 |
Filed: |
February 13, 2001 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
60193354 |
Mar 28, 2000 |
|
|
|
Current U.S.
Class: |
148/437 ;
148/438; 148/439; 148/440; 72/256 |
Current CPC
Class: |
C22F 1/04 20130101; C23C
14/3414 20130101; Y10S 72/70 20130101 |
Class at
Publication: |
148/437 ; 72/256;
148/438; 148/439; 148/440 |
International
Class: |
C22C 021/00; B21C
023/00 |
Claims
1. A method of forming an aluminum-comprising physical vapor
deposition target, comprising: deforming an aluminum-comprising
mass by equal channel angular extrusion, wherein the mass is at
least 99.99% aluminum and further comprises less than or equal to
about 1000 ppm of one or more dopant materials comprising elements
selected from the group consisting of Ac, Ag, As, B, Ba, Be, Bi, C,
Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir,
La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni, O, Os, P, Pb, Pd, Pm, Po, Pr,
Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te,
Ti, Ti, Tm, V, W, Y, Yb, Zn and Zr; after the deforming, shaping
the mass into at least a portion of a physical vapor deposition
target.
2. The method of claim 1 wherein the physical vapor deposition
target is a monolithic target.
3. The method of claim 1 wherein the one or more dopant materials
comprise materials selected from the group consisting of B, Ba, Be,
Ca, Ce, Co, Cr, Dy, Er, Eu, Gd, Ge, Hf, Ho, La, Ni, Nd, Pd, Pm, Pr,
Sb, Sc, Si, Sm, Sr, Tb, Te, Ti, Tm, Y, Yb and Zr.
4. The method of claim 1 wherein the one or more dopant materials
comprise materials selected from the group consisting of Si, Sc, Ti
and Hf.
5. The method of claim 1 wherein the mass consists of aluminum and
from about 10 ppm to about 100 ppm of the one or more dopant
elements.
6. The method of claim 1 wherein the mass consists of Al and from
about 10 ppm to about 100 ppm of one or more of Si, Sc, Ti, and
Hf.
7. The method of claim 1 wherein the mass consists of Al and from
about 10 ppm to about 100 ppm of Hf.
8. The method of claim 1 wherein the mass consists of Al and from
about 10 ppm to about 100 ppm of Ti.
9. The method of claim 1 wherein the mass consists of Al and from
about 10 ppm to about 100 ppm of Sc.
10. The method of claim 1 wherein the mass consists of Al and from
about 10 ppm to about 100 ppm of Si.
11. A method of forming an aluminum-comprising physical vapor
deposition target, comprising: deforming an aluminum-comprising
mass by equal channel angular extrusion; and after the deforming,
shaping the mass into at least a portion of a physical vapor
deposition target, the physical vapor deposition target having an
average grain size less than or equal to 45 microns.
12. The method of claim 11 wherein the mass is formed into an
entirety of the physical vapor deposition target, and further
comprising mounting the mass to a backing plate.
13. The method of claim 11 wherein the mass is at least 99.99%
aluminum and consists of Al and less than 100 ppm of one or more of
Si, Sc, Ti and Hf.
14. The method of claim 11 wherein the mass is at least 99.99%
aluminum, and further comprises greater than 0 ppm and less than or
equal to about 100 ppm of one or more dopant materials comprising
elements selected from the group consisting of Ac, Ag, As, B, Ba,
Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf,
Ho, In, Ir, La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni, O, Os, P, Pb, Pd,
Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr,
Ta, Tb, Te, Ti, Ti, Tm, V, W, Y, Yb, Zn and Zr.
15. The method of claim 11 wherein the mass consists essentially of
aluminum.
16. The method of claim 11 wherein the mass consists essentially of
aluminum, and less than or equal to about 100 ppm of one or more
dopant materials comprising elements selected from the group
consisting of Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu,
Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N,
Nb, Nd, Ni, O, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru,
S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Ti, Tm, V, W, Y, Yb,
Zn and Zr.
17. The method of claim 11 wherein the shaping comprises one or
more of forging and rolling of the aluminum-comprising mass at a
temperature of less than or equal to about 200.degree. C.
18. The method of claim 11 wherein the deforming comprises at least
three extruding steps, each of the at least three extruding steps
comprising passing the mass through two intersecting passages
having approximately equal cross-sections.
19. The method of claim 11 wherein the deforming comprises at least
four extruding steps, each of the at least four extruding steps
comprising passing the mass through two intersecting passages
having approximately equal cross-sections.
20. The method of claim 11 wherein the deforming comprises at least
six extruding steps, each of the at least six extruding steps
comprising passing the mass through two intersecting passages
having approximately equal cross-sections.
21. A physical vapor deposition target consisting essentially of
aluminum and less than or equal to 1000 ppm of one or more dopant
materials comprising elements selected from the group consisting of
Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu,
Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni,
O, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc,
Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb, Zn and Zr;
the physical vapor deposition target having an average grain size
of less than 100 microns.
22. The physical vapor deposition target of claim 21 having an
average grain size of less than or equal to 45 microns.
23. The physical vapor deposition target of claim 21 consisting of
Al and less than 100 ppm of one or more of Si, Sc, Ti; and Hf.
24. The physical vapor deposition target of claim 21 consisting of
Al and from 10 ppm to 100 ppm of one or more of Si, Sc, Ti; and
Hf.
25. The physical vapor deposition target of claim 21 consisting of
Al and from 10 ppm to 100 ppm of Sc; the target having an average
grain size of less than or equal to 45 microns.
26. The physical vapor deposition target of claim 21 consisting of
Al and from 10 ppm to 100 ppm of Si; the target having an average
grain size of less than or equal to 35 microns.
27. The physical vapor deposition target of claim 21 consisting of
Al and from 10 ppm to 100 ppm of Ti.
28. The physical vapor deposition target of claim 21 consisting of
Al and from 10 ppm to 100 ppm of Hf.
29. A film sputtered from a target, the film consisting essentially
of aluminum and less than or equal to 1000 ppm of one or more
dopant materials comprising elements selected from the group
consisting of Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu,
Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N,
Nb, Nd, Ni, O, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru,
S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb,
Zn and Zr.
30. The film of claim 29 consisting of Al and less than 100 ppm of
one or more of Si, Sc, Ti and Hf.
31. The film of claim 29 consisting of Al and from 10 ppm to 100
ppm of one or more of Si, Sc, Ti and Hf.
Description
RELATED APPLICATION DATA
[0001] This application claims priority to U.S. provisional
application Ser. No. 60/193,354, which was filed Mar. 28, 2000.
TECHNICAL FIELD
[0002] The invention pertains to methods of forming
aluminum-comprising physical vapor deposition targets, and to
target constructions. In particular applications, the invention
pertains to methods of utilizing equal channel angular extrusion
(ECAE) to deform an aluminum-comprising mass in forming a physical
vapor deposition (PVD) target for use in the manufacture of flat
panel displays (FPDs), such as, for example, liquid crystal
displays (LCDs).
BACKGROUND OF THE INVENTION
[0003] PVD is a technology by which thin metallic and/or ceramic
layers can be sputter-deposited onto a substrate. Sputtered
materials come from a target, which serves generally as a cathode
in a standard radio-frequency (RF) and/or direct current (DC)
sputtering apparatus. For example, PVD is widely used in the
semiconductor industry to produce integrated circuits.
[0004] A relatively new application for sputtering technologies is
fabrication of FPDs, such as, for example, LCDs. The LCD market has
experienced rapid growth. This trend may accelerate in the next few
years due to the diversified applications of LCDs in, for example
the markets of laptop personal computers (PCs), PC monitors, mobile
devices, cellular phones and LCD televisions.
[0005] Aluminum can be a particularly useful metal in forming LCDs,
and it accordingly can be desired to form aluminum-comprising
physical vapor deposition targets. The targets can contain a small
content (less than or equal to about 100 parts per million (ppm))
of doping elements. The aluminum, with or without small additions
of dopants, is generally desired to be deposited to form a layer of
about 300 nm which constitutes the reflecting electrode of LCD
devices. Several factors are important in sputter deposition of a
uniform layer of aluminum having desired properties for LCD
devices. Such factors including: sputtering rate; thin film
uniformity; and microstructure. Improvements are desired in the
metallurgy of LCD aluminum targets to improve the above-discussed
factors.
[0006] LCD targets are quite large in size, a typical size being
860.times.910.times.19 mm.sup.3, and are expected to become bigger
in the future. Such massive dimensions present challenges to the
development of tooling and processing for fabrication of suitable
aluminum-comprising targets.
[0007] Various works demonstrate that three fundamental factors of
a target can influence sputtering performance. The first factor is
the grain size of the material, i.e. the smallest constitutive part
of a polycrystalline metal possessing a continuous crystal lattice.
Grain size ranges are usually from several millimeters to a few
tenths of microns; depending on metal nature, composition, and
processing history. It is believed that finer and more homogeneous
grain sizes improve thin film uniformity, sputtering yield and
deposition rate, while reducing arcing. The second factor is target
texture. The continuous crystal lattice of each grain is oriented
in a specific way relative to the plane of target surface. The sum
of all the particular grain orientations defines the overall target
orientation. When no particular target orientation dominates, the
texture is considered to be a random structure. Like grain size,
crystallographic texture can strongly depend on the preliminary
thermomechanical treatment, as well as on the nature and
composition of a given metal. Crystallographic textures can
influence thin film uniformity and sputtering rate. The third
factor is the size and distribution of structural components, such
as second phase precipitates and particles, and casting defects
(such as, for example, voids or pores). These structural components
are usually not desired and can be sources for arcing as well as
contamination of thin films.
[0008] In order to improve the manufacture of LCD targets it would
be desirable to accomplish one or more of the following relative to
aluminum-based target materials: (1) to achieve predominate and
uniform grain sizes within the target materials of less than 100
.mu.m; (2) to have the target materials consist of (or consist
essentially of) high purity aluminum (i.e. aluminum of at least
99.99% (4N) purity, and preferably at least 99.999% (5N) purity,
with the percentages being atomic percentages); (3) to keep oxygen
content within the target materials low; and (4) to achieve large
target sizes utilizing the target materials.
[0009] The thermomechanical processes (TMP) used traditionally to
fabricate LCD targets can generally only achieve grain sizes larger
than 200 .mu.m for 5N Al with or without dopants. Such TMP
processes involve the different steps of casting, heat treatment,
forming by rolling or forging, annealing and final fabrication of
the LCD target. Because forging and rolling operations change the
shape of billets by reducing their thickness, practically
attainable strains in today's TMP processes are restricted.
Further, rolling and forging operations generally produce
non-uniform straining throughout a billet.
[0010] The optimal method for refining the structure of high purity
aluminum alloys (such as, for example, 99.9995% aluminum) would be
intensive plastic deformation sufficient to initiate and complete
self-recrystallization at room temperature immediately after cold
working.
[0011] High purity aluminum is typically provided as a cast ingot
with coarse dendrite structures (FIG. 1 illustrates a typical
structure of as-cast 99.9995% aluminum). Forging and/or rolling
operations are utilized to deform the cast ingots into target
blanks. Flat panel display target blanks are optimally to be in the
form of large thin plates. The total strains which can be obtained
for any combination of forging and/or rolling operations can be
expressed as .epsilon.=(1-h/H.sub.0)*100%; where H.sub.0 is an
ingot length, and h is a target blank thickness. Calculations show
that possible thickness reductions for conventional processes range
from about 85% to about 92%, depending on target blank size to
thickness ratio. The thickness reduction defines the strain induced
in a material. Higher thickness reductions indicate more strain,
and accordingly can indicate smaller grain sizes. The conventional
reductions of 85% to 92% can provide static recrystallization of
high purity aluminum (for instance, aluminum having a purity of
99.9995% or greater) but they are not sufficient to develop the
fine and uniform grain structure desired for flat panel display
target materials. For example, an average grain size after 95%
rolling reduction is about 150 microns (such is shown in FIG. 2).
Such grain size is larger than that which would optimally be
desired for a flat panel display. Further, the structures achieved
by conventional processes are not stable. Specifically, if the
structures are heated to a temperature of 150.degree. C. or greater
(which is a typical temperature for sputtering operations), the
average grain size of the structures can grow to 280 microns or
more (see FIG. 3). Such behavior occurs even after intensive
forging or rolling.
[0012] FIG. 4 summarizes results obtained for a prior art high
purity aluminum material. Specifically, FIG. 4 shows a curve 10
comprising a relationship between a percentage of rolling reduction
and grain size (in microns). A solid part of curve 10 shows an
effect of rolling reduction on a 99.9995% aluminum material which
is self-recrystallized at room temperature. As can be seen, even a
high rolling reduction of 95% results in an average grain size of
about 160 microns (point 12), which is a relatively coarse and
non-uniform structure. Annealing at 150.degree. C. for 1 hour
significantly increases the grain size to 270 microns (point 14).
An increase of reduction to 99% can reduce the grain size to 110
microns (point 16 of FIG. 4), but heating to 150.degree. C. for 1
hour increases the average grain size to 170 microns (point 18 of
FIG. 4).
[0013] Attempts have been made to stabilize recrystallized high
purity aluminum structures by adding low amounts of different
doping elements (such as silicon, titanium and scandium) to the
materials. A difficulty that occurs when the doping elements are
incorporated is that full self-recrystallization can generally not
be obtained for an entirety of the material, and instead partial
recrystallization is observed along grain boundaries and triple
joints. For example, the structure of a material comprising
99.9995% aluminum with 30 ppm Si doping is only partly
recrystallized after rolling with a high reduction of 95% (see FIG.
6) in contrast to the fully recrystallized structure formed after
similar rolling of a pure material (see FIG. 2). Accordingly,
additional annealing of the rolled material at a temperature of
150.degree. C. for about 1 hour is typically desired to obtain a
fully recrystallized doped structure. Such results in coarse and
non-uniform grains (see FIG. 7).
[0014] FIG. 5 illustrates data obtained for 99.9995% aluminum with
a 30 ppm silicon dopant. The curve 20 of FIG. 5 conforms to
experimental data of 99.9995% aluminum with 30 ppm silicon after
rolling with different reductions. A dashed part of the curve 20
corresponds to partial self-recrystallization after rolling, while
a solid part of the curve corresponds to full
self-recrystallization. The full self-recrystallization is attained
after intensive reductions of more than 97%, which are practically
not available in commercial target fabrication processes. The point
22 shows the average grain size achieved for the as-deformed
material as being about 250 microns, and the point 24 shows that
the grain size reduces to about 180 microns after the material is
annealed at 150.degree. C. for 1 hour. The points 22 and 24 of FIG.
5 correspond to the structures of FIGS. 6 and 7.
[0015] For the reasons discussed above, conventional
metal-treatment procedures are incapable of developing the fine
grain size and stable microstructures desired in high purity
aluminum target materials for utilization in flat panel display
technologies. For instance, a difficulty exists in that
conventional deformation techniques are not generally capable of
forming thermally stable grain sizes of less than 150 microns for
both doped and non-doped conditions of high purity metals. Also,
particular processing environments can create further problems
associated with conventional metal-treatment processes.
Specifically, there is a motivation to use cold deformation as much
as possible to refine structure, which can remove advantages of hot
processing of cast materials for healing pores and voids, and for
eliminating other casting defects. Such defects are difficult, if
not impossible, to remove by cold deformation, and some of them can
even be enlarged during cold deformation. Accordingly, it would be
desirable to develop methodologies in which casting defects can be
removed, and yet which achieve desired small grain sizes and stable
microstructures.
SUMMARY OF THE INVENTION
[0016] In one aspect, the invention includes a method of forming an
aluminum-comprising physical vapor deposition target. An
aluminum-comprising mass is deformed by equal channel angular
extrusion, with the mass being at least 99.99% aluminum and further
comprising less than or equal to about 1,000 ppm of one or more
dopant materials comprising elements selected from the group
consisting of Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu,
Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N,
Nb, Nd, Ni, 0, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru,
S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb,
Zn and Zr. After the aluminum-comprising mass is deformed, the mass
is shaped into at least a portion of a sputtering target. The
sputtering target can ultimately be formed to be either a
monolithic or mosaic sputtering target.
[0017] In another aspect, the invention encompasses a method of
forming an aluminum-comprising physical vapor deposition target
which is suitable for sputtering aluminum-comprising material to
form an LCD device. An aluminum-comprising mass is deformed by
equal channel angular extrusion. After the mass is deformed, it is
shaped into at least a portion of a physical vapor deposition
target. The physical vapor deposition target has an average grain
size of less than or equal to 45 microns.
[0018] In yet another aspect, the invention encompasses a physical
vapor deposition target consisting essentially of aluminum and less
than or equal to 1,000 ppm of one or more dopant materials
comprising elements selected from the group consisting of Ac, Ag,
As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga,
Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni, 0, Os,
P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc, Se, Si,
Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb, Zn and Zr. The
physical vapor deposition target has an average grain size of less
than or equal to 100 microns.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Preferred embodiments of the invention are described below
with reference to the following accompanying drawings.
[0020] FIG. 1 is an optical micrograph of a cast structure of
99.9995% aluminum (magnified 50 times).
[0021] FIG. 2 is an optical micrograph of 99.9995% aluminum showing
a self-recrystallized structure after 95% cold rolling reduction
(magnified 50 times).
[0022] FIG. 3 is an optical micrograph of 99.9995% aluminum
illustrating a structure achieved after 95% cold rolling reduction
and annealing at 150.degree. C. for 1 hour (magnified 50
times).
[0023] FIG. 4 is a graph illustrating an effect of prior art
rolling reduction processes on grain size of 99.9995% aluminum
which is self-recrystallized at room temperature.
[0024] FIG. 5 is a graph illustrating the effect of prior art
rolling reduction on grain size of a material comprising 99.9995%
aluminum with 30 ppm Si, with such material being partly
self-recrystallized at room temperature.
[0025] FIG. 6 is an optical micrograph of 99.9995% aluminum plus 30
ppm Si after 90% cold rolling reduction (magnified 50 times).
[0026] FIG. 7 is an optical micrograph of 99.9995% aluminum plus 30
ppm Si after 90% cold rolling reduction and annealing at
150.degree. C. for 1 hour (magnified 50 times).
[0027] FIG. 8 shows a flow chart diagram of a method encompassed by
the present invention.
[0028] FIG. 9 is an optical micrograph showing the structure of
99.9995% aluminum after 2 passes through an equal channel angular
extrusion (ECAE) device (magnified 50 times).
[0029] FIG. 10 is an optical micrograph of 99.9995% aluminum after
6 passes through an ECAE device (magnified 50 times).
[0030] FIG. 11 is a graph illustrating the effect of ECAE on grain
size of 99.9995% aluminum which is self-recrystallized at room
temperature.
[0031] FIG. 12 is a graph illustrating the effect of ECAE passes on
grain size of a material comprising 99.9995% aluminum and 30 ppm
Si. The graph illustrates the grain size after
self-recrystallization of the material at room temperature.
[0032] FIG. 13 is an optical micrograph showing the structure of a
material comprising 99.9995% aluminum and 30 ppm Si after 6 passes
through an ECAE device (magnified 100 times).
[0033] FIG. 14 is an optical micrograph showing the structure of a
material comprising 99.9995% aluminum and 30 ppm Si after 6 passes
through an ECAE device, 85% cold rolling reduction, and annealing
at 150.degree. C. for 16 hours (magnified 100 times).
[0034] FIGS. 15A and 15B show optical micrographs of a material
comprising aluminum and 10 ppm Sc after 6 ECAE passes via route D
(i.e., a route corresponding to billet rotation of 90.degree. into
a same direction after each pass through an ECAE device). FIG. 15A
shows the material in the as-deformed state and FIG. 15B shows
material after 85% rolling reduction in thickness.
[0035] FIG. 16 is a diagrammatic top-view of a tiled target
assembly composed of nine billets.
[0036] FIG. 17 is a diagrammatic cross-sectional side-view of the
target assembly of FIG. 16 shown along the line 17-17.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0037] A deformation technique known as equal channel angular
extrusion (ECAE) is used with advantage for the manufacture of
physical vapor deposition targets, and in particular aspects of the
invention is utilized for the first time in the manufacture of FPD
and LCD targets. The ECAE technique was developed by V. M. Segal,
and is described in U.S. Pat. Nos. 5,400,633; 5,513,512; 5,600,989;
and 5,590,390. The disclosure of the aforementioned patents is
expressly incorporated herein by reference.
[0038] The general principle of ECAE is to utilize two intersecting
channels of approximately identical cross-section and extrude a
billet through the channels to induce deformations within the
billet. The intersecting channels are preferably exactly identical
in cross-section to the extent that "exactly identical" can be
measured and fabricated into an ECAE apparatus. However, the term
"approximately identical" is utilized herein to indicate that the
cross-sections may be close to exactly identical, instead of
exactly identical, due to, for example, limitations in fabrication
technology utilized to form the intersecting channels.
[0039] An ECAE apparatus induces plastic deformation in a material
passed through the apparatus. Plastic deformation is realized by
simple shear, layer after layer, in a thin zone at a crossing plane
of the intersecting channels of the apparatus. A useful feature of
ECAE is that the billet shape and dimensions remain substantially
unchanged during processing (with term "substantially unchanged"
indicating that the dimensions remain unchanged to the extent that
the intersecting channels have exactly identical cross-sections,
and further indicating that the channels may not have exactly
identical cross-sections).
[0040] The ECAE technique can have numerous advantages. Such
advantages can include: strictly uniform and homogeneous straining;
high deformation per pass; high accumulated strains achieved with
multiple passes; different deformation routes, (i.e., changing of
billet orientation at each pass of multiple passes can enable
creation of various textures and microstructures); and low load and
pressure.
[0041] ECAE can enable a decrease in the grain size of high purity
aluminum and aluminum alloys used for the manufacture of LCDs by at
least a factor of three compared to conventional practices.
[0042] Various aspects of the present invention are significantly
different from previous ECAE applications. Among the differences is
that the present invention encompasses utilization of ECAE to
deform high purity materials (such as, for example, aluminum having
a purity of greater than 99.9995% as desired for FPD targets), in
contrast to the metals and alloys that have previously been treated
by ECAE. High purity metals are typically not heat treatable, and
ordinary processing steps like homogenizing, solutionizing and
aging can be difficult, if not impossible, to satisfactorily apply
with high purity metals. Further, the addition of low
concentrations of dopants (i.e., the addition of less than 100 ppm
of dopants) doesn't eliminate the difficulties encountered in
working with high purity metals. However, the present invention
recognizes that a method for controlling structure of single-phase
high purity materials is a thermo-mechanical treatment by
deformation, annealing and recrystallization. Also, as high purity
metals are generally not stable and cannot be refined by dynamic
recrystallization in the same manner as alloys, the present
invention recognizes that static recrystallization can be a more
appropriate methodology for annealing of high purity metals than
dynamic recrystallization. When utilizing static recrystallization
annealing of materials, it is preferred that the static
recrystallization be conducted at the lowest temperature which will
provide a fine grain size. If strain is increased to a high level
within a material, such can reduce a static recrystallization
temperature, with high strains leading to materials which can be
statically recrystallized at room temperature. Thus,
self-recrystallization of the materials can occur immediately after
a cold working process. Such can be an optimal mechanism for
inducing desired grain sizes, textures, and other microstructures
within high purity metal physical vapor deposition target
structures.
[0043] In one aspect, the present invention utilizes ECAE to form a
physical vapor deposition target for LCD applications. The target
comprises a body of aluminum with a purity greater than or equal to
99.99% (4N). The aluminum can be doped with less than or equal to
about 1000 ppm of dopant materials. The dopant materials are not
considered impurities relative to the doped aluminum, and
accordingly the dopant concentrations are not considered in
determining the purity of the aluminum. In other words, the percent
purity of the aluminum does not factor in any dopant
concentrations.
[0044] An exemplary target can comprise a body of aluminum having a
purity greater than or equal to 99.9995%. A total amount of dopant
material within the aluminum is typically between 5 ppm and 1,000
ppm, and more preferably between 10 ppm and 100 ppm. The amount of
doping should be at least the minimal amount assuring the stability
of material microstructures during sputtering, and less than the
minimum amount hindering the completion of full dynamic
recrystallization during equal channel angular extrusion.
[0045] The dopant materials can, for example, comprise one or more
elements selected from the group consisting of Ge, Group IIA
elements, Group IIIA elements, Group VIA elements, Group VA
elements, Group IIIB elements, Group IVB elements, Group VIB
elements, Group VIII elements, and Rare Earth elements.
Alternatively, the dopant materials can comprise one or more of Ac,
Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe,
Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni, 0,
Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc, Se,
Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, TI, Tm, V, W, Y, Yb, Zn and Zr.
[0046] The elements of the dopant materials can be in either
elemental or compound form within the materials. The dopant
materials can be considered to comprise two different groups of
materials. The first group comprises dopant materials having
effectively no room temperature solid solubility relative to an
aluminum matrix, and having no intermediate compounds. Such first
type of dopant materials are Be, Ge and Si. The second type of
dopant materials have effectively no room temperature solid
solubility in aluminum, and are not toxic, refractory or precious
metals, and further possess relatively high melting temperatures.
The second type of materials include various elements selected from
the Group IIA elements; the Group IIIB elements; the Group IVB
elements; the Group VIB elements; the Group VIII elements; the
Group IIIA elements; the Group VA elements; the Group VIA elements,
and the Rare Earth elements (i.e., the lanthanides).
[0047] The dopant materials can be in the form of precipitates or
solid solutions within the aluminum-material matrix. Preferably,
the target is composed of aluminum with purity greater than or
equal to 99.99% (4N), and with one or more dopant materials
comprising elements selected from the group consisting of Si, Sc,
Ti, and Hf.
[0048] The present invention can provide a physical vapor
deposition target for LCD applications comprising a body of
aluminum with purity greater than or equal to 99.99% (4N), alone or
doped with less than 1000 ppm of dissimilar elements selected from
a group consisting of one or more of Ac, Ag, As, B, Ba, Be, Bi, C,
Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, In, Ir,
La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni, 0, Os, P, Pb, Pd, Pm, Po, Pr,
Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te,
Ti, TI, Tm, V, W, Y, Yb, Zn and Zr. Further the target can consist
of aluminum and one or more of the listed dissimilar elements, or
can consist essentially of aluminum and the one or more of the
listed dissimilar elements.
[0049] The LCD target can be made of a body of Al with purity
greater than 99.99% (4N), alone or doped with less 100 ppm of one
or more dissimilar elements listed above, and the total doping
content of any element listed above can be higher than the
solubility limit of this element at the temperature at which ECAE
is performed.
[0050] Particularly preferred materials for LCD targets consist of
Al and less than 100 ppm of Si; Al and less than 100 ppm of Sc; Al
and less than 100 ppm of Ti; or Al and less than 100 ppm of Hf.
[0051] A preferred LCD target possesses: a substantially
homogeneous composition throughout; a substantial absence of pores,
voids, inclusions and any other casting defects; a predominate and
controlled grain size of less than about 50 micrometers; and a
substantially uniform structure and controlled texture throughout.
Very fine and uniform precipitates with average grain diameters of
less than 0.5 micrometers can also be present in a preferred target
microstructure.
[0052] LCD physical vapor deposition targets of the present
invention can be formed from a cast ingot comprising, consisting
of, or consisting essentially of aluminum. The aluminum material
can be extruded through a die possessing two contiguous channels of
equal cross section intersecting each other at a certain angle. The
ingot material can also be subjected to annealing and/or processing
with conventional target-forming processes such as rolling,
cross-rolling or forging, and ultimately fabricated into a physical
vapor deposition target shape. The extrusion step can be repeated
several times via different deformation routes before final
annealing, conventional processing and fabrication steps to produce
very fine and uniform grain sizes within a processed material, as
well as to control texture strength and orientation within the
material.
[0053] Processes of the present invention can be applied to large
flat panel display monolithic targets, or targets comprised of two
or more segments.
[0054] Particular embodiments of the present invention pertain to
formation of aluminum-comprising physical vapor deposition targets,
such as, for example, formation of aluminum-comprising physical
vapor deposition targets suitable for liquid crystal display (LCD)
applications. FIG. 8 shows a flow-chart diagram of an exemplary
process of the present invention. In a first step, an
aluminum-comprising cast ingot is formed, and in a second step the
ingot is subjected to thermo-mechanical processing. The material
resulting from the thermo-mechanical processing is an
aluminum-comprising mass. The mass is subsequently deformed by
equal channel angular extrusion (ECAE). Such deformation can be
accomplished by one or more passes through an ECAE apparatus.
Exemplary ECAE apparatuses are described in U.S. Pat. Nos.
5,400,633; 5,513,512; 5,600,989; and 5,590,390. The
aluminum-comprising mass can consist of aluminum, or can consist
essentially of aluminum. The mass preferably comprises at least
99.99% aluminum. The mass can further comprise less than or equal
to about 100 parts per million (ppm) of one or more dopant
materials comprising elements selected from the group consisting of
Ac, Ag, As, B, Ba, Be, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu,
Fe, Ga, Gd, Ge, Hf, Ho, In, Ir, La, Lu, Mg, Mn, Mo, N, Nb, Nd, Ni,
0, Os, P, Pb, Pd, Pm, Po, Pr, Pt, Pu, Ra, Rf, Rh, Ru, S, Sb, Sc,
Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb, Zn and Zr.
The aluminum-comprising mass can consist of aluminum with less than
or equal to about 100 ppm of one or more of the dopant materials
described above, or consist essentially of aluminum with less than
or equal to about 100 ppm of one or more of the dopant materials
described above.
[0055] ECAE is utilized in methodology of the present invention for
addressing problems found during formation of PVD targets of
high-purity materials. ECAE is a process which utilizes a simple
shear deformation mode, which is different from a dominant
deformation mode achieved by uniaxial compression of forging or
rolling. In high purity metals, the intensive simple shear of ECAE
can manifest itself by developing very thin and long shear bands.
The strains achieved inside these bands can be many times larger
than the strains achieved outside the bands. The shear bands occur
along a crossing plane of the channels utilized during ECAE. If a
processing speed is sufficiently low to eliminate adiabatic heating
and flow localization at the macro-scale, shear bands in pure
metals can have a thickness of only a few microns with a near
regular spacing between each other of a few tenths of a micron. The
bands can be observed after a single ECAE pass. However, if the
number of ECAE passes increases the spacing between shear bands can
reduce to a stable size. The actual size can vary depending on the
material being subjected to ECAE, and the purity of such material.
A strain inside of the shear bands can be equivalent to very high
reductions (specifically, reductions of about 99.99% or more), and
static recrystallization is immediately developed in the bands. The
static recrystallization can lead to new fine grains growing in
spacing between the bands.
[0056] FIGS. 9 and 10 show fully recrystallized structures of
99.9995% aluminum after ECAE with 2 passes and 6 passes,
respectively. The grains within the material attained a stable size
after 6 passes. Experiments have shown that processing with a route
corresponding to billet rotation of 90.degree. into a same
direction after each pass can provide the most uniform and
equiaxial recrystallized structures for high purity materials. Such
route is defined as route "D" in accordance with the standard
definitions that have been utilized to described ECAE processing in
previous publications.
[0057] FIG. 11 shows a curve 30 demonstrating the change manifested
in grain size of a high-purity aluminum material subjected to
varying numbers of ECAE passes. Curve 30 of FIG. 11 can be compared
with the curve 10 of FIG. 4 to illustrate advantages in grain size
reductions attained by an ECAE process relative to the conventional
processes utilized to generate the curve 10 of FIG. 4.
[0058] The ECAE structures are found to not only have small grain
sizes, but also to be stable during additional annealing to
sputtering-type temperatures. For example, after annealing at
150.degree. C. for 1 hour, a material subjected to six ECAE passes
shows only a relatively insignificant increase in grain size of
from 40 microns (point 32 in FIG. 11) to 50 microns (point 34 in
FIG. 11). However, the structures diagrammed at FIG. 11 were found
to be relatively unstable when subjected to rolling procedures,
even when the rolling procedures accomplished only moderate
reductions. For instance, a significant increase of grain size from
40 microns after 6 ECAE passes to 160 microns occurred after
rolling with the reduction of 75% (point 36 on FIG. 11).
[0059] Generally, ECAE can be effectively performed only when a
ratio of billet size to thickness is from about 4 to 8, while flat
panel display targets typically have a ratio of up to 100 or more.
Accordingly, additional rolling of ECAE processed billets may be
desired to fabricate the thin targets desired for FPD. Thus, it
would be desirable to develop methodologies which avoided the
structure coarsening evidenced by point 36 of FIG. 11. One way to
avoid such structure coarsening is to eliminate rolling. This can
be achieved if an ECAE processed billet has a sufficiently large
size to fabricate FPD targets by splitting the billet thickness for
a number of thin plates. However, this can be a complicated process
since FPD targets have a typical size of 1000 millimeters, or
larger; and ECAE of such large billets is typically not practical.
Another method for incorporating ECAE processed billets into FPD
targets is to fabricate mosaic targets by using a large number of
small pieces cut from ECAE billets (see, for example, FIGS. 16 and
17). However, mosaic targets are typically expensive to fabricate,
and also typically do not provide good performance in sputtering
applications.
[0060] Another method which can be utilized to avoid grain size
growth within ECAE processed materials is to provide doping
elements within the ECAE materials. However, while the addition of
dopants can typically be utilized for structure refinement when
static recrystallization is performed as a separate annealing
operation at sufficiently high temperatures after mechanical
working, it cannot generally be applied in the case of
self-annealing at room temperature during or immediately after
deformation performed by forging or rolling because the doping can
make even heavily deformed structures more stable.
[0061] ECAE can be utilized for grain refinement of high purity
metals, even if the metals have some dopant material therein. For
instance, 99.9995% aluminum having 30 ppm of silicon therein is
found to be almost fully recrystallized after 2 passes through an
ECAE apparatus. If the material is subjected to 3 to 6 passes
through the apparatus, it is found to have a fine and uniform
structure, with such structure remaining substantially unchanged
after 6 passes through the device. FIG. 12 illustrates a curve 50
corresponding to the change in grain size of 99.9995% aluminum
having 30 ppm silicon therein, with various numbers of ECAE passes.
A dashed part of curve 50 corresponds to partial recrystallization,
and a solid part of curve 50 corresponds to full recrystallization
at room temperature immediately after ECAE.
[0062] The structure after 6 passes is illustrated in FIG. 13. Such
structure is a substantially perfectly recrystallized, uniform,
very fine and equiaxial structure having an average grain size of
about 15 microns. Such properties can provide exceptional stability
of the structure during subsequent rolling and annealing. For
instance, subsequent rolling with a reduction of up to 90%, and
long-term annealing of about 16 hours at a temperature of
150.degree. C. causes only a moderate grain growth, with the
resulting structure having an average grain size of about 30
microns. Further, structure uniformity is maintained, as
illustrated in the optical micrograph of FIG. 14. Such stability of
the small grain size microstructures achieved with ECAE is
substantially different than what can be accomplished with
conventional processes of forging, rolling or other deformation
techniques. Accordingly, ECAE can provide improved methodology for
fabricating high purity targets with fine and stable
microstructures for physical vapor deposition applications. It is
found that ECAE processing utilizing from 3 to 6 passes through an
ECAE device is typically suitable for forming a physical vapor
deposition target blank. In particular, ECAE with 4 passes of route
"D" (i.e., rotation of 90.degree. into the same direction after
each pass) can be an optimal processing schedule.
[0063] Experiments have been performed on doping selection and
concentration. Specifically, the doping elements Si, Sc and Ti have
been tested. Concentrations ranged from 5 ppm to 100 ppm for each
of the elements. In all of the tested cases, the effects achieved
with the elements were found to be qualitatively about the same,
with some quantitative differences. For instance, it was found that
silicon doping can provide the best refinement, provided that a
doping concentration is from about 5 ppm to about 100 ppm.
[0064] Among the benefits of utilizing ECAE for forming target
blanks of high-purity materials, relative to utilizing conventional
processes, is that ECAE can be utilized in combination with a
hot-forging operation. Specifically, ECAE removes restrictions on
attainable deformation during processing from a cast ingot to a
target blank, and accordingly removes requirements on the original
structures subjected to ECAE. A material can be subjected to hot
forging prior to ECAE. Such hot forging can result in substantially
entire elimination of casting defects, which can further result in
improved performance of targets formed by methodology of the
present invention relative to targets formed by conventional
processes.
[0065] In a fourth step of the FIG. 8 flow-chart diagram, the
deformed aluminum-comprising mass is shaped into a PVD target, or
at least a portion of a target. Such shaping can comprise, for
example, one or more of rolling, cross-rolling, forging, and
cutting of the aluminum-comprising mass. The mass can be formed
into a shape comprising an entirety of a physical vapor deposition
target, or alternatively can be formed into a shape comprising only
a portion of a physical vapor deposition target. An exemplary
application wherein the mass is formed into a shape comprising only
a portion of a physical vapor deposition target is an application
in which the mass is utilized to form part of a so-called mosaic
target. If the aluminum-comprising mass is utilized in a mosaic
target, and further utilized for LCD applications, it can be
desired that all of the various target portions of the mosaic
target be aluminum-comprising masses which have been deformed by
equal channel angular extrusion prior to incorporation into the
mosaic target.
[0066] In the fifth step of the FIG. 8 process, the shaped mass is
mounted to a backing plate to incorporate the mass into a target
structure. Suitable backing plates and methodologies for mounting
aluminum-comprising targets to backing plates are known in the art.
It is noted that the invention encompasses embodiments wherein an
aluminum-comprising mass is utilized directly as a physical vapor
deposition target without being first mounted to a backing plate,
as well as embodiments in which the mass is mounted to a backing
plate.
[0067] Processes of the present invention can be utilized to
fabricate aluminum-comprising masses into targets having very fine
and homogenous grain structures, with predominate sizes of the
grains being less than about 50 micrometers. Such targets can be
particularly suitable for sputtering applications in forming LCD
materials. The present invention recognizes that improvements in
grain refinement can be provided by ECAE technology relative to
processing of aluminum-comprising materials. The ECAE is preferably
conducted at a temperature and speed sufficient to achieve desired
microstructures and provide a uniform stress-strain state
throughout a processed billet.
[0068] The number of passes through an ECAE device, and the
particular ECAE deformation route selected for travel through the
device can be chosen to optimize target microstructures. For
instance, grain refinement can be a consequence of radical
structural transformations occurring during intense straining by
simple shear through an ECAE device.
[0069] FIGS. 15A illustrates grains obtained for aluminum +10 ppm
Sc after ECAE processing. The grains shown in FIG. 15A have an
average size of about 20 microns, and are relatively fine,
equiaxial, and homogenous. The structure shown in FIG. 15A has an
average grain size that is at least a factor of 3 smaller than the
sizes produced by conventional target-forming methods.
[0070] At least three different aspects of ECAE contribute to the
remarkable reduction of grain size and improvement of grain
uniformity achieved by treating aluminum-comprising masses in
accordance with the present invention. These three aspects are an
amount of plastic deformation imparted by ECAE, the ECAE
deformation route, and simple shear forces occurring during
ECAE.
[0071] After a material has been subjected to ECAE in accordance
with methods of the present invention, the material can be shaped
by conventional methods of forging, cross-rolling and rolling to
form the material into a suitable shape to be utilized as a target
in a sputtering process. The ultrafine grain sizes created during
ECAE are found to remain stable and uniform, and to show limited
grain growth upon further conventional processing; even during
processing comprising a high reduction in thickness of a material.
Such is exemplified by FIG. 15, which compares various
microstructures of as-deformed ECAE samples (FIG. 15A) to those
submitted to further unidirectional rolling at an 85% thickness
reduction (FIG. 15B) for aluminum +10 ppm Sc.
[0072] Preferably, traditional forming operations utilized for
shaping a material after ECAE processing are conducted at
temperatures which are less than those which will occur during
sputtering. For instance, if sputtering processes are anticipated
to occur at about 150.degree. C., then conventional processing of,
for example, rolling, cross-rolling, or forging occurring after
ECAE will preferably occur at temperatures below 150.degree. C. By
conducting such processing at temperatures below the sputtering
temperature, the likelihood of the conventional processing
increasing grain sizes beyond those desired in a physical vapor
deposition target is reduced. Typically, target shaping steps occur
at temperatures of less than or equal to about 200.degree. C., and
more preferably occur at temperatures less than or equal to about
150.degree. C., to keep the target shaping steps at temperatures
below an ultimate sputtering temperature of a target.
[0073] The microstructures created during ECAE are found to exhibit
exceptional stability upon annealing relative to microstructures
created by conventional processes. For example, it is found that a
sample of aluminum +30 ppm Si which has been subjected to ECAE
shows a limited and progressive increase in average grain size from
approximately 12 microns to about 30 microns after annealing at
150.degree. C. for 1 hour. Such average grain size does not
significantly change after annealing at 150.degree. C. for 16
hours. In contrast, samples submitted solely to rolling to an 85%
reduction in thickness (a conventional process), show a dramatic
grain growth up to average grain sizes larger than 250 micron after
annealing at only 125.degree. C. for 1 hour.
[0074] Utilization of ECAE for processing aluminum targets can
enable control of a texture within the targets, with the term
"texture" referring to a crystallographic orientation within the
target. If a large number (i.e. a vast majority) of the grains in a
material have the same crystallographic orientation as one another,
the material is referred to as having strong texture. In contrast,
if the grains do not have the same crystallographic orientation,
the material is referred to as having a weak texture. Note that the
referred-to crystallographic orientation is not to imply that the
grains are part of a single crystal. Various textures can be
created utilizing methodology of the present invention.
[0075] A particular application of the invention is directed to the
manufacture of targets of especially large size. FIGS. 16 and 17
display this aspect of the invention. In FIGS. 16 and 17, the
construction of a target 190 in the form of a tiled assembly is
provided. Such comprises joining two or more billets 200 of
identical shape, dimensions and processing history to a backing
plate 210, machining the surface of the resulting assembly, and
fabricating the final target 190. Preferably, the backing plate is
made of a high strength material and possesses a length and width
close to those of the final target. Joining is realized by known
methods such as soldering, brazing, welding or diffusion bonding at
an interface 220 between the backing plate and the bottom of each
single billet and at sufficient time, pressure and temperature.
Preferably, techniques such as brazing or soldering will be used
because they can utilize lower temperatures than some of the other
methods. Also, lateral forces along the three different directions
X, Y and Z shown in FIGS. 16 and 17 are exerted with appropriate
tooling. The forces along the directions X and Y keep all the
billets held tightly together, while the force along the Z
direction participates to the joining operations and keeps the
surface of the final target flat. Also, as shown in FIGS. 16 and
17, one side of the bottom of each billet is preferably machined to
leave a space 230 at the bottom between adjacent billets. Such
space can have materials provided therein which are used for
joining the billets together (the space is shown in dashed-line
phantom view in FIG. 16). This space can also prevent the materials
utilized for soldering, brazing, welding and diffusion bonding from
going between billets and contaminating the target surface and the
volume to be sputtered.
[0076] The method described with reference to FIGS. 16 and 17 can
present several advantages for the production of very large
targets. First, current equipment and tooling can be employed.
Second, contrary to current known methods, intensive rolling and/or
cross-rolling are not used to reach final target size; therefore,
for example, as-deformed ECAE billets can be directly joined
together and retain their advantages in terms of grain size and
texture. Third, the procedure is easily adaptable to any future
evolution of the size of LCD targets.
EXAMPLES
Example 1
High-purity Aluminum Having 30 ppm Si Therein, and Processed in
Accordance With Methodology of the Present Invention
[0077] As-cast material defined as 5N5 Al and 30 ppm Si is
processed via hot forging at 75% reduction and ECAE for 6 passes
via route D. The material has a fully recrystallized structure with
grain size of 15 .mu.m. Subsequent rolling with a reduction of 85%
grew the average grain size to 20 .mu.m with an aspect ratio of
about 1.5. Annealing at a temperature of 150.degree. C. for 1 hour,
which was estimated as the highest temperature expected during a
subsequent sputtering process, resulted in an insignificant grain
growth to 23 .mu.m. During a long (16 hours) exposure to
150.degree. C., grains grew to 28 .mu.m. Also, a temperature
increase to 200.degree. C. for 1 hour yielded a similar grain size
of about 30 .mu.m. Therefore, ECAE plus rolling provides a fine and
uniform structure for a material of 5N5 Al and 30 ppm Si, with an
average grain size of less than or equal to about 30 .mu.m which is
stable for sputtering target applications.
Example 2
High-Purity Aluminum Having 10 ppm Silicon Therein, and Processed
in Accordance With Methodology of the Present Invention
[0078] Samples were cast, hot forged at 74% reduction and ECAE
extruded for 6 passes via route D. A Structure after ECAE is fully
dynamically recrystallized with an average grain size of about 19
.mu.m. Subsequent rolling at 85%, and annealing at 150.degree. C.
for 1 hour yields a fully recrystallized grain size of around 35
.mu.m.
Example 3
High-Purity Aluminum Having 10 ppm Sc Therein, and Processed in
Accordance With Methodology of the Present Invention.
[0079] Samples were cast, hot forged at 74% reduction, and ECAE
extruded for 6 passes via route D. A structure after ECAE is fully
dynamically recrystallized with an average grain size of about 26
.mu.m. During rolling up to a reduction of 60%, the structure
remains stable and typical for heavily-rolled materials. After 70%
reduction, first recrystallized grains are observed. At 85% rolling
reduction, about 60% of the sample area was fully recrystallized
with an average grain size of about 45 .mu.m.
Example 4
Aluminum Having 30 ppm Silicon Therein, and Processed in Accordance
With Prior Art Technologies
[0080] The present example was run to allow comparison of previous
results of ECAE (examples 1-3) with data obtained utilizing
conventional processing technologies. The same 5N5 Al+30 ppm Si
material was used for this example as was used in Example 1. A
cast, hot forged at 74% reduction and annealed sample was
subsequently cold rolled with a reduction of 85%. Its structure is
not fully recrystallized and fine dynamically recrystallized grains
can be observed only along boundaries of original grains.
Additional annealing at 125.degree. C. for 1 hour provides full
recrystallization but the microstructure has a highly non-uniform
distribution with an average grain size of about 150 .mu.m.
Annealing at higher temperatures further increases the average
grain size. The example illustrates that conventional processing
techniques only provide a moderate refinement of the structure of
5N5 Al with 30 ppm Si doping. Specifically, the grain size achieved
is well above a desired limit of 100 .mu.m, and, in fact, is
greater than 150 .mu.m.
[0081] In compliance with the statute, the invention has been
described in language more or less specific as to structural and
methodical features. It is to be understood, however, that the
invention is not limited to the specific features shown and
described, since the means herein disclosed comprise preferred
forms of putting the invention into effect. The invention is,
therefore, claimed in any of its forms or modifications within the
proper scope of the appended claims appropriately interpreted in
accordance with the doctrine of equivalents.
* * * * *