CN103058241A - High-efficiency synthetic method of nanometer aluminum particle - Google Patents
High-efficiency synthetic method of nanometer aluminum particle Download PDFInfo
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- CN103058241A CN103058241A CN2012105599072A CN201210559907A CN103058241A CN 103058241 A CN103058241 A CN 103058241A CN 2012105599072 A CN2012105599072 A CN 2012105599072A CN 201210559907 A CN201210559907 A CN 201210559907A CN 103058241 A CN103058241 A CN 103058241A
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Abstract
The invention relates to a high-efficiency synthetic method of a nanometer aluminum particle. Products can be used for manufacturing thin film solar cell materials in order to improve the photoelectric conversion efficiency; the products can also be used for solid rocket fuel push agent. The invention belongs to the field of preparing novel functional materials. The nanometer aluminum particle regards a hyperbranched polymer as solvent, reducing agent and dispersing agent. After the hyperbranched polymer is contacted with trivalent aluminum ion, a spontaneous reduction reaction happens in the aqueous solution and a core-shell structure material is generated. An outer sphere of the core-shell structure material is an overrunning compound, and an inner sphere of the core-shell structure material is the nanometer aluminum particle. When a reaction system is placed in a strong magnetic field generator to be used for controlling the strength and the action time of the magnetic field, the reduction reaction efficiency and the product productivity can be improved by various degrees.
Description
Technical field
The present invention relates to a kind of high efficiency preparation method of nano aluminum particle, in normal-temperature water solution, the spontaneous reduction trivalent aluminium ion of a kind of hyperbranched polymer generates the nano aluminum particle, and product has the nucleocapsid structure of " over-expense compound parcel nano aluminum particle "; Can improve speed of reaction and productive rate after reaction system placed high-intensity magnetic field.
Background technology
Nano material is the important researchdevelopment direction of in the nano science, has caused widely in many scientific domains in recent years and has paid attention to, and becomes the focus of Materials science research; As an aspect of nano material, metal and alloy nano particle thereof are serving as important role in modern industry, national defence and hi-tech development; Nanoparticle refers to be of a size of the ultrafine particle of 1-100 nm, the surface atom of nanoparticle sharply increases along with reducing of particle diameter with the ratio of total atom number, demonstrates strong volume effect (being small-size effect), quantum size effect, surface effects and macro quanta tunnel effect; The metal nanoparticle special performance that has good performance and show with the other materials compound tense wherein, a lot of fields in national economy all have broad application prospects, useful as catalysts, medical material,, electromagnetic functional material, absorbing material, sensor element material and nano composite material etc.
Organize net according to U.S. physicist: by behind depositing nano aluminum particulate on the solar film battery, can improve the electricity conversion of battery; The nano aluminum particle can prevent escape and the reflection of light, so that more directing light directly enters solar cell, and the application cost of aluminum particulate is more much lower than noble metal; So use the Core Superiority of nano aluminum particle to be at solar cell: the firstth, the light acquisition performance of nano aluminum particle is stronger, can significantly improve electricity conversion, the secondth, the production cost of reduction solar cell, and the market competitiveness of enhancing solar cell, make solar cell become lighter and thinner more efficient, have stronger Research Significance and commercial value; In addition, the nano aluminum particle can be used as the solid fuel propelling agent because of its special combustion-supporting performance, is widely used in national defence and aerospace field.
From present nano aluminum particle technology of preparing, as main take physical method, mechanical friction block materials, evaporative condenser and template type electrochemical deposition etc., principle is evaporation block aluminium when nearly boiling temperature, the condensation that continues, the evaporation thermal source is from high frequency electric source, laser, direct current-arc plasma heating, electrical explosion etc.; Find by analyzing, Physical prepares the problem that there be " nearly boiling point ultrahigh-temperature preparation, nano-particles size is large, particle size range is wide, preparation efficiency is lower " and " passivating process control difficulty is large; the aluminum particulate loss is serious " in the nano aluminum particle, therefore thinks: explore that chemical method prepares the nano aluminum particle when causing concern under the normal temperature; The method that prepare at present metal nanoparticle in the liquid phase is numerous, and chemical reduction method, microemulsion method, Radiation Synthesis Method etc. are arranged, but comprehensive at present document sees, domestic and international report about Liquid preparation methods nano aluminum particle seldom.
Ghanta used lithium aluminium hydride reduction AlCl in the Three methyl Benzene solution of polyvinylpyrrolidone or methyl methacrylate is arranged in 2010
3Prepare the nano aluminum particle, 165 ℃ of sustained reactions 24 hours are being arranged when stirring, prepared the matrix material of different al/polymer ratio by liquid phase synthesizing method; Main Problems is: long reaction time, the nanoparticle range scale 47-158nm for preparing, there is the problem that yardstick is large and particle size range is wide, also affect the stable performance of particle, and have non-spherical particle to occur in resultant, it is unfavorable that the disunity of pattern and size is brought into play its functional performance to the nano aluminum particle.
Prepare the weak point that exists in the nano aluminum particle for existing chemical method, the present invention is take the application demand of nano aluminum particle on solar cell as foundation, take " high-level efficiency, high-performance, low cost, the low pollution " of fabrication of new materials as governing principle, provide a kind of hyperbranched polymer as solvent, dispersion agent and reductive agent, by " Transfer Radical Polymerization " preparation nano aluminum particle, particle has the nucleocapsid structure of polymer overmold at normal temperatures; On the product feature, the preparation major requirement of metal nanoparticle is: (1) particle surface cleaning; (2) particle shape, particle diameter and size-grade distribution can be controlled, and the particle aggregation tendency is little; (3) collect easily, preferably thermostability is arranged, easily preserve; (4) production efficiency is high, and productive rate, output are large, wherein control particle size and enhance productivity and productive rate significant, the invention is intended in this.
Moreover, chemical reaction has higher speed and productive rate is the essential condition that a kind of technique realizes industrialization, development trend from the material preparation, suitable physical field is introduced reaction system and positive to interfere reaction process be effective, also be to improve and improve the functional important channel of novel material, at present, applicable physical field has electromagnetic field, electric field and ultrasonic field and the coupled field thereof etc. of varying strength; Wherein magnetic field is and temperature, the same important physical parameter of pressure, especially, high-intensity magnetic field is as the particular electrical magnetic field form under a kind of extreme condition, high-intensity energy contactlessly can be delivered to the atomic scale of material, change the behaviors such as arrangement, coupling and migration of atom and molecule, thereby tissue and performance to material produce huge and deep effect, high-intensity magnetic field processing has become a kind of important technical of development of new material, in solid state physics and condensed state physics tremendous development is arranged; In the organic materials preparation field, impulse magnetic field can change the motor behavior of compound electronics, activity and life-span to free radical, ion have a great impact, thereby can improve the activity and selectivity of reactant, regulation and control chemical reaction and polymerization process, can bring out the physicochemical change that can't realize under the general condition, or the physicochemical change that can carry out under the acceleration general condition.
Summary of the invention
Content of the present invention: be as raw material with a kind of hyperbranched polymer and trivalent aluminium ion solution, in the aqueous solution, prepare the core-shell material of homodisperse " over-expense compound parcel nano aluminum particle ", after reaction system is placed strong magnetic field circumstance, controlling magnetic field intensity and the action of a magnetic field time, can improve speed of reaction and productive rate.
The objective of the invention is to be achieved through the following technical solutions:
By " hydrophobicity hyperbranched polyether " and " poly-diethylamide ylmethyl ethyl propenoate " synthetic a kind of hyperbranched polymer, the solvent during as reduction reaction, reductive agent and dispersion agent; The concrete building-up process of this polymkeric substance is: select the brominated hyperbranched polyether of hydrophobicity of degree of branching 20-40% as macromole evocating agent, select cupric bromide as catalyzer, select the hexamethyl Triethylenetetramine (TETA) as many nitrogen ligands; Brominated hyperbranched polyether and cupric bromide are put into the dry reaction tube of crossing, with syringe in vitro injecting tetrahydrofuran (THF), as the middle grade solvent, the add-on of tetrahydrofuran (THF) is as the criterion to guarantee that brominated hyperbranched polyether dissolves therein fully, dropwise inject the hexamethyl Triethylenetetramine (TETA) again until behind the solution becomes au bleu, dropwise inject poly-diethylamide ylmethyl ethyl propenoate; The control solution temperature is between 65-75 ℃ the time, react between the reactant until reach certain viscosity, when at the uniform velocity rocking test tube, compare with the aqueous solution, solution has the hysteresis of flowing, and wall cling phenomenon occurs and be as the criterion, show that reaction finishes, stop to inject poly-diethylamide ylmethyl ethyl propenoate; After reaction finishes, dilute with tetrahydrofuran (THF) further, when at the uniform velocity rocking test tube, the free-flowing without lagging behind that the conventional aqueous solution occurs gets final product, with solution by as the solid-state alkali alumina of siccative to remove the cupric bromide as catalyzer, and in hexane, precipitate, namely obtain required " starlike-the hydrophobicity hyperbranched polyether-polymerization diethylamide ylmethyl ethyl propenoate " hyperbranched polymer, hereinafter to be referred as " hyperbranched polymer or polymkeric substance ".
Described certain viscosity refers to that viscosity number is 0.18-0.22 Pas.
Described viscosity with solution after the tetrahydrofuran (THF) dilution is 0.08-0.12 Pas.
Then in being 1 hydrochloric acid soln, the pH value dissolves hyperbranched polymer, adjust pH value to proper level 8.5 ~ 9 with NaOH solution, can avoid this moment the self-assembly of polymer billet to reunite, and numerical values recited does not affect reaction efficiency and product feature in this scope, dropwise add the trivalent aluminium ion solution of 0.5mol/L ~ 1 mol/L in the solution, polymer concentration is at 1 mg/mL ~ 2 mg/mL in the control solution, after at room temperature mixing solutions being stirred, insert the high-intensity magnetic field generating unit, and regulation and control high-intensity magnetic field magnetic induction density and the action of a magnetic field time, magnetic induction density is set as 2 ~ 40 T, be 5 ~ 40 ms the action time of a pulse, and applying pulse number is 5 ~ 30; After having applied emp, magnetic field treatment finishes; Magnetic field treatment places normal temperature air with solution after finishing, and leaves standstill until react end.
The described reaction times inserts the high-intensity magnetic field generating unit from solution and begins to count, and the reaction times is controlled at 200-250min, and time of repose is the reaction times to deduct the time that has applied emp.
Described trivalent aluminium ion solution is AlCl
3, Al
2(SO
4)
3Or NaAlO
2Solution.
Because the capacitor charging process is arranged, so that pulse applies is discontinuous; And according to the magnetic field means feature, the recurrent interval is relevant with magnetic induction density, and magnetic induction density is larger, and the recurrent interval is larger; The action of a magnetic field has improved Al
3+The reactive behavior of ion and hyperbranched polymer has improved reduction reaction rate, impels the nano aluminum rates of particles to increase, and on the product feature, the particle size range that generates the nano aluminum particle is 1-10nm, and the size distribution interval is narrow; Particle disperses in solution and is stable, does not reunite, and extracts easily.
After preparation finishes, extract the nucleocapsid structure particle in the solution, can directly be used as the solid rocket fuel propelling agent; Also can be placed on the atmosphere kiln roasting, control furnace atmosphere, maturing temperature and roasting time are overspend the carbon coating that compound is transformed into conduction with coating, form the coated nano aluminum particulate material of carbon; Prepared material can deposit on the thin-film solar cells, is used for improving the photoelectric conversion performance.
Compare with other documents, preparation technology's advantage of nano aluminum particle provided by the invention be mainly reflected in following some:
(1) the aluminum particulate size is tiny, and size range is 1 ~ 10 nm, and the size-grade distribution interval is narrow;
(2) aluminum particulate disperses in solution, does not reunite, and good stability easily extracts;
(3) finish experiment under the normal temperature, do not need the high temperature energy consumption;
(4) apply high-intensity magnetic field in short-term after, reduction efficiency and productive rate improve synchronously.
Description of drawings
When Fig. 1 is 2T, 30 pulses, 245min, use AlCl
3Quantity and pattern with hyperbranched polymer reduction preparation nano aluminum particle;
When Fig. 2 is 20T, 20 pulses, 225min, use Al
2(SO
4)
3Quantity and pattern with hyperbranched polymer reduction preparation nano aluminum particle;
When Fig. 3 is 40T, 5 pulses, 200min, use NaAlO
2Quantity and pattern with hyperbranched polymer reduction preparation nano aluminum particle.
Embodiment
The invention will be further elaborated below in conjunction with embodiment, and embodiment only is used for explanation the present invention, rather than limits by any way the present invention.
Embodiment one
Synthesis of super branched polymkeric substance: select the brominated hyperbranched polyether of hydrophobicity of the degree of branching 20% as macromole evocating agent, select cupric bromide as catalyzer, select the hexamethyl Triethylenetetramine (TETA) as many nitrogen ligands; Brominated hyperbranched polyether and cupric bromide are put into the dry reaction tube of crossing, with syringe in vitro injecting tetrahydrofuran (THF), as the middle grade solvent, the add-on of tetrahydrofuran (THF) is as the criterion to guarantee that brominated hyperbranched polyether dissolves therein fully, dropwise inject the hexamethyl Triethylenetetramine (TETA) again until behind the solution becomes au bleu, dropwise inject poly-diethylamide ylmethyl ethyl propenoate; The control solution temperature is between 65 ℃ the time, reacts between the reactant until to reach the viscosity of solution be 0.18Pas, stops to inject poly-diethylamide ylmethyl ethyl propenoate; After reaction finishes, with tetrahydrofuran (THF) dilution, the viscosity of solution is 0.08 Pas after the dilution further, with solution by as the solid-state alkali alumina of siccative to remove the cupric bromide as catalyzer, and in hexane, precipitate, namely obtain needed hyperbranched polymer.
Dissolve hyperbranched polymer in the HCl of pH=1 solution, the NaOH solution of usefulness is adjusted pH value to 8.5, with the AlCl of concentration 0.5mol/L
3Solution dropwise adds, the regulation and control polymer concentration is at 1mg/mL, after at room temperature solution being stirred, insert the high-intensity magnetic field generating unit, magnetic induction density is set as 2T, be 50ms the action time of a pulse, apply altogether 30 pulses (because process of charging is arranged, so pulse applies discontinuous), after magnetic field treatment finishes, take out test tube and place normal temperature air, leave standstill until the reaction times reaches rear end preparation process.
The particle size range that generates the nano aluminum particle is 1-10nm, and the size distribution interval is narrow; Particle disperses in solution and is stable, does not reunite, and extracts easily.
When not adding magnetic field, the time of finishing reduction reaction is 350min, apply the magnetic field of above-mentioned intensity and time after, the reaction times shortens to 245min, speed of reaction improves 30%; Increasing 10%(when the nano aluminum number of particles does not add magnetic field demarcates by weighing).
Embodiment two
Synthesis of super branched polymkeric substance: select the brominated hyperbranched polyether of hydrophobicity of the degree of branching 30% as macromole evocating agent, select cupric bromide as catalyzer, select the hexamethyl Triethylenetetramine (TETA) as many nitrogen ligands; Brominated hyperbranched polyether and cupric bromide are put into the dry reaction tube of crossing, with syringe in vitro injecting tetrahydrofuran (THF), as the middle grade solvent, the add-on of tetrahydrofuran (THF) is as the criterion to guarantee that brominated hyperbranched polyether dissolves therein fully, dropwise inject the hexamethyl Triethylenetetramine (TETA) again until behind the solution becomes au bleu, dropwise inject poly-diethylamide ylmethyl ethyl propenoate; The control solution temperature is between 70 ℃ the time, reacts between the reactant until to reach the viscosity of solution be 0.20Pas, stops to inject poly-diethylamide ylmethyl ethyl propenoate; After reaction finishes, with tetrahydrofuran (THF) dilution, the viscosity of solution is 0.10 Pas after the dilution further, with solution by as the solid-state alkali alumina of siccative to remove the cupric bromide as catalyzer, and in hexane, precipitate, namely obtain needed hyperbranched polymer.
In the HCl of pH=1 solution, dissolve hyperbranched polymer, adjust pH value to 8.8 with NaOH solution, with the Al of concentration 0.7 mol/L
2(SO
4)
3Solution dropwise adds, the regulation and control polymer concentration reaches 1.5 mg/mL, after at room temperature solution being stirred, insert the high-intensity magnetic field generating unit, magnetic induction density is set as 20T, be 20ms the action time of a pulse, apply altogether 10 pulses (because process of charging is arranged, so pulse applies discontinuous), after magnetic field treatment finishes, take out test tube and place normal temperature air, leave standstill until the reaction times reaches rear end preparation process.
The particle size range that generates the nano aluminum particle is 1-10nm, and the size distribution interval is narrow; Particle disperses in solution and is stable, does not reunite, and extracts easily.
When not adding magnetic field, the time of finishing reduction reaction is 300min, apply the magnetic field of above-mentioned intensity and time after, the reaction times shortens to 225min, speed of reaction improves 25%; Increasing 15%(when the nano aluminum number of particles does not add magnetic field demarcates by weighing).
Embodiment three
Synthesis of super branched polymkeric substance: select the brominated hyperbranched polyether of hydrophobicity of the degree of branching 40% as macromole evocating agent, select cupric bromide as catalyzer, select the hexamethyl Triethylenetetramine (TETA) as many nitrogen ligands; Brominated hyperbranched polyether and cupric bromide are put into the dry reaction tube of crossing, with syringe in vitro injecting tetrahydrofuran (THF), as the middle grade solvent, the add-on of tetrahydrofuran (THF) is as the criterion to guarantee that brominated hyperbranched polyether dissolves therein fully, dropwise inject the hexamethyl Triethylenetetramine (TETA) again until behind the solution becomes au bleu, dropwise inject poly-diethylamide ylmethyl ethyl propenoate; The control solution temperature is between 75 ℃ the time, reacts between the reactant until to reach the viscosity of solution be 0.22Pas, stops to inject poly-diethylamide ylmethyl ethyl propenoate; After reaction finishes, with tetrahydrofuran (THF) dilution, the viscosity of solution is 0.12Pas after the dilution further, with solution by as the solid-state alkali alumina of siccative to remove the cupric bromide as catalyzer, and in hexane, precipitate, namely obtain needed hyperbranched polymer.
In the HCl of pH=1 solution, dissolve hyperbranched polymer, adjust pH value to 9 with NaOH solution, with the NaAlO of concentration 1 mol/L
2Solution dropwise adds, the regulation and control polymer concentration reaches 2 mg/mL, after at room temperature solution being stirred, insert the high-intensity magnetic field generating unit, magnetic induction density is set as 40T, be 40ms the action time of a pulse, applies altogether 5 pulses (because process of charging is arranged, so pulse applies discontinuous); Take out test tube after burst process finishes, take out test tube and place normal temperature air, leave standstill until the reaction times reaches rear end preparation process.
The particle size range that generates the nano aluminum particle is 1-10nm, and the size distribution interval is narrow; Particle disperses in solution and is stable, does not reunite, and extracts easily.
When not adding magnetic field, the time of finishing reduction reaction is 250min, apply the magnetic field of above-mentioned intensity and time after, the reaction times shortens to 200min, speed of reaction improves 20%; When adding magnetic field, the nano aluminum number of particles do not increase by 20%.
Claims (4)
1. the high-efficiency synthesis method of a nano aluminum particle is characterized in that comprising the steps:
(1) preparation hyperbranched polymer: select the brominated hyperbranched polyether of hydrophobicity of degree of branching 20-40% as macromole evocating agent, select cupric bromide as catalyzer, select the hexamethyl Triethylenetetramine (TETA) as many nitrogen ligands; Brominated hyperbranched polyether and cupric bromide are put into the dry reaction tube of crossing, with syringe in vitro injecting tetrahydrofuran (THF), as the middle grade solvent, the add-on of tetrahydrofuran (THF) is as the criterion to guarantee that brominated hyperbranched polyether dissolves therein fully, dropwise inject the hexamethyl Triethylenetetramine (TETA) again until behind the solution becomes au bleu, dropwise inject poly-diethylamide ylmethyl ethyl propenoate; The control solution temperature is between 65-75 ℃ the time, react between the reactant until reach certain viscosity, when at the uniform velocity rocking test tube, compare with the aqueous solution, solution has the hysteresis of flowing, and wall cling phenomenon occurs and be as the criterion, show that reaction finishes, stop to inject poly-diethylamide ylmethyl ethyl propenoate; After reaction finishes, dilute with tetrahydrofuran (THF) further, when at the uniform velocity rocking test tube, the free-flowing without lagging behind that the conventional aqueous solution occurs gets final product, with solution by as the solid-state alkali alumina of siccative to remove the cupric bromide as catalyzer, and in hexane, precipitate, namely obtain required " starlike-the hydrophobicity hyperbranched polyether-polymerization diethylamide ylmethyl ethyl propenoate " hyperbranched polymer;
(2) obtain solution, finish reaction: in the pH value is 1 hydrochloric acid soln, dissolve hyperbranched polymer, adjust pH value to proper level 8.5 ~ 9 with NaOH solution, dropwise add the trivalent aluminium ion solution of 0.5mol/L ~ 1 mol/L in the solution, polymer concentration is at 1 mg/mL ~ 2 mg/mL in the control solution, after at room temperature mixing solutions being stirred, insert the high-intensity magnetic field generating unit, and regulation and control high-intensity magnetic field magnetic induction density and the action of a magnetic field time, magnetic induction density is set as 2 ~ 40 T, be 5 ~ 40 ms the action time of a pulse, and applying pulse number is 5 ~ 30; After having applied emp, magnetic field treatment finishes; Magnetic field treatment places normal temperature air with solution after finishing, and leaves standstill until react end; The described reaction times inserts the high-intensity magnetic field generating unit from solution and begins to count, and the reaction times is controlled at 200-250min, and time of repose is the reaction times to deduct the time that has applied emp.
2. the high-efficiency synthesis method of a kind of nano aluminum particle as claimed in claim 1, it is characterized in that: described certain viscosity refers to that viscosity number is 0.18-0.22 Pas.
3. the high-efficiency synthesis method of a kind of nano aluminum particle as claimed in claim 1 is characterized in that: described viscosity with solution after the tetrahydrofuran (THF) dilution is 0.08-0.12 Pas.
4. the high-efficiency synthesis method of a kind of nano aluminum particle as claimed in claim 1, it is characterized in that: described trivalent aluminium ion solution is AlCl
3, Al
2(SO
4)
3Or NaAlO
2Solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109834289A (en) * | 2017-11-24 | 2019-06-04 | 阜阳师范学院 | A kind of preparation method of nanometer aluminium powder |
| CN109834288A (en) * | 2017-11-24 | 2019-06-04 | 阜阳师范学院 | A kind of preparation method of the uniform nanometer aluminium powder of particle diameter distribution |
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| CN101654284A (en) * | 2009-09-04 | 2010-02-24 | 上海交通大学 | Preparation method of magnetic ferroferric oxide nanocrystal |
| CN101871089A (en) * | 2009-04-22 | 2010-10-27 | 中国科学院半导体研究所 | Method for preparing ordered aluminum nanoparticles |
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| US20070259437A1 (en) * | 2005-12-14 | 2007-11-08 | Oxonica, Inc. | Nanoparticulate Chemical Sensors Using SERS |
| CN101053907A (en) * | 2006-04-10 | 2007-10-17 | 辽宁师范大学 | Method for preparing nanometer size aluminium powder |
| CN101871089A (en) * | 2009-04-22 | 2010-10-27 | 中国科学院半导体研究所 | Method for preparing ordered aluminum nanoparticles |
| CN101654284A (en) * | 2009-09-04 | 2010-02-24 | 上海交通大学 | Preparation method of magnetic ferroferric oxide nanocrystal |
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| CN109834289A (en) * | 2017-11-24 | 2019-06-04 | 阜阳师范学院 | A kind of preparation method of nanometer aluminium powder |
| CN109834288A (en) * | 2017-11-24 | 2019-06-04 | 阜阳师范学院 | A kind of preparation method of the uniform nanometer aluminium powder of particle diameter distribution |
| CN109834288B (en) * | 2017-11-24 | 2022-04-29 | 阜阳师范学院 | Preparation method of nano aluminum powder with uniform particle size distribution |
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