WO2022023991A1 - Équipement sportif - Google Patents

Équipement sportif Download PDF

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Publication number
WO2022023991A1
WO2022023991A1 PCT/IB2021/056849 IB2021056849W WO2022023991A1 WO 2022023991 A1 WO2022023991 A1 WO 2022023991A1 IB 2021056849 W IB2021056849 W IB 2021056849W WO 2022023991 A1 WO2022023991 A1 WO 2022023991A1
Authority
WO
WIPO (PCT)
Prior art keywords
sports equipment
matrix
cellulose nanocrystals
cellulose
cellulosic material
Prior art date
Application number
PCT/IB2021/056849
Other languages
English (en)
Inventor
Roberto Gazzara
Original Assignee
NOXI S.r.l.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NOXI S.r.l. filed Critical NOXI S.r.l.
Publication of WO2022023991A1 publication Critical patent/WO2022023991A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
    • A43B1/00—Footwear characterised by the material
    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
    • A43B13/00—Soles; Sole-and-heel integral units
    • A43B13/02—Soles; Sole-and-heel integral units characterised by the material
    • A43B13/026—Composites, e.g. carbon fibre or aramid fibre; the sole, one or more sole layers or sole part being made of a composite
    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
    • A43B23/00—Uppers; Boot legs; Stiffeners; Other single parts of footwear
    • A43B23/02—Uppers; Boot legs
    • A43B23/0205—Uppers; Boot legs characterised by the material
    • A—HUMAN NECESSITIES
    • A43—FOOTWEAR
    • A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
    • A43B5/00—Footwear for sporting purposes
    • A43B5/04—Ski or like boots
    • A43B5/0486—Ski or like boots characterized by the material
    • A43B5/049—Ski or like boots characterized by the material with an upper made of composite material, e.g. fibers or core embedded in a matrix
    • A—HUMAN NECESSITIES
    • A63—SPORTS; GAMES; AMUSEMENTS
    • A63B—APPARATUS FOR PHYSICAL TRAINING, GYMNASTICS, SWIMMING, CLIMBING, OR FENCING; BALL GAMES; TRAINING EQUIPMENT
    • A63B49/00—Stringed rackets, e.g. for tennis
    • A63B49/02—Frames
    • A63B49/10—Frames made of non-metallic materials, other than wood
    • A—HUMAN NECESSITIES
    • A63—SPORTS; GAMES; AMUSEMENTS
    • A63B—APPARATUS FOR PHYSICAL TRAINING, GYMNASTICS, SWIMMING, CLIMBING, OR FENCING; BALL GAMES; TRAINING EQUIPMENT
    • A63B53/00—Golf clubs
    • A63B53/10—Non-metallic shafts
    • A—HUMAN NECESSITIES
    • A63—SPORTS; GAMES; AMUSEMENTS
    • A63C—SKATES; SKIS; ROLLER SKATES; DESIGN OR LAYOUT OF COURTS, RINKS OR THE LIKE
    • A63C5/00—Skis or snowboards
    • A63C5/12—Making thereof; Selection of particular materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C08J5/249—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs characterised by the additives used in the prepolymer mixture
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41B—WEAPONS FOR PROJECTING MISSILES WITHOUT USE OF EXPLOSIVE OR COMBUSTIBLE PROPELLANT CHARGE; WEAPONS NOT OTHERWISE PROVIDED FOR
    • F41B5/00—Bows; Crossbows
    • F41B5/14—Details of bows; Accessories for arc shooting
    • F41B5/1403—Details of bows
    • A—HUMAN NECESSITIES
    • A63—SPORTS; GAMES; AMUSEMENTS
    • A63B—APPARATUS FOR PHYSICAL TRAINING, GYMNASTICS, SWIMMING, CLIMBING, OR FENCING; BALL GAMES; TRAINING EQUIPMENT
    • A63B2209/00—Characteristics of used materials
    • A63B2209/02—Characteristics of used materials with reinforcing fibres, e.g. carbon, polyamide fibres
    • A63B2209/023—Long, oriented fibres, e.g. wound filaments, woven fabrics, mats
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B62—LAND VEHICLES FOR TRAVELLING OTHERWISE THAN ON RAILS
    • B62K—CYCLES; CYCLE FRAMES; CYCLE STEERING DEVICES; RIDER-OPERATED TERMINAL CONTROLS SPECIALLY ADAPTED FOR CYCLES; CYCLE AXLE SUSPENSIONS; CYCLE SIDE-CARS, FORECARS, OR THE LIKE
    • B62K19/00—Cycle frames
    • B62K19/02—Cycle frames characterised by material or cross-section of frame members
    • B62K19/16—Cycle frames characterised by material or cross-section of frame members the material being wholly or mainly of plastics
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins

Definitions

  • the invention relates to sports equipment, such as a racket, comprising at least one layer of composite material.
  • the equipment of the present invention may in particular find application in sports activities such as tennis, padel, paddle-ball, squash, badminton, pickleball, beach tennis, fronton, and touchtennis.
  • the sports equipment of the present invention may also be intended for use in other sports, such as cycling, golf, snowboarding, skiing, footwear, etc., in which the sports equipment of the present invention may be used in the form of a frame or component.
  • the main objectives traditionally sought in the design of sports equipment are the possibility of providing the user with a competitive advantage by improving performance, increasing the durability of the equipment, improving user comfort, or protecting the user from injury.
  • pre-impregnated composite material also referred to as "pre-preg"
  • pre-preg "pre-impregnated” composite material
  • fillers require complex and difficult-to-control production processes, with potential quality problems.
  • some fillers are poorly dispersible in resins and are therefore difficult to combine with resins.
  • some fillers have features that are potentially harmful to health and require rather complex disposal at the end of their useful life.
  • the technical problem underlying the present invention is how to provide an item of sports equipment that is structurally and functionally designed to at least partially solve one or more of the drawbacks mentioned in reference to the prior art cited above.
  • one object of the present invention is to provide an item of sports equipment that has high mechanical properties without using materials that significantly affect the cost of manufacture
  • a further object is to provide sports equipment in which there is no increased use of non-recyclable materials, or materials that are not easy to dispose of, than in the known solutions.
  • An object of the present invention is also to provide an item of sports equipment that uses a composite material in which a filler of natural origin is present, and which therefore has a low impact from an environmental perspective.
  • Yet another object is to provide an item of sports equipment in which no potentially health-threatening materials are used.
  • the sports equipment in the present invention comprises at least one layer of a composite material including a matrix and reinforcing fibres that are at least partially surrounded by the matrix, wherein the composite material further includes a cellulosic material dispersed in the matrix.
  • cel lulosic material means material extracted from cellulose.
  • the cel lulosic material acts as a filler.
  • the cellulosic material acts as a reinforcing filler to improve the mechanical properties of the composite layer or even of the different layers of composite material if the equipment is formed by superimposing several pre-preg layers.
  • the cellulosic material is micrometric or nanometric in size. It should be noted that, in this context, "nanometric size" preferably means a size smaller than 1 micrometre, even more preferably smaller than or equal to 500 or 400 nanometres and, more particularly, smaller than or equal to 200 or 100 nanometres.
  • the cellulosic material is in the form of nanocrystals.
  • cellulose nanocrystals means cellulose crystals preferably having an elongated shape, for example substantially cylindrical (preferably a "nano rod” shape), with a length expediently less than or equal to 500 or 400 nm (preferably a length less than or equal to 300 or 200 nm and more specifically less than or equal to 100 nm) and, again preferably, a transverse dimension or diameter of a few nm units (preferably a transverse dimension or diameter less than or equal to 10 or 20 nm and more specifically between 3 and 5 nm).
  • CNC cellulose nanocrystals
  • the cellulose crystals are obtained by removing the amorphous part of the cellulose.
  • cellulose is made up of cellulose nanofibrils, also called cellulose nanofibres (CNF), each of which contains crystalline cellulose domains separated by amorphous cellulose domains. These crystalline cellulose domains may be released by removing the amorphous cellulose domains, thus obtaining cellulose nanocrystals (CNC).
  • CNF cellulose nanofibrils
  • CNC cellulose nanocrystals
  • CNFs and CNCs differ significantly in both chemical nature and size.
  • CNF Cellulose nanofibres
  • CNC cellulose nanocrystals
  • CNFs and CNCs differ in length: cellulose nanofibres may extend several micrometres and are therefore significantly longer than cellulose nanocrystals.
  • nanocrystals Due to their chemical nature and their size, cellulose nanocrystals are capable of dispersion in a host matrix on a nanoscale (so-called “nanodispersion”), which allows high-performance nanocomposites to be produced.
  • nanoscale dispersion of cellulose nanocrystals in the host matrix may improve the mechanical properties of the material at very low concentrations of nanocrystals.
  • the addition of cellulose nanocrystals to the composition of the matrix may increase the workability of the material and ensure sufficient cohesion to prevent their fragmentation caused by impacts.
  • NCC nanocrystalline cellulose
  • cellulose nanocrystals cellulose nanocrystals
  • cellulose nanocrystals may fill in any gaps left by the matrix, thereby improving the mechanical properties of said material.
  • cellulose nanocrystals combine high axial stiffness, high Young's modulus, high tensile strength, low thermal expansion coefficient, high thermal stability, and low density.
  • cellulose improves in particular the mechanical properties of the matrix of the composite material. Therefore, cellulose nanocrystals improve the anisotropic properties of the composite material.
  • the matrix comprises a resin, such as an epoxy resin.
  • At least one layer of composite material is a pre-preg layer.
  • pre-preg means a fibre- reinforced composite material "pre-impregnated” with a matrix material (e.g., epoxy resin).
  • cellulose preferably in the form of nanocrystals, is evenly dispersed in the matrix.
  • the cellulose nanocrystals are dispersed in the matrix uniformly but with a random orientation. In this way, the cellulose nanocrystals advantageously create a lattice that increases the elastic modulus and mechanical strength of the matrix in all directions.
  • cellulose nanocrystals improve the mechanical properties of the matrix to an extent that depends on the formulation of the composite material.
  • a plurality of layers of the composite material is provided.
  • the layers are at least partially superimposed on each other.
  • the presence of the cellulose nanocrystals not only improves the mechanical properties of each individual layer, but also improves the adhesion between adjacent superimposed layers of composite material, thereby considerably increasing the shear strength and thus also the fatigue strength and elastic modulus of the article comprising the plurality of layers of the composite material.
  • the sports equipment comprises a racket.
  • the racket is of a type suitable for at least one activity chosen from tennis, padel, paddle-ball, squash, badminton, pickleball, beach tennis, fronton, and touchtennis. It is understood that the racket may be replaced by other types of sports equipment such as a golf club, snowboard, skis, footwear, etc.
  • At least one layer of the composite material is used in the manufacture of a sports equipment frame or a sports equipment component which preferably has a structural function. Therefore, the present invention may also be applied to the manufacture of equipment for other sports activities, such as cycling, golf, etc.
  • the sports equipment may comprise one or more components of a bicycle such as the frame, fork, handlebars, and so on.
  • the bicycle may be a pedal-assisted bicycle.
  • the sports equipment may include archery equipment, and preferably may include an archery bow or a bow component.
  • - Fig. 1 represents a layer of a composite material of an item of sports equipment according to the invention
  • - Fig. 2 represents two superimposed layers of Fig. 1 seen in cross- section and enlarged in detail;
  • - Fig. 3 is a perspective view of a racket according to an embodiment of the invention
  • - Fig. 4 is a side view of a bicycle according to an embodiment of the invention
  • FIG. 5 is a front view of a golf club according to an embodiment of the invention.
  • FIG. 6 is a perspective view of a snowboard according to an embodiment of the invention.
  • Fig. 7 is a perspective view of a pair of skis according to an embodiment of the invention.
  • - Fig. 8 is a perspective view of an archery bow according to an embodiment of the invention
  • - Fig. 9 is a perspective view of a shoe according to an embodiment of the invention.
  • a layer of a composite material for sports equipment 100 is collectively referred to as 1.
  • the sports equipment 100 comprises at least one layer 1 of composite material including a matrix 2 and reinforcing fibres 3 at least partially surrounded by the matrix 2.
  • the sports equipment 100 comprises a frame 10 or component 11 including the at least one layer 1 of the composite material.
  • the sports equipment 100 may include one or more items of equipment chosen from a racquet 101, a bicycle 102, a golf club 103, a snowboard 104, a pair of skis 105, an archery bow 106, footwear 107, or a component 11 of any of the sports equipment just mentioned.
  • the sports equipment 100 comprises a plurality of layers 1, 1' of the composite material.
  • the layers 1, 1' may be laminated together.
  • the at least one layer 1 may be of the pre-preg type comprising the matrix 2 reinforced with fibres 3 that are at least partially surrounded by the matrix 2.
  • the reinforcing fibres 3 may be at least partially woven or at least partially non-woven, arranged in one direction or in several directions, and may include short fibres and/or long fibres.
  • the reinforcing fibres 3 may comprise a selection of one or more of the following fibres: carbon fibres, boron fibres, glass fibres, silicon carbide fibres, ceramic fibres and/or aramid fibres of the type available under the trade name KEVLAR.
  • the reinforcing fibres 3 may be arranged in a single layer and/or in a plurality of layers, which may be laminated together.
  • the matrix 2 preferably includes a resin, cured by a curing process or otherwise solidified.
  • the matrix 2 may advantageously include a thermosetting resin or a thermoplastic resin.
  • the thermosetting resin may be selected from one among the following resins: an epoxy resin, a polyester resin, or a vinylester resin.
  • cellulose 4 preferably in the form of nanocrystals 6, is provided to reinforce the composite material comprising the matrix 2 and the fibres 3.
  • the crystallinity of the cellulose 4 may be equal to or greater than 60%, more preferably equal to or greater than 70%.
  • the maximum rate of crystallinity of the cellulose 4 is not particularly limited but may be for example 99%.
  • cellulose nanocrystals 6 some embodiments of the present invention also include the use of cellulose 4 in another form, provided it is nanometric or at least micrometric in size, as in the case of nanocellulose and cellulose nanofibrils.
  • the use of cellulose 4 exclusively or at least predominantly in the form of nanocrystals 6 is preferred, more particularly nanocrystals of the type commercially available from Anomera Inc. Canada under the brand name DextraCel.
  • the cellulose nanocrystals 6 may be extracted from agricultural, forestry (lignocellulosic biomass), and/or bacterial sources, in a sustainable way and without impacting the environment.
  • these sources represent derivatives or waste from other productions (both industrial and food-related), for the benefit of sustainability and circularity.
  • cellulose nanocrystals 6 have an elongated shape and are to a certain extent comparable to nanofibres, i.e., fibres with structural dimensions on the nanometric scale, it being advantageous for cellulose nanocrystals 6 to be distinguished from nanofibres by the fact that they do not comprise amorphous cellulose (apart from possible impurities).
  • cellulose nanocrystals 6 have a length of up to 500 nm and more particularly up to 100 nm and a thickness of 3 to 5 nm, for example.
  • thickness preferably means the dimension transverse to the longitudinal extension of the cellulose nanocrystals 6.
  • the cellulose nanocrystals 6 could have a length of up to 200, 300, or 400 nm.
  • the minimum length of cellulose nanocrystals 6 is not particularly limited but may, for example, be 5 or 10 nm.
  • the cellulose nanocrystals 6 are mixed with and/or used as a filler and/or additive in the matrix 2. Mixing may take place in the resin of the matrix 2 in liquid form, before the resin enriched with cellulose nanocrystals 6 is used to make the pre-preg layers.
  • the cellulose nanocrystals 6 are dispersed in the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially 5% or less than 5% of a mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially 5% or less than 5% by weight and/or volume of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially 3% or less than 3% of a mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially 3% or less than 3% by weight and/or volume of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.005% and 2% of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.005% and 2% by weight and/or volume of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.005% and 1.5% of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.005% and 1.5% by weight and/or volume of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.5% and 1.5% of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • the cellulose nanocrystals 6 constitute substantially between 0.5% and 1.5% by weight and/or volume of the mixture that the cellulose nanocrystals 6 form with the matrix 2.
  • composition of the mixture in one or more of these ranges, an optimal distribution and/or dispersion of the cellulose nanocrystals 6 in the matrix 2 may be ensured, and a deterioration of the physical properties of the mixture due to non-uniform distribution and/or dispersion may be avoided.
  • the volumetric content of the reinforcing fibres 3 in the layer 1 may be substantially between 10% and 85%.
  • By setting the volumetric content of the reinforcing fibres 3 in this range it is possible to achieve a balance between the strength in the plane of layer 1, which may be mainly based on the strength imparted by the reinforcing fibres 3, and other types of strength such as the compressive strength of the layer 1, which may be mainly based on the strength imparted by the matrix 2.
  • the cellulose nanocrystals 6 improve the mechanical properties of the composite material between two adjacent superimposed layers 1, 1', as shown in the example in Fig. 2.
  • the cellulose nanocrystals 6 arranged in the interlaminar region 5 considerably increase the shear strength between adjacent layers 1, 1' and reduce the delamination phenomena.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Physical Education & Sports Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • General Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Cyclones (AREA)
  • Devices For Conveying Motion By Means Of Endless Flexible Members (AREA)
  • Lubricants (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Équipement sportif comprenant au moins une couche d'un matériau composite comprenant une matrice et des fibres de renfort entourées au moins partiellement par ladite matrice.
PCT/IB2021/056849 2020-07-28 2021-07-28 Équipement sportif WO2022023991A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT102020000018310 2020-07-28
IT102020000018310A IT202000018310A1 (it) 2020-07-28 2020-07-28 Attrezzatura sportiva

Publications (1)

Publication Number Publication Date
WO2022023991A1 true WO2022023991A1 (fr) 2022-02-03

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2021/056849 WO2022023991A1 (fr) 2020-07-28 2021-07-28 Équipement sportif

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IT (1) IT202000018310A1 (fr)
WO (1) WO2022023991A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2965789A1 (fr) * 2014-07-11 2016-01-13 NOXI s.r.l. Équipement de sport avec une structure tubulaire renforcée
US20160177084A1 (en) * 2013-08-06 2016-06-23 Dic Corporation Reinforcing material, reinforced matrix resin, fiber-reinforced resin composite, and method for manufacturing reinforcing material
WO2019221155A1 (fr) * 2018-05-15 2019-11-21 地方独立行政法人大阪産業技術研究所 Matériau de renforcement d'un plastique renforcé par des fibres de carbone et matériau de renforcement d'un plastique

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160177084A1 (en) * 2013-08-06 2016-06-23 Dic Corporation Reinforcing material, reinforced matrix resin, fiber-reinforced resin composite, and method for manufacturing reinforcing material
EP2965789A1 (fr) * 2014-07-11 2016-01-13 NOXI s.r.l. Équipement de sport avec une structure tubulaire renforcée
WO2019221155A1 (fr) * 2018-05-15 2019-11-21 地方独立行政法人大阪産業技術研究所 Matériau de renforcement d'un plastique renforcé par des fibres de carbone et matériau de renforcement d'un plastique

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DIETER KLEMM ET AL: "Nanocelluloses: A New Family of Nature-Based Materials", ANGEWANDTE CHEMIE INTERNATIONAL EDITION, vol. 50, no. 24, 20 May 2011 (2011-05-20), pages 5438 - 5466, XP055167698, ISSN: 1433-7851, DOI: 10.1002/anie.201001273 *
GABR M. ET AL: "IMPROVING FRACTURE TOUGHNESS OF CARBON FIBRE/EPOXY COMPOSITE FILLED WITH NANO-CELLULOSE MODIFIED WITH LIQUID RUBBER", vol. 15, no. 15, 1 May 2012 (2012-05-01), pages 1 - 12, XP055794389, Retrieved from the Internet <URL:https://amme.journals.ekb.eg/article_36943_9b2cda9a0f4862d7bc43019bca7ae5b5.pdf> DOI: 10.21608/amme.2012.36943 *

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