Nissan North America, Inc.v.Diamond Coating Technologies, LLC

Patent Trial and Appeal Board

Apr 20, 2016

09045163 (P.T.A.B. Apr. 20, 2016)

Trials@uspto.gov Paper 49
571-272-7822 Date: April 20, 2016

UNITED STATES PATENT AND TRADEMARK OFFICE
____________

BEFORE THE PATENT TRIAL AND APPEAL BOARD
____________

NISSAN NORTH AMERICA, INC. and
HITACHI AUTOMOTIVE SYSTEMS, LTD.,
Petitioner,

v.

DIAMOND COATING TECHNOLOGIES, LLC,
Patent Owner.

____________

Case IPR2014-01546
Patent No. 6,066,399
____________

Before CHRISTOPHER L. CRUMBLEY, JO-ANNE M. KOKOSKI, and
BRIAN P. MURPHY, Administrative Patent Judges.

CRUMBLEY, Administrative Patent Judge.

FINAL WRITTEN DECISION
35 U.S.C. § 318 and 37 C.F.R. § 42.73

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I. INTRODUCTION
In this inter partes review trial, instituted pursuant to 35 U.S.C. § 314,
Petitioner Nissan North America, Inc. and Hitachi Automotive Systems, Ltd.
(collectively, “Petitioner”) challenge the patentability of claim 1 of
U.S. Patent No. 6,066,399 (Ex. 1001, “the ’399 patent”), owned by Diamond
Coating Technologies, LLC (“Patent Owner”).
We have jurisdiction under 35 U.S.C. § 6(c). This Final Written
Decision, issued pursuant to 35 U.S.C. § 318(a) and 37 C.F.R. § 42.73,
addresses issues and arguments raised during trial. For the reasons
discussed below, we determine that Petitioner has met its burden to prove,
by a preponderance of the evidence, that claim 1 of the ’399 patent is
unpatentable.
A. Procedural History
On September 26, 2014, Petitioner requested an inter partes review of
claim 1 of the ’399 patent. Paper 1, “Pet.” Patent Owner filed a Patent
Owner Preliminary Response. Paper 13.1 We authorized Petitioner to file
additional briefing regarding real party in interest issues raised in the
Preliminary Response, pursuant to which Petitioner filed a Reply to the

1 The Preliminary Response was filed as “Parties and Board Only,”
accompanied by a Motion to Seal. Paper 14. A redacted version of the
Preliminary Response was included as Exhibit A to the Motion to Seal. Id.
In an Decision issued today, we grant Patent Owner’s Motion to Seal, unseal
the Motion, and direct Patent Owner to file a copy of the redacted
Preliminary Response (Exhibit A) as a separate Paper in the record.
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Preliminary Response. Paper 17.2 In a Decision on Institution of Inter
Partes Review (Paper 223, “Dec.”), we determined that the Petition named
all real parties in interest, and instituted trial of claim 1 based on the
following grounds:
1. Whether claim 1 is unpatentable under 35 U.S.C. § 102 as
anticipated by Menu;4 and
2. Whether claim 1 is unpatentable under 35 U.S.C. § 102 as
anticipated by Hirochi.5
Dec. 19.
Following institution of trial, Patent Owner filed a Patent Owner
Response (Paper 33, “PO Resp.”), and Petitioner filed a Reply (Paper 38,
“Reply”).
Petitioner supported its Petition with the Declaration of Dr. Mark C.
Hersam (Ex. 1007), and Patent Owner took the cross-examination of
Dr. Hersam via deposition. Ex. 2022. With its Response, Patent Owner
submitted the Declaration of Dr. Richard B. Kaner (Ex. 2028), and Petitioner
took the cross-examination of Dr. Kaner via deposition. Ex. 1017.

2 Petitioners filed a sealed version of the Reply, accompanied by a Motion to
Seal with a redacted version of the Reply as Exhibit A. Paper 16. As with
the Preliminary Response, we grant the Motion and direct Petitioners to file
a copy of Exhibit A as a separate Paper in the record.
3 Paper 22 is a redacted version of the Decision; an unredacted version was
issued under seal as Paper 18.
4 Ex. 1002, US 5,837,331 to Menu et al., (Nov. 17, 1998).
5 Ex. 1005, US 4,877,677 to Hirochi et al., (Oct. 31, 1989).
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No Motions to Exclude or Motions for Observation were filed by
either party. Oral hearing was requested by both parties, and a hearing was
held January 6, 2016. A transcript of the oral hearing is included in the
record. Paper 48, “Tr.”
B. The ’399 Patent
The ’399 patent relates to a hard carbon thin film formed on a
substrate, wherein the film has a graded structure. Ex. 1001, Abstract.
Specifically, the ’399 patent discloses varying the type of carbon-carbon
bonding in the film to achieve improved properties. Id. at 2:10–14.
According to the ’399 patent, it is generally known that the carbon-carbon
bonds in graphite are predominantly sp2 type, whereas diamond contains
predominantly sp3 bonds. Id. at 2:42–46. In the films of the ’399 patent, the
ratio of sp2 to sp3 bonding is varied through the thickness of the film, such
that the interior of the film has a lower sp2/sp3 ratio than the outer edges. Id.
at 2:33–41. This graded structure is illustrated in Figure 5 of the patent,
shown below:

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Figure 5 of the ’399 patent depicts the relationship between sp2/sp3 ratio and
the distance from the film/substrate interface.

The ’399 patent discloses that an increased proportion of sp2 bonding
(higher sp2/sp3 ratio) results in a decrease in internal stress in the film and
provides better adhesion to a substrate, while an increased proportion of sp3
bonding (lower sp2/sp3 ratio) leads to increased hardness and internal stress.
Id. at 2:58–64.
C. Challenged Claim
Claim 1 is the only challenged claim of the ’399 patent, and recites:
1. A hard carbon thin film arrangement comprising a hard
carbon thin film having a surface and an interface opposite said
surface with a thickness direction extending through said thin
film from said interface to said surface, and having a graded
carbon composition in which a ratio of sp2 to sp3 carbon-carbon
bonding in said thin film decreases in said thickness direction
from said interface to a minimum at an internal location of said
thin film between said interface and said surface, and increases
from said minimum at said internal location toward said surface
of said thin film.

Ex. 1001, 23:1–11.
II. DISCUSSION
A. Claim Construction
For purposes of our Decision to Institute, we analyzed each claim
term in light of its broadest reasonable interpretation, as understood by one
of ordinary skill in the art and as consistent with the specification of the ’399
patent. 37 C.F.R. § 42.100(b); see In re Cuozzo Speed Techs., LLC, 793
F.3d 1268, 1278–79 (Fed. Cir. 2015), cert. granted, Cuozzo Speed Techs.
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LLC v. Lee, 84 U.S.L.W. 3218 (U.S. 2016). In the Decision, we determined
that no claim term required an explicit construction at that stage of the
proceeding. See Dec. 10–11 (citing Vivid Techs., Inc. v. Am. Sci. & Eng’g,
Inc., 200 F.3d 795, 803 (Fed. Cir. 1999)).
During the course of the trial, the parties’ dispute focused on the claim
term hard carbon thin film, and the parties proffered competing
constructions of that term. Petitioner maintains that an explicit construction
of the term is unnecessary, but that, if the Board construes the term, it should
be interpreted to mean “a carbon film having a significant amount of sp3–
hybridized carbon, including a crystalline diamond carbon thin film, an
amorphous diamond-like carbon thin film, and a diamond-like carbon thin
film having a partial crystalline structure.” Pet. 10–11; Reply 7–8. Patent
Owner, by contrast, proposes the construction “a film that contains
significant amounts of sp3-hybridized carbon and that excludes graphitic
carbon.” PO Resp. 12.
Petitioner also informs us that, in a copending District Court patent
infringement action between the parties, the court construed hard carbon
thin film under the standards set forth by the Federal Circuit in Phillips v.
AWH Corp., 415 F.3d 1303 (Fed. Cir. 2005) (en banc), and arrived at the
construction “a film containing a significant fraction of sp3-hybridized
carbon. Hard carbon film excludes graphitic or polymer-like carbon film.”
Pet. 10; Ex. 1015, 8. The court also noted that “[b]oth parties now agree that
the term excludes graphitic or polymer-like carbon film.” Ex. 1015, 8.
While the court acknowledged that the construction would require the trier
of fact to determine what constitutes a “significant fraction of sp3-hybridized
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carbon,” Judge Pfaelzer found that the “Koidl reference,” cited during
prosecution of a related patent issued to the same inventors, “may serve as a
guide.” Id. at 8–10 (“Significant variation from the ratios expressed in the
Koidl reference may be evidence that a film is not hard carbon and does not
reflect the properties of hard carbon: hardness, resistivity, and chemical
stability.”). While neither party has introduced the Koidl reference—or the
prosecution history of the ’399 patent—into the record of this proceeding,
we understand from the District Court’s opinion that the Koidl reference
disclosed an sp3:sp2:sp1 ratio of 68:30:2 in hard carbon, as opposed to a
53:45:2 ratio in polymer-like carbon. Id. at 9.
We have taken into consideration Judge Pfaelzer’s construction of
hard carbon thin film, recognizing that the District Court claim construction
standard differs from that applied during inter partes review of an unexpired
patent. In an inter partes review, “[a] claim in an unexpired patent shall be
given its broadest reasonable construction in light of the specification of the
patent in which it appears.” 37 C.F.R. § 42.100(b). Under this standard, we
construe claim terms using “the broadest reasonable meaning of the words in
their ordinary usage as they would be understood by one of ordinary skill in
the art, taking into account whatever enlightenment by way of definitions or
otherwise that may be afforded by the written description contained in the
applicant’s specification.” In re Morris, 127 F.3d 1048, 1054 (Fed. Cir.
1997). We presume that claim terms have their ordinary and customary
meaning. See In re Translogic Tech., Inc., 504 F.3d 1249, 1257 (Fed. Cir.
2007) (“The ordinary and customary meaning is the meaning that the term
would have to a person of ordinary skill in the art in question.”) (internal
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quotation marks omitted). A patentee may rebut this presumption, however,
by acting as his own lexicographer and providing a definition of the term in
the specification with “reasonable clarity, deliberateness, and precision.” In
re Paulsen, 30 F.3d 1475, 1480 (Fed. Cir. 1994).
Before turning to the contentions of the parties, a background on the
chemistry of carbon films is helpful. As the ’399 patent acknowledges, it
was generally known that carbon made up exclusively, or predominantly, of
sp2-bonded carbon is graphite, whereas exclusively or predominantly sp3-
bonded carbon is diamond. Ex. 1001, 2:42–46. In between these extremes
lie a number of intermediate forms of carbon which are amorphous6 or
polycrystalline in nature. Ex. 1007, 54–55. The forms may be characterized
as “graphitic,” which are soft, or “diamond-like,” which are hard. Tr. 31
(Patent Owner’s counsel agreeing it is nonsensical to describe a hard
graphitic film, or a soft diamond-like film). Dr. Hersam testified that this
continuum can be depicted on a “ternary phase diagram” (Ex. 2022, 13), a

6 An amorphous structure is one that lacks long-range order. See Ex. 2022
(Hersam cross-examination), 62; Ex. 1002 (Menu) 3:60–63.
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version of which appears in the Robertson7 reference submitted by Patent
Owner:

Figure 2 of Robertson depicts a ternary phase diagram having vertices of sp2,
sp3, and H, as well as regions of graphitic carbon, amorphous carbon (a-C),
tetrahedral amorphous carbon (ta-C), and hydrogenated amorphous carbon
(a-C:H and ta-C:H). Ex. 2021, 130–131.

The continuum of pure carbon films ranging from graphite to diamond
lies along the left-hand side of the ternary phase diagram, and has a small
region of graphitic carbon followed by larger regions of amorphous carbon
and tetrahedral amorphous carbon. Id. The ternary phase diagram also
depicts carbon films that contain varying amounts of hydrogen, called
hydrogenated carbon films. Id. Dr. Kaner testified that the hard carbon

7 J. Robertson, Diamond-Like Amorphous Carbons, 37 MATERIAL SCI. AND
ENGINEERING REP. 129 (2002) (Ex. 2021).
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films of the ’399 patent may include both pure carbon films as well as films
containing hydrogen. Ex. 1017, 151.
The parties’ experts disagree on the exact transition point between
hard (diamond-like) carbon films and soft (graphitic) carbon films.
According to Dr. Hersam, a “few percent” of sp3 bonding is sufficient to
move the film beyond the graphitic range. Ex. 2022, 10–11. Dr. Kaner
disagreed slightly, testifying that a film would need to have up to about 15%
sp3 bonding before it became non-graphitic. Ex. 1017, 69–70. Both experts
agreed, however, that a carbon film can contain a large amount of sp2 carbon
and still be diamond-like in character. This is in accordance with the
disclosure of the ’399 patent itself; claim 3 of the patent, which depends
from claim 1, recites that the hard carbon film may have an sp2/sp3 ratio
ranging from 0–3, meaning that carbon films may be up to 75% sp2 and still
considered hard within the usage of the patent.
Resolution of this inter partes review trial does not require us to
determine exactly where the transition between soft carbon films and hard
carbon films occurs on the continuum of sp2/sp3 ratios, or define what
constitutes a “significant” fraction of sp3-hybridized carbon as used in the
District Court’s construction of the term. The ternary phase diagram from
Robertson, depicted above, shows that a wide range of compositions—
including compositions having very high percentages of sp2 bonding—are
within the scope of amorphous hard carbon films. Ex. 2021, Fig. 2. Indeed,
only a comparably small range of films in the lower left corner of the
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diagram are classified as graphitic carbon films, which the parties agree is
outside the scope of the claims.
Returning to the disclosure of the ’399 patent itself, the specification
sets forth three exemplary forms of carbon that fall within the scope of the
claim term hard carbon thin film: “crystalline diamond carbon thin film,”
“amorphous diamond-like carbon thin film,” and “diamond-like carbon thin
film having a partial crystalline structure.” Ex. 1001, 3:1–5; see also claim 4
(dependent claim specifying types of films within claim 1). This disclosure
confirms that hard carbon thin film covers a wide range of the ternary phase
diagram, including the top vertex (diamond film) as well as much of the left
border and interior (amorphous and polycrystalline films).
As noted above, Patent Owner asks that we adopt a construction that
specifically excludes “graphitic carbon.”8 PO Resp. 12. We decline to do
so. To the extent that Patent Owner’s proposed “graphitic carbon” exclusion
could be interpreted to exclude films which are diamond-like overall, but
which have regions of sp2 (graphitic) bonding, it is improper. As Petitioner
correctly notes, diamond-like carbon films necessarily have regions of sp2
bonding within the amorphous structure. Reply 5 (citing Ex. 1017 (Kaner
cross-examination), 77); see also Ex. 2028 (Kaner direct testimony) ¶¶ 49–

8 We note that this differs from the District Court’s construction, which only
excludes graphitic carbon films (i.e., films that are—as a whole—graphitic).
Ex. 1015, 8.
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51 (diamond-like carbon is a combination of diamond and graphite that has
clusters of sp2-carbon bonding).
Nor do we consider it necessary to adopt, as Petitioner suggests, a
construction that includes examples of films within the scope of the term,
namely “a crystalline diamond carbon thin film, an amorphous diamond-like
carbon thin film, and a diamond-like carbon thin film having a partial
crystalline structure.” Reply 8. As noted above, these examples are set forth
in the ’399 patent itself, including in dependent claim 4, meaning that claim
1’s hard carbon thin film must encompass them. We decline to adopt a
construction that expressly recites these examples, to the extent it might
imply that all other types of carbon films are excluded.
For these reasons, we determine that the broadest reasonable
interpretation of hard carbon thin film in light of the specification is “film
containing a significant fraction of sp3-hybridized carbon.” This
construction is not inconsistent with that adopted by the District Court,9 and
we agree with the court that it excludes graphitic carbon films. While it is
unnecessary to determine the exact boundary of the hard carbon film
domain, we note that “a significant fraction of sp3” encompasses a wide
range of sp3/sp2 ratios that may even be a majority sp2-bonding, extending to
at least 75% sp2.

9 We decline to adopt the District Court’s reliance on a 68:30 ratio of sp3/sp2
bonding as indicative of “a significant fraction,” as the Koidl reference upon
which that ratio is based is not in the record of this proceeding, nor does it
appear to have been cited during the prosecution history of the ’399 patent.
Ex. 1001, References Cited.
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B. Anticipation by Menu
Petitioner contends that claim 1 is unpatentable under 35 U.S.C. § 102
as anticipated by Menu. Pet. 11–24. To establish anticipation, Petitioner
must prove that each and every element in a claim may be found in Menu,
arranged as recited in the claim. Net MoneyIN, Inc. v. VeriSign, Inc., 545
F.3d 1359, 1369 (Fed. Cir. 2008); Karsten Mfg. Corp. v. Cleveland Golf Co.,
242 F.3d 1376, 1383 (Fed. Cir. 2001). For the following reasons, Petitioner
has established by a preponderance of the evidence that Menu anticipates
claim 1.
Menu discloses amorphous carbon multi-layered structures, also
called amorphous superlattice structures, and an improved method for
making such structures. Ex. 1002, 1:5–10. The properties of the structures’
layers are predetermined, and may have varying degrees of resistivity,
electronic emission, band gap, density, hardness, and stress. Id. at 4:6–7.
To form the layers, a precursor such as graphite is vaporized to form carbon
ions, which are then impinged upon a substrate to form a solid carbon layer.
Id. at 3:63–4:3. By varying the total ion impinging energy during
deposition, Menu discloses that the proportion of sp2- and sp3-bonded carbon
in the resulting layers can be controlled. Id. at 4:30–50. This relationship
between the amount of sp3 bonding in a layer and the total ion impinging
energy is depicted in Figure 2 of Menu:
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Figure 2 of Menu shows “a graphical depiction of per cent sp3-bonding in a
deposited carbon layer as a function of total ion impinging energy.” Id. at
30–32.

Figure 3 of Menu shows the variation of applied voltage over time
during the deposition process, and indicates a period of high voltage ǀUsǀmax,
followed by low voltage ǀUsǀmin, followed by high voltage ǀUsǀmax again. Id. at
Fig. 3. Menu discloses that ǀUsǀmax has a value corresponding to the low %
sp3 range in the graph of Figure 2. Id. at 5:25–27.
Drawing on these disclosures, Petitioner reasons that the voltage pattern
of Figure 3 would result in a graded carbon film having a region of lower sp3
bonding (higher sp2/sp3 ratio), followed by an interior region of higher sp3
bonding (lower sp2/sp3 ratio), followed by a surface region of lower sp3
bonding again. Pet. 14. According to Petitioner, this satisfies claim 1’s
requirement of a graded carbon composition in which the sp2/sp3 ratio
decreases from the substrate “interface to a minimum at an internal location
of said thin film between said interface and said surface, and increases from
said minimum at said internal location toward said surface of said thin film.”
Id.
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Patent Owner raises two substantive arguments10 in response. First,
Patent Owner contends that the structures of Menu are not hard carbon thin
film, as required by the claims. Second, Patent Owner argues that the
structures of Menu are not graded carbon compositions. We discuss each
argument in turn below.
1. hard carbon thin film
Patent Owner argues that Menu’s disclosure that the structure is
“amorphous” carbon does not necessarily mean that it is diamond-like, or
hard. PO Resp. 19; see also Ex. 1017, 53 (Q: “Are amorphous carbon films
diamond-like carbon films?” KANER: “Not necessarily.”). Rather, Patent
Owner directs us to Menu’s disclosure that its first-phase (outer) layers are
“rich in sp2 bonds,” as compared to the second-phase (inner) layer that is
“rich in sp3 bonds.” PO Resp. 20 (citing Ex. 1002, 7:53–57). In addition,
Menu discloses that its layers have distinct physical, chemical, and electrical
properties, and that the outer layers have a low resistivity. Ex. 1002, 3:4–25.
From these disclosures, Patent Owner contends that a person of ordinary

10 Patent Owner also raises two arguments directed to the sufficiency of the
analysis set forth in the Petition, claiming that it fails to establish a “clear
and unambiguous disclosure” of the elements of claim 1 (“Petitioner’s
anticipation ‘analysis’ with regard to Menu must fail as it is the epitome of
ambiguity”), or fails to set forth the elements “arranged as in the claim”
(“the Petition reads more like an obviousness analysis picking and choosing
multiple distinct teachings”). PO Resp. 14–19. We consider these
objections to be without merit, as the Petition identifies the grounds with
sufficient particularity to comply with the statute and our Rules. See 35
U.S.C. § 312(a)(3); 37 C.F.R. § 42.104(b)(4).
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skill in the art would have understood that the outer layers of Menu are
graphitic, while the inner layer is diamond-like, taking the structure of Menu
outside the scope of claim 1’s hard carbon thin film. PO Resp. 21.
Petitioner disagrees, arguing that Menu equates the term “amorphous
carbon” with “diamond-like carbon,” and thus the disclosed “amorphous
carbon multi-layered structures” are diamond-like in character overall.
Reply 11. Menu also discloses that its structures may be used in “hard
coatings.” Id. (citing Ex. 1002, 12:58). Petitioner contends that a person of
ordinary skill in the art would not have understood Menu’s description of the
outer layers as “rich in sp2 bonds” to imply that the layers were graphitic,
noting that the ’399 patent itself uses the phrase “sp2-rich” in the context of a
hard carbon film. Id. at 13–14 (citing Ex. 1001, 18:55–61). Rather,
Petitioner argues, the description of layers as “rich” in sp2 or sp3 bonding
merely describes the composition of the layers in relative terms. Id. at 14.
Upon review of the reference, the expert testimony, and the parties’
arguments, we find that the amorphous carbon structures of Menu are hard
carbon thin films. While we agree with Dr. Kaner’s testimony that the
general usage of “amorphous carbon films” may encompass both diamond-
like and graphitic carbon, we also agree with Dr. Hersam that Menu is using
the term in a more limited way, as synonymous with “diamond-like carbon.”
See Ex. 2022, 62. Menu discusses “the need for an improved method for
fabricating DLC [diamond-like carbon] superlattice structures” (Ex. 1002,
1:38–40), and it is reasonable to conclude that the method disclosed is
directed to addressing this need. In addition, as Petitioner points out, Menu
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refers initially to “amorphous carbon, or ‘diamond-like carbon’ (DLC)” (id.
at 1:25–28), implying that the terms are being used synonymously.
The reference to Menu’s first-phase outer layers as “rich in sp2 bonds”
(id. at 53–56) does not persuade us otherwise. As Petitioner notes, the ’399
patent uses the same terminology when referring to hard carbon films,
suggesting that “rich in sp2” does not imply graphitic. Furthermore, as
discussed above, there is a wide range of carbon films within the scope of
hard carbon thin films, including films having at least 75% sp2 bonding.
Such films can reasonably be termed “rich in sp2” bonds, yet still fall within
the domain of diamond-like carbon.
Finally, the disclosure that Menu’s layers have distinct properties does
not convince us that the first phase must be graphitic while the second is
diamond-like. At the oral hearing, Patent Owner’s counsel agreed that two
compositions within the diamond-like carbon domain could have distinct
chemical, physical, or electrical properties. Tr. 43. This is consistent with
the ternary phase diagram of Robertson, which shows various types of
diamond-like carbon having distinct properties. Ex. 2021, Figure 2. For
example, Table 1 of Robertson shows tetrahedral amorphous carbon (ta-C)
having a hardness of 80 GPa and a band gap of 2.5 eV, whereas hard
hydrogenated amorphous carbon (a-C:H hard) has a hardness of 10–20 GPa
and a band gap of 1.1–1.7 eV. Id. at 130. We conclude that Menu’s layers
could have distinct properties, while still remaining within the domain of
hard carbon thin films.
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2. graded carbon composition
Patent Owner also contends that Menu’s structure cannot be a graded
carbon composition, as required by claim 1, for two reasons. PO Resp. 23–
25. First, Figure 3 of Menu is said to disclose a second application of
ǀUsǀmin, which would result in a fourth layer similar in composition to the sp3-
rich, second-phase inner layer. Id. at 24 (citing Ex. 1002, Fig 3). Second,
Patent Owner points to the “transition layers” of Menu, labeled as 104 in
Figure 1 below:

Figure 1 of Menu depicts “a cross-sectional view of a structure which is
realized by performing various steps of a method in accordance
with the [Menu] invention.” Ex. 1002, 2:37–39.
Figure 1 of Menu depicts a multi-layered structure, comprising “first-
phase layers 102 includ[ing] layers of amorphous carbon which are rich in
sp2 bonds, and second-phase layer 103 includ[ing] a layer of amorphous
carbon which is rich in sp3 bonds.” Ex. 1002, 7:54–57. As Patent Owner
emphasizes, however, Figure 1 also discloses transition layers 104, which
have “chemical compositions” that “are not the same due to the different
deposition conditions at the time the voltage step changes are made.” Id. at
7:67–8:2. The voltage changes are fast, however, “so that transition layers
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104 have thicknesses, t, which are less than one atomic layer.” Id. at 7:65–
67.
According to Patent Owner, “any alleged gradation in sp²/sp³ ratio
from first-phase layer 102 to second-phase layer 103 back to first-phase
layer 102 is interrupted by two additional layers of an unknown and
uncertain composition.” PO Resp. 25. Characterizing the composition of
the transition layers as “unknown,” Patent Owner posits that the layers 104
could have more sp3 bonding than the interior second-phase layers 103,
resulting in an increase in sp3 bonding towards the exterior of the
composition at the 103/104 transition. Id. at 25. Patent Owner argues that
this would mean that the structure of Menu cannot be a graded carbon
composition as used in the ’399 patent claims.
We find that a preponderance of the evidence supports a finding that
Menu discloses a graded carbon composition, and do not find either of
Patent Owner’s arguments to the contrary to be persuasive. First, contrary to
Patent Owner’s interpretation of Figure 3 of Menu, the embodiment of
Figure 1 clearly depicts only three layers, with two extremely thin transition
layers in between. In any event, we do not consider a four-layer
embodiment, with alternating sp2 and sp3 content, to fall outside the scope of
graded carbon composition. The claim language only requires that the
sp2/sp3 ratio decreases toward an internal location of the thin film, and then
increases from a minimum toward the surface of the film. Nothing in the
claim, or elsewhere in the ’399 patent, requires that the sp2/sp3 ratio only
increase once past the minimum, or that the increase continue all the way to
the surface; it merely requires that it increase toward the surface for some
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distance. Importantly, the ’399 patent discloses that a stepwise change in
sp2/sp3 ratio is a graded carbon composition, irrespective of the fact that the
ratio is constant in between the stepwise changes. Ex. 1001, 25–30. Nor
does the claim language exclude the presence of multiple minima or more
than three layers; claim 1 uses the transition phrase “comprising,” and
therefore permits the inclusion of additional elements.
Similarly, we do not conclude that the existence of transition layers
104 in the Menu structure prevents it from being a graded carbon
composition. As just noted, nothing in the claim restricts the number of
layers present in the film. Nor does Patent Owner’s speculation that
transition layers 104 could have a higher sp3 content than second-phase layer
103 convince us otherwise. Because the ion impinging energy is
transitioning between ǀUsǀmax and ǀUsǀmin—or vice versa—at the time
transition layers 104 are formed, it is more reasonable to conclude that
transition layers 104 have sp2/sp3 ratios somewhere between that of first-
phase layers 102 and second-phase layer 103. Even if Patent Owner were
correct that transition layers 104 have high sp3 content, this would merely
mean the sp2/sp3 ratio reaches its minimum at the transition layer before
increase again toward the surface into the first-phase layer. Such an
arrangement would also fall within the scope of claim 1, which does not
require the sp2/sp3 to be located in any particular layer.
For the foregoing reasons, we find that Menu discloses a hard carbon
thin film having a graded carbon composition as set forth in claim 1 of the
’399 patent. We, therefore, conclude that Menu anticipates claim 1.
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C. Anticipation by Hirochi
Petitioner also asserts that claim 1 is unpatentable under 35 U.S.C.
§ 102 as anticipated by Hirochi. Pet. 39–51. Upon review of the Petition,
the experts’ testimony, and the reference, we find that Hirochi discloses all
of the elements of claim 1.
Hirochi discloses hard carbon films formed by ion-beam sputtering on
the surface of a substrate. Ex. 1005, Abstract. In its third embodiment,
Hirochi discloses that a buffer film is first formed adjacent to the substrate,
followed by a hard carbon film, and then a lubricative film. Id. at 3:55–4:7.
This embodiment is depicted in Figure 4 of Hirochi:

Figure 4 of Hirochi depicts an embodiment comprising substrate 11, buffer
film 31, hard carbon film 12, and lubricative film 13.

The film of Hirochi is formed by sputtering a carbon target using an
ion-beam of argon gas, in which the hydrogen component of the argon gas
can be varied. Id. at 4:21–28. Buffer layer 31 containing both carbon and
hydrogen is first formed on a substrate, and the hydrogen content gradually
increases as the layer is deposited, reaching a maximum at hard carbon film
12. Id. at 3:58–61. The hydrogen content is held steady within hard carbon
film 12, and then decreases gradually to the surface of lubricative layer 13.
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Id. at 3:61–66. This gradual increase and decrease of hydrogen
concentration is depicted in Figure 4A, below:

Figure 4A of Hirochi depicts the gradual change in hydrogen content over
the distance from the substrate surface.

According to Hirochi, Raman spectroscopic analysis of the
embodiment of Figure 4 “confirmed that the structures of the lubricative film
13 and the buffer film 31 are of graphite-like carbon and that of the hard
carbon film 12 is of diamond-like carbon.” Ex. 1005, 4:61–66. Dr. Hersam
concludes from this disclosure that the lubricative film and buffer film have
relatively high sp2/sp3 ratios, while the hard carbon film has a low sp2/sp3
ratio. Ex. 1007 ¶ 102. Petitioner, therefore, contends that Hirochi discloses
all elements of claim 1.
As with Menu, Patent Owner makes two substantive arguments
regarding the disclosure of Hirochi. First, Hirochi allegedly does not
disclose a hard carbon thin film. Second, Patent Owner argues that Hirochi
does not vary the sp2/sp3 ratio of its layers, but rather adjusts the hydrogen
content. We discuss each argument below.
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1. hard carbon thin film
As it did with Menu, Patent Owner first argues that Hirochi does not
disclose a hard carbon thin film. In particular, Patent Owner directs us to
Hirochi’s disclosure that the outer layers (buffer and lubricative films) are
graphitic carbon. PO Resp. 29–31 (citing Ex. 1005, 4:61–66). As such,
these layers cannot be part of the hard carbon thin film as claimed. Patent
Owner, therefore, argues that the only layer of Hirochi that may be
considered for anticipation purposes is the hard carbon film inner layer. Id.
at 32. As depicted in Figure 4A, however, this layer has a constant
composition across its thickness and therefore is not “graded” as required for
claim 1. Id.
Petitioner responds by arguing that the outer layers of Hirochi are
hard carbon, noting that the reference states that the lubricative film may be,
“for instance, a hard carbon film.” Ex. 1005, 4:13–14. Arguing that the
term “graphite-like” is used only in a sense relative to the harder, diamond-
like inner layer, Petitioner contends that the films overall have
characteristics sufficient to make them hard carbon films. Reply 21–23.
Upon review of the reference and the experts’ testimony, we agree
that Hirochi uses conflicting terminology in describing the composition of
its buffer and lubricative layers. Patent Owner correctly notes that Hirochi
characterizes the layers, at least as formed in the process described in
column 4 of the specification, as “graphite-like carbon.” Claim 18 of
Hirochi, cited in the Petition, also requires the buffer layer to have a
“graphitic structure.” Ex. 1005, 7:37–8:3. At the same time, Petitioner is
also correct that the lubricative layer is said to be “hard carbon film.” We
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also note that the lubricative film is described as a carbon film having
“hydrogen concentration . . . equal to or smaller than that of the hard carbon
film,” but that in addition to such carbon films the lubricative layer can also
be graphite. Id. at 2:37–50. Claim 18 is similarly broad, indicating that the
lubricative film consists essentially of at least one constituent selected from
a group that includes “graphitic-structure carbon” and “carbon with up to 50
percent hydrogen,” implying that the lubricative film can be either graphitic
or non-graphitic.
Regardless of this ambiguity, however, we find that Hirochi discloses
the claimed hard carbon thin film. As Petitioner notes, even if the outer
portions of the lubricative and buffer layers are graphitic, Figure 4A shows
that the structure changes gradually over the thickness of the layers. Reply
22 (citing Ex. 1005, 3:55–66). The inner portions of the lubricative and
buffer layers of Hirochi have compositions with only slightly less
hydrogen—and, therefore, that are only slightly less hard—than the hard
carbon film layer, which the parties agree is diamond-like. As argued by
Petitioner, “[a]t a minimum, the claim limitations would be met by
considering hard carbon film 12, and at least the initial portions of films 31
and 13 where the transition begins and entails a rise in the sp2/sp3 ratio, as
required by claim 1.” Reply 23. We agree with Petitioner that these inner
portions of Hirochi’s film meet the hard carbon thin film requirement of
claim 1. As discussed above with respect to Menu, claim 1 is an open-ended
“comprising” claim, and, therefore, the inclusion of additional, graphitic
layers on the outer portions of the film does not remove Hirochi from the
scope of claim 1.
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2. ratio of sp2 to sp3 carbon-carbon bonding
As Patent Owner correctly notes, Hirochi does not discuss the amount
of sp2 or sp3 bonding in the layers of its film, or indeed mention the type of
carbon-carbon bonds at all. PO Resp. 33. Petitioner instead relies on
Hirochi’s description of the physical characteristics of the layers to infer the
degree of sp2 and sp3 bonding. Pet. 40–41; Ex. 1007 ¶ 102. Patent Owner
disagrees with this conclusion, arguing that the characteristics of the layers
are varied by changing the hydrogen content of the film, not by varying the
sp2/sp3 ratio in the layer. PO Resp. 33–34. Dr. Kaner testified that a person
of ordinary skill in the art “would have found it difficult to understand how
or why the variation in hydrogen content varies the sp2/sp3 carbon-carbon
bonding ratio in the films.” Ex. 2028 ¶ 116.
On cross-examination, however, Dr. Kaner contradicted this
testimony, testifying that:
[O]ne of the things that hydrogen does is it actually eats sp2
graphitic-type carbon. It also actually eats sp3 diamond-like
carbon. However, it eats the graphitic carbon at a much faster
rate. Often on the order of three orders of magnitude faster. So
by controlling the amount of hydrogen in the deposition, you
can control the sp2/sp3 ratio.

Ex. 1017, 94. In fact, Dr. Kaner specifically stated that in the context of the
’399 patent, “hydrogen is used to scavenge the sp3. And so to control the
ratio of sp2/sp3.” Id. at 108; see also Ex. 1001, 14:14–19 (varying sp2/sp3
ratio by varying the supply of hydrogen into the reaction chamber).
Later in his testimony, Dr. Kaner attempted to distinguish the ’399
patent’s use of hydrogen to control the sp2/sp3 ratio from Hirochi’s use of
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hydrogen, which he said was used to make hydrogenated films (in other
words, to incorporate hydrogen into the film itself). Ex. 1017, 155. We do
not find this distinction to be credible. Both the ’399 patent and Hirochi use
hydrogen in the same manner, by introducing it as a gas into the reaction
chamber during formation of the carbon film. Compare Ex. 1001, 13:14–17,
25–29 (hydrogen introduced into chamber containing argon and methane
gas) with Ex. 1005, 4:30–32 (hydrogen component of argon gas in chamber
is varied). Patent Owner does not explain, nor does the record reflect, any
reason why Hirochi’s methods would result in incorporation of hydrogen
into the film while the ’399 patent methods do not. Furthermore, as
Dr. Kaner acknowledges, the hard carbon thin films of the ’399 patent
include hydrogenated films. Ex. 1017, 151.
From this record, we conclude that the use of hydrogen in Hirochi
achieves the same result as disclosed in the ’399 patent; namely, variation of
the ratio of sp2/sp3 bonding. By increasing the hydrogen content of the
chamber during formation of the film, Hirochi also increases the amount of
sp3 bonding relative to sp2 bonding, causing the sp2/sp3 ratio to decrease to a
minimum in the inner hard carbon film layer. Similarly, gradually
decreasing the amount of hydrogen causes the sp2/sp3 ratio to increase from
the minimum toward the surface of the Hirochi film. We find that Hirochi
discloses a graded carbon composition in which the sp2/sp3 ratio is varied, as
required by claim 1.
For the foregoing reasons, we find that Hirochi discloses a hard
carbon thin film having a graded carbon composition as set forth in claim 1
of the ’399 patent. We, therefore, conclude that Hirochi anticipates claim 1.
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III. CONCLUSION
We conclude that Petitioner has demonstrated, by a preponderance of
the evidence, that claim 1 of the ’339 patent is unpatentable under 35 U.S.C.
§ 102 as anticipated separately by Menu and Hirochi.
IV. ORDER
Accordingly, it is
ORDERED that claim 1 of U.S. Patent No. 6,066,399 is unpatentable;
FURTHER ORDERED that, pursuant to 35 U.S.C. § 318(b), upon
expiration of the time for appeal of this decision, or the termination of any
such appeal, a certificate shall issue canceling claim 1 in U.S. Patent No.
6,066,399; and
FURTHER ORDERED that, because this is a final decision, parties to
the proceeding seeking judicial review of the decision must comply with the
notice and service requirements of 37 C.F.R. § 90.2.
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PETITIONER:

Reginald J. Hill
rhill@jenner.com

Chad J. Ray
cray@jenner.com

Pavan K. Agarwal
pagarwal@foley.com

Michael R. Houston
mhouston@foley.com

PATENT OWNER:

Jason D. Eisenberg
jasone-PTAB@skgf.com

John P. McGroarty
jmcgroarty-PTAB@skgf.com

Robert Greene Sterne
rsterne-PTAB@skgf.com

Nicholas J. Nowak
nnowak-PTAB@skgf.com

Jonathan H. Takei
jonathan.takei@ipvalue.com

Boaz Brinkman
boaz.brinkman@ipvalue.com