Armour Research Foundation of Illinois Institute of Technology v. C. K. Williams & Co. (170 F. Supp. 871, 1959)

JUERGENS, District Judge.

This litigation was commenced by the plaintiff Armour Research Foundation of Illinois Institute of Technology (hereinafter referred to as Armour) against C. K. Williams & Co., Inc. (hereinafter referred to as Williams), defendant in Civil Action No. 3200 and plaintiff Armour against Technical Tape Corporation (hereinafter referred to as Technical Tape), defendant in Civil Action No. 3438. Minnesota Mining and Manufacturing Company (hereinafter referred to as Minnesota) was subsequently, by order of this Court, brought in as a necessary party plaintiff. The two suits were consolidated for trial.

The plaintiffs charge infringement by the defendants of United States Letters Patent No. 2,694,656, issued to Marvin Camras, who filed his application with the United States Patent Office on July 25, 1947. The patent issued November 16, 1954. The inventor Marvin Camras assigned the patent to Armour. Minnesota is an Armour licensee and has the exclusive right to grant sub-licenses under the patent.

The defendants filed their separate answers to the respective complaints, alleging invalidity and unenforceability of the patent and denying infringement. In addition, Williams filed its counterclaim seeking an adjudication of the invalidity and non-infringement of the patent in suit and counterclaimed against both plaintiffs for violation of the AntiTrust Law.

This Court has jurisdiction under the patent laws of the United States.

In support of their allegations of infringement the plaintiffs rely on claims 3, 8, 10, 14, 25 and 26 of the patent in suit. These claims are as follows:

“3. A ferromagnetic iron oxide material adapted to form an element of a magnetic impulse record member, said material consisting essentially of acicular crystalline particles uniformly small in size and not over 6 microns in their greatest dimension of a synthetic magnetic oxide of iron selected from the group consisting of magnetic ferrosofer-ric oxide FesOá, and magnetic gamma ferric oxide, Fe203, the selected synthetic magnetic oxide of iron having a cubic lattice structure, and said material having a coercive force value of between 200 and 550 oersteds and a ratio of Bfm/Br at H-1000 of not over 3 to 1.

“8. The method of making permanent magnet material which comprises precipitating a non-magnetic ferric oxide from solution in acicular crystalline form, heating said nonmagnetic ferric oxide in a reducing hydrogen atmosphere to a temperature of about 750° F. for a sufficient length of time to reduce said ferric oxide to a magnetic ferroso-ferrie oxide, cooling the ferrosofer-ric oxide in the presence of a reducing atmosphere to room temperature and then exposing said ferro-soferric oxide to the air to recover a ferrosoferric oxide having a coercive force value between 200 and 550.

“10. The method of making magnetic material, which comprises precipitating a non-magnetic ferric oxide from solution in acicular crystalline form and of a particle size less than 6 microns in greatest dimension heating said non-magnetic ferric oxide to a temperature between 500 and 1000° F. in a reducing atmosphere until the reduced oxide turns almost black, stopping the reaction at that point by cooling said reduced oxide in a reducing atmosphere to around room temperature and recovering ferrosoferric oxide of the same crystalline form and same order of particle size but having permanent magnet properties including a coercive force of over 200 oersteds and a B£m/Br (H-1000) of not over 3 to 1 and reoxi-dizing said ferrosoferric oxide in the presence of oxygen at a temperature between 300° F. and 900° F. to produce a magnetic iron oxide consisting essentially of gamma Fe20s.

“14. The method of making magnetic iron oxide which comprises providing a synthetic non-magnetic ferric oxide in acicular crystalline form and of particle size not over 6 microns in its greatest dimension, reducing said non-magnetic oxide at elevated temperatures to produce a ferrosoferric oxide and oxidizing said ferrosoferric oxide to gamma ferric oxide having permanent magnet properties including a coercive force of at least 200 oersteds.

“25. Ferromagnetic iron oxide selected from the group consisting of a synthetic ferrosoferric oxide, FesOi, and of a synthetic gamma ferric oxide, Fe2C>3, adapted to form an element of a magnetic impulse record member, said iron oxide consisting essentially of uniformly small elongated crystals of less than about 1.5 microns maximum dimension having a length-to-width ratio of about 2.5 to 1 and higher, and having a cubic crystal lattice structure and a coercive force, H0, within the range of 245 to 330 and rema-nence, Br, of above about 500 gauss.

“26. A magnetic impulse record' member having a non-magnetic carrier and a coating adherently bonded thereto of a binder and magnetic material, said magnetic material being the ferromagnetic iron oxide defined in claim 25 and having a Br versus H characteristic that rises most rapidly at fields between 200 and 600 oersteds and relatively slowly at fields between 0 and 200 oersteds and at fields above 600 oersteds.”

The patent in suit relates to a permanent magnetic material and to a method of making same. This permanent magnetic material is then impregnated or coated on a non-magnetic carrier to produce a magnetic impulse record member.

Magnetic recording was first discovered prior to the beginning of the present century by Valdemar Poulsen, a Danish physicist. He found that a mass of magnetizable material may be impressed with impulses varying in intensity in successive adjacent portions of the magnetizable mass which will retain these impulses. It was learned that a sound wave could be converted into a varying electric signal and it was further determined that by energizing an electromagnet with the electric signal a corresponding magnetic signal would be impressed on the record member as the record member was caused to pass over the electromagnet. It was further observed that when the same record member was again moved past the same or a similar electromagnet, an electric signal would be introduced into the electromagnet corresponding to the magnetic signal which had been impressed on the record member by its prior exposure to the effects of the electromagnet. These early experiments were in great part conducted using wire or metal tapes as the record member.

Prior to World War II the Germans had developed magnetic recorders using non-magnetic tape materials coated with magnetic iron oxides as the recording media. This use of magnetic iron oxide tapes as a recording media continued and was advanced throughout the war years. These tapes were used on two different machines, the “Magnetophon” and the “Tonsehreiber”. The Magnetophon was used by the German radio and broadcasting industry for recording broadcasts which were subsequently replayed and transmitted. This recording machine was a bulky instrument, having a tape speed of approximately 30 inches per second. This required large reels in order to provide programs of any extended length. The Tonsehreiber was primarily used by the German armed forces in transmitting messages and could be set to operate at any speed from 0 to approximately 30 inches per second. Both of these machines utilized the German low coercive force oxide tapes.

During the period referred to above the magnetic recording art in the United States was limited to the use of wire or tape. Iron oxides were not generally used as recording media in the United States until after the conclusion of World War II when the Brush Development Company of Cleveland, Ohio, placed on the market the Brush “Sound-mirror”. This machine used as a recording media a low coercive force magnetic oxide tape similar to that used by the Germans in their Magnetophon and Tonsehreiber. The basic difference between the German and Brush machines was that the Soundmirror operated at a speed of 7% inches per second. This speed has become the standard speed of American tape recorders.

While the work on the Soundmirror was progressing — it became the first American machine for home use — the Indiana Steel Products Company had produced a tape recorder designed to use high coercive force tapes in order to obtain high frequency response at low speeds. The tape used with this machine had a coercive force of around 250 oer-steds and utilized a magnetic powder having particle sizes in the 1 micron range for the recording media. The coating material used on this tape was not the magnetic iron oxides claimed as an invention in the patent in suit nor was it similar to that used on the German tapes.

On June 1, 1946 Marvin Camras, the inventor of the patent in suit, applied for a patent on an “apparatus for magnetic recording” and on October 31, 1950 Patent No. 2,528,261 issued (Dx. N). In that patent he claimed as his invention a magnetic recorder designed to use a recording media having a permeability of less than 50 and a coercive force of over 100 oersteds, preferably over 250 oersteds. With the advent of this magnetic recorder the first great need for high coercive force and low permeability tapes arose.

On July 25, 1947 Marvin Camras filed his application and on November 16, 1954 the patent in suit was issued.

The important criteria of his patent, according to Mr. Camras, are:

(1) A relatively high coercive force, generally between 200 and 550 oersteds.

(2) Initial magnetization curve with a relatively gentle slope to an H0 point of about 250 gauss.

(3) A rapid rise from about 200 to 600 oersteds.

(4) A high remanence above about 500 gauss and a B(m/Br ratio of less than 3 to 1.

(5) A synthetic material comprised of particles of preferably less than 1.5 microns and not more than 6 microns in maximum dimensions and consisting of acicular or elongated particles.

The defendants assert the invalidity of the patent and declare that the patent should not have been issued.

One of the asserted grounds of invalidity is that the oxides claimed as an invention by Camras are old in the art, as was also the use of magnetic iron oxides for magnetic impulse record members.

In support of this contention the defendants point to the Johnson patent (British Patent No. 466,023) (Dx. F) dated November 18, 1936. This patent is entitled “Improvement in the Manufacture and Production of Sound Record Carriers” and claims invention of electromagnetic recording and reproduction of sound according to the known process suggested by Poulsen whereby sound carriers have been employed, which consist of coherent magnetic materials, preferably in the form of strips or wires of magnetic metals. The patent claims that it has also been proposed to make use of finely divided magnetic material and that magnetic metal oxides in a finely divided state are eminently suitable for electromagnetic recording and reproduction of sound by means of sound carriers consisting of magnetic materials on or in a non-magnetic carrier material. The oxides FesOi and gamma Fe2C>3 are especially suitable.

“A suitable process for the preparation of the oxides in a very finely divided state consists in the decomposition of complex metal salts, as for example iron ammonium salts, or complex metal compounds which contain organic radicals such as pyridine. Such methods of preparing oxides are known per se, but it was hitherto not known that magnetic metal oxides when prepared in such a way are highly suitable for sound recording purposes * * *

“It has been found that the oxides to be used according to this invention fulfil the said requirements to a high degree. The main reason for this is the extreme fineness and the very great uniformity in the size of the particles. For example it is possible to incorporate the magnetic material according to this invention in the sound record carrier in a particle size of Yiooo millimetre or less; with the processes hitherto proposed for the purpose this is either impossible or only possible with difficulty. The magnetic properties of the oxides, in particular their induction and remanence with low field strengths, are favourable for their use as sound record carriers. The high coercive force ensures a good stability of the sound recording. * * *

“The following Examples will further illustrate how the said invention may be carried out in practice but the invention is not restricted to these Examples.”

Johnson sets out five examples of methods of preparing oxides for use in the invention. However, the patent clearly indicates that the method of preparation of the oxide is not restricted to the examples.

The Patent Examiner rejected several claims of the Camras patent as being unpatentable over the Johnson British patent (p. 48, Dx. G). To overcome this objection (p. 48, Dx. G) Camras conducted experiments of three examples of the British patent. By following these methods low coercive force materials were obtained (pp. 63, 64, Dx. G).

On page 64 of this exhibit the effect of temperature upon the magnetic properties of hydroxides was illustrated. Crystals of Fe203.H20 in the form of light yellow acicular crystals of a particle size from % to about 1 Y% microns in length and Yio to %o microns in width were produced according to the reactions described in the Camras application. The resulting particles were then reduced in an atmosphere of hydrogen at temperatures of 300° F., 400° F. and 1200° for varying periods of time. The resulting oxides proved in the case of the 300° F. and 400° F. reductions to have coercive force values and remanence values too low to obtain a measurement, and in the case of the 1200° F. reduction a coercive force of 30 was attained.

Since Camras in his experiments failed to follow the teachings of the prior publications for the method of reducing both synthetic and natural iron oxides, it is not surprising that he obtained the low coercive force above indicated.

The Williams and Thewlis article (Dx. 1-Y) dealing with heat treatment of gamma monohydrate of ferric oxide (1931) disclosed that reduction of gamma hydrate at the temperature of 350° C. was necessary for practically complete dehydration. Temperatures below this point did not show a satisfactory dehydration while temperatures in excess of 500° C. showed the beginning of a conversion from the gamma to the alpha oxide. The gamma hydrate used in the Williams and Thewlis teachings was prepared from a dilute solution of ferrous chloride, by precipitation with calcium hydroxide in the form of a suspension in water and subsequent oxidation at room temperature.

At the Inter-Partes demonstration at Easton, Pennsylvania, the Williams and Thewlis publication was followed in conducting the H series demonstration. In this demonstration the hydrate was reduced at 350° C. (R. 2049). The particles of the oxide produced in the H demonstration were found to be acicular and smaller than 1 micron in maximum dimension (R. 2051) (Dx. 1-B-1, p. 33). The oxides produced in this demonstration showed a coercive force of over 200 oersteds and a B£m/Br ratio of less than 3 to 1 (R. 3166, 3167).

By following the teachings of the Williams and Thewlis publication, as was done at the Inter-Partes H demonstrations, an oxide clearly conforming to the patented oxide was obtained.

Another prior publication showing the effect of heat treatment on magnetic properties of iron oxides is found in the Kraeber and Luyken publication (Dx. 1 — Z—1 and l-Z-2).

This article was published in Germany in 1936 by the German-Kaiser-Wilhelm Institute. It discloses methods by which iron oxides may be reduced and oxidized in order to provide certain magnetic properties. At the Easton Inter-Partes demonstrations an oxide, identical to Camras’ oxide, was produced by following the disclosures of the publication.

The plaintiffs contend that the article fails to anticipate the Camras patent, notwithstanding the fact that oxides identical to those disclosed in the Camras patent were produced by following the teachings of Kraeber and Luyken at the Easton demonstrations. They assert that the publication does not disclose the use of these oxides for magnetic recording media; that the Camras measurements, which are necessary in order to determine that the oxide sought has been obtained, are not disclosed anywhere in the article; and that the starting material used at the Easton demonstration was not the Merck iron hydroxide but rather was a product of the defendant Williams Company. This latter objection is strongly urged by the plaintiffs in their claim that the Camras oxide was not anticipated by this publication.

The defendants used a substitute hydroxide (a commercial product of defendant Williams known as YLO-1788); this iron hydroxide corresponds to the Merck iron hydroxide prescribed as a starting material in the publication. The Court finds that the defendants have justified their use of the substitute hydroxide by showing that:

(1) They attempted to obtain the Merck iron hydroxide as prescribed by Kraeber and Luyken, but none was available. (p. 73, Dx. 3-E).

(2) The substitute starting material (YLO-1788) was of the same extremely small particle size as Merck iron hydroxide. The evidence discloses that the particle size of the prescribed and the substitute hydroxides are the same. (p. 11, Dx. 3-E) (pp. 16, 17, Dx. 1-Z (2)) (p. 14, Dx. 3-E).

(3) The Merck and the YLO-1788 hydroxides both consisted of acicular particles. This is borne out by the evidence, (pp. 62 and 69, Dx. 3-E, and pp. 8, 16 and 17, Dx. l-Z-2).

Except for the use of a substitute starting material, the procedures outlined in the Kraeber and Luyken article were followed in producing the P series demonstration oxides. The starting material (p. 11, Dx. 3-E) was roasted at a temperature of 400° C. for one-half hour in the presence of carbon monoxide gas (pp. 8, 9, Dx. 3-E). The kiln was then removed from the heating blanket with nitrogen continually passing through and was placed on the floor to cool down to room temperature (pp. 18, 19, Dx. 3-E). This procedure follows test No. 3, table 5, page 30 of the Kraeber and Luyken article (Dx. 1-Z (2), p. 8, Dx. 3-E). In the second step in the procedure materials produced in the first step were placed in a rotary kiln and heated to 200° C. This temperature was maintained for a period of one hour as air passed through the kiln. The kiln was then removed from the heating blanket and cooled down to room temperature (p. 27, Dx. 3-E). The second step of the procedure follows the procedure outlined in experiment 7, table 6, page 36 of the publication (Dx. 1-Z (2)).

The oxide and tapes produced correspond in all respects to the Camras patent material (pp. 2-5, Dx. l-B-3) pp. 1-3, Dx. l-B-4).

The United States Department of Interior Bureau of Mines Bulletin No. 425, dealing with the Magnetic Separation of Ores, at page 136, teaches the Effect of Heat Treatment on Iron Oxides, Ferrites and Ilmenite and provides as follows:

“Properties of Gamma Fe203 and Ferrites

“It has long been known that under certain conditions Fe2Ü3 is ferromagnetic. This form has been shown by X-ray spectrometry to be cubic, whereas the ordinary paramagnetic form is hexagonal.

“Of the various methods for preparing this ferromagnetic Fe203 two may be used to treat minerals for magnetic separation. By the first method Fe30 3 by reacting a solution of ferric nitrate with ammonia and then reducing the Fe2Ü3 in a mixture of hydrogen and water vapor. The reference teaches how to control the concentration of hydrogen and water vapor in relation to the temperature so as to obtain ferrosoferric oxide (FesOd), which is then oxidized to produce Fe2(>3 by heating at a prescribed temperature in air (Dx. 2-A-l and 2-A-2).

The reduction and oxidation disclosed in this article are very similar to those disclosed in the patent.

Oxides were produced at the Easton Inter-Partes demonstrations by following the Huggett teachings. These oxides showed coercive forces of Hc at 1000 in the neighborhood of 200 to 210, Bfm/Br ratio at 3 to 1 or less, rapid rise from 200 to 600 (Dx. 1-B-l, p. 12; Dx. l-B-2, p. 5; R. 2104-2114).

By following the procedure set out in the Huggett publication, oxides having the magnetic properties claimed by Cam-ras as his invention were obtained. The Huggett procedure however failed to produce an oxide comprised of predominantly acicular particles and due to this failure it cannot be said that Huggett anticipated the patented oxides.

The defendants also refer to a German patent (Reich’s Letter Patent No. 587,-916) issued October 26, 1933 to Siemens and Halske (Dx. 0-1 and 0-2). This invention concerns a process for the manufacture of sound writing carriers for use in electromagnetic recording of sounds, such as conversation and music. The patent refers to the prior use of permanent magnetizable splinter shaped particles and claims as its invention the alignment of the splinter shaped particles on the tape.

There is no disclosure as to the type nor the magnetic properties of the material used. This publication does not anticipate the Camras oxides except possibly to show the preferred use of acicu-lar or, as described in the patent, splinter-like particles so that orientation of the particles on the nonmagnetic carrier is possible.

The Sappa article (Dx. 1-X-l and 1— X-2) deals with the properties of ferro magnetic substance; however, this reference is concerned with natural ores and therefore does not anticipate the patent in suit.

The Lehrer German Patent No. 675,-490, issued June 12, 1936, (Dx. 1-W-l and l-W-2) teaches the use of magnetic oxide powders for use in producing magnetic recording media. The teachings of this patent were followed at the Inter-Partes demonstrations and oxides were produced which were found not to • be acicular. When the oxide was produced it was.in a solid form and had to be removed by chiseling it from the kiln. The oxide was then crushed by a jar crusher. It was then necessary to air classify the materials to obtain particles sufficiently small to coat on tape. The unclassified materials showed an Hc value of considerably less than 200 (R. 2154-2155).

On the basis of the failure to produce an oxide at the demonstrations which would conform to the patented oxides, this patent (Lehrer) does not anticipate the patent in suit.

The OSRD Report No. 5325, published June 30, 1945, (Dx. 1-B) deals, among other things, with the use of iron oxides in making magnetic recording media and describes in detail the method of preparation. The publication teaches the use of iron oxides of gamma Fe203 and Fe sO