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WO2018174814A1 - Matériau de protection - Google Patents

Matériau de protection Download PDF

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Publication number
WO2018174814A1
WO2018174814A1 PCT/SG2017/050142 SG2017050142W WO2018174814A1 WO 2018174814 A1 WO2018174814 A1 WO 2018174814A1 SG 2017050142 W SG2017050142 W SG 2017050142W WO 2018174814 A1 WO2018174814 A1 WO 2018174814A1
Authority
WO
WIPO (PCT)
Prior art keywords
protective material
windows
protective
rare
material according
Prior art date
Application number
PCT/SG2017/050142
Other languages
English (en)
Inventor
Seok Khim ANG
Wei-Pin Ernest LAU
Original Assignee
Dso National Laboratories
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 Dso National Laboratories filed Critical Dso National Laboratories
Priority to PCT/SG2017/050142 priority Critical patent/WO2018174814A1/fr
Priority to SG11201906564PA priority patent/SG11201906564PA/en
Priority to BR112019014894-9A priority patent/BR112019014894A2/pt
Publication of WO2018174814A1 publication Critical patent/WO2018174814A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H5/00—Armour; Armour plates
    • F41H5/02—Plate construction
    • F41H5/04—Plate construction composed of more than one layer
    • F41H5/0407—Transparent bullet-proof laminatesinformative reference: layered products essentially comprising glass in general B32B17/06, e.g. B32B17/10009; manufacture or composition of glass, e.g. joining glass to glass C03; permanent multiple-glazing windows, e.g. with spacing therebetween, E06B3/66
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/14—Layered products comprising a layer of synthetic resin next to a particulate layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B32B27/365—Layered products comprising a layer of synthetic resin comprising polyesters comprising polycarbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B3/10—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material
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    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina

Definitions

  • Various embodiments refer to a protective material, such as a ballistic resistant material, and articles formed therefrom. Characterization of the protective material and evaluation of the articles fabricated with the protective material were also carried out according to embodiments, and are detailed herein.
  • Protective materials refer broadly to substances that may be used to hinder destruction and/or damage to, or exposure of an object, and may find application in a myriad of items ranging from consumer goods such as eyewear and protective cover on watches and electronic gadgets, to construction materials such as windows and shower screens, to parts of vehicles such as windscreens of cars, and to military items such as ballistic resistant materials.
  • the protective materials may be applied on a surface of the object to be protected, such that the protective materials are in direct contact with the object. This may be the case for a protective screen on an electronic device such as a smartphone or watch.
  • the protective materials are spaced apart from the object or structure, for example, as an enclosure containing the object or as a shield protecting the object from external elements, such as windscreen of a vehicle or eyewear.
  • various materials may be used as the protective material.
  • glass treated with an ion-exchange strengthening process have been used as a protective cover for displays and touch screens in electronic devices such as smart phones, tablet computers, and televisions.
  • Polymeric materials such as poly(methyl methacrylate) have been used as substitutes for glass in applications where transparency, high strength and resistance to shattering is required, such as in windows and aircraft canopies.
  • bullet-proof materials include armored glass and sapphire single crystals.
  • Armored glass in particular, is readily available for use in bullet-proof windows. Due to its low hardness and strength, however, thicknesses in the range of about 50 to 150 mm are often necessary for bullet-proof applications. As such, there is still much room for improvement in terms of weight and volume.
  • Sapphire has improved material hardness and strength over that of armored glass. Accordingly, it may be made thinner and lighter in weight in various applications. Sapphire, however, is an anisotropic crystal and may therefore not be optically uniform. Hence, it cannot be considered to be a general-purpose material. Moreover, it has a very high melting point of 2100 °C, which may lead to high production costs. Hardness of the material may also result in increased processing costs. Further, as strength of the material is dependent on the crystal axes due to its anisotropy, damage may be catastrophic in the weaker crystal planes.
  • Spinel for example, may be synthesized by adding sintering additives such as LiF followed by hot-pressing. It may be difficult to obtain transparency in Spinel unless sintering additives are used. As this material has a cubic structure, it does not exhibit optical or mechanical anisotropy. Due to the use of LiF additives, grain growth may occur during sintering to result in final average grain sizes of about 30 to 100 microns. Single crystal Spinel has hardness and bending strength of 11 GPa and 270 MPa, respectively.
  • polycrystalline Spinel with additives while having the same level of hardness, has a reduced bending strength of about 90 to 140 MPa.
  • using the hot press method to fabricate Spinel is not ideal for production as only one sample may be produced per cycle. This may lead to cost-related issues.
  • Aluminum oxynitride has a hardness between that of Spinel and sapphire. Its bending strength is about 250 to 300 MPa, which is as good as single crystal Spinel, making it a promising candidate. Synthesis of this material, however, requires solid reaction of the raw materials AI2O3 and A1N, which is difficult to achieve. Generally, one has to use ⁇ - alumina under reducing atmosphere while at the same time reacting with nitrogen or ammonia under a temperature of higher than 1800 °C in order to produce AION powder.
  • a protective material comprising a rare-earth garnet ceramic.
  • the rare-earth garnet ceramic has general formula
  • R 1 is selected from the group consisting of Y, Yb, and combinations thereof
  • R 2 is selected from the group consisting of Eu, Gd, Tb, Ho, Tm, Lu, and combinations thereof, R 1 being present in an amount that is more than 90 atomic % of total amount of R 1 and R 2 , and R 2 being present in an amount that is 10 atomic % or less of total amount of R 1 and R 2 , and a is in the range from about 3 to about 3.015.
  • a ballistic resistant article comprises
  • a third aspect use of the protective material according to the first aspect in goggles, safety glasses, personal protective equipment, window, screen, windscreen, panel, optical sensor, imager, windows of aircrafts, windows and bridges of ships, windows of building infrastructure, structural member of a military equipment or a vehicle, vehicles as jet fighter canopies, aircraft windows, helicopter canopies or windows; windows, barriers or doors in police or military installations, jails, schools, sport halls, prisons, or hospitals; protective shields for police or military personnel; lenses and windows in optical devices, goggles, safety glasses, windows, screens, eyeglass lenses, camera lenses, microscope lenses, telescope lenses; LED (light-emitting diode) lenses and windows; protective cover for watches and clocks; diffusers, protective and/or decorative covers and bulb materials for artificial lighting, automotive headlights, highway, parking lot lighting is provided.
  • BRIEF DESCRIPTION OF THE DRAWINGS BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1A is an optical image showing small cracks covering strike face of an yttrium aluminum garnet (YAG) ceramics tile.
  • YAG yttrium aluminum garnet
  • FIG. IB is an optical image showing back face of the panel depicted in FIG. 1A showing no penetration of the bullet.
  • FIG. 2A is an optical image showing a transparent ceramics armor panel.
  • FIG. 2B is an optical image showing a transparent ceramics armor panel.
  • FIG. 3 is an optical image showing rare earth aluminum garnet ceramics of different size and shape.
  • FIG. 4A is an optical image showing strike face of a typical transparent armor panel, with multiple shots tested on the panel demonstrating its protection capability.
  • FIG. 4B is an optical image showing back face of the transparent armor panel depicted in FIG. 4A, with multiple shots tested on the panel demonstrating its protection capability.
  • a protective material according to embodiments disclosed herein has exhibited excellent scratch resistant properties at almost 3 times harder than glass, as well as excellent energy absorbing performance.
  • the protective material according to embodiments may also possess high optical transparency, which renders their suitability for use in a wide range of applications for land, sea and air platforms, such as, but not limited to, in vehicles as jet fighter canopies, aircraft windows, helicopter canopies and windows; protective windows, barriers and doors, such as for use in police and/or military installations such as prisons, and other installations such as schools, sport halls, hospitals, offices, and factories; protective shields for military and/or police personnel as a ballistic resistant or bullet proof material; lenses and windows in optical devices such as eyeglass lenses, goggles, camera lenses, microscope and/or telescope lenses, LED (light-emitting diode) lenses and windows; protective cover for watches and clocks; diffusers, protective and/or decorative covers and bulb materials for lightings, such as automotive headlights, highway and/or parking lot lighting.
  • the protective material disclosed herein is also suitable as a ballistic resistant material.
  • a high degree of hardness has been considered as a pre -requisite for ballistic resistant materials.
  • the protective material disclosed herein may accordingly be used as a ballistic resistant material or a bullet proof material in various applications, for example, in the fabrication of goggles, safety glasses, personal protective equipment, window, screen, windscreen, panel, optical sensor, imager, structural member of a military equipment or a vehicle, to name only a few.
  • a protective material refers to a material which is able to provide a defense or shield of an object to be protected from harm.
  • the protective material may hinder destruction and/or damage to, or exposure of the object by functioning as a physical barrier to inhibit direct contact between an outer surface of the object and its environment.
  • the protective material may comprise a rare-earth garnet ceramic.
  • the term "rare-earth garnet ceramic” refers to rare earth ceramics having the general formula (R 1 R 2 )aAlsOi2.
  • the term "rare-earth” refers generally to an element of the lanthanide and of the actinide series. Accordingly, in various embodiments, the rare-earth refers to an element selected from the group consisting of yttrium (Y), ytterbium (Yb), europium (Eu), gadolinium (Gd), terbium (Tb), holmium (Ho), thulium (Tm), lutetium (Lu), and combinations thereof. [0026] As disclosed herein, rare-earth elements Y and/or Yb, and optionally Eu, Gd, Tb, Ho, Tm, and/or Lu are used to form the rare-earth garnet ceramic.
  • rare-earth garnet ceramic may have a very narrow solid solution region, a change in chemical composition may have a significant effect on optical and mechanical characteristics of the rare-earth garnet ceramic, and in turn the protective material.
  • R 1 may be selected from the group consisting of Y, Yb, and combinations thereof, and may be present in an amount that is more than 90 atomic % of the total amount of R 1 and R 2 .
  • R 1 may be present in an amount that is at least 91, at least 92, at least 93, at least 95, at least 97, or at least 99 atomic % of the total amount of R 1 and R 2 .
  • R 1 is present in an amount in the range of about 91 atomic % to about 99 atomic %, about 92 atomic % to about 99 atomic %, about 95 atomic % to about 99 atomic %, about 97 atomic % to about 99 atomic %, about 91 atomic % to about 97 atomic %, about 91 atomic % to about 95 atomic %, about 91 atomic % to about 93 atomic %, or about 93 atomic % to about 97 atomic % of the total amount of R 1 and R 2 .
  • R 1 and R 2 make up the total amount of R 1 and R 2 , i.e. they add up to 100 atomic %. This means that when R 1 is at x atomic % for example, R 2 is at (100 - x) atomic %. In some embodiments, R 2 is not present, i.e. R 1 is present as 100 atomic % of total amount of R 1 and R 2 .
  • Y and/or Yb may confer stable optical and mechanical characteristics on the protective material, and render the process of manufacturing the protective material economically viable.
  • R 1 is Y.
  • the rare-earth garnet ceramic may have formula (YR 2 )aAlsOi2, with R 2 and a as being defined above.
  • protective materials comprising Y may be preferred in applications since it is lighter.
  • R 2 is optionally present, and may be considered a rare-earth dopant of the rare- earth garnet ceramic.
  • R 2 is selected from the group consisting of Eu, Gd, Tb, Ho, Tm, Lu, and combinations thereof.
  • amount of R 2 may be 10 atomic % or less of total amount of R 1 and R 2 .
  • R 2 may be present in an amount that is 8 % or less, 6 % or less, 4 % or less, 2 % or less of total amount of R 1 and R 2 .
  • R 2 is not present in the rare-earth garnet ceramic, i.e. the rare-earth garnet ceramic has general formula R ⁇ A On.
  • a may be in the range from about 3 to about 3.015, such as about 3.005 to about 3.015, about 3.01 to about 3.015, about 3 to about 3.01, or about 3.005 to about 3.01. In various embodiments, a is 3.
  • the rare-earth garnet ceramic may comprise at least one of Y3AI5O12 or Yb 3 Al50i2 having purity of at least 99.8 %.
  • purity this means that at least one of Y 3 Ai50i2 or Yb 3 Ai50i2 may constitute at least 99.8 % by weight of the rare-earth garnet ceramic.
  • the at least one of Y 3 AlsOi2 or Yb 3 AlsOi2 may constitute at least 99.8 % by weight of the rare-earth garnet ceramic, such as at least 99.9 % or 100 % by weight of the rare-earth garnet ceramic.
  • the rare earth garnet ceramic may be made up of multiple grains connected in a continuous network.
  • the term "grain” is used herein to describe an internal structure of the protective material, and refers to individually recognizable crystals or particles that form the continuous matrix of the material.
  • a sintering agent may be added to prepare the protective material.
  • the term "sintering agent” as used herein refers to a material that is capable of enhancing densification of the rare-earth garnet ceramics.
  • sintering time of the protective material may be shortened by using a sintering agent. Transparency of the protective material may also be improved.
  • the sintering agent is at least one of a metal oxide or a metal fluoride.
  • the sintering agent may, for example, be selected from the group consisting of S1O2, MgO, CaO, MgF2, CaF2, YF 3 , A1F, and combinations thereof.
  • the sintering agent constitutes less than 1000 ppm of the protective material.
  • the sintering agent may constitute less than 900 ppm, less than 800 ppm, less than 700 ppm, less than 600 ppm, less than 500 ppm, less than 400 ppm, less than 300 ppm, less than 200 ppm, or less than 100 ppm of the protective ballistic resistant material.
  • Mechanical characteristics of the protective material may be varied by varying grain size of the rare-earth garnet ceramic. This allows tailoring of the protective material to specific requirements of intended application.
  • a decrease in grain size of the rare-earth garnet ceramic may provide improved mechanical characteristics.
  • the grain size may be affected by composition of the rare-earth garnet ceramic. For example, grain size may be affected by the presence or absence of additives at the same composition. While addition of sintering agent may have effect of shortening the sintering time, average grain size may still be kept to within 20 ⁇ .
  • the term "size" as used herein refers to the maximal length of a line segment passing through the centre and connecting two points on the periphery of grains. Average size of the grains may be calculated by dividing the sum of a maximal length of each grain by the total number of grains.
  • the rare-earth garnet ceramic may comprise grains having an average size in the range of about 1 ⁇ to about 20 ⁇ , such as about 3 ⁇ to about 20 ⁇ , about 5 ⁇ to about 20 ⁇ , about 8 ⁇ to about 20 ⁇ , about 10 ⁇ to about 20 ⁇ , about 12 ⁇ to about 20 ⁇ , about 15 ⁇ to about 20 ⁇ , about 1 ⁇ to about 15 ⁇ , about 1 ⁇ to about 12 ⁇ , about 1 ⁇ to about 10 ⁇ , about 1 ⁇ to about 8 ⁇ , about 5 ⁇ to about 15 ⁇ , or about 8 ⁇ to about 12 ⁇ .
  • average grain size of the rare- earth garnet ceramic is in the range of about 1 ⁇ to about 5 ⁇ .
  • grain size of the protective material is closely related to ballistic resistance or bullet-resistance performance.
  • a protective material according to embodiments disclosed herein may be used as a ballistic resistant material.
  • the term "ballistic resistant material” as used herein refers to a material which is able to absorb or resist impact of a moving object, such as a projectile. Although it may not be completely impenetrable to all types of projectiles under different situations, the ballistic resistant material as described herein is intended to stop, or at least severely retard, the progress of a projectile, such as a bullet. In some embodiments, the ballistic resistant material functions as a bullet-proof material.
  • the protective material further comprises one or more pores. Air gaps or voids in and between the grains of the rare-earth garnet ceramic are referred to herein as pores within the rare-earth garnet ceramic.
  • the pores may not be regular in shape and/or be of the same shape.
  • size for pores may accordingly refer to the maximal length of a line segment passing through the centre and connecting two points on the periphery of a pore. Average size of the pores may be calculated by dividing the sum of a maximal length of each pore by the total number of pores.
  • the one or more pores have an average size of about 100 ⁇ or less.
  • the one or more pores may have an average size of about 80 ⁇ or less, about 60 ⁇ or less, about 40 ⁇ or less, about 20 ⁇ or less, or about 10 ⁇ or less.
  • average pore size of the rare-earth garnet ceramic is about 100 ⁇ or less, preferably less than 5 ⁇ . Size of the pores may be minimized using a pressure compacting process or a high pressure sintering process, such as Hot Press and/or hot isostatic press (HIP) for sintering.
  • a pressure compacting process or a high pressure sintering process such as Hot Press and/or hot isostatic press (HIP) for sintering.
  • HIP hot isostatic press
  • pores in the protective material may affect optical characteristics, therefore, from an optics perspective, it is better to have a lesser number of pores. From the perspective of protective performance, however, zero pores may reduce protective performance such as ballistic-resistance as a portion of void or pores may function as crack absorbance band. It has been found by the inventors that an average pore size of about 10 ⁇ or less is the best condition for both optical and mechanical strength aspects.
  • the protective material may have a pore volume in the range of about 10 ppm to about 1000 ppm, such as about 50 ppm to about 1000 ppm, about 100 ppm to about 1000 ppm, about 200 ppm to about 1000 ppm, about 500 ppm to about 1000 ppm, about 800 ppm to about 1000 ppm, about 10 ppm to about 800 ppm, about 10 ppm to about 600 ppm, about 10 ppm to about 400 ppm, about 10 ppm to about 200 ppm, about 100 ppm to about 800 ppm, about 200 ppm to about 600 ppm, or about 300 ppm to about 500 ppm.
  • the protective material disclosed herein has the same level of mechanical strength as single crystal for high bullet-resistance.
  • the protective material may have a three-point bending strength in the range of about 150 MPa to about 450 MPa, such as about 200 MPa to about 450 MPa, about 300 MPa to about 450 MPa, about 350 MPa to about 450 MPa, about 150 MPa to about 400 MPa, about 150 MPa to about 350 MPa, about 150 MPa to about 300 MPa, about 150 MPa to about 250 MPa, about 250 MPa to about 350 MPa, or about 300 MPa to about 400 MPa.
  • surfaces of the protective material may be mirror polished so that the protective material may have an optical transmittance of more than 65 %. This may be measured on a sample of the protective material having a thickness of about 1 cm and using a radiation having a wavelength of about 550 nm. Depending on the composition of the protective material, for example, 80 % to about 84 % may be a theoretical limit regarding optical transmittance of the protective material.
  • optical transmittance of the protective material disclosed herein may be in the range of about 65 % to about 84 %, such as about 65 % to about 80 %, or about 65 % to about 75 %, as measured on a sample of the protective material having a thickness of about 1 cm and using a radiation having a wavelength of about 550 nm. At these linear optical transmittances, an end user may be able to see through the protective material.
  • the protective material according to embodiments disclosed herein has exhibited excellent scratch resistant properties and energy absorbing performance, and may also possess high optical transparency. These attributes may render their suitability for use in applications such as, but not limited to, in vehicles as jet fighter canopies, aircraft windows, helicopter canopies and windows; protective windows, barriers and doors, such as for use in police and/or military installations such as prisons, and other installations such as schools, sport halls, hospitals, offices, and factories; protective shields for military and/or police personnel as a ballistic resistant or bullet proof material; lenses and windows in optical devices such as eyeglass lenses, goggles, camera lenses, microscope and/or telescope lenses, LED (light-emitting diode) lenses and windows; protective glass for watches and clocks; diffusers, protective and/or decorative covers and bulb materials for lightings, such as automotive headlights, highway and/or parking lot lighting.
  • the protective material disclosed herein may be used as a ballistic resistant material in the fabrication of goggles, safety glasses, personal protective equipment, window, screen, windscreen, panel, optical sensor, imager, structural member of a military equipment or a vehicle.
  • various embodiments refer in a further aspect to a ballistic resistant article.
  • the ballistic resistant article may comprise a polymeric support attached to the protective material disclosed herein.
  • Choice of the polymeric support is not particularly limited, and may comprise a polymer selected from the group consisting of acrylic, perspex, butyrate, polycarbonates, copolymers thereof, and combinations thereof.
  • One or more tiles comprising the protective material may be attached to the polymeric support.
  • the term "tile" refers to a relatively thin and substantially planar object having two principal sides lying in planes that are substantially parallel. The sides may be joined together by at least three and usually four, sides or peripheral sides which are small in relation to the areas of the principal sides.
  • the one or more tiles has a shape capable of tessellation.
  • tiles are generally rectangular or square in shape, they may have more or less than four peripheral faces and may have shapes such a square, a rectangle, or a hexagon.
  • a regular polygon shape such as a square, a rectangle or a hexagon is preferred as this may provide flexibility in arrangement of the tiles on the polymeric support to form the ballistic-resistant article.
  • a circular tile of the protective material may be attached to the polymeric support and used singularly.
  • a thickness of less than 10 mm may be good enough to protect against 7.62 mm rounds.
  • Transparency requirements may limit material thickness to less than 25 mm, hence it may be preferable to use a thickness that is less than 25 mm.
  • the one or more tiles comprising the protective material may have a thickness that is less than 25 mm, such as about 0.1 mm to about 25 mm, about 0.5 mm to about 25 mm, about 5 mm to about 25 mm, or about 10 mm to about 25 mm.
  • tile size of the protective material is not particularly constrained, in practice, probability of bullets hitting the same tile may be higher for a tile having an area greater than 10 x 10 cm 2 . As such, it may be difficult for the same tile to protect against multiple shots. Furthermore, the fabrication yield and cost may become problematic. By using relatively small area tiles of the protective material and attaching them to a polymeric support to form the ballistic resistant article, the bonding of multiple tiles into a single panel allows multi-shot protection, though the shots may not be on the same point.
  • the one or more tiles comprising the protective material have a cross-sectional area in the range of about 16 cm 2 to about 100 cm 2 and an aspect ratio of 2 or less.
  • the specified cross-sectional area and aspect ratio may avoid damage to surrounding tiles due to ballistic impact, which may otherwise take place for a tile area smaller than 16 cm 2 and aspect ratio greater than 2.
  • the one or more tiles comprising the protective material may be attached to the polymeric support.
  • the one or more tiles comprising the protective material are attached to the polymeric support by an adhesive. Any suitable adhesives that are within the knowledge of the person skilled in the art may be used, so long as the adhesive holds the protective material and the polymeric support together. Examples of such adhesives may include, but are not limited to polyurethane, polyvinyl acetate, epoxy, cyanoacrylate or combinations thereof. In some embodiments, epoxy or polyurethane may be used to bond the protective material to the polymeric support.
  • the ballistic resistant article may have a refractive index of around 1.80
  • the one or more tiles comprising the protective material are attached to the polymeric support by an adhesive having a refractive index in the range of about 1.7 to about 1.9. In so doing, this may avoid refractive index mismatch at the bonding interfaces, which may be the case for normal adhesives having refractive index of around 1.4.
  • Such adhesives may, for example, have a main composition of organic materials or a mixture of organic material and inorganic particles with refractive indices greater than 2.0 and sizes smaller than 100 nm. In this way, problem(s) relating to visual discomfort due to the joints may be mitigated.
  • the adhesive has a refractive index in the range of about 1.7 to about 1.9, about 1.7 to about 1.8, or about 1.75 to about 1.85.
  • an adhesive that may have a refractive index in this range may include cyanoacrylates and/or nanoparticles doped adhesives.
  • the adhesive is selected from the group consisting of cyanoacrylates, nanoparticles doped adhesives, and combinations thereof.
  • the one or more tiles comprising the protective material may be arranged to form a panel.
  • panel it is meant an arrangement of the one or more tiles comprising the protective material such that they are placed adjacent to each other so as to cover a larger area for various applications.
  • the ballistic resistant article is a goggle, a safety glass, personal protective equipment, window, screen, windscreen, panel, optical sensor, imager, structural member of a military equipment or a vehicle, such as a helicopter, an airplane, a car, a tank, a boat, a ship, to name only a few.
  • Various embodiments refer to a method of preparing the protective material disclosed herein, which is provided herein for purposes of illustration only.
  • the method may comprise preparing a mixture comprising aluminum oxide and an oxide of R 1 in a suitable solvent, where R 1 is as defined above.
  • R 1 is as defined above.
  • the oxide of R 1 is selected from the group consisting of Y2O3, Yb 2 03, and combinations thereof.
  • the oxide of R 1 comprises Y2O3.
  • suitable solvent examples include, but are not limited to, alcohol based solvents such as methanol, ethanol, and/or propanol, to name only a few.
  • the aluminum oxide and the oxide of R 1 may independently have a size in the range of about 1 ⁇ to about 10 ⁇ , such as about 3 ⁇ to about 10 ⁇ , about 5 ⁇ to about 10 ⁇ , about 7 ⁇ to about 10 ⁇ , about 1 ⁇ to about 8 ⁇ , about 1 ⁇ to about 5 ⁇ , about 1 ⁇ to about 3 ⁇ , about 3 ⁇ to about 8 ⁇ , or about 4 ⁇ to about 6 ⁇ .
  • the mixture further comprises an oxide of R 2 , where R 2 is as defined above.
  • R 2 is selected from the group consisting of Eu, Gd, Tb, Ho, Tm, Lu, and combinations thereof.
  • R 2 is optionally present, and may function as a rare-earth dopant of the rare-earth garnet ceramic.
  • the mixture further comprises a sintering agent.
  • a sintering agent examples include a sintering agent.
  • the method may include physically working the mixture to form a slurry. Physically working the mixture may be carried out by any suitable technique, such as milling, ball milling, and/or grinding.
  • physically working the mixture is carried out by ball milling.
  • the ball milling may be carried out, for example, at a speed in the range of about 10 to about 100 rpm, and for a time period in the range of about 1 hour to about 48 hours.
  • the slurry may be dried to form a powder. Drying the slurry may be carried out using any suitable techniques, such as by oven drying or spray drying.
  • a pressure in the range of about 100 MPa to about 200 MPa such as about 100 MPa to about 150 MPa, about 120 MPa to about 180 MPa or about 140 MPa to about 160 MPa, may be applied to the powder to form a compact, which may be carried out using a cold isostatic pressed (CIP) process.
  • CIP cold isostatic pressed
  • the compact Upon forming the compact, it may be heated in two steps by calcining the compact at a temperature in the range of about 500 °C to about 1000 °C, and sintering the compact following calcination at a temperature in the range of about 1600 °C to about 1800 °C in vacuum to obtain the protective material.
  • the calcination step may be carried out for a time period sufficient to burn off organic constituents, and may be in the range of about 1 hour to about 12 hours. Sintering the compact following calcination, on the other hand, may be carried out for a time period sufficient to obtain transparency in the protective material, such as in the range of about 1 hours to about 50 hours.
  • a pressure in the range of about 100 MPa to about 200 MPa may be applied to the protective material at a temperature in the range of about 1600 °C to about 1800 °C to reduce the pore size within the ceramics.
  • a smaller pore size within the ceramics may enhance mechanical strength of the protective material.
  • a surface of the protective material may be polished so as to improve transparency of the protective material.
  • the polishing may be carried out using commercially available grinder and polisher as would be understood by a person of average skill in the art.
  • Various embodiments refer in a further aspect to use of the protective material according to the first aspect in goggles, safety glasses, personal protective equipment, window, screen, windscreen, panel, optical sensor, imager, windows of aircrafts, windows and bridges of ships, windows of building infrastructure, structural member of a military equipment or a vehicle, vehicles as jet fighter canopies, aircraft windows, helicopter canopies and windows; windows, barriers and doors in police and/or military installations, jails and prisons, hospitals; protective shields for police and/or military personnel; lenses and windows in optical devices, goggles, safety glasses, windows, screens, eyeglass lenses, camera lenses, microscope lenses, telescope lenses, LED (light-emitting diode) lenses and windows, protective glass for watches and clocks, diffusers, protective and/or decorative covers and bulb materials for artificial lighting, automotive headlights, highway, parking lot lighting and combinations thereof.
  • Various embodiments relate generally to a rare-earth garnet ceramic, such as a transparent aluminum garnet ceramics with Y and/or Yb as the main composition, with high optical transmittance in the visible to infrared wavelength range and possessing excellent mechanical strength.
  • a rare-earth garnet ceramic such as a transparent aluminum garnet ceramics with Y and/or Yb as the main composition, with high optical transmittance in the visible to infrared wavelength range and possessing excellent mechanical strength.
  • the rare-earth garnet ceramic may comprise or consist of a transparent garnet material (R 1 R 2 )aAlsOi2, wherein R 1 is Y and/or Yb, and R 2 is one or more types of rare-earth selected from the group consisting of Eu, Gd, Tb, Ho, Tm, Lu, and combinations thereof, R 1 being present in an amount that is 90 % or more of total amount of R 1 and R 2 , R 2 being present in an amount that is 10 % or less of total amount of R 1 and R 2 , and a is in the range from about 3 to about 3.015.
  • R 1 R 2 transparent garnet material
  • R 1 is Y and/or Yb
  • R 2 is one or more types of rare-earth selected from the group consisting of Eu, Gd, Tb, Ho, Tm, Lu, and combinations thereof
  • R 1 being present in an amount that is 90 % or more of total amount of R 1 and R 2
  • R 2 being present in an amount that is 10 % or less
  • the transparent garnet ceramic material may be Y3AI5O12, YbsAlsOn, or their solid solution with purity of 99.8 % or higher.
  • the transparent garnet ceramic material may have average grain size within a range of 1 to 20 microns.
  • the transparent garnet ceramic material may have a residual pore amount in the range of 10 ppm to 1000 ppm and average pore size of smaller than 100 micron, or preferably, smaller than 5 microns.
  • the transparent garnet ceramic material may have a three-point bending strength in the range of about 150 MPa to 450 MPa.
  • the transparent garnet ceramic material may have an optical transmittance of more than 65 % for a thickness of 1 cm at 550 nm.
  • the transparent garnet ceramic material may be used as a transparent armor material.
  • the transparent garnet armour material may be made of transparent garnet ceramic tiles with an area in the range of about 16 cm 2 to 100 cm 2 .
  • the tiles may be bonded in a horizontal manner to form a plate, and be bonded into one piece of panel using a polymeric backing material for application as a composite bullet-proof panel.
  • the bulletproof panel may be made of tiles having a thickness of less than 25 mm, an area of between 16 cm 2 to 100 cm , and an aspect ratio of smaller than 2.
  • the tiles may be bonded using transparent adhesives, which may be commercially available, and in combination with polymeric material as a backing to form the whole transparent ceramics armor panel.
  • the transparent garnet ceramics tiles may have a shape structure that is not limited to just 4 sides like a square, and may include other tessellation structures such as hexagon, and rectangle. It can be used singularly as a circle.
  • the tiles may be bonded using commercially available transparent adhesives, and may be bonded to a suitable polymeric backing material to form the bullet-proof panel.
  • the bullet-proof panel may have excellent bullet-resistance even in the case of two or more shots fired on the same panel.
  • the transparent garnet ceramic tiles disclosed herein may further be used in military systems that feature the application of bullet-proof protective screens such as protection for optical sensors and imagers, windows, windscreens, and panels; for platforms which include but is not limited to various land, air and sea platforms such as for e.g. fighter jets, helicopters, airplanes, cars, armored vehicle windows, windows of boats and ships etc.
  • bullet-proof protective screens such as protection for optical sensors and imagers, windows, windscreens, and panels
  • platforms which include but is not limited to various land, air and sea platforms such as for e.g. fighter jets, helicopters, airplanes, cars, armored vehicle windows, windows of boats and ships etc.
  • garnets While naturally occurring garnets may be composed of oxides of Ca, Si, Al, Fe, etc., garnets may be prepared using various other elements from the periodic table. Amongst them, although rare-earth aluminum garnets may be used as materials for laser devices, they cannot be applied as bullet-resistant materials. The reasons are:
  • Material hardness is only half that of sapphire, and it lacks the ability to deform the bullet shot at its surface.
  • the length of crack was longest for sapphire. It was observed that for YAG, the cracks were concentrated around the centre portion where impact with the steel ball occurred. The inventors determined that the propagation of the cracks was the least for YAG as it was hard for cracks to spread to the surrounding.
  • rare-earth elements Y and/or Yb were to form the garnet ceramics as a basic/principle composition.
  • the rare-earth elements Y and/or Yb may confer ability to obtain stable optical and mechanical characteristics, and to render the process economically viable.
  • FIG. 2 shows a panel made by bonding 16 pieces of tiles of 80 mm x 80 mm using adhesives. The joints are visible but it is not a problem practically.
  • Example 2 General preparation method
  • Y2O3 powder particle size >1 micron
  • AI2O3 particle size > 1 micron
  • Milling balls with suitable quantity of solvents as pulverization and mixing media, were mixed together with additives, and milled from a few hours to tens of hours depending on the mixing requirements.
  • Sintering agents such as MgO, CaO, MgF2, CaF2, AIF, and/or S1O2 with weight% of less than 1000 ppm may also be added.
  • the slurries obtained were spray- dried to form powders.
  • CIP cold isostatic pressed
  • the compacts were first calcined using temperatures in the range from a few hundred degrees up to a 1000 degrees Celsius. After that, they were sintered in vacuum from a few hours to tens of hours under a temperature in the range of about 1600 °C to about 1800 °C to obtain transparency. HIP was applied at a pressure of 100 MPa to 200 MPa between 1600 °C to 1800 °C for another few hours.
  • Transparent tiles were obtained by polishing the surface of the sintered body, which were carried out using commercially available grinder and polisher.
  • Transparent panels were obtained by bonding the polished tiles on the edges with adhesives to form a flat transparent ceramics panel and then bonding the ceramics panel to a polymeric support.
  • the material composition was analyzed with X-ray fluorescence (XRF), or for the case of powder, X-ray diffraction (XRD), to quantify the garnet or rare-earth amounts.
  • XRF X-ray fluorescence
  • XRD X-ray diffraction
  • Average grain size of the ceramic was measured by thermal etching of mirror polished material to expose the grain boundary part, and then using scanning electron microscopy (SEM) to observe 10 random positions to obtain the grain size via image analysis.
  • SEM scanning electron microscopy
  • Amount of residual pores was measured either by visually observing the size and number of voids or by image analysis of a two- side mirror-polished sample under an optical microscope.
  • the bending strength was measured in accordance to ASTM (American Standard Testing Method), and may be measured using any relevant international standard.
  • the transmittance was measured by preparing a 10 mm thick mirror-polished sample and using a commercially available UV-vis spectrophotometer.
  • Example 4 Implementation examples [00121] To verify the effect of embodiments exemplified herein, the inventors fabricated materials as illustrated in FIG. 3, and having different characteristics as listed in TABLE 3 to TABLE 8 (the inventors used test samples where each piece is 40 X 40 mm with both faces mirror polished).
  • TABLE 7 lists panels that were formed by bonding 16 pieces of fabricated tiles using adhesives, where the tiles have different sizes. The panels were all bonded to polymeric backing and their bullet resistance were evaluated under conditions the same as those in TABLE 3 to TABLE 6.
  • the shooting test followed the procedure described earlier.
  • the panel is 4 x 4 pieces of test tiles bonded with adhesives and with a polymeric backing material similar to that illustrated in FIG. 1.
  • the panel that is obtained by bonding relatively small tiles is furthermore able to withstand multiple shots and hence provides much higher probability of protecting lives.
  • the fabrication of rare-earth aluminum garnet tiles is much less costly compared to the fabrication costs of sapphire single crystal, AION, Spinel ceramics, etc., and hence, it is also highly advantageous economically.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Aiming, Guidance, Guns With A Light Source, Armor, Camouflage, And Targets (AREA)
  • Helmets And Other Head Coverings (AREA)

Abstract

L'invention concerne un matériau de protection transparent comprenant une céramique de grenat de terres rares. La céramique de grenat de terres rares possède la formule générale (R1 R2)aAl50i2, où R1 est choisi dans le groupe constitué par Y, Yb et des associations de ces derniers, et R2 est choisi dans le groupe constitué par Eu, Gd, Tb, Ho, Tm, Lu et des associations de ces derniers, R1 étant présent en une quantité qui est supérieure à 90 % atomique de la quantité totale de R1 et R2, et R2 étant présent en une quantité qui est inférieure ou égale à 10 % atomique de la quantité totale de R1 et R2, et a étant dans la plage d'environ 3 à environ 3,015. Selon un mode de réalisation préféré, le grenat d'yttrium-aluminium (YAG) est utilisé en tant que matériau de protection transparent. De plus, l'invention concerne également un article résistant aux balles constitué dudit matériau de protection transparent.
PCT/SG2017/050142 2017-03-23 2017-03-23 Matériau de protection WO2018174814A1 (fr)

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SG11201906564PA SG11201906564PA (en) 2017-03-23 2017-03-23 A protective material
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WO2009038674A2 (fr) * 2007-09-14 2009-03-26 The Penn State Research Foundation Procédé de fabrication de céramiques transparentes
US20100102464A1 (en) * 2008-10-24 2010-04-29 Hollingsworth Joel P Transparent ceramics and methods of preparation thereof
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JP2008097014A (ja) * 2003-08-05 2008-04-24 Sumitomo Electric Ind Ltd 液晶パネル用透明基板
US20060024528A1 (en) * 2004-07-30 2006-02-02 Strangman Thomas E Protective coating for oxide ceramic based composites
WO2009038674A2 (fr) * 2007-09-14 2009-03-26 The Penn State Research Foundation Procédé de fabrication de céramiques transparentes
US20100102464A1 (en) * 2008-10-24 2010-04-29 Hollingsworth Joel P Transparent ceramics and methods of preparation thereof
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US20140374931A1 (en) * 2011-11-10 2014-12-25 Ceramtec-Etec Gmbh Method for producing transparent ceramic objects by means of fluidized bed granulation
CN105904790A (zh) * 2016-06-12 2016-08-31 浙江美盾防护技术有限公司 透明装甲板

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