US20070102672A1 - Ceramic radiation shielding material and method of preparation - Google Patents

Ceramic radiation shielding material and method of preparation Download PDF

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Publication number
US20070102672A1
US20070102672A1 US11/441,833 US44183306A US2007102672A1 US 20070102672 A1 US20070102672 A1 US 20070102672A1 US 44183306 A US44183306 A US 44183306A US 2007102672 A1 US2007102672 A1 US 2007102672A1
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United States
Prior art keywords
phosphate
radiation shielding
matter
composition
group
Prior art date
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Abandoned
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US11/441,833
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English (en)
Inventor
Judd Hamilton
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CO-OPERATIONS Inc
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CO-OPERATIONS Inc
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 CO-OPERATIONS Inc filed Critical CO-OPERATIONS Inc
Priority to US11/441,833 priority Critical patent/US20070102672A1/en
Priority to CN200680045960.3A priority patent/CN101496112B/zh
Priority to NZ568903A priority patent/NZ568903A/en
Priority to RU2008127341/07A priority patent/RU2446490C2/ru
Priority to CA2632764A priority patent/CA2632764C/en
Priority to EP06851936.2A priority patent/EP1958210B1/en
Priority to MX2008007245A priority patent/MX339802B/es
Priority to AU2006350740A priority patent/AU2006350740A1/en
Priority to ES06851936.2T priority patent/ES2657928T3/es
Priority to JP2008544509A priority patent/JP5469342B2/ja
Priority to PCT/US2006/046722 priority patent/WO2008060292A2/en
Priority to BRPI0620029-0A priority patent/BRPI0620029A2/pt
Priority to KR1020157019158A priority patent/KR101749946B1/ko
Priority to KR1020087016382A priority patent/KR101523235B1/ko
Priority to CN201510679756.8A priority patent/CN105390171B/zh
Priority to KR1020147006035A priority patent/KR101578697B1/ko
Priority to DK06851936.2T priority patent/DK1958210T3/da
Assigned to CO-OPERATIONS, INC. reassignment CO-OPERATIONS, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAMILTON, JUDD D., HAMILTON, VERNON D.
Publication of US20070102672A1 publication Critical patent/US20070102672A1/en
Priority to IL191901A priority patent/IL191901A/he
Priority to US12/133,209 priority patent/US8440108B2/en
Priority to US13/869,724 priority patent/US20130277616A1/en
Priority to JP2013116194A priority patent/JP5850881B2/ja
Priority to US14/712,853 priority patent/USRE46797E1/en
Priority to JP2015198391A priority patent/JP6084266B2/ja
Priority to US15/954,495 priority patent/USRE48014E1/en
Abandoned legal-status Critical Current

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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/06—Ceramics; Glasses; Refractories
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
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    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
    • C04B28/342—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition as a mixture of free acid and one or more reactive oxides
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    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/19—Alkali metal aluminosilicates, e.g. spodumene
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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    • C04B35/6303—Inorganic additives
    • C04B35/6306—Binders based on phosphoric acids or phosphates
    • C04B35/6313—Alkali metal or alkaline earth metal phosphates
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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Definitions

  • the present invention relates to the field ceramics and particularly to a cold fired zeolite (alumino-silicate) containing ceramic having radiation shielding characteristics.
  • Radioactive materials including medical wastes, industrial wastes, wastes from depleted uranium ordinance, and the like also experience the same storage, shielding, and containment issues.
  • electronic devices such as cellular telephones, microwave ovens, and the like may require electromagnetic energy shielding which blocks radiated energy from being directed towards the user.
  • the medical diagnostic field also makes extensive use of radioactive materials to aid in detection of human maladies.
  • Radioactive medical diagnostics make extensive use of lead as a shielding material.
  • a patient may wear a lead lined vest to minimize exposure during an x-ray.
  • the x-ray machine itself may require significant shielding, such as provided by lead sheeting, to prevent undue human exposure to radioactive materials.
  • Metallic lead shielding is extensively utilized because it allows for efficient shielding without unduly consuming space. For example, a sheet of lead less than one inch thick may be implemented to shield an x-ray machine.
  • Lead shielding drawbacks include the mass of lead, the difficulty in forming structures for holding the lead sheeting in place, the desire for aesthetically pleasing structures, and the like.
  • cementitious based shielding and containment systems may hinder the utilization of cementitious based shielding and containment systems due to their size, mass and generally inferior ability to shield radioactive energy without additives included for this purpose.
  • cement based shielding may require additional building supports thereby preventing retrofitting without extensive reconstruction.
  • Portland cement matrices also require extensive curing (twenty-one days) to ensure proper matrix formation.
  • Other alternatives such as a polymeric based matrix may offer lower porosity but, may degrade when exposed to organic solvents and either high or low pH materials.
  • Cement matrices also are susceptible to corrosive attack from a variety of materials typically found in radioactive wastes.
  • Fired or high temperature curing ceramic materials do not offer a viable alternative to cement structures.
  • High curing temperatures may prevent the materials from being utilized in waste containment and shielding applications as high temperature firing (above several hundred degrees Celsius) requires the components be formed and fired in a remote location prior to transport and assembly in the desired location.
  • High temperature cured ceramics may not be practical for forming large components due to the firing requirements.
  • In-situ formation of fired ceramics for waste containment may be problematic because of the wastes being contained and the location of final storage.
  • Ammonia may be liberated during the firing process. Inclusion of ammonia in the ceramic matrix may be detrimental to the resultant formation.
  • ceramic structures may form low porosity structures in comparison to Portland cement structures.
  • magnesium oxide/phosphoric acid reaction may be characteristic: MgO+H 3 PO 4 +H 2 O ⁇ MgHPO 4 .3H 2 O
  • contemplated metal oxides included aluminum oxides, iron oxides, calcium oxides. Minimizing the pH of the reaction, in comparison to a phosphoric acid (i.e., a more basic reaction) may be achieved through utilization of a carbonate, bicarbonate, or hydroxide of a monovalent metal reacting with the phosphoric acid prior to reacting with the metal oxide or metal hydroxide.
  • M′ contemplated metals
  • potassium, sodium, and lithium being potassium, sodium, and lithium.
  • a partial exemplary reaction being: H 3 PO 4 +M 2 CO 3 +M′Oxide ⁇ M′HPO 4
  • suitable monvalent metal dihydrogen phosphates being sodium dihydrogen phosphate and potassium dihydrogen phosphate. Each being utilized in a hydrated form.
  • the present invention is directed to a phosphate bonded ceramic including a zeolite with radiation shielding characteristics for containment, electromagnetic shielding, attenuation of electromagnetic energy, and construction applications.
  • composition of matter and method of forming a radiation shielding member at ambient temperatures in which the composition of matter includes a phosphate bonded ceramic, a radiation shielding material dispersed in the phosphate bonded ceramic matrix is disclosed.
  • the present invention is directed to a composition of matter and method for forming a radiation shielding member at ambient conditions.
  • composition of matter of the present invention may be utilized for shielding and attenuation of various forms of radiation included in the electromagnetic spectrum from alpha, beta, or gamma emissions; microwaves; energy from electron-beam welding (bremsstrahlung radiation or secondary radiation) and the like.
  • the composition of matter and method provides an efficient composition for utilization in constructing members which exhibit radiation shielding capability in a region of the electromagnetic spectrum.
  • the resultant material may be formed at ambient conditions in a rapid time frame (two days curing to one-half hour of curing). This allows for formation of a phosphate bonded ceramic matrix with radiation shielding inclusion materials without the high temperature firing typically required.
  • Typical high temperature firing may exceed several hundred degrees Celsius and usually may occur in the range about 1800° C. (one thousand eight hundred degrees Celsius). While the present method of cold firing (curing at ambient temperatures) may occur at or below 100° C. (one hundred degrees Celsius).
  • a structure formed in accordance with the present invention may allow for a fully cured wall partition to be formed in the time frame of several days.
  • a wall partition formed in the foregoing manner may be less massive then a Portland concrete system.
  • the utilization of a phosphate bonded ceramic material of the present invention may minimize the mass and size (i.e., thickness) required for a shielding component over a Portland concrete based matrix (for the same effective shielding) as disclosed in U.S. Pat. No. 6,565,647.
  • a composition of matter of the present invention implements a phosphate bonded ceramic material to form a matrix for including additional radiation shielding material therein.
  • a phosphate bonded ceramic matrix may be formed by the incorporation of a metal oxide with a phosphates containing substance or material.
  • the resultant phosphate ceramic may be a hydrated form based on the constituent metal phosphate.
  • Suitable metal oxides may include metal oxides in which the cationic component is associated with radiation shielding such that the resultant metal phosphate ceramic may exhibit radiation shielding capability.
  • Suitable phosphate containing substances or materials include phosphoric acid, an acid phosphate, monohydrogen phosphates, dihydrogen phosphates and the like.
  • Suitable oxides include magnesium, iron(II or III), calcium, bismuth, cerium(III or IV), barium, depleted uranium(III) (substantially uranium 238), or aluminum.
  • the resultant phosphate ceramics may include MgHPO 4 .3H 2 O (magnesium hydrogen phosphate trihydrate), MgHPO 4 magnesium hydrogen phosphate, Fe 3 (HPO 4 ) 2 (iron(II) phosphate), Fe 3 (HPO 4 ) 2 .8H 2 O (iron(II) phosphate octahydrate), FeHPO 4 (iron(III) phosphate), FeHPO 4 .2H 2 O (iron(III) phosphate dihydrate) AlPO 4 aluminum phosphate, AlPO 4 .1.5H 2 O (aluminum phosphate hydrate), CaHPO 4 (calcium hydrogen phosphate), CaHPO 4 .2H 2 O (calcium hydrogen phosphate dihydrate), BiPO 4 (bismuth phosphate), CePO 4 (cerium(III) phosphate), CePO 4 .2H 2 O (cerium(III) phosphate dihydrate), BaHPO 4 (barium hydrogen phosphate), and UPO 4 (depleted ura
  • Suitable multiple metal phosphates may include magnesium hydrogen phosphate, iron(III) phosphate, aluminum phosphate, calcium hydrogen phosphate, bismuth phosphate, cerium(III) phosphate, and barium hydrogen phosphate.
  • the ceramic matrix is of the formula: ceramic matrix is of the formula: MHPO 4 .xH 2 O in which M is a divalent cation selected from the group consisting of: Mg (magnesium), Ca (calcium), Fe (iron(II)), and Ba (barium); wherein x is at least one of 0 (zero), 2 (two), 3 (three), or 8 (eight).
  • the phosphate based ceramic matrix is of the formula: MPO 4 .xH 2 O in which M is a trivalent cation selected from: Al (aluminum), Ce (cerium (III)), U 238 (depleated uranium) ; and Fe (iron(III)); and x is at least one of 0 (zero), 1.5 (one point five), or 2 (two).
  • a multiple layer structure is formed to provide effective attenuation across a range of kilovolt-peak (kVp) ranges.
  • a multiple layer material is formed via a casting or spray application to form a mono structure exhibiting shielding and attenuation across a range.
  • the layers may be formed of differing combinations of ceramics/shielding materials to achieve the desired shielding/attenuation.
  • a first layer is formed with a bismuth shielding material while a second layer is formed of a cerium based ceramic.
  • a third layer of a ceramic including a barite shielding material may be included as well.
  • cerium oxide is included for its attenuation X-rays at 120 kVp at a material thickness of 0.5 inches. Greater material thickness may effectively attenuate x-radiation at higher levels of energy.
  • suitable radiation shielding materials may be dispersed in the matrix.
  • suitable radiation shielding materials may be incorporated in a matrix to provide attenuation across a portion of the electromagnetic spectrum, such as X-rays, microwaves, and the like regions or portions of regions of the electromagnetic spectrum. Examples include powders, aggregates, fibers, woven fibers and the like.
  • Exemplary materials include barite, barium sulfate, bismuth metal, tungsten metal, annealed leaded glass fibers and powders, cerium oxide, zeolite, clinoptilotite, plagioclase, pyroxene, olivine, and celestite.
  • a zeolite may be approximately by weight percentage 52.4% (fifty two point four percent) SiO 2 (silicon dioxide), 13.13% (thirteen point one three percent) Al 2 O 3 (alumina oxide), 8.94% (eight point nine four percent) Fe 2 O 3 (ferric oxide), 6.81% (six point eight one percent) CaO (calcium oxide), 2.64% (two point six four percent) Na 2 O (sodium oxide), 4.26% (four point two six percent) MgO (magnesium oxide).
  • barite may be approximately 89% (eighty nine percent) BaSO 4 (barium sulfate) and 5.8% (five point eight percent) silicates with the remainder consisting of naturally varying percentages of titanium dioxide, calcium oxide, magnesium oxide, manganese oxide, and potassium oxide. The foregoing approximation being dependent on naturally occurring weight percentage variations.
  • a method of constructing a shielding member includes mixing a metal oxide, such as a metal oxide including divalent metal cation with a phosphate containing material.
  • Suitable phosphate containing materials include phosphoric acid, hydrogen phosphate substances (such as monohydrogen phosphates and dihydrogen phosphates) and the like.
  • a radiation shielding material may be incorporated into the metal oxide and phosphate containing material mix. Incorporating may include dispersing aggregate, powder, fibers. Woven fibers may be incorporated as part of a casting process, a layering process, or the like.
  • the incorporated radiation shielding material and metal phosphate ceramic may be cured to hardness (maximum compressive strength) at ambient conditions.
  • the member may be cast in place and the curing reaction being conducted at ambient conditions (i.e., ambient temperature).
  • ambient conditions i.e., ambient temperature
  • the reaction and curing of the radiation shielding member occurs at or at less than 100° C. (one hundred degrees Celsius).
  • the porosity of the resultant member may be varied based on the reagents selected.
  • a radiation shielding member composed of a composition of matter of the present invention is constructed by mixing 1 lb. (one pound) of a metal oxide and monopotassium phosphate mixture with 1 lb. (one pound) of radiation shielding mater such as a aggregate, powder, fiber filler material, H 2 O (water) is added to approximately 20% (twenty percent) by weight and the resultant “cold-fired” material allowed to cure.
  • the metal oxide to monopotassium phosphate ratio by weight, is 1 ⁇ 3 (one third) metal oxide, such as magnesium oxide, to two thirds monopotassium phosphate, or MKP(KH 2 PO 4 ).
  • various carbonates, bicabonate (such as sodium bicarbonate, potassium bicarbonate and the like) or metal hydroxides reagents may be reacted in a two step process with an acid phosphate to limit the maximum reaction temperature of the metal oxide and the result of the carbonate, bicabonate or hydroxide reaction with an acid phosphate.
  • other acids may be implemented to form a resultant metal phosphate ceramic based material.
  • the selection of the acid may be based on the metal oxide to be utilized, suitable metal oxides include divalent and trivalent metals (including transition metals and lanthanide series and actinide series metals).
  • suitable acids include boric acid and hydrochloric acid.
  • exemplary compositions were formed by mixing the selected ceramic cement with the desired shielding material.
  • the following specific examples being only exemplary and utilized to explain the principles of the present invention.
  • the following procedures were conducted in ambient conditions (e.g., temperature, pressure). For instances, carried out at a room temperature of between 65° F. to 85° F. (sixty-five degrees Fahrenheit to eighty-five degrees Fahrenheit) under atmospheric pressure. No attempt was made to fully homogenize the material to obtain uniform particles, while substantially uniform distribution of shielding material within the ceramic cement was attempted.
  • the ceramic is hydrolized and cast in contact with the fabric. In instances in which powdered shielding materials are incorporated, the particle size varied depending on the material.
  • Water is added to hydrolyze the dry mixture.
  • the combination water/ceramic cement/shielding material is mixed for a sufficient duration and with sufficient force to cause the material to exhibit an exothermic rise of between 20%-40% (twenty percent. to forty percent) of the original temperature of the mixture.
  • the hydrolyzed mix was compacted via vacuum or vibratory, or equivalent method to eliminate voids. Compaction being conducted in a container, such as a polymeric container formed from polypropylene or polyethylene, having a low coefficient of friction to facilitate removal.
  • the samples were allowed to harden to the touch (at least twenty-four hours) at ambient conditions. The samples were submitted for testing.
  • the samples submitted for testing were formed when a metal oxide such as MgO (Magnesium Oxide) and radiopaque additives as set forth in the present invention, are stirred in an acid-phosphate solution, (such as mono potassium phosphate and water).
  • an acid-phosphate solution such as mono potassium phosphate and water.
  • the dissolution of the metal oxide forms cations that react with the phosphate anions to form a phosphate gel.
  • This gel subsequently crystallizes and hardens into a ceramic.
  • Dissolution of the oxide also raises the pH of the solution, with the ceramic being formed at a near-neutral pH.
  • the chemically bonded phosphate ceramic is produced by controlling the solubility of the oxide in the acid-phosphate solution.
  • Oxides or oxide minerals of low solubility are good candidates to form chemically bonded phosphate ceramics because their solubility can be controlled.
  • the metal oxide in the sample formulations is known “deadburn” Magnesium Oxide (MgO), calcinated at 1300° C. or above in order to lower the solubility in the acid-phosphate solution.
  • Such “deadburn” magnesium oxide can then be reacted at room temperature with any acid-phosphate solution, such as potassium hydrogen phosphate, to form a ceramic of the magnesium potassium phosphate.
  • magnesium potassium phosphate a mixture of MgO (Magnesium Oxide) and KH 2 PO 4 (Potassium Phosphate) can simply be added to water and mixed from 5 minutes to 25 minutes, depending on the batch size. Potassium Phosphate dissolves in the water first and forms the acid-phosphate solution in which the MgO dissolves.
  • the chemically bonded phosphate ceramics are formed by stirring the powder mixture of oxides and additives such as retardants and radiopaque fillers as have been clearly defined by this invention, into an acid-phosphate solution in which the MgO dissolves and reacts with the phosphate and sets into a ceramic material.

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US11/441,833 US20070102672A1 (en) 2004-12-06 2006-05-26 Ceramic radiation shielding material and method of preparation
KR1020087016382A KR101523235B1 (ko) 2005-12-06 2006-12-06 화학 결합된 세라믹 방사선 차폐재 및 제조방법
CN201510679756.8A CN105390171B (zh) 2005-12-06 2006-12-06 化学键合的陶瓷辐射屏蔽材料及制备方法
NZ568903A NZ568903A (en) 2005-12-06 2006-12-06 Chemically bonded ceramic radiation shielding material and method of preparation
KR1020147006035A KR101578697B1 (ko) 2005-12-06 2006-12-06 화학 결합된 세라믹 방사선 차폐재 및 제조방법
EP06851936.2A EP1958210B1 (en) 2005-12-06 2006-12-06 Chemically bonded ceramic radiation shielding material and method of preparation
MX2008007245A MX339802B (es) 2005-12-06 2006-12-06 Material protector contra radiación, de cerámica enlazada químicamente y método para su preparación.
AU2006350740A AU2006350740A1 (en) 2005-12-06 2006-12-06 Chemically bonded ceramic radiation shielding material and method of preparation
ES06851936.2T ES2657928T3 (es) 2005-12-06 2006-12-06 Material cerámico de blindaje contra la radiación unido químicamente y método de preparación
JP2008544509A JP5469342B2 (ja) 2005-12-06 2006-12-06 化学結合性セラミック放射線遮蔽材料および製造方法
PCT/US2006/046722 WO2008060292A2 (en) 2005-12-06 2006-12-06 Chemically bonded ceramic radiation shielding material and method of preparation
BRPI0620029-0A BRPI0620029A2 (pt) 2005-12-06 2006-12-06 material cerámico de blindagem contra radiação ligado quimicamente e método de preparação
KR1020157019158A KR101749946B1 (ko) 2005-12-06 2006-12-06 화학 결합된 세라믹 방사선 차폐재 및 제조방법
CN200680045960.3A CN101496112B (zh) 2005-12-06 2006-12-06 化学键合的陶瓷辐射屏蔽材料及制备方法
RU2008127341/07A RU2446490C2 (ru) 2005-12-06 2006-12-06 Химически связанный керамический радиационно-защитный материал и способ его подготовки
CA2632764A CA2632764C (en) 2005-12-06 2006-12-06 Chemically bonded ceramic radiation shielding material and method of preparation
DK06851936.2T DK1958210T3 (da) 2005-12-06 2006-12-06 Kemisk bundet keramisk strålingsafskærmningsmateriale og fremgangsmåde til fremstilling deraf
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US12/133,209 US8440108B2 (en) 2005-12-06 2008-06-04 Chemically bonded ceramic radiation shielding material and method of preparation
US13/869,724 US20130277616A1 (en) 2005-12-06 2013-04-24 Chemically bonded ceramic radiation shielding material and method of preparation
JP2013116194A JP5850881B2 (ja) 2005-12-06 2013-05-31 化学結合性セラミック放射線遮蔽材料および製造方法
US14/712,853 USRE46797E1 (en) 2005-12-06 2015-05-14 Chemically bonded ceramic radiation shielding material and method of preparation
JP2015198391A JP6084266B2 (ja) 2005-12-06 2015-10-06 化学結合性セラミック放射線遮蔽材料および製造方法
US15/954,495 USRE48014E1 (en) 2005-12-06 2018-04-16 Chemically bonded ceramic radiation shielding material and method of preparation

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