case 3:14-cv-01771-RLM-CAN document 1 filed 08/01/14 page 1 of 7
`
`IN THE UNITED STATES DISTRICT COURT
`FOR THE NORTHERN DISTRICT OF INDIANA
`SOUTH BEND DIVISION
`
`CERAMEDIC LLC,
`
`Plaintiff,
`
`Civil Action No. 14-cv-1771
`
`y.
`
`JURY DEMAND
`
`DEPUY ORTHOPAEDICS, INC.,
`
`Defendant.
`
`COMPLAINT
`
`CeraMedic LLC ("CeraMedic") hereby asserts claims of patent infringement against
`
`DePuy Orthopaedics, Inc. ("DePuy") and alleges as follows:
`
`THE PARTIES
`
`1 .
`
`CeraMedic is a Florida limited liability company having a place of business at
`
`2400 Dallas Parkway, Suite 200, Plano, TX 75093.
`
`2.
`
`On information and belief, DePuy Orthopaedics, Inc. is an Indiana corporation
`
`having a principal place of business at 700 Orthopaedic Drive, Warsaw, IN 46582.
`
`PATENT-IN-SUIT
`
`3.
`
`U.S. Patent No. 6,066,584 ("the '584 patent"), entitled "Sintered AL203 Material,
`
`Process for Its Production and Use of the Material" was lawfully issued on May 23, 2000, with
`
`the original assignee Fraunhofer-Gesellschaft zur Förderung der Angewandten Forschung e.V.,
`
`Germany ("Fraunhofer") . CeraMedic is the owner, through assignment, of the title, interest, and
`
`rights to enforce and collect damages for all past, present, and future infringements of the '584
`
`Exhibit 2322 Page 001
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

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`case 3:14-cv-01771-RLM-CAN document 1 filed 08/01/14 page 2 of 7
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`patent by the accused products and the use thereof. A copy of the '584 patent is attached as
`
`Exhibit A.
`
`BACKGROUND
`
`4.
`
`Fraunhofer is Europe' s largest application-oriented research organization. Its
`
`research efforts are geared entirely to people' s needs: health, security, communication, energy
`
`and the environment. As a result, the work undertaken by its researchers and developers has a
`
`significant impact on people' s lives. Fraunhofer was honored by Thomson Reuters as one of the
`
`Top 100 Global Innovators in 2013.
`
`5.
`
`Fraunhofer is the assignee of over 1,500 U.S. patents and was the original
`
`assignee of the '584 patent. In early 2014, Fraunhofer assigned ownership of the '584 patent to
`
`CeraMedic.
`
`6.
`
`The '584 patent relates to the field of ceramics and concerns sintered A1203
`
`compositions and methods for the use of such material as medical implants or tool material.
`
`7.
`
`On information and belief, CeramTec GmbH ("CeramTec") developed and
`
`manufactures BIOLOX® Delta, an aluminum oxide matrix composite ceramic comprising
`
`approximately 82% alumina (A1203), 17% zirconia (Zr02), and other trace elements.
`
`8.
`
`BIOLOX® Delta is
`
`incorporated into DePuy products,
`
`such as DePuy
`
`ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral Heads and DePuy 5-ROM® BIOLOX®
`
`Delta Ceramic Femoral Heads.
`
`9.
`
`DePuy ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral Heads and DePuy
`
`S-ROM® BIOLOX® Delta Ceramic Femoral Heads can be used in conjunction with compatible
`
`DePuy acetabular and femoral stem components for primary and revision total hip arthroplasty.
`
`2
`
`Exhibit 2322 Page 002
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

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`case 3:14-cv-01771-RLM-CAN document i
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`filed 08/01/14 page 3 of 7
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`10.
`
`On information and belief, DePuy is knowledgeable about the science behind
`
`BIOLOX® Delta material,
`
`including its composition, performance characteristics, and
`
`manufacture.
`
`11.
`
`On information and belief, DePuy designs, develops, manufactures, offers for
`
`sale, sells, uses, distributes, and markets hip implants, many of which include DePuy
`
`ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral Heads and/or DePuy S-ROM®
`
`BIOLOX® Delta Ceramic Femoral Heads.
`
`JURISDICTION AND VENUE
`
`12.
`
`This Court has subject matter jurisdiction pursuant to 28 U.S.C. § 1331 and 1338
`
`because this action arises under the patent laws of the United States, including 35 U.S.C. § 271 et
`
`seq.
`
`13.
`
`This Court has personal jurisdiction over DePuy because, among other things,
`
`DePuy' s headquarters are located in Warsaw, Indiana and because, on information and belief,
`
`DePuy engages in substantial and ongoing business in this District.
`
`14.
`
`On information and belief, DePuy offers to sell, sells, and distributes its DePuy
`
`ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral Heads and DePuy 5-ROM® BIOLOX®
`
`Delta Ceramic Femoral Heads, which infringe the '584 patent, to healthcare institutions and/or
`
`medical professionals within this District.
`
`15.
`
`Venue is proper in this judicial district pursuant to 28 U.S.C. §
`
`1391 and
`
`1400(b).
`
`COUNT I - INFRINGEMENT OF THE '584 PATENT
`
`16.
`
`CeraMedic realleges and incorporates by reference each of the preceding
`
`paragraphs.
`
`3
`
`Exhibit 2322 Page 003
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document i
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`filed 08/01/14 page 4 of 7
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`17.
`
`On information and belief, DePuy, directly or through the actions of its
`
`employees, divisions, and/or subsidiaries, has infringed and continues to infringe the '584 patent
`
`directly, literally, and/or by equivalents.
`
`18.
`
`On information and belief, DePuy has infringed and continues to infringe the '584
`
`patent literally and/or by equivalents under 35 U.S.C. § 27 i(a) by, among other things, importing
`
`BIOLOX® Delta ceramics, and making, using, offering for
`
`sale, and selling DePuy
`
`ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral Heads and DePuy 5-ROM® BIOLOX®
`
`Delta Ceramic Femoral Heads, individually and/or as part of hip replacement products.
`
`19.
`
`On information and belief, DePuy has infringed and continues to infringe the '584
`
`patent literally and/or by equivalents under 35 U.S.C. § 271(g) by, among other things, importing
`
`BIOLOX® Delta ceramics manufactured by CeramTec outside of the United States, which
`
`manufacture by CeramTec would infringe the ' 5 84 patent if it occurred in the United States.
`
`20.
`
`On information and belief, DePuy has infringed and continues to infringe the '584
`
`patent literally and/or by equivalents under 35 U.S.C. § 271(g) by, among other things, using,
`
`offering for sale, and selling DePuy ARTICUL/EZE® BIOLOX® Delta Ceramic Femoral
`
`Heads, DePuy 5-ROM® BIOLOX® Delta Ceramic Femoral Heads, and/or other products that
`
`include BIOLOX® Delta, individually and/or as part of hip replacement products, which
`
`products include BIOLOX® Delta manufactured by CeramTec outside of the United States,
`
`which manufacture by CeramTec would infringe the ' 584 patent if it occuned in the United
`
`States.
`
`2 1 .
`
`On information and belief, at least as of the filing of this Complaint, because
`
`DePuy knew of the '584 patent and knew of the science behind BIOLOX® Delta, including its
`
`manufacture, DePuy has ignored and/or disregarded that DePuy's
`
`actions
`
`constituted
`
`Exhibit 2322 Page 004
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

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`case 3:14-cv-01771-RLM-CAN document 1 filed 08/01/14 page 5 of 7
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`infringement of a valid patent and DePuy continues to ignore and/or disregard an objectively
`
`high risk that DePuy' s actions constitute infringement of a valid patent.
`
`22.
`
`On information and belief, at least as of the filing of this Complaint, DePuy' s
`
`infringement of the '584 patent is and has been willful and deliberate, and, further, DePuy' s
`
`continued infringement after the filing of this Complaint shall constitute willful and deliberate
`
`infringement of the ' 5 84 patent.
`
`DAMAGES AND RELIEF
`
`23.
`
`As a consequence of DePuy's infringement of the '584 patent, CeraMedic has
`
`been damaged in an amount not yet determined and will suffer additional ineparable damage
`
`unless DePuy' s infringing acts are enjoined by this Court.
`
`PRAYER FOR RELIEF
`
`WHEREFORE, CeraMedic respectfully requests that the Court enter judgment against
`
`DePuy:
`
`A.
`
`Determining that DePuy has infringed and continues to infringe one or more
`
`claims of the '584 patent;
`
`B .
`
`Preliminarily and permanently enjoining DePuy, its respective officers , agents,
`
`servants, directors, employees, and attorneys, and all persons acting in concert or participation
`
`with it, directly or indirectly, or any of them who receive actual notice of the judgment, from
`
`further infringing the ' 584 patent;
`
`C.
`
`Ordering DePuy to account for and pay to CeraMedic all damages suffered by
`
`CeraMedic as a consequence of DePuy' s infringement of the ' 584 patent, together with all pre-
`
`judgment and post-judgment interest and costs as fixed by the Court;
`
`5
`
`Exhibit 2322 Page 005
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document 1 filed 08/01/14 page 6 of 7
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`D.
`
`Trebling or otherwise increasing CeraMedic' s damages under 35 U.S.C. § 284 on
`
`the grounds that DePuy' s infringement of the '584 patent was deliberate and willful;
`
`E.
`
`Declaring that this case is exceptional and awarding ceraMedic its costs and
`
`reasonable attorneys' fees in accordance with 35 U.S.C. § 285; and
`
`F.
`
`Granting CeraMedic such other and further relief as the Court may deem just and
`
`proper.
`
`JURY DEMAND
`
`Pursuant to Rule 38 of the Federal Rules of Civil Procedure, CeraMedic hereby requests
`
`a trial by jury for all issues so triable.
`
`Exhibit 2322 Page 006
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document i
`
`filed 08/01/14 page 7 of 7
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`Dated: August 1, 2014
`
`By:
`
`Is! Laurie Stempler
`Laurie Stempler
`
`DESMARAIS LLP
`John M. Desmarais (pro hac vice forthcoming)
`Email: jdesmarais @desmaraisllp.com
`Laurie Stempler
`Email: lstempler@desmaraisllp.com
`Kevin K. McNish
`Email: kmcnish@desmaraisllp.com
`230 Park Avenue
`New York, NY 10169
`Telephone: (212)-351-3400
`Facsimile: (212)-351-3401
`
`James M. Lewis (15784-71)
`jlewis@thklawfirm.com
`Michael J. Hays (23606-7 1)
`mhays@thklawfirm.com
`TUESLY HALL KONOPA LLP
`212 E. LaSalle Avenue, Suite 100
`South Bend, IN 46617
`Telephone: 574-232-3538
`Facsimile: 574-232-3790
`
`Attorneysfor CeraMedic LLC
`
`'i
`
`Exhibit 2322 Page 007
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document 1-1 filed 08/01/14 page 1 of 12
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`EXHIBIT A
`
`Exhibit 2322 Page 008
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3: 14cvO1771R LMCAN docu rijflIflhjIIIJD I11IH1III11]I11 IflllhII IHHHID II
`US006066584A
`
`United States Patent
`
`H
`
`KrcII et al.
`
`Iii]
`
`[45]
`
`Patent Number:
`
`6,066,584
`
`Date of Patent:
`
`May 23, 2000
`
`[54] SINTERED ALO MATER1ÀL, PROCESS
`FOR ITS PRODUCTION AND USE 01 THE
`MATERIAL
`
`[58J Field ofSeareh ..................................... O1/127, 153,
`501/128, 132; 51/307, 309; 264/621, 653,
`603, 645
`
`[75]
`
`tnventørs: Andreìs Krell; PuI Blank, both of
`Dresden, Germany
`
`[56]
`
`References Cited
`U.S. PATENT DOCUMENTS
`
`[73] Assignee: Fraunhofer-GeseIIscjrnfL zur
`Förderung der Angewandten
`Forschung e.V.. Germany
`
`[21] App!. No.:
`
`0S1727,409
`
`[22]
`
`PCI Filed:
`
`Apr. 19, 1995
`
`[86]
`
`PCT No.:
`
`PCT/EI'95/01474
`Jan. 31, 1997
`§ 371 I)ate:
`§ tO(e) Date: Jan. 31, 1997
`[87] PCI Pub. No.: W095/28364
`PCI Pub. Date: Oct. 26, 1995
`Foreign Application Priority Datn
`
`[30]
`
`European Pat. Off ............... 94106040
`Apr. 19, 1994
`[EP]
`hit. CI.7 ..................................................... CO4B 35/tO
`31]
`[52] U.S. Cl ........................... Oh/127; 501/128; 01/132;
`501/153; 264/653; 2M/603; 264/645
`
`4,052,538 10/1977 Eddy et al ................................ 264f56
`811990 Hayashi el al .......................... 501/153
`4,952,537
`5/1992 Kunzea1 .............................. 501/127
`5,114,891
`6/1993 Halanaka et al ........................ 501/153
`5,215,551
`5,261,930 11/1993 Fliedner ei a] ........................... 51/309
`8/1996 Cornwell et al ........................ 501/153
`5,547,479
`7/1997 Moiiree et al .......................... 501/153
`5,645,618
`Primary Fxa,,iner-MichaeI Marcheschi
`Attorney, Ageni, or t7rm-Medlen & Carroll, LLP
`ABSTRACT
`[57]
`
`The invention relates to the field of ceramics and concerns
`sinteredAl,03 compositions prodticed from corundum pow-
`der and alsø methods for the lise of the invented coruposi-
`tions as medical implants or tool material. To produce such
`materials, an initially unsintered precursor having a relative
`density of p55% is produced from a..A1203 powder hay-
`ing defined properlies using at least two different dispersing
`methods, this precursor is subsequently subjected to heat
`treatment and sin tering.
`
`53 Claims, No Drawings
`
`Exhibit 2322 Page 009
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document 1-1 filed 08/01/14 page 3 of 12
`
`6,066,584
`
`i
`SINTERED AL2O MATERIAL, PROCESS
`FOR ITS PRODUCTION AND USE OF TIlE
`MATERIAL
`
`The iuventioii relates to the field of ce[amics and cou-
`cerns sintered ALO materials and processes for their pro-
`duction. The sintered materials can be used as medical
`implants, as wear products, as cutting tools or as abrasives.
`The inlerisive efforts of recent years aimed at pruduciug
`monolilhic Sjj]te[ed AL,Ø products having grain sizes of
`less than 2 pm and improved mechanical properties from
`corundum powder followed essentially two routes:
`use of very flue submicron or nanosize powders,
`addition uf substances to lower the temperature required
`for sintering lo lull density.
`Although the very flue starting materials have the desired
`high sintering activity, owing to their poor densification
`behaviour they at the same time bring with them consider-
`able problems in shaping. l'he low-cost uniaxial dry pressing
`process, which has hitherto been predominanily employed,
`leads to insufficient green density or to density inhomoge-
`neities in the shaped body and, on sintering, defects which
`reduce the hardness and strength. for these reasons, other
`shaping processes such as culd isustatic pressing, extrusiun,
`pressure or centrifugal casting or gel casting are empinyed.
`An Al,03 grain size ¡n the sintered body of 0.8 pm and a
`hardness ofHV2O'192O have been achieved by extrusion of
`ceramic compositions comprising submicron pnwders and
`siotering at 14(10° C. (G. Riedel, et al., Silicates Industriels
`(1989) 1/2,2Q-35). The powder used here had a mean
`particle size of 0.45 pm and a d
`value, which describes the
`width of the coarse particle fraction of the particle size
`distribution, of 1.0 pm.
`In the case ofvery fine AlO powders having d0<0.4um
`and a d8, value, which describes the width of the coarse
`particle fraction of the particle size distribution, of <0.7 pm,
`slip casting has also been successfully used recently (T-5h.
`Ych et al., .1. Am. Ceram. Soc. (1988), pp. 841-844), also in
`combination with the application of pressure (jressure Ill-
`tration: F. F. Lange et al., Bull. Aro. Ceram. Soc. (1987), pp.
`1498-1504; Vacuum Pressure Filtration: H. Mizuta et al., J.
`Arrt. Ceram. Soc. (1992), pp. 49-473). As shown, for
`example, by Mizuta et al., these complicated processes
`enable tI-ic best mechanical properties up to now for pure
`sintered corundum to be achieved, but according to this prior
`art no Vickers low-load hardnesses of
`2000 or flexural
`80O Mla were measured even when hot
`strengths of
`isostatic pressing (HIPping) was employed.
`The usefulness of pressureless casting processes such as
`gel casting or enzyme-controlled coagulation for producing
`pure AlO ceramics has hitherto been restricted to corun-
`dum powders having mean particle sizes of more than 0.4
`pm (A. C. Young, et al., J. Am. Ceram. Soc. (1991)3,
`612-618), so that the mean grain sizes of the dense sintered
`microstructures produced were always greater than 1.5 pm.
`lo the example cited, the strengths achieved remained below
`300 MPa.
`The opportunities for improving tEte mechanical pmper-
`ties and the grain fineness of sintered AlO products
`produced from corundum powder by addition of substances
`which promote sintering are very limited. The temperature
`required for siotering submicron AIM3 powders to full
`density is, in particular, reduced to 12O0 and less by
`addition of more than 1% of dopants which form liquid
`phases during sintering, but the strengths remain at the level
`usual for traditional siotered corundum, viz. about 4U) MPa
`(L. A. Xue et al., J. Am. Ceram. Soc., (1991), pp.
`
`15
`
`25
`
`30
`
`2
`201 1-2013), and the widespread ftrmation of grain hound-
`ary phases brings with it unfavourable high-temperature
`properties.
`Although the relationship between defect structure and
`strength of brittle solids has been well known for a long
`time, most studies are restricted to the purely qualitative
`determination of relevant defect types; even a characteriza-
`tiofl of only relative defect size distributions (l-l. E. Exner et
`al., Mater. Sci. Eng. 16 (1974), pp. 231-238) is rare. As
`lo regards the technology dependence ofthe actually important
`absolute defect frequency per volume or analysed area, as
`studied, for example, for glass (J. R. Matthews et al., J. Aro.
`Ceram. Soc. 59 (1976), pp. 304-308), nothing is known fur
`Al203 ceramics. There are absolutely no prior studies on the
`effect of such defects on the Vickers hardness.
`In evaluating the hardness of A1203 ceramics thus
`produced, the influence of the test loading used for the
`indenter first has to be taken into account. The Vickers
`hardness of MO3 is, for a single-crystal as well as poly-
`crystalline material, dependent on the load in a complex way
`20 (A. Krell, Kristall und 1'echnik (198(1) 12,1467-74). lhe
`following material behaviour is typical:
`relatively little load influence at a relatively high test load
`50 N,
`decreasing loading first produces increasing hardness
`values,
`when the test load is reduced further to from <I to 5 N,
`the hardness can fall again.
`Similar behaviour ¡s found for the Knoop hardness,
`although there are certain systematic differences between the
`numerical results by the Kioup and Vickers methods.
`According to the prior art described below fûr the sintered
`Al:Oa products produced by means of known processes
`from corundum powder, the long-established recognition
`that, independently of the respective test load, a grain size
`reduction in the range 2--O.2 pm cannot make possible a
`hardness increase beyond the known upper limits of
`HVIO-2000 (low-load hardness) or HVO.2
`2500
`(microhardness) applies (S. D. Skrovanek et al., J. Am.
`Ceram. Soc. (.1919)3/4, 215-.216). For the above reasons, a
`comparison of hardness data io the literature is only infor-
`mative when the load dependence of the hardness bas been
`examined and the associated test conditions are indicated.
`This is particularly true because the influence of the test load
`Varies greatly even within a material group, Iòr example
`sintered corundum, as a function uf additives, residual
`porosity and, in particular. the state of the surface. Owing to
`the wide variety of data in the prior art, for which specific
`details are rarely given, the data for the particle size influ-
`ence on ttie microhardness and low-load hardness or mac-
`50 rohardness Iluctilate within wide limits.
`Microhardness HV (in the range HVO.1-HVO.5. i.e. in the
`range of the possible maximum of the hardness-load curve)
`for single crystals: 2300-2700 (A. G. Evans et al., J. Am.
`Ceram. Suc. (1976)7/8, 371-372)
`for sintered corlindum with I)2 pm at relative density
`p99%; 2000-2600 (S. I). Skrovanek et al., J. Am.
`Ceram. Soc. (1979)3/4,215-216
`Vickers low-load hardness and macrohardness (test load
`l0N)
`for single crystals: 1400-1700 (A. KmH, Kristall und
`Technik (1980)12,1467-1476)
`for sintered corundum with D2 pm at relative density
`p99%: 1650-1850 (A. Krell, Kristall und Technik
`(1980)12,1467-1476)
`for sintered corundum pmducLs with l)O.45 pin, pro-
`duced by powder technology, at relative density
`
`35
`
`40
`
`45
`
`55
`
`60
`
`65
`
`Exhibit 2322 Page 0010
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-R LM-CAN document 1-1 filed 08/01/14 page 4 of 12
`
`6,066,584
`
`5
`
`J O
`
`15
`
`-
`-'o
`
`p98-983%: 1900-2000 (G. Riedel ei al., Silicates
`Industriels (1989)1/2, 29-35).
`Specific studies by Skrovanck cl al. on the dependence of
`hardness on grain size iii virtually fully densified ho t-p resed
`sintered co[ufldugjs having a gradated reduction io giain size
`showed a hardness increase proportional to D" only down
`to the range 3-4 um. According to general opinion, this is
`caused by the increasing hindrance of' the displacement
`motion in the smaller grains. I lowever, further grain size
`reductions down to 1.7 um gave no further increase in the
`hardness; the hardness remained constant in this range of
`small grain sizes. This finding has hitherto never been
`contradicted because, according to general opinion a further
`mercase in hindrance of the displacement motion with
`decreasing grain size, and therefore increasing hardness, can
`no longer be expected when the grain sizes are uf the size
`range of the displacements. Since typical sizes of displace-
`ments (displacement loops) observed in corundum by means
`of transmission electron microscopy are in the micron range.
`the reduction in the grain size effect on the hardness at grain
`sizes of less than 3-4 pm was :
`self-evident that this
`question was not examined in more detail.
`The disadvantage of the sintered M203 products known
`from the prior art and produced from corundum powder is
`that no sintered Al2°3 products having a very low level of
`defect and very high hardness or high hardness and strength
`are known and able to be produced. Without conclusive
`solutions of the problems having become known up to now,
`current developments are being concentrated internationally
`on two directions which are regarded as promising (T. J.
`Carbone. p. 107 iii: L. D. Hart (Editor), "Alumina Chemicals
`Science and Technology Handhûok", The Am. Ceram. Soc.,
`Westerville, ohio, l99O)
`(1) improvement of the sol/gel technologies with addi-
`tions of nuclei (e.g. G. L. Messing and M. Kumagai in
`Bull. Am. Ceram. Soc. 73(1994)88.-91),
`(2) the development and use ut' powders extremely tini-
`form particle size believed to be ideal ("monosized",
`"uniform-sized") as described by K. Yamada iii "Alu-.
`mina Chemicals Science and Technology Handbook"
`(Editor L. D.
`Hart, The Am. (2eram. Soc., Westerville, Ohio, 1990, page
`564)
`It is an object of the invention to provide sintered A1O
`materials havmg improved mechanical properties, in par-
`ticular having high hardness and/or strength.
`The sintered Al2() materials of the invention having an
`MO3 content of from 95 to 100% by volume and a Vickers
`low-load hardness of 2OOO at a test load of from 10 N to
`100 N (HVI to HV1O) have a relative sintered density of
`p9S.S%, microstructures having meangrain sizesof
`1.5
`um and a frequency of inhomogeneities of <5Ox1O m2.
`The inhomogeneities belong to one or more of the fol-
`lowing categories:
`a) cracks and/or porous regions along the boundaries of
`powder aggregates/powder agglomerates,
`b) nest-like regions in the micmstnicture having a boa-
`ened structure with many pores,
`e) pores having a diameter exceeding twice the grain size.
`Inhomogeneities of the following category may also be
`taken into account:
`d) grains of >10
`and/or agglomerates of individual
`grains having an agglomerate size of greater than 10
`pm and a diameter which exceeds five times the mean
`grain size.
`In addition, all pores having a diameter of
`0.3 pm may
`be taken into account in the case of the inhomogeneities of
`the category e).
`
`The frequency of the inhomogeneities is advantageously
`2Ox1O m2. In contrast, in the case ofsintered corundum
`ofthe prior art, the frequency of the inhomogeneities is more
`than 5Ox109 m2.
`Advantageously, even sintered microstructures having
`mean grain sizes below 0.8 tm can be obtained using the
`process of the invention.
`The sintered material advantageously has a microstruc-
`turc having a predominantly irregular orientation ol the
`crystallites.
`In a further embodiment of the invention, importance is
`attached to achieving both a comparatively high hardness
`and a high flexural strength. The additional requirement of
`a high flexural strength in this embodiment requires a
`sintered material which also has a certain size distribution of
`the defects or mhomogeneities as qualifying feature. This in
`turn requires the characterization of the sintered material uf
`the invention by means of a dimensionte&s defect density
`defined as the sum of the squares of the defect sizes per area
`analysed. as was originally introduced for the evaluation of
`microcrack densities (A. Krell et al., J. Mater. Sci. (1987)9,
`3304-08). bIere, the defect size employed is the maximum
`recognizable extent uf the defect io any direction in the
`analysed plane. In the case of ceramic materials of the prior
`15 art, the frequency of such inhomogeneities is more than
`-- 30x103. The further embodiment of the invention is char-
`acterized by a content uf from 95 tu 100% by volume uf
`AlOa and a Vickers bow-load hardness of
`1750 at a test
`loadoffrom lONto 100N(HV1 toHVlO)and afiexural
`strength of
`80O MPa, with the sintered material having a
`relative sintered density of p983%, a microstmcture with
`a mean grain size of
`2 jtm and a dimensionless defect
`density of <3Ox1O, where the defects belong to one or
`more of the following categories:
`a) cracks and/or porous regions along the boundaries of
`powder aggregates/powder agglomerates,
`b) nest-like regions in the microstmcture having a boos-
`ened stracture with many pores,
`e) pores having a diameter exceeding twice the mean
`graiii size,
`d) grains of >10 im and/or agglomerates of individual
`grainS having an agglomerate size of greater than 10
`pm arid a diameter which exceeds five times the mean
`grain size.
`The microstructure of the sintered material which com-
`bines high hardness with high flexiiral strength also advan-
`tageously has a predominantly irregular nentation of the
`crystabbites.
`The sintered products of the invention can also contain, in
`50 addition to corundum (a-Al,03), up to 5% by volume of
`other substances as long as the ahovemeotioned permissible
`limits uf the relative density, the frequency of the inhumo-
`geneitios mentioned or the dimensionless defect density are
`still adhered to. The fracture toughness (K,) of the products
`55 ofthe invention can considerably exceed the level typical for
`sintered corundum, depending on measurement method
`between about 3 and 4.5 MPaVm. However, this is not a
`condition for implementing the invention. For determining
`the fracture toughness, it has to be noted that, in particular,
`the measurement method used has a strong and difficult-to-
`quantify influence on the measured value found, so that
`measured values can frequently not be compared with one
`another.
`A process for producing a sintered AlO material of the
`65 invention comprises the following steps:
`a) conversion of an aAl:()3 powder having a mean
`particle size d0 of O.30ini and a chemical purity uf
`
`30
`
`35
`
`40
`
`45
`
`60
`
`Exhibit 2322 Page 0011
`
`CeraMedic Ex. 2322
`CeramTec GmbH v. CeraMedic LLC
`Case IPR2015-01328
`
`

`
`case 3:14-cv-01771-RLM-CAN document 1-1 filed 08/01/14 page 5 of 12
`
`6,066,584
`
`99_9% ofAJ2O iii a liquid juLo a stable suspension of
`dispersed particles by means of simultaneous and/or
`sequential use of at
`least two different dispersing
`methods,
`b) poduclion of an unsititered precuior having a relative
`density of p 55
`by means oC shaping,
`e) heat treatment and sintering ot the precursor.
`The process of the invention does not require use of very
`expensive powders of uniform ("monosized", "uniform-
`sized") particle size, but rather it can be advantageously
`carried out using a very muet-i cheaper a-AlO3 powder
`having the following particle size distribution: d>OO65
`pm, d0O.3O pm, d1O45 pm. This is a particular advan-
`tage of the invention since it makes possible the production
`of correspondingly high-value sintered materials at lower
`cost than in the case of the prior art. Eentjal to the success
`ol: the production process of the invention is the preparation
`of a stable (and particularly homogeneous) suspension of the
`dispersed particles by simultaneous and/or sequential use of
`at least two different dispersing methods.
`Advantageously, the c-Al2O3 powder used in step a) has
`a speciìc surface area, detenijined by the BET method of
`from 10 to 17 m2/g.
`The abovementioned particle size distribution of the
`a-A1203 starting powder used is of particular importance to
`the success of the invention. Larger mean particle sizes than
`permissible, higher amounts of coarse material (d84 shifted
`to higher values) and correspondingly lower specific surface
`areas reduce the sintering activity, increase the sintering
`temperature required and thus lead to unacceptable coarse
`microstructures. Smaller irtean particle sizes or higher
`amounts of very fine material (d shifted to lower values)
`cause problems in the subsequent shaping and sintering: the
`resulting reduced green density (i.e. the density of the
`unsintered products) and an increased defect frequency
`likewise require increased sinteritig temperatures, so that
`coarser sintered products having more inhomogeneities and
`defects are formed. A reduced purity of the powder raw
`material below the value indicated according to the in ven-
`tion leads, at least locally, to formation of liquid phases
`during sintering, so that the microstructures produced con-
`tain amorphous grain boundary phases, precipitates,
`micropores and other undesired microdefects. Even when
`amutphuus phases cannot he detected, a reduction oIT the
`powder purity to he adhered to according tu the invention
`leads to uncontrollable grain growth processes during sin-
`tering.
`To produce a sintered a203 material in which impur-
`taflce is not exclusively attached tu a particularly high
`hardness, hut in which a high flexural strength is sought at
`the expense ofa somewhat reduced hardness. the production
`process of the invention can be modified so as io employ the
`following steps:
`a) conversion uf an (1-Al203 powder having a particle size
`distribution determined by the parameters d1>O.O6$
`m, 0.2 pmdO.4 um, 0.45 pmd.O.8 im and
`a chemical purity of 99.9% of A1O in a liquid into
`a stable suspension of dispersed particles by means of
`simultaneous and/or sequential use of at least two
`different dispersing methods,
`b) production of an uiisintered precursor having a relative
`density of p 55% by means of shaping,
`e) heat treatment and sintering of the precursor.
`The difference between this and the first-mentioned pro-
`cesS is that a slightly higher rucan particle size and a
`somewhat higher proportion of coarse material may be
`
`6
`permissible. Ii is thus possible to use au even more irtex-
`pensive starting material. Here too, mean particle sizes
`which are larger than permissible, higher proportions of
`coarse material (d54 shifted to higher values) and corre-
`spondingly lower specific surface areas reduce the sintering
`activity, increase the sintering temperature in an unaccept-
`able way and thus lead to microstructures which are too
`coarse-grained to achieve the ahovementioned mechanical
`properties. Iligher proportions of very fine material (d1
`lo shifted to lower values) and a reduced purity of the powder
`raw material here also cause the same problems as discussed
`above.
`The a-A1203 powder used as starting material in this
`modification of the pmduction process of the invention
`15 advantageously has a specific surface area determined by the
`BET method of 8-17 m2/g.
`The sintering processes used for the purposes of the
`invCntion can he pressureless or employ pressure (e.g. hut
`pressing Or hot isostatic pressing). However, a particular
`20 advantage of the invention is that a-ALO materials of high
`hardness and/or strength are also obtained when using
`
`pressureless sinteringpS
`
`In this context, it may he pointed out that pressureless
`sintering in air compared with hot pressing or hot isostatic
`25 pressing (HIPping) leads, owing to the differences in the
`surrounding atmosphere (in particular the oxygen partial
`pressure), to considerable structural differences which in
`turn alter diffusion coefficients and mechanical, optical and
`electrical properties dependent thereon (S. K. Mohapatra et
`30 al., J. Am. Ceram. Soc. (1978), Issue 3/4, 106-109; 5. K.
`Mohapatra et al., J. Am. Ceram. Soc. (1979). Issue 1/2.
`50-51).
`i lot pressing or hot isostatic pressing are usually carried
`out in a protective gas atmosphere (argon), so that there is a
`35 reduced oxygen partial pressure and, on the other hand, the
`carbon-containing materials used for the purposes of the
`pressing process result in a CC) partial pressure which has a
`reducing action which produces oxygen vacancies as point
`defects distributed over the entire corundum lattice and
`40 leading to the abovementioned changed properties. Among
`other things, there results a dark grey coloration of the
`corundum in contrast to the typical pale appearance uf
`sintered M,O materials produced by pressureless sintering
`in air (T. Nagatome et al., J. Ceram. Soc. Japan, mt. Ed.
`45