Ex Parte Drzal et al

Board of Patent Appeals and Interferences

Sep 27, 2011

11435471 (B.P.A.I. Sep. 27, 2011)

UNITED STATES PATENT AND TRADEMARKOFFICE
UNITED STATES DEPARTMENT OF COMMERCE
United States Patent and Trademark Office
Address: COMMISSIONER FOR PATENTS
P.O. Box 1450
Alexandria, Virginia 22313-1450
www.uspto.gov
APPLICATION NO. FILING DATE FIRST NAMED INVENTOR ATTORNEY DOCKET NO. CONFIRMATION NO.
11/435,471 05/17/2006 Lawrence T. Drzal MSU 4.1-799 6292
7590 09/28/2011
Ian C. McLeod
McLeod & Moyne, P.C.
2190 Commons Parkway
Okemos, MI 48864
EXAMINER
NILAND, PATRICK DENNIS
ART UNIT PAPER NUMBER
1762
MAIL DATE DELIVERY MODE
09/28/2011 PAPER
Please find below and/or attached an Office communication concerning this application or proceeding.
The time period for reply, if any, is set in the attached communication.
PTOL-90A (Rev. 04/07)
1

UNITED STATES PATENT AND TRADEMARK OFFICE
________________

BEFORE THE BOARD OF PATENT APPEALS
AND INTERFERENCES
________________

Ex parte LAWRENCE T. DRZAL and
HIROYUKI FUKUSHIMA
________________

Appeal 2010-005104
Application 11/435,471
Technology Center 1700
________________

Before LINDA M. GAUDETTE, MARK NAGUMO, and
MICHAEL P. COLAINNI, Administrative Patent Judges.

GAUDETTE, Administrative Patent Judge.

DECISION ON APPEAL
Appellants appeal under 35 U.S.C. § 134(a) from the Examiner’s
decision1 finally rejecting claims 1-26, the only claims pending in the
Application.2 We have jurisdiction under 35 U.S.C. § 6(b).
We AFFIRM.
The invention relates to polymer-expanded graphite composites.
(Spec.3 [0004].) The expanded graphite used in the composites “is one
which has been heated with radiofrequency waves and microwaves in a

1 Final Office Action mailed Sep. 11, 2007.
2 Supplemental Appeal Brief filed Aug. 14, 2009 (“App. Br.”).
3 Specification filed May 17, 2006.
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gaseous atmosphere to separate individual platelets of graphite.” (Spec.
[0072].) “The use of microwave energy or RF induction heating” is said to
“provide[] a fast and economical method to produce expanded graphite
nanoflakes, graphite nanosheets, or graphite nanoparticles.” (Spec. [0073].)
Independent claim 1 is representative of the invention, and is
reproduced below from the Claims Appendix to the Appeal Brief:
1. A composite composition which comprises in admixture:
(a) a polymer; and
(b) microwave or radiofrequency wave expanded graphite platelets,
which were expanded from a graphite containing an intercalcant by boiling
the intercalcant with radiofrequency or microwaves for up to five minutes
and are optionally pulverized, in admixture in the polymer, wherein the
platelets are present in an amount which provides electrical conductivity
properties or provides barrier properties to gases or liquids or a combination
of these properties.
Appellants request review of the following rejections (App. Br. 6):
1. Claims 1-26 under 35 U.S.C. §112, first paragraph, as failing to
comply with the written description requirement (Ans.4 3);
2. Claims 1-9, 11-16, 18-20 and 22-26 under 35 U.S.C. §102(b) as
anticipated by Saito (US 6,024,900, issued Feb. 15, 2000) (Ans. 3-6);
3. Claims 1-9, 11-16, 18-20 and 22-26 under 35 U.S.C. §103(a) as
unpatentable over Saito (Ans. 6-9); and
4. Claims 10 and 17 under 35 U.S.C. §103(a) as unpatentable over
Saito in view of Krassowski (US 6,395,199 B1, issued May 28, 2002) (Ans.
9-10).

4 Examiner’s Answer mailed Jun. 6, 2008.
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Rejection under 35 U.S.C. §112, first paragraph,
written description requirement
The Examiner finds the Application, as originally filed, fails to
provide support for “boiling the intercalcant” for time periods within the
entire claim range of “for up to five minutes” as required by each of the
independent claims, claims 1, 3, 7, 13, 14, 15, 16 and 23. (Final 2, Ans. 3.)
Appellants have not argued the Examiner’s reasons are insufficient to meet
the initial burden of establishing lack of support under 35 U.S.C. § 112, ¶ 1.
(See App. Br. 7.) Thus, the sole issue raised for our consideration with
respect to the first ground of rejection is:
Have Appellants identified disclosure in the originally filed
Application which clearly allows one of ordinary skill in the art to recognize
that Appellants invented a composite composition comprising “graphite
platelets, which were expanded from a graphite containing an intercalcant by
boiling the intercalcant with radiofrequency or microwaves for” time periods
over the entire range of “up to five minutes” as recited in each of the
independent claims?5
Appellants rely on Specification paragraphs [0075] and [0080] for
written description support. (See Rep. Br.6 5.) Paragraph [0075] reads, in
relevant part: “Heating for 3 to 5 minutes removes the expanding chemical.

5 “The test for sufficiency of a written description is ‘whether the disclosure
clearly “allow[s] persons of ordinary skill in the art to recognize that [the
inventor] invented what is claimed.”’” Crown Packaging Technology, Inc. v.
Ball Metal Beverage Container Corp., 635 F.3d 1373, 1380 (Fed. Cir. 2011)
(quoting Ariad Pharms., Inc. v. Eli Lilly & Co., 598 F.3d 1336, 1351 (Fed.
Cir. 2010) (en banc) (quoting Vas–Cath Inc. v. Mahurkar, 935 F.2d 1355,
1562-63 (Fed. Cir. 1991))).
6 Reply Brief filed Jul. 3, 2008.
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The graphite absorbs the RF or microwave energy very quickly without
being limited by convection and conduction heat transfer mechanisms. The
intercalant heats up past the boiling point and causes the graphite to expand
to many times its original volume.” Paragraph [0080] describes EXAMPLE
1, in which expanded graphite was prepared by exposing “[i]ntercalated
graphite flakes . . . to microwave energy, typically at 2.45 GHz frequency,
for a few seconds to a few minutes in an oven.”
The claims require “graphite platelets, which were expanded from a
graphite containing an intercalcant by boiling the intercalcant with radio
frequency or microwaves for up to five minutes.” (Claims 1, 3, 7, 13, 14, 15,
16 and 23 (emphasis added).) Appellants argue, and we agree, that the
phrase “for up to five minutes” does not encompass 0 minutes, since the
claims require “boiling,” which must necessarily take place for some period
of time. (App. Br. 7.) However, we interpret the phrase “for up to five
minutes” as encompassing a fraction of second. Appellants have not
identified, nor do we find, any basis in the Specification or claims which
supports a narrower interpretation of the claimed range.
The Specification provides support for exposing graphite flakes to
microwave energy for a minimum time period of “a few seconds” and a
maximum time period of five minutes. However, the Specification fails to
indicate at what point during the exposure to radio frequency or microwaves,
the intercalcant begins to boil. Appellants have not directed us to any
evidence which demonstrates that one of ordinary skill in the art would have
understood from the originally filed Application that the inventors were in
possession of a composite composition comprising “expanded graphite
platelets, which were expanded from a graphite containing an intercalcant by
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boiling the intercalcant with radiofrequency or microwaves for up to five
minutes.” (Claims 1, 3, 7, 13, 14, 15, 16 and 23 (emphasis added).) See
Carnegie Mellon Univ. v. Hoffmann-La Roche Inc., 541 F.3d 1115, 1122
(Fed. Cir. 2008) (explaining that to satisfy the written description
requirement, an “applicant must ‘convey with reasonable clarity to those
skilled in the art that, as of the filing date sought, he or she was in possession
of the invention,’ and demonstrate that by disclosure in the specification.”
(quoting Vas-Cath Inc. v. Mahurkar, 935 F.2d 1555, 1563-64 (Fed. Cir.
1991))).
Accordingly, we affirm the rejection of claims 1-26 under 35 U.S.C.
§112, first paragraph, as failing to comply with the written description
requirement.
Rejections under 35 U.S.C. §102(b) & §103(a)
With respect to the prior art rejections, Appellants do not advance
arguments in support of separate patentability of any particular claim or
claim grouping. Rather, Appellants’ traversal of the prior art rejections is
based on their contention that Saito fails to disclose graphite platelets “which
were expanded from a graphite containing an intercalcant by boiling the
intercalcant with radio frequency or microwaves for up to five minutes” as
required by each of the independent claims. (See App. Br. 8.) Appellants
concede that Saito does disclose graphite platelets expanded from a graphite
by a conventional high temperature treatment. (See App. Br. 9.) The
Examiner has correctly noted that the argued claim language is not a
structural limitation, but describes the graphite platelets by the process used
to obtain them. (See Final 3; Ans. 4; App. Br. 10 (“The graphite platelets in
the claims of the present application have been described by a product-by-
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process limitation.”).) Thus, the sole issue raised for our consideration with
respect to the above-listed grounds of rejection 2-4 is:
Have Appellants met their burden to show that the claimed graphite
platelets are structurally different from Saito’s graphite platelets?7
Saito discloses that production of expanded graphite can be conducted
from a known process, such as by mixing concentrated sulfuric acid with
hydrogen peroxide to form peroxomonosulfuric acid, adding raw material
graphite with stirring to give rise to a reaction for about 1 hour to 1 day, and
heating the reacted graphite at 500-1000 ºC. (Col. 2, ll. 59-65.) According
to Appellants, this is a conventional heating process to expand graphite.
(App. Br. 9.)
As evidence of a difference between the claimed graphite platelets and
those prepared by a conventional heating process, Appellants rely on
evidence in the Specification and the Declaration of Lawrence T. Drzal8, a
named inventor in the present application. Prof. Drzal relies on the

7 See In re Thorpe, 777 F.2d 695, 697 (Fed. Cir. 1985) (citations omitted)
(“The patentability of a product does not depend on its method of
production.”); In re Best, 562 F.2d 1252, 1255 (CCPA 1977) (citations
omitted) (“Where . . . the claimed and prior art products are identical or
substantially identical, or are produced by identical or substantially identical
processes, the PTO can require an applicant to prove that the prior art
products do not necessarily or inherently possess the characteristics of his
claimed product. Whether the rejection is based on ‘inherency’ under 35
U.S.C. § 102, on ‘prima facie obviousness’ under 35 U.S.C. § 103, jointly or
alternatively, the burden of proof is the same, and its fairness is evidenced
by the PTO's inability to manufacture products or to obtain and compare
prior art products.”); In re Spada, 911 F.2d 705, 708 (Fed. Cir. 1990).

8 Declaration under 37 C.F.R. § 1.132, executed Jun. 21, 2006 (“Dec.”),
included in the Evidence Appendix to the Appeal Brief.
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dissertation of Mr. Hiroyuki Fukushima (Dec. ¶ 4 (citing Exhibit A9)), also a
named inventor in the present application. (See App. Br. 11-13.) Appellants
contend the evidence shows that graphite expanded by a microwave or
radiofrequency process for up to 5 minutes has a higher degree of expansion,
less residual expander, and a cleaner surface than graphite expanded by a
heat treatment. (App. Br. 11.)
The experiments described in the Specification were conducted using
“a commercial microwave oven operating at 2.45 GHz.” (Spec. [0076].)
FIG. 4 of the Specification reveals that the experiments included preparing
expanded graphite by microwaving at 1040W for 3 minutes.
According to Mr. Fukushima,
[t]here are several methods to expand GICs [(graphite
intercalated compounds)]. The most commonly used technique
is the rapid heating in a furnace. This is widely used in the
commercial stage. Other methods can include infrared laser,
microwave, and electric current. Among these, microwave
systems are available in many sizes and power levels.

(p. 71 (emphasis added).) Mr. Fukushima investigated the effects of
“temperature, microwave power, and the size of graphite flakes on degree of
expansion” and “the surface chemistry of the exfoliated graphite samples.”
(p. 71.)
A comparison was made between expanded graphite prepared from
various sizes of graphite flakes by heating at 900 ºC for 5 minutes (p. 76)
and by microwaving at 900W, 2.45 GHz for 5 seconds (p. 8210). With

9 The appeal record includes pages 70-98 of the Fukushima dissertation.
The date of the dissertation is not identified in the appeal record.
10 Contra p. 83, Figure 2.6, which identifies the samples as microwaved at
1300 W.
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respect to the heating process, Mr. Fukushima “concluded that graphite
flakes of 75 µm or larger size show good expansion, and those of 180 µm or
larger show the maximum expansion.” (p. 76.) With respect to the
microwave process, Mr. Fukushima concluded “the larger the size, the better
the expansion.” (p. 82.) According to Mr. Fukushima, the comparison
revealed “that microwave process could give the same or better degree of
expansion for graphite flakes.” (p. 82 (emphasis added).)
A comparison was also made between expanded graphite prepared
from graphite 160-50A11 by heating for 3 minutes at temperatures of 300,
400, 500, 600, 700, 800, 900 and 1000 ºC (p. 75), and by microwaving at
powers of 650, 780, 910, 1040, 1170, and 1300 W for an undisclosed time
period (p. 87, Figure. 2.10). According to Mr. Fukushima, the comparison
“revealed that overall microwave treatment showed a better degree of
expansion than conventional heating process.” (p. 84.)
“BET surface areas of heat or microwave treated samples were
measured to estimate the degree of expansion.” (p. 84.) According to Mr.
Fukushima, “[t]he surface areas of microwave exfoliated graphite samples
were more than 4 times larger than those of the heat exfoliated samples.”
(Id.) The copy of the dissertation in the appeal record does not include the
details of the heat and microwave treatments used to prepare the samples on
which the BET surface areas were measured.
On page 89 of the dissertation, Mr. Fukushima explains:

11 “Grafguard ™160-50A[:] . . . ‘160’ refers to the onset temperature at
which intercalated acid begins to be released and exfoliation of the graphite
occurs. ‘50’ indicates the average size of the flakes is 50 mesh, which is 300
µm. A, B, and N show the conditions of the sample surface, which are
acidic, basic, and neutral.” (p. 72.)
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To investigate the surface condition of expanded graphite, XPS
(X-Ray Photoelectron Microscopy) data were collected and
analyzed. Figure 2.15 shows the sulfur/carbon and
nitrogen/carbon ratio of the expanded graphite. Sulfur content
suggests the existence of sulfuric acid while nitrogen implies
nitric acid. At 600°C treatment, the sulfur and nitrogen
components were detected even after 10 minutes of treatment.
At 800°C, these components were almost removed from the
sample after 5 minutes of treatment. At l000 °C, it required
about 2 minutes to remove these components. Figure 2.16
shows the XPS results of expanded graphite by microwave
treatment. In this case, the sulfur and nitrogen component were
removed after 2 minutes treatment at 910W and 1300W. This
implies that the microwave treatment also has advantage over
conventional heating process in terms of removal of the residual
intercalates.

(Emphasis added.) Figure 2.16 shows that the sulfur and nitrogen
components were not removed after a 5 minute treatment at 780W. (p. 93.)

Evidence of secondary considerations must be reasonably
commensurate with the scope of the claims. This does not
mean that an applicant is required to test every embodiment
within the scope of his or her claims. If an applicant
demonstrates that an embodiment has an unexpected result and
provides an adequate basis to support the conclusion that other
embodiments falling within the claim will behave in the same
manner, this will generally establish that the evidence is
commensurate with scope of the claims.

In re Kao, 639 F.3d 1057, 1068 (Fed. Cir. 2011) (citations omitted).

Appellants’ “claims are silent regarding wattage of the claimed
microwaves or radiowaves, the particulars of the devices used to apply the
microwaves or radiowaves, the amount of power applied to the graphite, and
any other parameters required to particularly point out what exactly is made
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by the microwaving or radio frequency treating of graphite.” (Ans. 12.) The
claims do not recite the particle size of the graphite, identify the particular
intercalcant or its reaction time with the graphite. (See Ans. 13.) “Thus, the
[] claims read on a wide variety of [compositions and] products due to these
unknown and unclaimed factors.” (Ans. 12; cf. Spec. [0076] (“microwave
frequency across a wide range can be used”); Fukushima dissertation p. 71
(“microwave systems are available in many sizes and power levels”).)
The Examiner finds Appellants’ evidence is not commensurate in
scope with the claims, and concludes that Appellants have not demonstrated
a difference between the claimed and prior art expanded graphite platelets.
(Ans. 13-14.) We agree for the reasons detailed by the Examiner in the
Answer.
We have taken into account Prof. Drzal’s testimony that Mr.
Fukushima’s dissertation “illustrates [] graphite expanded by a microwave
process has superior properties as compared to graphite expanded by a heat
treatment.” (Dec. ¶4.) However, even accepting this statement as accurate,
we find the evidence in the dissertation (and in the Specification) insufficient
to support a conclusion that graphite expanded under conditions which were
not tested, but still fall within the scope of the claims, would be expected to
behave in the same manner. For example, the dissertation evidence shows
residual intercalcates can be removed in the same amount of time, 2 minutes,
using either conventional heating conditions, i.e., l000 °C (see Saito col. 2,
ll. 59-65), or microwave treatments at 910W and 1300W. However,
complete removal of residual intercalates is not possible at a microwave
treatment of 780W for 5 minutes. Thus, a conventional heat treatment of the
type used by Saito would appear to provide superior cleanness results to a
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microwave treatment falling within the scope of the claims. Likewise, as
acknowledged by Mr. Fukushima, particle size has an effect on expansion.
(See Fukushima dissertation p. 82 supra p. 8) Therefore, depending on the
particle size of the graphite, a microwave treatment may only give “the
same” degree of expansion as conventional heating. (Id.) While Mr.
Fukushima conducted heat treatments and microwave treatments over a
number of different temperatures and microwave powers, there is no
evidence the same results would be achieved for different treatment times,
i.e., times which were either less than or greater than 3 minutes.
Accordingly, because Appellants have not shown a difference
between the claimed and prior art graphite platelets, we affirm the rejections
under 35 U.S.C. §102(b) & §103(a).
No time period for taking any subsequent action in connection with
this appeal may be extended under 37 C.F.R. § 1.136(a)(1).

AFFIRMED
1

NAGUMO, Administrative Patent Judge, concurring

I respectfully dissent from the affirmance of the rejection for lack of
written description of the process limitation of “boiling the intercalcant with
radiofrequency or microwaves for up to five minutes.” The purpose of the
written description requirement is to prevent an applicant from claiming, at
some date after filing the application for patent, an invention that was not
originally described. The majority is willing to accept that zero time is
excluded because the process of boiling requires a finite amount of time.
(Op. 4.) The Specification states that “[t]he graphite absorbs the RF or
microwave energy very quickly without being limited by convection and
conduction heat transfer mechanisms.” (Spec. 21 [0075].) In my view, this
description provides support for boiling times down to the physical limits
afforded by the cross section for RF or microwave absorption by the
graphite and the processes by which that energy is converted to the random
motions of heat. This results in very broad claims indeed, but, in my view,
less broad than, for example, original claims 1-3, which specify no time
limits. I am unable to see what substantive value is gained by attempting to
impose a greater precision in claim language than the art normally requires.
The problems associated with providing such a broad definition of the
process are, in my view, more than adequately dealt with by requiring
Appellants to distinguish the claimed subject matter from the prior art. This
the Examiner has done. I join the majority in affirming the rejections over
prior art.

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