CN104477977B - The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder - Google Patents
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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- C01—INORGANIC CHEMISTRY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to the synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, comprises the following steps: (1) mixes dysprosia, titanium oxide and alkali metal salt ball milling, obtains mixed powder; (2) by dry step (1) gained mixed powder 6～10h; (3) after the material of the dry gained of step (2) is ground, pre-molding; (4) material after step (3) pre-molding is warming up to 800 DEG C～1400 DEG C, insulation calcining 1～4h; (5) washing, dry: the material after the calcining of step (4) gained is ground, then with deionized water washing, filter, by solid drying, to obtain final product. Invention is synthesized Dy by molten-salt growth method2TiO5Powder, compares with sol-gel technology, and without gel process, technique is simple, aggregate velocity is fast, production cost is low; The powder crystal grain that makes is little, size uniform, good dispersion, without crystal grain adhesion agglomeration.
Description
Technical field
The present invention relates to Dy2TiO5The preparation method of powder, is specifically related to the synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, belongs to field of inorganic nonmetallic material.
Background technology
Rare earth titanium hydrochlorate has higher initial thermal neutron absorbability and unique neutron-absorbing efficiency, has good anti-radiation performance, and its fusing point is high, coefficient of thermal expansion is little. In the core industry of present stage, main use is rich in10The materials such as the boron carbide of B are as command bundle rods for nuclear reactors and shielding protection material, this be mainly due to10B has high thermal neutron absorption cross section, but due to10B, being subject to, after irradiation, (n, α) reaction to occur, produces swelling, affects the stability of its use, causes shorten its service life; And the lanthanide oxide base pottery of fluorite structure shows good resistance to radiation damage, the safe operation in Muscovite MIR reactor of control rod of wherein preparing with metatitanic acid dysprosium pottery, since nineteen ninety-five, metatitanic acid dysprosium pottery has been applied to Russian VVER-1000 nuclear power generating sets (VDRisovany, EEVarlashova, DNSuslov, Dysprosiumtitanateasanabsorbermaterialforcontrolrods, J.Nucl.Mater., 2000,281:84-89). Metatitanic acid dysprosium pottery has does not emit gas and process does not produce the advantages such as radwaste after neutron irradiation, is the extremely potential neutron absorber material of one and command bundle rods for nuclear reactors material. As the Dy of the high neutron absorption efficiency of preparation2TiO5The raw material of pottery, Dy2TiO5Powder should have the features such as high-purity, epigranular, favorable dispersibility, therefore, and Dy2TiO5The preparation research of powder is significant.
The people such as AmitSinha are with Dy2O3，TiO2For raw material, with MoO3For stabilizing agent, adopt solid phase method to synthesize Dy2TiO5Powder (Developmentofdysprosiumtitanatebasedceramics, J.Am.Ceram.Soc., 2005,88[4]: 1064-1066). The people such as ChoongHwanJung are with Dy2O3，TiO2For raw material, with MoO3For stabilizing agent, adopt sol-gel process synthesis technique to synthesize Dy2TiO5Powder, (SynthesisandsinteringstudiesonDy2TiO5Preparedbypolymercarrierchemicalprocess, J.Nucl.Mater., 2006,354:137-142). But said method all comes with some shortcomings, such as: in solid phase method synthetic powder process, required calcining heat is high, and the powder reuniting phenomenon of preparing is serious, coarse grains, and sintering activity is low; In sol-gel synthesis powder process, reaction required time is long, yields poorly, and production efficiency is low, in a large amount of preparation process, need to consume large amount of organic, contaminated environment.
Molten-salt growth method, as preparing oxide ceramic powder body new technology, can reduce synthesis temperature, and Reaction time shorten to a certain extent; In the process of molten-salt growth method synthesizing inorganic powder, fused-salt medium between the particle of product, has stoped between product particle and has reunited all the time, makes the powder obtaining have good dispersiveness; Molten-salt growth method can be controlled the shape and size of powder product crystal grain effectively; By changing kind and the consumption of fused salt, the reaction temperature of system, reaction time and additive add the pattern that can effectively control molten-salt growth method synthesized crystal. In addition, utilize molten-salt growth method to be conducive to remove the impurity in product, obtain the advantages such as highly purified product has rapidly and efficiently, energy-conserving and environment-protective.
Summary of the invention
For the deficiencies in the prior art, the invention provides the synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, the method technique is simple, production cost is low, manufacturing cycle is short, and prepared product grains size uniform, dispersion effect are good.
Technical solution of the present invention is as follows:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, taking dysprosia, titanium oxide as raw material, taking alkali metal salt as fused-salt medium, the method comprises the following steps:
(1) batch mixing: dysprosia, titanium oxide and alkali metal salt ball milling are mixed, obtain mixed powder;
Described dysprosia: titanium oxide is 1:(0.8～1.2 in molar ratio) batching, described alkali metal salt: the mass ratio of (dysprosia+titanium oxide) is (0.5～3): 1;
(2) dry: by step (1) gained mixed powder dry 6～10h at 60～100 DEG C;
(3) pre-molding: after the material of the dry gained of step (2) is ground, pre-molding;
(4) calcining: the material after step (3) pre-molding is warming up to 800 DEG C～1400 DEG C by the heating rate of 3～7 DEG C/min from room temperature, insulation calcining 1～4h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, then with deionized water washing, filter, by solid dry 6～10h at 60～100 DEG C, obtain Dy2TiO5Powder.
According to the present invention, preferred, the dysprosia described in step (1) is Dy2O3, described titanium oxide is TiO2, described alkali metal salt is NaCl, KCl or/and LiCl, and ball-milling medium is absolute ethyl alcohol;
Preferably, described dysprosia: titanium oxide is 1:1 batching in molar ratio, described alkali metal salt: the mass ratio of (dysprosia+titanium oxide) is (0.5～1.5): 1.
According to the present invention, preferred, in step (3), the pressure of pre-molding is 50～200Mpa. Pre-molding, to combine closely between maintenance fused salt and raw material, promotes the carrying out of reaction.
According to the present invention, preferred, in step (4), calcining heat is 1150～1250 DEG C.
According to the present invention, preferred, while washing by deionized water in step (5), material is carried out to ultrasonic processing simultaneously. Ultrasonic processing can promote the dissolving of alkali metal salt, and improves the dispersiveness of powder.
Beneficial effect of the present invention:
1, the present invention synthesizes Dy by molten-salt growth method2TiO5Powder, compares with sol-gel technology, and without gel process, technique is simple, aggregate velocity is fast, production cost is low; Be conducive to the dispersiveness of crystal grain thinning and raising powder; Gained Dy of the present invention2TiO5Powder average grain diameter 2～3 μ m.
2, the present invention adopts molten-salt growth method, and fused salt can reuse after cleaning, and reduce production costs, and the powder crystal grain making is little, size uniform, good dispersion, without crystal grain adhesion agglomeration.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of the embodiment of the present invention 1 prepared sample.
Fig. 2 is the SEM photo of the embodiment of the present invention 1 prepared sample.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described further, but institute of the present invention protection domain is not limited to this.
Raw materials usedly in embodiment be conventional raw material, device therefor is conventional equipment, commercial product.
In embodiment, ball-milling medium is absolute ethyl alcohol.
Embodiment 1:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, step is as follows:
(1) batch mixing: take 41gDy2O3、9gTiO2, 75gNaCl, by Dy2O3、TiO2Be placed in high-speed mixing ball mill with NaCl and mix, obtain mixed powder; Dy in powder2O3：TiO2Mol ratio is 1:1, NaCl quality and Dy2O3、TiO2Total mass ratio is 1.5:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven to forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of the dry gained of step (2) is placed in to mortar, after grinding, is pre-molding under 50MPa at pressure;
(4) calcining: the material after step (3) pre-molding is placed in batch-type furnace, is warming up to 1200 DEG C with the heating rate of 5 DEG C/min from room temperature, insulation calcining 1h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, after powder after grinding washs by deionized water in ultrasonic machine, standing or suction filtration removes supernatant, carry out after 3～5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy2TiO5Powder.
The Dy that the present embodiment is prepared2TiO5Powder test X ray diffracting spectrum and SEM photo, as shown in Figure 1, 2.
As shown in Figure 1, the powder product obtaining is Dy2TiO5Powder. As shown in Figure 2, the Dy obtaining2TiO5The average grain diameter of powder approximately 2～3 μ m, particle diameter is evenly distributed, and good dispersion, without crystal grain adhesion agglomeration.
Embodiment 2:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, step is as follows:
(1) batch mixing: take 41gDy2O3、9gTiO2, 100gNaCl, by Dy2O3、TiO2Be placed in high-speed mixing ball mill with NaCl and mix, obtain mixed powder; Dy in powder2O3:TiO2Mol ratio is 1:1, NaCl quality and Dy2O3、TiO2Total mass ratio is the raw material of 2:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven to forced air drying 10h at 80 DEG C;
(3) pre-molding: dry step (2) gained material is placed in to mortar, after grinding, is pre-molding under 150MPa at pressure;
(4) calcining: the material after step (3) pre-molding is placed in batch-type furnace, is warming up to 1150 DEG C with the heating rate of 5 DEG C/min from room temperature, insulation calcining 2h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, after powder after grinding washs by deionized water in ultrasonic machine, standing or suction filtration removes supernatant, carry out after 3～5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy2TiO5Powder.
Embodiment 3:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, step is as follows:
(1) batch mixing: take 41gDy2O3、9gTiO2, 50gKCl, by Dy2O3、TiO2Be placed in high-speed mixing ball mill with KCl and mix, obtain mixed powder; Dy in powder2O3:TiO2Mol ratio is 1:1, KCl quality and Dy2O3、TiO2Total mass ratio is the raw material of 1:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven to forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of the dry gained of step (2) is placed in to mortar, after grinding, is pre-molding under 100MPa at pressure;
(4) calcining: the material after step (3) pre-molding is placed in batch-type furnace, is warming up to 1250 DEG C with the heating rate of 5 DEG C/min from room temperature, insulation calcining 2h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, after powder after grinding washs by deionized water in ultrasonic machine, standing or suction filtration removes supernatant, carry out after 3～5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy2TiO5Powder.
Embodiment 4:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, step is as follows:
(1) batch mixing: take 41gDy2O3、9gTiO2, 50gLiCl, by Dy2O3、TiO2Be placed in high-speed mixing ball mill with LiCl and mix, obtain mixed powder; Dy in powder2O3:TiO2Mol ratio is 1:1, LiCl quality and Dy2O3、TiO2Total mass ratio is the raw material of 1:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven to forced air drying 10h at 80 DEG C;
(3) pre-molding: dry step (2) gained material is placed in to mortar, after grinding, is pre-molding under 150MPa at pressure;
(4) calcining: the material after step (3) pre-molding is placed in batch-type furnace, is warming up to 1250 DEG C with the heating rate of 3 DEG C/min from room temperature, insulation calcining 2h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, after powder after grinding washs by deionized water in ultrasonic machine, standing or suction filtration removes supernatant, carry out after 3～5 washings, gained powder is placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy2TiO5Powder.
Embodiment 5:
The synthetic Dy of a kind of molten-salt growth method2TiO5The method of powder, step is as follows:
(1) batch mixing: take 41gDy2O3、9gTiO2, 100gNaCl-KCl, NaCl-KCl mass ratio is 1:1, by Dy2O3、TiO2Be placed in high-speed mixing ball mill with NaCl-KCl and mix, obtain mixed powder; Dy in powder2O3:TiO2Mol ratio is 1:1, NaCl-KCl quality and Dy2O3、TiO2Total mass ratio is the raw material of 2:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven to forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of the dry gained of step (2) is placed in to mortar, after grinding, is pre-molding under 150MPa at pressure;
(4) calcining: the material after step (3) pre-molding is placed in batch-type furnace, is warming up to 1250 DEG C with the heating rate of 5 DEG C/min from room temperature, insulation calcining 2h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, after powder after grinding washs by deionized water in ultrasonic machine, standing or suction filtration removes supernatant, carry out after 3～5 washings, gained powder is placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy2TiO5Powder.
It should be noted that, what more than enumerate is only several specific embodiments of the present invention, and obviously the present invention is not limited only to above embodiment, can also have other distortion. Those skilled in the art directly derives or all distortion of amplification indirectly from the disclosure of invention, all should think protection scope of the present invention.
Claims (6)
1. the synthetic Dy of molten-salt growth method2TiO5The method of powder, taking dysprosia, titanium oxide as raw material, is situated between taking alkali metal salt as fused saltMatter, the method comprises the following steps:
(1) batch mixing: dysprosia, titanium oxide and alkali metal salt ball milling are mixed, obtain mixed powder;
Described dysprosia: titanium oxide is 1:(0.8 ~ 1.2 in molar ratio) batching, described alkali metal salt: the matter of (dysprosia+titanium oxide)Amount is than being (0.5 ~ 3): 1;
(2) dry: by step (1) gained mixed powder dry 6 ~ 10h at 60 ~ 100 DEG C;
(3) pre-molding: after the material of the dry gained of step (2) is ground, pre-molding;
(4) calcining: by the material after step (3) pre-molding by the heating rate of 3 ~ 7 DEG C/min from room temperature be warming up to 1150 ~1250 DEG C, insulation calcining 1 ~ 4h;
(5) washing, dry: the material after the calcining of step (4) gained is ground, then with deionized water washing, filter, solid is existedAt 60 ~ 100 DEG C, dry 6 ~ 10h, obtains Dy2TiO5Powder.
2. the synthetic Dy of molten-salt growth method according to claim 12TiO5The method of powder, is characterized in that, described in step (1)Dysprosia be Dy2O3, described titanium oxide is TiO2, described alkali metal salt is that NaCl, KCl are or/and LiCl.
3. the synthetic Dy of molten-salt growth method according to claim 12TiO5The method of powder, is characterized in that, described in step (1)Dysprosia: titanium oxide is 1:1 batching in molar ratio.
4. the synthetic Dy of molten-salt growth method according to claim 12TiO5The method of powder, is characterized in that, described in step (1)Alkali metal salt: the mass ratio of (dysprosia+titanium oxide) is (0.5 ~ 1.5): 1.
5. the synthetic Dy of molten-salt growth method according to claim 12TiO5The method of powder, is characterized in that, precompressed in step (3)The pressure of moulding is 50 ~ 200MPa.
6. the synthetic Dy of molten-salt growth method according to claim 12TiO5The method of powder, is characterized in that, step spends in (5)When ionized water washing, material is carried out to ultrasonic processing simultaneously.
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| CN105161144B (en) * | 2015-08-07 | 2017-09-08 | 厦门大学 | A kind of preparation method of nuclear reactor neutron absorber material metatitanic acid dysprosium pellet |
| CN107572573A (en) * | 2017-10-26 | 2018-01-12 | 贵州大学 | A kind of preparation method of the nano ceric oxide particle of polyhedral structure |
| CN107601546A (en) * | 2017-10-26 | 2018-01-19 | 贵州大学 | A kind of environment-friendly preparation method thereof of nano ceric oxide particle |
| CN112340777A (en) * | 2020-10-30 | 2021-02-09 | 中科立民新材料（扬州）有限公司 | Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate |
| CN113213916B (en) * | 2021-05-19 | 2022-02-11 | 山东大学 | Fluorite-structured dysprosium titanate reactor control rod and preparation method thereof |
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| CN102701273A (en) * | 2012-05-22 | 2012-10-03 | 山东大学 | Preparation method of nano dysprosium titanate powder |
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| CN102701273A (en) * | 2012-05-22 | 2012-10-03 | 山东大学 | Preparation method of nano dysprosium titanate powder |
Non-Patent Citations (3)
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| Ion-irradiation-induced structural transitions in orthorhombic Ln2TiO5;Jiaming Zhang et al.;《Acta Materialia》;20130430;第61卷;第4191-4199页 * |
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