29
. . -( SN Ofqwt)w HIGH POWER X-lUY WELDING OF METAL-MATRIX COMPOSITES Richard A. Rosenberg George A. Goeppner John R. Noonan William J. Farrell Qing Ma .— “.--. . - .,

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Page 1: HIGH POWER X-lUY WELDING OF METAL-MATRIX COMPOSITES/67531/metadc... · energy made available the electric arc for welding applications, with attendant improvements including gas tungsten

..

-(

SN Ofqwt)w

HIGH POWER X-lUY WELDING OF METAL-MATRIX COMPOSITES

Richard A. RosenbergGeorge A. GoeppnerJohn R. NoonanWilliam J. FarrellQing Ma

.— —“. —— —_______

——— . . . . . . . . .——. _—. —.—..- —. . . ._ . . . “.--. — . - .,

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08/974, 167~ Ctil

HIGH POWER X-RAY WELDING OF Richard A. Rosenberg W-31 -1 09-ENG-38METAL-MATRIX COMPOSITES George A. Goeppner

John R. NoonanWilliam J. FarrellQing Ma

II

I

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DISCLAIMER

This report was,.prepared as an account of work sponsoredby an agency of the United States Government. Neitherthe United States Government nor any agency thereof, norany of their employees, make any warranty, express orimplied, or assumes any legal liability or responsibility forthe accuracy, completeness, or usefulness of anYinformation, apparatus, product, or process disclosed, orrepresents that its use would not infringe privately ownedrights. Reference herein to any specific commercialproduct, process, or service by trade name, trademark,manufacturer, or otherwise does not necessarily constituteor imply its endorsement, recommendation, or favoring bythe United States Government or any agency thereof. Theviews and opinions of authors expressed herein do notnecessarily state or reflect those of the United. StatesGovernment or any agency thereof.

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DISCLAIMER

Portions of this document may be illegiblein electronic image products. Images areproduced from the best available originaldocument.

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CONTRACTUAL ORIGIN OF THE INVENTION

The United States Government has rights in this invention pursuant to

Contract Number W-3 1-109-ENG-38 between the United States Government and

Argonne National Laboratory.

TECHNICAL FIELD

The present invention relates to x-ray welding, and, in particular, a method

for using high power x-rays as a volumetric heat source for welding metal-matrix

composites.

BACKGROUND OF INVENTION

Metal-matrix composites (MMCs) are composed of a metal and a reinforcing

material distributed within the metal. The metal matrix is usually comprised of

titanium (Ti) or aluminum (Al), and the reinforcing material is usually comprised of

alumina (A120q)or silicon carbide (SiC), in the form of particulate, whiskers, wires,

fibers, or flakes. MMCS are lighter and have superior mechanical and thermal

properties than the metals comprising the matrix alone, including higher specific

strength, operating temperature, and wear resistance. MMCS are increasingly

2

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. ~.J-. ---rT.--7--- .— -,,7-C- - - —--”-..-, .— ----

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.

important in a growing number of applications, including use in the aerospace

industry, high speed mechanical systems, and electronic packaging. The potential

use of MMCS, however, is largely unrealized because MMC elements must be joined

together to produce integrated structures, and methods for joining MMC elements by

5 autogenous welding have been largely unsuccessful.

Welding technology has developed according to new sources of thermal

energy required for directed, localized heating and melting. For example, elec&ical

energy made available the electric arc for welding applications, with attendant

improvements including gas tungsten arc (GTA), gas metal arc (GMA), and

10 submerged-arc welding. A major problem associated with using conventional

electric arc welding for joining MMCS is that chemical and metallurgical reactions

occur between the metal matrix and the reinforcing material, causing brittle and

excessively porous welds having poor structural strength. For example, attempts to

fusion weld MMCS reinforced with SiC cause undesirable, irreversible chemical

15 reactions rendering the joints unusable.

Electron beam welding tightly focuses an electron beam to effectively drill a

hole through the thickness of the target material, permitting single pass and deep

penetrating welds. In the deep penetrating welding process, a beam of relatively high

velocity electrons (50 KeV to 150 KeV) is directed at the joint to be welded. The

beam is focused to produce a power density of about 10Gwatts/cm2 at the target20

3

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surface, superheating the surface layers of the work piece and causing violent

vaporization, particularly in the central region of the beam, whereby a slightly

conical hole, referred to as a keyhole, is bored through the thickness of the material

to be welded. The keyhole, having a diameter usually slightly less than the beam

5 diameter, is filled with products of the fision, evaporation, and sublimation process.

Thermal interaction of the metal being welded by relative beam movement occurs at

the front wall of the vapor-gas channel (the keyhole), and molten metal moves from

the front wall, along the channel walls, and to the rear of the keyhole, due to the

dynamic balance between the pressure of gases, vapors, and molten metal. Provided

10 the established condition produces a stable keyhole, a high quality, full penetration

welded joint is produced. A lower quality, or slightly defocused, electron beam at a

specific power of about 104watts/cm2 behaves similarly to a GTA weld, i.e.

penetration is limited by heat conductance into the thickness of the metal from the

heat area on the surface.

Conditions of laser beam energy sources are similar to the electron beam

sources, however, the specific energy of the laser beam must be greater than about 5

x 10Gwatts/cm2 to produce a keyhole, due to lower coupling efficiency of the laser

beam, as well as metallurgical reactions of the molten metal and the atmosphere.

C02 lasers are used for welding thin sheet metal components because of the high

welding speed made possible by the high power of the focused laser beam.

4

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However, as the thickness of the welding joint increases, a gas plume forms from

metal vaporized by the high intensity beam. The metal vapor is ionized due to laser

irradiation which obstructs the beam transfer into the weld pool. A jet of helium gas

must be used to blow the plume away from the work surface. Alternatively, laser

5 beam welding is conducted in a vacuum where the metal vapor expands so rapidly

that no blocking plume can form.

All energy sources currently utilized for fixsionwelding, including oxy-fiel,

electric arc, GTA, GMA, plasma arc, electron beam, and laser energy sources,

essentially depend on surface heating and the resultant conductive heat flow for

10 penetration of the melt into the thickness of the weld. A relatively large temperature

difference must be created between the face and root of the weld in order to achieve

full penetration, and, therefore, the surface layer of the melt is superheated.

Subjecting the surface layer of MMCs to superheating causes melting and

vaporization of the reitiorcement material, destroying or decreasing the strength of

15 the MMCS. Thus, conventional fb.sion welding processes cause pronounced changes

in the distribution of the reinforcement material of the MCCS in the solidified weld

metal. For example, for an MCC reinforced with AlzOJmaterial, fusion welding

results in a joint strength essentially equivalent to the unretiorced aluminum matrix

alloy.

A need still exists in the art for a method of directed, localized heating for20

5

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welding metal-matrix composites, without excessive melting and/or vaporization.

The development of synchrotronsradiation sources has made high energy x-

rays available as a volumetric heat source for material processing. In contrast to

conventional welding methods, the photons of the x-ray beam penetrate the complete

5 thickness of the work piece, nearly instantaneously heating the volume through

which they pass. Thus, the surface layers of the work piece are not subjected to

superheating. High energy x-rays have the ability to penetrate deeply into light

alloys at selected power densities, without causing violent vaporization and/or holes

in the target material. The absorption coefficient of x-rays are atom and energy

10 dependent, and therefore the behavior of the target material exposed to x-rays is

vastly different than the behavior of the same material subjected to electron or laser

irradiation.

The present method uses x-rays having relatively short wave lengths, such as

1-8 Angstroms, and a relatively high energy power, such as 105watts/cm2, to weld

metal-matrix composites. A high power x-ray is directed to the weld line between

two adjacent MMCS materials, generating an irradiated region or melt zone. The

metal matrices are fused together in the melt zone, while the reinllorcing material of

the metal-matrix composites is not vaporized, but remains uniformly distributed in

the melt zone. In an alternate embodiment, high power x-rays are used to provide the

volumetric heat required to weld metal elements, including metal elements

6

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comprised of metal alloys.

Therefore, in view of the above, a basic object of the present invention is to

provide a method for welding metal matrix composites, metals, and metal alloys.

Another object of this invention is to provide a method for welding that

penetrates deep into a metal matrix composite without causing vaporization of the

reinforcement material.

Additional objects, advantages and novel features of the invention will be set

forth in part in the description which follows, and in part will become apparent to

those skilled in the art upon examination of the following or may be learned by

practice of the invention. The objects and advantages of the invention maybe

realized and attained by means of instrumentation and combinations particularly

pointed out in the appended claims.

BRIEF SUMMARY OF THE INVENTION

The present method uses high power x-rays as a volumetric heat source for

welding metal-matrix composites.

Briefly, the method provides for welding metal-matrix composites (MMCS)

by directing an x-ray to the weld line between two adjacent MMCS materials to melt

the matrices. The x-rays have a power density greater than about 104watts/cm2 and

provide the volumetric heat required to join the MMC materials. Importantly, the

reinforcing material of the metal-matrix composites remains uniformly distributed in

7

. . . . ... . . .. ——-—...—— ... ... ..- . . . .. —-—. —...... ..- -,-— —--- . . . .. .... . . . . ..

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the irradiated region, and the strength of the MMC is not diminished. In an alternate

embodiment, high power x-rays are used to provide the volumetric heat required to

weld metal elements, including metal elements comprised of metal alloys.

BRIEF DESCRIPTION OF THE DRAWINGS

The appended claims set forth those novel features which characterize the

invention. However, the invention itself, as well as further objects and advantages

thereof, will best be understood by reference to the following detailed description of

a preferred embodiment taken in conjunction with the accompanying drawings,

where like reference characters identi@ like elements throughout the various figures,

10 in which:

FIG. 1 shows a cross-section scanning electron micrograph (SEM) image of

the melt zone of an x-ray weld, including the entire width of the sample;

FIG. 2 shows a cross-section scanning electron micrograph (SEM) image of

the melt zone of an x-ray weld, including an enlarged region of the area where the x-

rays impinged on a sample metal-matrix composite;

FIG. 3 shows a cross-section scanning electron micrograph (SEM) image of

the melt zone of an x-ray weld, including an enlarged region of the area where the x-

rays exited a sample metal-matrix composite;

FIG. 4 shows a cross-section scanning electron micrograph (SEW image of

an unirradiated region of a metal matrix composite; and

8

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FIG. 5 shows a cross-section scanning electron micrograph ($EM) image of

the melt zone of an electron beam weld of a sample metal-matrix composite.

DETAILED DESCRIPTION OF THE INVENTION

The present invention is a method for using high power x-rays as a

volumetric heat source for welding metal-matrix composites (MMCS).

MMCS are composed of a metal and a reinforcing material distributed within

the metal, wherein the metal matrix is usually comprised of titanium (Ti) or

aluminum (Al), and the reinforcing material is usually comprised of alumina (A120J)

or silicon carbide (SiC), in the form of particulate, whiskers, wires, fibers, or flakes.

High-intensity x-ray synchrotronsradiation sources produce high heat-flux x-

ray beams having power densities of greater than 104watts/cm2 which are focusable

on a 1-2 mm target. The energies of the x-rays range from about 3 to about 200 keV

and have penetration lengths on the order of about 0.001 to about 50 mm for various

materials.

The present method uses high power x-rays as a volumetric heat source for

welding MMC elements. The method comprises directing x-ray(s) having a power

density greater than about 104watts/cm2 to a weld line between two adjacent MMC

elements to melt the matrices. Preferably, the beam power must be sufllciently high

for a welding speed of about 15-20 inhnin. In a 3.3 mm thick MMC element. The x-

rays produce volumetric heating in the melt zone along the weld line, whereby the

9

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MMCelements are fused together atthe weld line. Thex-rays donot cause cracking

or destruction of the MMC elements, and importantly, the reinforcing material

remains uniformly distributed in the irradiated region or melt zone along the weld

line.

Experiments were performed at the Advance Photon Source (APS) at

Argonne National Laboratory. The APS is a 7 GeV, third-generation synchrotrons

radiation source. The insertion device (ID) used in the beamline was a 72-period, 3.3

cm period length undulator capable of reaching a peak magnetic field of 0.849 T

when the undulator gap is closed to its minimum setting of 10.5 cm, resulting in a

peak x-ray heat flux of approximately 180 W/mm2 at the location of the experiment

(30 m from the source), for a storage ring beam current of 100 mA. At the first

harmonic energy of 3.2 keV, calculations predict a spot size FWHM of 2.0 mm

horizontal and 1.1 mm vertical. As the undulator gap is increased, the energy of the

first harmonic increases from 3.2 ke V to 12 ke V at 25 cm, while the peak heat flux

decreases to 35 W/mm*.

A1/A120~MMC samples were comprised of a 6061 Al alloy matrix reinforced

with 20V0calcined A120~powder particulate having an average size of 20.8+ 6 pm.

The MMC samples were approximately 25 x 100x 3.3 mm in size.

Welds were pefiormed in air by irradiating a spot on the sample for

approximately 16 seconds at a storage ring beam currentof91 mA. The x-ray beam

10

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was normal to the surface of the sample.

Welding trials were pefiormed on the A1/A120~MMC samples on beamline

l-ID with the undulator gap set to 11 mm, resulting in a peak heat flux of 170

W/mm2 and a first harmonic energy of 3.5 ke V. A fixed mask limited the beam size

5 to 2.5 mm horizontal and 1.0 mm vertical. Cross-section scanning electron

micrograph (SEM) images of the melt zone irradiated for approximately 16 seconds

at a storage ring beam current of 91 mA are shown in FIGS. 1-4. FIG. 1 shows the

melt zone, indicating where x-rays were incident on the sample at the lower left and

exited from the sample at the upper right. Although some vaporization of matrix

10 material did occur, most of the material was still intact and, more importantly, the

distribution of particulate stayed uniform. FIG. 2 shows an enlarged region of the

area where the x-rays impinged on the sample, demonstrating that the density of

particulate is even slightly higher in this region, which is most probably a result of

selective vaporization of the Al matrix (TV,P= 2467” C), leaving behind an excess of

AlzOqparticulate (TV,P= 2980°C). FIG. 3 shows an enlarged view of the region

where the x-rays exited. In the exiting region, the distribution of the particles is

uniform when compared to an unirradiated region, as shown in FIG. 4. These

examples show that fill penetration heating of a 3.3 mm thick sample by x-ray

welding occurs with minimal disruption to metallurgical integrity.

Importantly, although melting occurred throughout the irradiated region, the

11

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reinforcing particulate were unperturbed. This is a significant improvement over

the disruptive effect electron beam and laser sources have on the particulate, or

other reinforcement material, of the metal-matrix composite, including violent

vaporization and destruction of particulate, wherein the work piece was cut rather

5 than fused. FIG. 5 shows an SEM micrograph of an electron-beam-welded MMC,

including a very low density of reinforcing particulate in the vicinity of the melt

zone and a crack extending nearly completely through the work piece. The low

10

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density of the reitiorcing particulate is probably due to vaporization of the

particulate or dissolution of the A120~in the molten Al. Similar behavior has also

been observed in laser welding of A1/SiC MMCS.

Also important is the total absence of cracks in the weld zones according to

the present method, as illustrated in FIGS. 2-5. The matrix metal, 6061 Al, is known

for solidification cracking when welded autogenously using conventional methods.

The absence of cracks in the MMCS subjected to x-ray welding is probably because

the volumetric heating results in relatively slow heating and cooling rates, decreasing

strain on the material in the melt zone.

In an alternate embodiment, high power x-rays are used as a volumetric heat

source for welding metal and/or metal alloy elements, such as aluminum 6061 and

aluminum 7075, as opposed to metals matrices comprised of reinforcing materials.

As in the MMC embodiment above, the x-ray beam has a power density of at least

12

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104W/cm2, a total power of at least 300 watts, and energies in the range of between

about 2 keV and 200 keV. The x-ray beam is directed along the weld line formed by

the juxtaposition of the structures to be welded, creating a melt zone. The structures

are fused together as the x-ray beam causes melting along the weld line.

h additional significant advantage of x-ray welding is that the welding can

be performed at atmospheric pressure. The MMC or metal or metal alloy surfaces to

be joined are generally prepared by removing any oxide layer by filing or other

means known in the art. An inert atmosphere may further be provided, by purging

for example, in the work area containing the MMC or metal or metal alloys to be

welded and wherein the welding is performed.

The foregoing description of a preferred embodiment of the invention has

been presented for purposes of illustration and description. It is not intended to be

exhaustive or to limit the invention to the precise form disclosed, and obviously

many modifications and variations are possible in light of the above teaching. The

embodiments described explain the principles of the invention and practical

applications and should enable others skilled in the art to utilize the invention in

various embodiments and with various modifications as are suited to the particular

use contemplated. While the invention has been described with reference to details

of the illustrated embodiment, these details are not intended to limit the scope of the

invention, rather the scope of the invention is to be defined by the claims appended

13

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hereto.

14

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w

Io01+

‘t

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ABSTIL4CT

A method for joining metal-matrix composites (MMCS) by using high power

x-rays as a volumetric heat source is provided. The method involves directing an x-

ray to the weld line between two adjacent MMCS materials to create an irradiated

region or melt zone. The x-rays have a power density greater than about 104

watts/cm2 and provide the volumetric heat required to join the MMC materials.

Importantly, the reinforcing material of the metal-matrix composites remains

uniformly distributed in the melt zone, and the strength of the MMCS are not

diminished. In an alternate embodiment, high power x-rays are used to provide the

volumetric heat required to weld metal elements, including metal elements

comprised of metal alloys. In an alternate embodiment, high power x-rays are used

to provide the voh.unetric heat required to weld metal elements, including metal

elements comprised of metal alloys.

18

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GCF 2050.3A(5-83)DOE S- 82.547

COMBINED DECLARATION AND POWER OF ATTORNEY

As the below named inventor(s), I (we) herebydeclarethat:My (Our) residence, post office address and citizenship(s) areas stated below next to my (our) name(s).I believe I am the original, first and sole inventor (if only one name is listed below) or an original, first and joint inventor (if

plural names are listed below) of the subject matter which is claimed and for which a patent is sought on the invention entitled

HIGH POWER X&4 Y WELDING (2F METAL-MATRIX COMPOSITES

x

..... ..>.,....7:..“..::,. ... is attached hereto ~~ was tiled as Serial No. and was amended on... .

(if applicable).I (We) hereby state that I (we) have reviewed and understand the contents of the above-identified specification, including

claims as amended by any amendment referred to above.I (We) acknowledge the duty to disclose information which is material to the examination of this application in accordance

with Title 37, Code of Federal Regulations, $1.56.I (We) hereby claim foreign priority benefits under Title 35, United States Code $119 of any foreign application(s) for

patent or inventor’s certificate listed below and have also identified below any foreign application for patentor inventor’s certificatehaving a filing date before that of the application on which priori~ is claimed:

PRIOR FOREIGN APPLICATION(S)Priority

Number Country Filed (Day/Month/Year)

claimed..,= .=,=-- -=,7-.:.---.,. ~-.‘~es No

I (We) hereby claim the benefit under Title 35, United States Code, $120 of any United States application(s) listed belowand insofar as the subject matter of each of the claims of this application is not disclosed in the prior United States application in themanner provided by the fwst paragraph of Title 35, United States Code $112, I acknowledge the duty to disclose material informationas defined in Title 37, Code of Federal Regulations, $1.56 which occurred between the filing date of the prior application and thenational of PCT international filing date of this application:

Serial No. Filing Date status

POWER OF ATTORNEY: As the named inventor(s), I (we) hereby appoint the following attorney(s) and/or agent(s) to prosecutehis application and transact all business in the Patent and Trademark Oftlce connected therewith.

Names and Registration Nos. Names and Registration Nos.

Paul A. Gottlieb 26,733 Robert J. Fisher 26,163William R. Moser 24,763 Mark P. Dvorscak 33,492Judson R. Hightower 26,603 Thomas G. Anderson 27,767Robert J. Marchick 27,057 Lisa M. Soltis 40,623

Send Correspondence To: Direct Telephone Calls To:Paul A. Gottlieb (Name and Telephone Numbers)Ass’t General Counsel for Technology Transfer

and Intellectual PropertyGC-62 (FORSTL) MS-6F-067 Lisa M. Soltis1000 Independence Ave. S.W. (630) 252-2042United States Department of EnergyWashington, D.C. 20585

Page 1 of 2 Pages U.S. DEPARTMENT OF ENERGY

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and Power of Attornev DOE S- 82,547

I (We) hereby declare that all statements made herein of my (our) own knowledge are true and that all statements made oninformation and belief are believed to be true; and further that these statements were made with the knowledge that willfid falsestatements and the like so made are punishable by fine or imprisonment, or both, under $1001 of Title 18 of the United States Codeand that such willful false statements may jeopardize the validity of the application or any patent issuing thereon.

Richard A. RosenbergW & .&.4?x -

Full Name of Inventor Signature

Naperville, IL 11/6/97

Residence (City, State or Foreign Country) Date

1609 Fordham Ct. Naperville, IL 60565 USA

Postal Address (Street, City, State, Zip Code) Citizenship

xxxxxxxxxxx~

George A. Goeppner /Q!!fy # . &fp*

Full Name of Inventor Signature

Orland ParQ IL 11/6/97

Residence (City, State or Foreign Country) Date

13634 Old Post Rd. Orland Park, IL 60467 USA

Postal Address (StreeL City, State, Zip Code) Citizenship

xxXOUXXXX~ xx~

John R. Noonan U/~

Full Name of Inventor Y Signature

Naperville, IL 11/6/97

Residence (City, State or Foreign Country) Date

1016 Kennebec Ln. Naperville, IL 60563 USA

Postal Address (StreeL Ci~, State, Zip Code) Citizenship

xxxxxxxx~ Xx.4 ,,

William J. Farrell &4N[/ll’”w”

Full Name of Inventor Signature

Flossmoor, IL 10/31/97

Residence (City, State or Foreign Country) Date

2908 MacFarlane Cr. Flossmoor, IL 60422 USA

Postal Address (StreeL City, State, Zip Code) Citizenship

Page 2 of 2 Pages U.S. DEPARTMENT OF ENERGY

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Combined Declaration and Power of Attornev DOE S- 82.547

1(We) hereby declare that all statements made herein of my (our) own knowledge are true and that allstatements made on information and belief are believed to be true; and iiu-ther that these statements were madewith the knowledge that willful false statements and the like so made are punishable by fine or imprisonment, orboth, under $1001 of Title 18 of the United States Code and that such willful false statements may jeopardizethe validity of the application or any patent issuing thereon.

Qing Ma- v

Full Name of Inventor / Signature

Westmont, IL 11/6/97

Residence (City, State or Foreign Country) Date

34, W. 65th St. #3, Westmont, IL 60559 China

Postal Address (Street, City, State, Zip Code) Citizenship

Full Name of Inventor Signature

Residence (City, State or Foreign Country) Date

Postal Address (Street, City, State, Zip Code) Citizenship

Full Name of Inventor Signature

Residence (City, State or Foreign Country) Date

Postal Address (Street, City, State, Zip Code) Citizenship

Full Name of Inventor Signature

Residence (City, State or Foreign Country) Date

Postal Address (Street, City, State, Zip Code) Citizenship

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Joint

PATENT ASSIGNMENT FORM

WHEREAS, we, Richard A. Rosenber~, George A. GoeDwer, John R. Noonan. and

William J. Farrell, citizens of the UnitedStates residing

in NatIervi[~e , County of Dupa~e , State of IL ;

in Orland Park . County of Cook , State of IL ;

in Na~erville , County of DuDage , State of IL ;

in Flossmoor , County of Cook , State of IL ;

and Qing Ma, citizen of the People’s Republic of China residing

in Westmont , County of Dupape , State of IL ;

have invented certain new and usejid improvements in HIGH POWER X-RA Y WELDING

OF METAL-MATRIX COMPOSITE$ for which a patent application identljied as Serial No._

wasfi[ed on and executed by us on the fldayof ‘ov: 1997 ; on the 6th

day of ~OV● , 1997 ; on the 6‘h day of Nov” 1997 ; on the31st day

of Oct. ,19 ‘7 ; and on the 6th day of ‘ov “ ,19 ‘7

WHEREAS,the Government of the UnitedStates desires to acquire the entire right, title,and interest in and to said invention and in and to any Letters Patent wherever they maybeissued thereon;

NOW, THEREFORE, to all whom it may concern, be it known thatfor and inconsideration of the sum of One Dollar to us in handpaid by the Government of the UnitedStates, andfor other good and valuable consideration, the rece@ of which is herebyacknowledged, we by these presents do sell, assign, and transfer unto the said Government of theUnitedStates, as represented by the unitedStates Department of Energy, andor its assigns, theentire right, title, and interest in and to the said invention and in and to any and all LettersPatent wherever they may be granted thereon as well as reissues and extensions of said LettersPatent are or maybe granted reissued or extended asfilly and entirely as the same wouldhave been held or enjoyed by us had this assignment not been made.

We agree to make, execute, and deliver unto the Government of the UnitedStates, or tothe UnitedStates Department of Energy, any and allpapers, documents, aj?davits, renewal,divisional and reissue applications, statements, or other instrumentsin such usual or otherforms, terms and contents as ma-ybe required by the UnitedStates Depar~ent of Energy, or itsduly authorized representative, in or incident to theprosecution or conduct of any and allapplications, before as well as ajler the issuance of any Letters thereon, or in the adjustment orsettlement of any interferences or other actions or proceedings that said applications mayencounter or in which they may become involved and we agree that we will encounter or inwhich they may become involved and we agree that we will aid the Government of the UnitedStates in every way inprotecting the inventions as may be requested by the UnitedStatesDepartment of Ener~ or its assigns, except that any expenses arising through extending suchassistance will be paidfor by proper arrangement with the Government of the UnitedStates.

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-2-

WITNESS:

WITNESS:

/ CL/

WITNESS:

WITNESS:

INVENTORS:

(SEAL)/ u

Date

Approved and consented to this day of , 19—“

ATTEST:

(SEAL)

Its

Accepted for the Benefit of the Government of the United States.

UNITED STATES Department OF ENERGYWITNESS:

BvAssistant Genera1 Counse1 for Patents

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DISCLOSUREVERIFICATION

TITLE :

DOE CASE NO:

INVENTOR(S):

Every inventorto disclose to

HIGH POWER X-RAY WELDING OF METAL-MA TRIX COMPOSITES

S-82,547

Richard A. Rosenberg, George A. Goeppner, John R. Noonan,William J. Farrell and Qing Ma

seeking patent protection for his invention has an obligationthe U.S. Patent and Trademark Office information of which he or

she is aware which is material to examination of the patent application. Suchinformation is material where there is a substantial likelihood that a reason-able examiner would consider it important in deciding whether to allow theapplication to issue as a patent. Information of this type WOU1d include, butnot be limited to, existing publications and any public use or sale of theinvention, or any aspect of it, or similar information such as related art,from which it COU1d be concluded that the invention WOU1d have been obvious toan individual skilled in this technology at the time of invention.

YOUR STRICT AllENTION TO COMPLETION OF THIS DISCLOSURE VERIFICATION IS VITALBECAUSE THE VALIDIN OF ANY PATENT ISSUED COVERING THIS INVENTION, IN PART,DEPENDS UPON YOUR MEETING THIS OBLIGATION.

To ensure that your obligation is met and that W known information of thistype pertaining to this invention is brought to the attention of the U.S.Patent and Trademark Office, please complete and sign the following:

In addition to the information set forth in the Invention Disclosure are youaware of any:

YES NO

❑ EY

E-m

❑ llr

LHr

❑ ti

Reduction to practice of the invention? If so, on what datedid the first reduction to practice occur?

Publication of the invention? If so, what is the dateof the first such publication?

Routine use of the invention? If so, describe the extentof use and give the date of the first routine use.

Experimental use of the invention? If SO, give the date

of the first experimental use.

Other U.S. or foreign patent applications prepared orfiled disclosing this invention?

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-2-

❑ ▼❉Sale or offer of sale of the invention? If so, what isthe date of first sale or offer of sale?

Information material to examination of the patent❑l# application which was not previously disclosed to DOE?

If the answer to anyone or more of the above questions is in the affirmative,please identify the date of each event, give other identifying data anddescribe the circumstances surrounding it. If a publication of the inventionhas occurred, attach a copy of the publication and indicate the date ofpublication first became available to the public. Copies of any materialreferences should also be provided and the references listed as an appendixhereto.

t /Inventor

tDate ,

Date’ ‘

Inventor

Date

ventor

9/2-s74 yDate

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TITLE :

DOE CASE NO:

INVENTOR(S):

Every inventorto disclose to

DISCLOSUREVERIFICATION

HIGH POWER X-RAY WELDING OF METAL-M4 T~X COMPOSITES

S-82,547

Richard A. Rosenberg, George A. Goeppner, John R. Noonan,William J Farrell and Qing Ma

seeking patent protection for his invention has an obligationthe U.S. Patent and Trademark Office information of which he or

she is aware which is material to examination of the patent application. Suchinformation is material where there is a substantial likelihood that a reason-able examiner would consider it important in deciding whether to allow theapplication to issue as a patent. Information of this type WOU1d include, butnot be limited to, existing publications and any public use or sale of theinvention, or any aspect of it, or similar information such as related art,from which it COU1d be concluded that the invention WOU1d have been obvious toan individual skilled in this technology at the time of invention.

YOUR STRICT AllENTION TO COMPLETION OF THIS DISCLOSURE VERIFICATION IS VITALBECAUSE THE VALIDITY OF ANY PATENT ISSUED COVERING THIS INVENTION, IN PART,DEPENDS UPON YOUR MEETING THIS OBLIGATION.

To ensure that your obligation is met and that W! known information of thistype pertaining to this invention is brought to the attention of the U.S.Patent and Trademark Office, please complete and sign the following:

In addition to the information set forth in the Invention Disclosure are youaware of any:

YES NO

dn

dn❑ n’❑ a’Em’

Reduction to practice of the invention? If so, on What datedid the first reduction to practice occur?

Publication of the invention? If so, what is the dateof the first such publication?

Routine use of the invention? If so, describe the extentof use and give the date of the first routine use.

Experimental use of the invention? If so, give the dateof the first experimental use.

Other U.S. or foreign patent applications prepared orfiled disclosing this invention?

.

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❑ H’❑ d

-2-

Sale or offer of sale of the invention? If so, what isthe date of first sale or offer of sale?

Information material to examination of the patentapplication which was not previously disclosed to DOE?

If the answer to anyone or more of the above questions is in the affirmative,please identify the date of each event, give other identifying data anddescribe the circumstances surrounding it. If a publication of the inventionhas occurred, attach a copy of the publication and indicate the date ofpublication first became available to the public. Copies of any materialreferences should also be provided and the references listed as an appendixhereto.

Inventor

Date

Inventor

Date

Inventor

,Invent&

Date

Inventor

Date