USOO734 1757B2

(12) United States Patent (10) Patent No.: US 7,341,757 B2

Yadav (45) Date of Patent: Mar. 11, 2008
(54) POLYMERNANOTECHNOLOGY 3,635,819 A 1/1972 Kaiser
3,700,575 A 10, 1972 Paine
(75) Inventor: Tapesh Yadav, Longmont, CO (US) 3,734,790 A 5/1973 Kirshenbaum
3,764,540 A 10, 1973 Khalafalla et al.
(73) Assignee: NanoProducts Corporation, 3.806.449 A 4, 1974 Kaiser
Longmont, CO (US) 3,905,109 A 9/1975 Cohen et al.
(*) Notice: Subject to any disclaimer, the term of this 3,917,538 A 11/1975 Rosensweig
patent is extended or adjusted under 35 3,981,844 A 9, 1976 Romankiw
U.S.C. 154(b) by O days. 4,017,820 A 4, 1977 ROSS
4,019,994 A 4/1977 Kelley
(21) Appl. No.: 11/054,786 4,094,804. A 6/1978 Shimoizaka
4,208,294 A 6, 1980 Khalafalla et al.
(22) Filed: Feb. 10, 2005 4,234,437 A 1 1/1980 Friberg et al.
(65) Prior Publication Data 4.252,678 A 2f1981 Smith
4,280,918 A 7/1981 Homola et al.
US 2005/0147747 A1 Jul. 7, 2005 4,315,827 A 2/1982 Bottenberg et al.
Related U.S. Application Data
(60) Division of application No. 10/143,995, filed on May
10, 2002, now Pat. No. 6,855.426, and a continuation- (Continued)
in-part of application No. 10/004,387, filed on Dec. 4, OTHER PUBLICATIONS
2001, now Pat. No. 6,652,967.
(60) Provisional application No. 60/357.946, filed on Feb. U.S. Appl. No. 10/424,395, filed Apr. 28, 2003.
19, 2002, provisional application No. 60/310,967, Continued
filed on Aug. 8, 2001. (Continued)
Primary Examiner Vivian Chen
(51) Int. Cl. (74) Attorney, Agent, or Firm—Foley & Lardner LLP
B05D 7/02 (2006.01)
A6 IK 9/14 (2006.01) (57) ABSTRACT
B32B I5/08 (2006.01)
B32B 8/00 (2006.01)
B32B 43/00 (2006.01) Size-confined nanocomposite powders and methods for their
(52) U.S. Cl. .................. 427/2.14; 427/123; 427/126.1: manufacture are provided by coating fine powders with a
427/126.3; 427/127; 427/212:427/222; 428/403; nanoscale powder of a different composition. The nanocom
428/404: 428/407; 264/109 posite plastics offer performance characteristics approaching
(58) Field of Classification Search ..................... None those of metals and alloys. The nanocomposite powders are
See application file for complete search history. alternatively used for dispersion strengthening of metals,
alloys, and ceramics. Materials based nanotechnology for
(56) References Cited energy devices and programmable drug delivery are
U.S. PATENT DOCUMENTS included.
3,531,413 A 9/1970 Rosensweig
3,565,676 A 2, 1971 Holz1 16 Claims, 2 Drawing Sheets

303 O O
A O O 9O
O O O O
O O

O
2. Co.
OO - O - O O A-305
OO og
O Oo C O
 US 7,341,757 B2
Page 2

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U.S. Patent Mar. 11, 2008 Sheet 1 of 2 US 7,341,757 B2

SELECT FINE POWDERS

SELECT NANOSCALE
POWDERS OF A 103
101 OF A FIRST SECOND COMPOSITION
COMPOSITION SUTABLE ASA FLLER
SUTABLE ASA MATRIX
OR DISPERSANT

BOND (COAT) THE

NANOSCALE POWDERS
ON THE SURFACE OF
105 THE FINE POWDERS
FIG. 1

COLLECT THE
107 RESULTING SIZE
CONFINED
NANOCOMPOSITE
POWDER MATERIAL

PRODUCE SIZE
CONFINED
NANOCOMPOSITE
POWDER 201

POST-PROCESS TO
SIMPLIFY PART
MANUFACTURING

205
FORM FINISHED PART
FROM SIZE-CONFINED
NANOCOMPOSITE
POWDER

FIG. 2
U.S. Patent US 7,341,757 B2

FIG. 3
 US 7,341,757 B2
1. 2
POLYMERNANOTECHNOLOGY sion strengthening is a method used to increase the strength
and high temperature performance of metal alloys by incor
RELATED APPLICATIONS porating a fine distribution of hard particulates within a
load-bearing matrix. These materials are formed, for
This application is a divisional of U.S. application Ser. example, by mixing particles with a matrix material com
No. 10/143,995. filed May 10, 2002, now U.S. Pat. No. prising the metal, metal alloy, or other material to be
6.855.426, which claims the benefit of U.S. Application No. strengthened. This method takes advantage of the fact that
60/357.946, filed Feb. 19, 2002, the specification of which dislocation motion is hindered by the presence of the fine
is incorporated herein by reference in its entirety, and is a particulate. It is expected that as nanoparticles replace
continuation-in-part of U.S. application Ser. No. 10/004, 10 microparticles in dispersion-strengthened materials, the per
387, filed Dec. 4, 2001, now U.S. Pat. No. 6,652,967, which formance of these materials will increase.
is incorporated herein by reference in its entirety, which However, it has been difficult to use nanoscale particu
claims the benefit of U.S. Application No. 60/310,967, filed lates in commercial dispersion strengthening applications
Aug. 8, 2001. because of poor bonding at the matrix and the nanoparticle
15 dispersant interface. The lack of an intimate, uniform bond
BACKGROUND OF THE INVENTION ing between the matrix and dispersant materials results in
Sub-optimal performance of the composite materials. Fur
1. Field of the Invention ther, conventional techniques experience difficulty in
The present invention relates, in general, to use of nano achieving and maintaining a homogeneous distribution of
technology, and, more particularly, methods to produce the nanoparticles in the matrix.
significantly improved material performance through the use In general, the commercial promise and Social benefits of
of composite nanoparticles. nanotechnology are currently limited by the difficulty in
2. Relevant Background post-processing nanoparticles into nanotechnology prod
Powders are used in numerous applications. They are the ucts. There is a need for a technology that can address these
building blocks of electronic, telecommunication, electrical, 25 post-processing limitations.
magnetic, structural, optical, biomedical, chemical, thermal,
and consumer goods. On-going market demands for Smaller, SUMMARY OF THE INVENTION
faster, Superior and more portable products have demanded
miniaturization of numerous devices. This, in turn, demands Briefly stated, the present invention involves the use of
miniaturization of the building blocks, i.e. the powders. 30 nanotechnology to produce composite nanoparticles, as well
Sub-micron and nano-engineered (or nanoscale, nanosize, as new classes of materials from those composite nanopar
ultrafine) powders, with a size 10 to 100 times smaller than ticles. The invention addresses known issues with the use of
conventional micron size powders, enable quality improve nanoparticles and offers unusual methods for making novel
ment and differentiation of product characteristics at Scales materials useful in a wide range of applications. More
currently unachievable by commercially available micron 35 specifically, the invention teaches method to create materials
sized powders. from plastics that can compete with metals and alloys in
Nanopowders in particular and Sub-micron powders in certain applications. The invention further teaches method to
general are a novel family of materials whose distinguishing create materials from resins, ceramics, metals or alloys that
feature is that their domain size is so Small that size are expected to dramatically improve the performance of the
confinement effects become a significant determinant of the 40 constituent materials they are fabricated from. Further, the
materials performance. Such confinement effects can, invention discloses some illustrative applications and their
therefore, lead to a wide range of commercially important commercial significance.
properties. Nanopowders, therefore, are an extraordinary
opportunity for design, development and commercialization BRIEF DESCRIPTION OF THE DRAWINGS
of a wide range of devices and products for various appli 45
cations. Furthermore, since they represent a whole new FIG. 1 shows an exemplary overall approach for produc
family of material precursors where conventional coarse ing unusual materials in accordance with the present inven
grain physiochemical mechanisms are not applicable, these tion; and
materials offer unique combination of properties that can FIG. 2 shows an exemplary overall approach for produc
enable novel and multifunctional components of unmatched 50 ing a product from the unusual materials in accordance with
performance. Yadav et al. in commonly assigned U.S. Pat. the present invention;
No. 6.569,397 which along with the references contained FIG. 3 illustrates and example of nanocomposite particle
therein are hereby incorporated by reference in full, teach production; and
Some applications of Sub-micron and nanoscale powders. FIG. 4 illustrates production of useful materials from
It has been anticipated by those skilled in the art that size 55 nanocomposite powders in accordance with the present
confinement could potentially produce materials with sig invention.
nificantly improved strength, toughness, hardness, and other
mechanical properties. However, size confinement has been DETAILED DESCRIPTION OF THE
difficult to reduce to commercial practice. The reasons for PREFERRED EMBODIMENTS
this failure, in part, include (a) current inability to retain the 60
nanoscale grain size when nanoparticles are post-processed This invention is generally directed to size-confined,
into a final commercial product, and (b) agglomeration and interface-fused nanocomposite particles and products pro
aggregation of nanoparticles that in turn produces defects duced from Such particles. Composite nanoparticles pro
and poor bonding at interfaces. duced in accordance with the present invention comprise,
Yet another method of improving the mechanical perfor 65 for example fine powders in which nanoscale particles are
mance of materials that is known to those in the art is to bonded to the Surfaces of nanoscale or micron scale particles
employ particles to dispersion strengthen materials. Disper of a matrix material. An important difference between other
 US 7,341,757 B2
3 4
methods that merely teach coating of a powder with another performing materials, Superior in strength, modulus, creep
Substance, is that in present invention the nanoscale particles and other commercially useful characteristics. Despite the
on the Surface and the coated powder chemically bond and potential outlined by theory, in practice this has not been
form a layer where the two compositions create a state reduced to commercial use. In part, this failure is because it
synergistically reducing the free energies from the bonding. is very difficult to retain the nanoscale dimensions as nano
Thus, the coated nanocomposite particles taught herein are particles are processed into final useful products. When used
characterized by the composition of the powder coated, as dispersants, it is difficult to disperse the nanoparticles
composition of the nanoparticles that form the coating, and homogeneously in a matrix. Further, it is difficult to process
the distinct composition of an interface that results from the the nanoparticles and a matrix to achieve intimate bonding
bonding process and consequent reduction in the chemical 10 at the interface; normally, defects or the presence of gases
potential. Therefore, unlike other techniques in the art that adsorbed onto the interfaces causes the bonding to be poor.
merely teach methods for forming coated powders, this Conventional methods of forming a product from nano
invention teaches a novel composition of matter. Also, particles or forming a nano-dispersion strengthened material
unlike prior approaches for forming composites materials, combines the process of forming the end product and
the present invention enables a high degree of control and 15 interface engineering. That is, both the product manufactur
flexibility in engineering the interface between the nanopar ing step and the interface-engineering step happen together,
ticle dispersant and the matrix material. Further, the result each affecting and often creating confounding interactions
ing powder is uniform at a fine powder scale to that when the with the other. To be more specific, numerous products
composite nanopowders are used to form materials, unifor prepared from powders require sintering which normally is
mity and homogeneity of the resulting material is readily practiced at elevated temperatures. These elevated tempera
controlled. tures, unfortunately, also cause grain coarsening and the loss
Definitions of nanoscale confinement. Similarly, dispersion of particu
For purposes of clarity the following definitions are lates in alloys is often done at elevated temperatures or in
provided to aid understanding of description and specific molten form of a metal or alloy. These processing conditions
examples provided herein: 25 lead to phase segregation or poor distribution and bubbling
“Fine powders', as the term used herein, are powders that out of the particles given that they have gases adsorbed at
their interface.
simultaneously satisfy the following: It is also common to prepare mixtures of powders in
particles with mean size less than 100 microns, preferably advance of the manufacturing processes used to make a
less than 10 microns, and 30 useful article. The prepared mixtures are packaged, stored,
particles with aspect ratio between 1 and 1,000,000. and handled in ways that affect the integrity of the powders.
“Submicron powders', as the term used herein, are fine For example, separation of the mixture reduces homogeneity
powders that simultaneously satisfy the following: leading to variability in performance of the material in the
1. particles with mean size less than 1 micron, and manufacturing processes.
particles with aspect ratio between 1 and 1,000,000. 35 In accordance with the present invention, the product
“Nanopowders” (or “nanosize powders' or “nanoscale manufacturing operation(s) and the interface-engineering
powders” or “nanoparticles'), as the term used herein, are operation(s) are separated. The interface engineering is done
fine powders that simultaneously satisfy the following: first in operations shown in FIG. 1, and at processing
1. particles with mean size less than 250 nanometers, conditions that prevent or limit the loss of size confinement
preferably less than 100 nanometers, and 40 effects. Next, the product manufacturing operations shown
2. particles with aspect ratio between 1 and 1,000,000. in FIG. 2 are conducted. Preferably, the nanocomposite
“Pure powders,” as the term used herein, are powders that powders produced in the interface engineering phase are
have composition purity of at least 99.9%, preferably Suitably rugged to preserve size confinement effects during
99.99% by metal basis. portions of the manufacturing operations shown in FIG. 2 in
“Powder, as the term used herein encompasses oxides, 45 which size confinement effects are relevant, as well as any
carbides, nitrides, chalcogenides, metals, alloys, and com packaging, storage, and handling operations that occur
binations thereof. The term includes hollow, dense, porous, between the interface engineering operations shown in FIG.
semi-porous, coated, uncoated, layered, laminated, simple, 1 and the manufacturing operations shown in FIG. 2.
complex, dendritic, inorganic, organic, elemental, non-el As shown in FIG. 1, matrix powders comprising fine
emental, composite, doped, undoped, spherical, non-spheri 50 powders of a composition suitable for the desired matrix are
cal, Surface functionalized, Surface non-functionalized, sto selected in 101, where the fine powders may be nanoscale,
ichiometric, and non-stoichiometric form or Substance. micron Scale, or in Some cases larger. In 103, nanoscale
The present invention involves size confinement, and in powders of a second composition, different than the matrix
particular involves size confinement through the use of material selected in 101, are selected. The composition of
nanoscale particles. 55 the material selected in 103 is selected to be suitable as a
One feature of the present invention involves forming filler or dispersant in the desired composite.
nanocomposite particles (also called nanocomposite pow In one embodiment, the nanoscale powders or Submicron
ders) that are size-confined in that they retain useful prop powders selected in 101 are coated in operation 105 with the
erties associated with size confinement when placed in powders selected in 103, preferably such that coating is
proximity with other matter as required by most useful 60 significantly thinner than the composite powder size. On
applications. weight basis, it is preferred that the loading of coated
It is known that the mechanical properties of materials can nanoparticulate material be less than or equal to 40% by
be improved by dispersion strengthening or hard working weight of the resultant nanocomposite powder, and more
the materials to introduce interfaces where dislocations get preferred to be less than 5% in some applications. In some
pinned. The emergence of nanotechnology has led those in 65 applications, this loading can be as Small as 0.25% to 2%, or
the art to theoretically suggest that materials having nanos lower than 0.25%, and in others it may be higher than 40%
cale dimensions could be used to form unusually Superior by weight. This coating can be done using techniques such
 US 7,341,757 B2
5 6
as chemical vapor deposition, physical vapor deposition, Some non-limiting illustrations of an alloy that can be
monolayer reactive deposition, precipitation, condensation, prepared using the nanocomposite powders in accordance
selective and controlled reaction, infiltration, laser deposi with this invention include alloys comprising two metals,
tion, and those taught by commonly owned co-pending U.S. alloys comprising three or more metals, alloys comprising
patent application Ser. No. 10/004,387 filed on Dec. 4, 2001 metals and semimetal or nomnetal or both. Some of the
entitled NANO-DISPERSED POWDERS AND METH preferred alloys for dispersion strengthening include those
ODS FOR THEIR MANUFACTURE, the specification of comprising steel, iron alloys, aluminum alloys, brass,
which is incorporated herein by reference. The particles so bronze, nickel alloys, molybdenum alloys, titanium alloys,
produced can Subsequently be processed into useful prod Superalloys, and alloys comprising of rare earth elements.
ucts. The presence of the coating prevents or limits the 10 Fine powders, Submicron powders, and nanoparticles for
coarsening of the nanoparticles and the coated powder, and this invention may be produced and processed by any
gives the manufacture greater control over the manner in method including those that have been discussed in com
which size confinement effects of the composite particles monly owned patents (U.S. Pat. Nos. 6,344.271, 6.228,904,
affect the properties of the useful article being produced. 6,202,471, 5,984,997, 5,952,040, 5,905,000, 5,851,507, and
In another embodiment, fine powders or Submicron pow 15 5,788,738) which along with the references cited therein are
ders or nanoscale powders of first composition of material incorporated herein by reference.
(selected in operation 101) are post-processed in operation The manufacturing processes shown in FIG. 2 generally
105 with nanoparticles of second composition selected in involve producing, selecting or otherwise obtaining size
operation 103. The post-processing produces composite confined nanocomposite powders in operation 201, Such as
particles where the nanoparticles of second composition coat described in reference to FIG. 1. Optionally, the nanocom
the powders of first composition. The coating bonds the posite powders may be post-processed to simplify part
interface between the first and the second composition. The manufacturing in 203. Post-processing operation 203 may
coating performed in 105 can be complete, partial, dense, involve any of a variety of processes such as thermal
porous, monolayer, multi-layer, uniform or non-uniform. treatment, drying, chemical treatment, Surface modification,
The composite particles so produced can then be collected in 25 de-agglomeration, agglomeration, reduction, oxidation, dis
operation 107, and processed into useful products as Sug persion, static removal, and the like that have an impact on
gested in FIG. 2. handling the nanocomposite powder during manufacture, or
The presence of the coating and interface bonding (a) alter the nanocomposite powder's performance in the manu
prevents or limits the coarsening of the nanoparticles, and factured product. In operation 203, a finished or partially
(b) helps retain the size confinement of the powders of first 30 finished part is manufactured from the size-confined nano
composition due the presence of the coating of second composite powder using techniques including injection
composition. For this embodiment, one or more of these molding, spray coating, pressing, hipping, tape casting,
methods can be employed to form the composite particles— screen printing, mold stamping, ink-jet printing, melt pro
cyogenic fusion, mechano-chemical fusion caused by vari cessing, electrophoresis, and the like.
ous variations of milling, chemical vapor deposition, physi 35 FIG.3 and FIG. 4 illustrate the nanocomposite production
cal vapor deposition, reactive deposition, precipitation, and manufactured product production processes described in
condensation, selective and controlled reaction of Surface, FIG. 1 and FIG. 2. As generally shown in FIG. 3, fine
infiltration, laser deposition, and those taught by a com powder particles 301, selected in operation 101, are pro
monly-pending U.S. patent application Ser. No. 10/004,387. cessed with nanoscale powders 303, selected in operation
Examples of a first composition selected in 103 in a 40 103, to form a nanocomposite 305. FIG. 3 illustrates an
composite particle can be a polymer, metal, ceramic, alloy or example nanocomposite particle 305 in cross-section in
a composite. The second composition can also be a polymer, which the nanoparticles 303 substantially completely bond
metal, ceramic, alloy or a composite; however, for this with the surface of fine powder particle 301. However, as
invention the Substance constituting the first composition is noted earlier, the Surface coverage degree and uniformity are
different in one or more way than the second composition. 45 a matter of design choice. Significantly, nanoparticles 303
Some non-limiting illustrations of a polymer useful as a form an energy favored bond with the surface of fine powder
first composition in 103 include polyethylene, polypropy particle 301 so that, absent application of external energy,
lene, polystyrene, polyurethane, polyacrylates, polycarbon particles 303 will remain bonded with the particle 301.
ates, polyamides, polyamines, polyimines, and any other In FIG. 4, once the nanocomposite powders 401 are
carbon containing polymeric compound.
50 selected in step 201, they may be post-processed (not
shown), and formed into a consolidated structure 405 by
Some non-limiting illustrations of a ceramic useful as a various manufacturing means. The consolidated structure
first composition in 103 include oxides, carbides, nitrides, 405 may be formed in a manner that retains the surface
borides, chalcogenides, halides, silicides, and phosphides. bonding of nanoparticles 303 and fine powder particles 301.
Ceramics for this invention can be single metal compounds 55 Alternatively, the manufacturing process may provide Suf
or multi-metal compounds. The composition selected in 103 ficient energy to break some or all of the bonds.
may also comprise complex compositions such as oxycar
bides, oxynitrides, carbonitrides, boro-nitrides, and non EXAMPLE 1.
Stoichiometric compositions.
Some non-limiting illustrations of a metal useful in as a 60 Dispersion Strengthening of Materials
first composition in 103 include transition metals, alkali
metals, alkaline earth metals, rare earth metals, and semi Dispersion strengthening is a method to increase the
metals. It is preferred that the metal be low cost and strength of metal alloys by incorporating a fine distribution
otherwise compatible with the processing and intended use of hard particulates. This method takes advantage of the fact
for the metal. Some of the preferred metals for dispersion 65 that dislocation motion is hindered by the presence of the
strengthening include those comprising copper, molybde fine particulate. This can be quantified by the following
num, iron, nickel, and cobalt. equation:
 US 7,341,757 B2
8
fillers are often nanoscale powders, Submicron powders or
fine powders (e.g., calcium carbonates, fumed silicas, car
bon black, talc). Everything else remaining same, the shape,
the size, and the concentration of mineral filler addition
determines the performance the filler-filled plastic. How
ever, an outstanding problem has been the ability to homo
where t-stress to force a dislocation through the particulate, geneously distribute nanostructured or Submicron mineral
G=shear modulus, b=Burger's vector, a spacing between fillers as these fillers have tendencies to agglomerate.
particulate. Another issue is the bonding of the filler interface to the
One of the primary variables in this equation (for a given 10 polymer. These reasons, in part, have limited the commer
chemistry) is the spacing between the particulate. This cially achieved performance of filled polymers.
spacing can be reduced by decreasing the size of the To fully appreciate the relevance of nanotechnology to
particulate, giving a resultant increase in the shear strength plastics, consider the constitutive equation for tensile
for a given Volume fraction of particulate. By decreasing the strength of a polymer,
size of the particulate, the total mass and Volume of par 15
ticulate in the composite need not change. In this manner,
valuable properties of the matrix material are expected to where,
remain constant or be improved by decreasing the size of the k: geometric constant
particulate rather than being altered or compromised as E: Young's modulus of the material
might occur if the particulate loading were increased. y: fracture energy (not surface energy per unit area to
For example, 10 um powders have a volume of about account for plastic flow)
5.24x10 cc/particle (for spheres), while 100 nm powders a: length of crack
have a volume of about 5.24x10 cc./particle. Everything This equation suggests that the tensile strength of a plastic
else remaining same and assuming uniform distribution, this is, in part, a function of the length of the naturally occurring
represents a six order of magnitude difference in the number 25
cracks in a compounded plastic. As a rule of thumb, for
of reinforcing particles in a given volume of the composite. compounded plastic powders of about 20 to 50 micron size,
The increased dispersant concentration by number signifi this naturally occurring crack length is usually between 1 to
cantly decreases the inter-particle spacing (W). By using 100
nm dispersant particles instead of 10 micron dispersant 10 microns. When a plastic fails, it is often because of
particles, the inter-particle spacing (W) can be reduced by 30
stresses that concentrate around these cracks and grow the
about 100 fold, which translates to a 100 fold enhancement crack. The presence of fillers tends to pin these cracks and
in failure stress, T. provide some limited improvement in the performance of
In order to improve the performance of the metals like the plastic.
copper and alloys like nickel aluminide, it is preferred that Everything else remaining same, if plastic powders can be
the nanoparticles be fused on the surface of the metal or 35
size-confined by a well-bonded mineral filler, the crack
alloy powder. This can be accomplished using Hosokawa length can be confined to a domain size less than the plastic
Micron's Mechanochemical Bonding R equipment. For powder size. This can significantly enhance the tensile
example, 1 wt % of aluminum oxide nanoparticles can be strength of the compounded plastic. Other mechanical prop
mechanochemically bonded with 5 to 20 micron copper erties can similarly be enhanced.
powders. Other weight loadings and different particle sizes 40
The Superior performing plastic can be achieved as fol
can be utilized as appropriate. The resulting nano-engi lows. Produce plastic powders of less than 5 microns,
neered composite particles are ready to be used for oxide preferably less than 1 micron, more preferably 0.5 micron,
dispersion strengthened materials. It is anticipated that the and most preferably 100 nm in size. Coat (with good
uniform distribution and the interface bonding of the pow interface bonding) or mechano-chemically bond a nanoscale
ders will significantly enhance the performance of the result 45
filler on the surface of this plastic powder by any technique
ing material. thereby forming coated size-confined plastic powders. Ulti
Alternatively, by using indium tin oxide or conductive mately, the present invention is used to produce a product
nanoparticle dispersant, the electrical properties of the from the coated size-confined plastic powder.
resulting oxide dispersion strengthened alloy can be In another embodiment, a further step can comprise
enhanced. Similarly, by using magnetic compositions, addi 50 processing the coated size-confined plastic powders with
tional functionality can be added to the dispersion strength additional plastic material to form a compounded plastic
ened metal or alloy. In yet other applications, the dispersant powder of a size Suitable for injection molding. Such process
composition may be chosen to be one that is thermodynami can include agglomeration with uncoated plastic powders or
cally stable with the matrix at processing and use tempera ball milling or any other technique, and performed, for
tures and environments. To illustrate, but not limit, the use 55
example, in post-processing operation 203 shown in FIG. 2.
of yttrium aluminum garnet instead of yttria in aluminum Table 1 presents specific data on the benefits of nanopar
alloys can prevent the degradation of yttria strengthened ticle enabled size-confined plastic powders in contrast with
aluminum alloy over time at high temperatures due to the conventional polymers, metals and alloys.
reaction thermodynamically favored between yttria and alu
minum. 60 TABLE 1.
MECHANICAL PROPERTIES OF MATERIALS
EXAMPLE 2
Typical Tensile Strength (Yield,
Superior Performing Plastics Material MPa)
65 20-50 micron Polypropylene with 30
Mineral fillers are commonly used in plastics to lower naturally occurring crack length = 5
cost or to enhance performance of the plastic. These mineral
 US 7,341,757 B2
9 10
In another embodiment, a further step can comprise
TABLE 1-continued processing the coated size-confined powders with additional
MECHANICAL PROPERTIES OF MATERLALS
material to form a compounded powder of a size suitable for
injection molding or other processing technique. Such pro
Typical Tensile Strength (Yield, cess can include agglomeration with uncoated powders or
Material MPa) ball milling or any other technique.
micron
Compared with parts produced using 20+ micron powders
Aluminum 103 of conventional metals, alloys, and ceramics, parts produced
Brass, Annealed 250 using size-confined materials prepared by the method out
Bronze, Annealed 270 10 lined above can improve tensile strengths by greater than
Nickel Superalloy 276 25%. Other mechanical, magnetic, electrical, thermal, opti
Low Carbon Steel 285
Stainless Steel 290 cal, and other properties of commonly available materials
Nanoparticle size-confined 95 can similarly be improved by 25% or more.
Polypropylene with crack length
confined to 500 nm 15
Uses
Nanoparticle size-confined
Polypropylene with crack length
212 This invention can be utilized to further improve the
confined to 100 nm
performance of known oxide dispersion strengthened alloys.
These alloys are particularly desirable for engines, lighting
parts, medical devices, X-ray imaging Systems, cryogenic
Table 1 Suggests that nanoparticle enabled size confine equipment, automotive parts, medical implants, nuclear
ment can enhance the tensile strength of a plastic to a level industry, offshore piping, dental alloys, sporting goods, parts
where they may be able to compete with certain metals and Subject to high temperatures or corrosion, and environmen
alloys. Size-confined nanocomposite plastics become par tal cleaning equipment.
ticularly attractive when the tensile strength exceeds 75 Size-confined materials that can offer significantly
MPa. Given that plastics can be injection molded and 25 improved performance are useful in wide range of new
formed by other techniques into net shape parts, this applications. Of particular interest are fuel cell System parts
approach can significantly reduce the cost of making com and micro-turbines given the importance of weight and costs
plex parts while delivering competitive structural perfor for their wide spread commercial acceptance.
This invention can also be used where dissimilar materials
mance. Plastics are lighter than metals and the consequent 30 need to be bonded. The filler, in such cases can be prepared
weight related savings could significantly enhance the sys with a composition of the dissimilar material thereby aiding
tem wide performance. Such enhanced plastics can be useful the bonding process between matrix and the dissimilar
in automobiles, mobile consumer products such as laptops, material.
phones and hand-held computers, architecture, and aircraft). Further, this invention can be used to engineer other
Additionally, size-confined plastic powders with 35 properties of materials, e.g., magnetic, electrical, electro
enhanced mechanical properties can also reduce capital, chemical, optical, chemical, catalytic, and thermal. This can
operating, and labor costs associated with Such tasks as be achieved because of the fact that the bonding of another
post-machining, finishing, and others that are necessary material on the Surface of a Submicron or nanoscale powder
when complex metal parts are being formed. The consequent isolates the core particle. To illustrate but not limit, by
reduction in environmental waste and the possibility of 40 coating magnetically soft nanoscale powders (less than 250
recycling or reuse further make Such nanotechnology attrac nm average size) on magnetically hard micron-scale pow
tive. At the end of their useful life, such materials can also ders (greater than 1 micron but less than 1000 microns), the
be used as precursors to make metal carbides and other nanocomposite produced is anticipated to exhibit unusual
inorganics through pyrolysis and related methods. magnetic performance Such as the hard magnetic domains
45 that are functionally isolated from the other similar domains.
EXAMPLE 3 Such materials are expected to be particularly useful in data
storage, signal transmission, signal interception, intelligence
Superior Performing Ceramics, Metals and Alloys gathering devices, and power conversion devices.
Similarly, by bonding electrically insulating nanoscale
As in example 2, nanoscale fillers can also be used with 50 powder compositions on magnetic micron-scale powders,
ceramics, metals and alloys to form Superior performing energy storage capacity can be increased while reducing
materials. The constitutive equation presented in example 2 losses due to eddy currents. In contrast, current technology
applies to other compositions of matter with the modifica using oxidized coatings to provide such insulation are lim
tion that many compositions do not experience plastic flow ited to magnetic materials that oxidize readily, and can not
and therefore fracture energy has to be replaced with surface 55 independently control the insulator composition or thick
energy per unit area or other Suitable quantity. ness. In this manner, the present invention enables produc
The Superior performing ceramic or metal or alloy can be tion of novel materials for electronic components and elec
achieved as follows. Produce powders of desired composi trical and energy devices. It is expected that these devices
tion of average size less than 50 microns, preferably less and components can significantly reduce losses and/or
than 5 micron, more preferably 0.5 micron, and most pref 60 improve energy efficiency and/or improve size to perfor
erably 100 nm in size. Coat (with good interface bonding) or mance ratio and/or weight to performance ratios by at least
fuse a nanoscale filler on the surface of this powder by any by 5% when compared with equivalent devices and com
technique thereby forming coated size-confined powders ponents prepared from uncoated micron-scale powders.
with an average domain size of the confinement of less than The use of appropriate composition on the Surface can
5 microns, preferably less than 1 micron, more preferably 65 help engineer the surface contributed electrical properties of
0.5 micron, and most preferably 100 nm in size. Produce a the composite particles. The disclosed materials can also be
product from the coated size-confined powder. used for enabling electrical conductivity in materials used
 US 7,341,757 B2
11 12
commercially at cryogenic or high temperatures or unusual sensor, electronic, telecom, optics, electrical, photonic, ther
environments or in materials processed at high temperatures mal, piezo, magnetic, catalytic and electrochemical prod
to produce a product where the electrical conductivity is uctS.
normally poor. Electrical conductivity can be achieved as Other embodiments of the invention will be apparent to
follows: (a) provide a powder that meets the thermal, those skilled in the art from a consideration of the specifi
structural, and other performance requirements of the prod cation or practice of the invention disclosed herein. It is
uct, (b) coat the powder with nanoparticles of an electrically intended that the specification and examples be considered
conducting Substance Such as metal or alloy or defect oxides as exemplary only, with the true scope and spirit of the
or nitride or carbide or boride to achieve a nanocomposite invention being indicated by the following claims.
form disclosed herein, (c) process the nanocomposite pow 10
What I claim is:
ders into a product. This method can enable multifunctional 1. A method of forming a product comprising:
materials, i.e. products that provide structural function and selecting a fine powder of a polymer of first composition;
provide one or more additional function. For example, selecting nanoparticles of a second composition different
aerospace parts can be produced with Such multifunctional than the first composition;
materials in order to provide structural Support during rou 15
chemically bonding the nanoparticles to the Surface of the
tine use and provide a method for non-destructive testing of polymer powders to form a nanocomposite plastic
the parts integrity during routine maintenance tests. If the powder,
part integrity is good, it is anticipated that the electrical forming a product from the nanocomposite plastic pow
conductivity of the part will not change. However, cracks der, wherein the product has Superior mechanical prop
and other incipient failures would change the electrical erty than the corresponding mechanical property of an
properties and therefore would be an easy way to detect equivalent product prepared from the fine powder of
incipient failure before the failure occurs. polymer.
Similarly, the use of appropriate composition on the 2. The method of claim 1 wherein the forming step is
Surface can help engineer the Surface contributed properties performed in an injection molding equipment.
of the composite particles. The disclosed materials can also 25
3. The method of claim 1 wherein the product comprises
be used for targeted drug delivery and programmable drug a net shaped part.
delivery vehicles. Targeted drug delivery can be achieved as 4. The method of claim 1 wherein the first composition is
follows: (a) provide a magnetic powder that is physiologi selected from the group consisting of polyethylene, polypro
cally acceptable, (b) coat the magnetic powder with the drug pylene, polyacrylates, polycarbonates, polystyrene, and
or a polymer containing the drug or a slow-release formu 30
polyurethane.
lation of the drug in a composite particle form disclosed 5. The method of claim 1 wherein the second composition
herein, (c) administer the drug orally, by injection, as skin is selected from the group consisting of oxide, carbide,
cream, as fluid drops, using Surgical procedures, or through nitride, boride, polymer, metal, and alloy.
inhalation, (d) apply electromagnetic field to concentrate the 6. The method of claim 1 wherein the fine powder of
drug in the area of interest to deliver the drug in the area of 35
polymer of first composition is a Submicron powder.
interest.
Programmable drug delivery can be achieved as follows: 7. The method of claim 1 wherein the fine powder of
(a) provide a fine powder, Submicron powder or nanoscale polymer of first composition is a nanoscale powder.
powder with electromagnetic characteristics that is physi 8. The method of claim 1 wherein the product formed
ologically acceptable, (b) coat the powder with the drug or 40 from the nanocomposite plastic powder has a tensile
a polymer containing the drug or a slow-release formulation strength greater than that of a product produced from the fine
of the drug into a composite particle form disclosed herein, powder of a polymer of first composition.
(c) if the drug diffuses rapidly, add a diffusion barrier coating 9. The method of claim 1 wherein the nanocomposite
that controls the diffusion rate to the preferred rate (d) plastic powder comprises a drug.
administer the drug orally, by injection, as skin cream, as 45 10. The method of claim 1 wherein the nanocomposite
fluid drops, using Surgical procedures, or through inhalation, plastic powder comprises a means to deliver drug.
(e) apply magnetic or electrical field to concentrate the drug 11. The method of claim 1 wherein the nanocomposite
in the area of interest to deliver the drug in the area of plastic powder comprises a means for targeted drug delivery.
interest, (f) develop a program for preferred administration 12. The method of claim 1 wherein the nanocomposite
of the drug, (g) in accordance with this program, apply an 50 plastic powder comprises an electrically conducting Surface.
electromagnetic field of Sufficient intensity causing the elec 13. The method of claim 1 wherein the nanocomposite
tromagnetic powders to warm up and thereby thermally plastic powder comprises a magnetic composition.
inducing increased drug diffusion and delivery rates. Such 14. The method of claim 1 wherein the nanocomposite
drug delivery procedures can be combined with blood or plastic powder comprises an electrically insulating Surface.
other body fluid monitors that monitor the administered drug 55 15. The method of claim 1 wherein the nanocomposite
or a resultant marker or a byproduct of the drug or a waste plastic powder provides a means for non-destructive testing
product of the drug to provide real time information to make of the product.
the drug delivery administration program safer, cost effec 16. The method of claim 1 wherein the nanocomposite
tive, and more physiologically optimal. plastic powder provides a means for drug administration.
Fine powders have numerous applications in industries 60
Such as, but not limiting to biomedical, pharmaceuticals, k k k k k