CN116041052B - Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof - Google Patents
Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof Download PDFInfo
- Publication number
- CN116041052B CN116041052B CN202310035630.1A CN202310035630A CN116041052B CN 116041052 B CN116041052 B CN 116041052B CN 202310035630 A CN202310035630 A CN 202310035630A CN 116041052 B CN116041052 B CN 116041052B
- Authority
- CN
- China
- Prior art keywords
- lithium
- core
- powder
- lithium titanate
- orthosilicate
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000011258 core-shell material Substances 0.000 title claims abstract description 61
- 239000008188 pellet Substances 0.000 title claims abstract description 54
- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- ZYJNJMHGRZIEST-UHFFFAOYSA-N dilithium dihydroxy(dioxido)silane Chemical compound [Si]([O-])([O-])(O)O.[Li+].[Li+] ZYJNJMHGRZIEST-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 22
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 22
- 230000035755 proliferation Effects 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 91
- 239000002243 precursor Substances 0.000 claims abstract description 52
- 238000000498 ball milling Methods 0.000 claims abstract description 39
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 34
- YTZVWGRNMGHDJE-UHFFFAOYSA-N tetralithium;silicate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-][Si]([O-])([O-])[O-] YTZVWGRNMGHDJE-UHFFFAOYSA-N 0.000 claims abstract description 32
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 235000015895 biscuits Nutrition 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000853 adhesive Substances 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims abstract description 9
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 43
- 239000004677 Nylon Substances 0.000 claims description 24
- 229920001778 nylon Polymers 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- 229910010093 LiAlO Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 150000002641 lithium Chemical group 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21B—FUSION REACTORS
- G21B1/00—Thermonuclear fusion reactors
- G21B1/11—Details
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62818—Refractory metal oxides
- C04B35/62821—Titanium oxide
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
- C04B2235/3234—Titanates, not containing zirconia
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- General Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a lithium orthosilicate-lithium titanate core-shell structure ceramic pellet for tritium proliferation and a preparation method thereof, which adopts LiOH.H 2 O and H 2 SiO 3 Mechanically mixing raw materials, presintering, and performing heat treatment to obtain lithium orthosilicate precursor powder; by LiOH H 2 O and H 2 TiO 3 Mechanically mixing raw materials, presintering, and performing heat treatment to obtain lithium titanate precursor powder; mixing the precursor powder with PVB solution to obtain precursor powder coated with an adhesive; preparing PVB coated lithium orthosilicate precursor powder into a spherical inner core through ball milling granulation, and then adding PVB coated lithium titanate precursor powder for continuous rotary granulation until forming a core-shell structure biscuit pellet; finally, sintering to obtain the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet. The invention solves the problem of mismatching of sintering shrinkage rates of lithium orthosilicate and lithium titanate ceramics.
Description
Technical Field
The invention belongs to the technical field of fusion reactors, and particularly relates to a lithium orthosilicate-lithium titanate core-shell structure ceramic pellet for tritium proliferation and a preparation method thereof.
Background
Tritium breeder acts as a key material in the tritium-producing cladding of a nuclear fusion reactor and functions to react with neutrons to provide the tritium necessary for fuel recycling. Li (Li) 4 SiO 4 Tritium breeder is identified by chinese fusion engineering laboratory reactor (CFETR) as the first choice due to its high lithium atom density, low neutron activation characteristics and outstanding low temperature tritium release rate. However, li 4 SiO 4 Has strong water absorption tendency, and is easy to be combined with H 2 O reacts to form Li 2 SiO 3 And LiOH alike, making it difficult to maintain phase and structural stability in a wet environment, presenting challenges to the storage, transfer and loading of the material. Therefore, new ideas and new methods are introduced into Li 4 SiO 4 Improving the moisture stability and mechanical property of the lithium ion battery to obtain the lithium ion battery Li 4 SiO 4 Important problems to be solved in the application process of tritium breeder are urgent. At present, for Li at home and abroad 4 The modification research of SiO4 tritium breeder mainly includes the following three types: (1) by doping TiO 2 、SiO 2 And ZrO(s) 2 The oxides are used for enhancing the mechanical property, but the method has very limited improved crushing strength and still needs to be further improved and Li is doped 2 O can even promote abnormal growth of grains; (2) direct Li incorporation 2 TiO 3 And LiAlO 2 The tritium proliferation material is used as a second phase and forms a complex phase ceramic structure, so that the performance complementation of a plurality of tritium proliferation agents can be formed while the grain growth is inhibited and the mechanical property is enhanced; (3) research on novel tritium proliferation ceramic materials. Researchers based on Li 4 SiO 4 And Li (lithium) 2 TiO 3 Diffusion performance difference during sintering, 50% Li is sintered at high temperature 2 TiO 3 -50％Li 4 SiO 4 When the ceramic microsphere is proliferated by the complex phase tritium, the complex phase ceramic microsphere with core-shell structure is obtained (the shell is Li) 2 TiO 3 The core is 50% Li 2 TiO 3 -50％Li 4 SiO 4 ) The special complex phase checkThe shell structure may significantly improve crush strength. Meanwhile, compared with the traditional composite material, the core-shell structure has the congenital advantage, and the stable shell structure can protect the inner core from the influence of factors such as the humidity environment outside the shell. However, from the viewpoint of the overall lithium density, the amount of the second phase material added to the composite ceramic is too high (Li 2 TiO 3 Up to 50%) sacrifice of Li 4 SiO 4 And thus impair the tritium proliferation ratio. On the basis, if pure-phase Li can be prepared 4 SiO 4 Inner core and pure phase Li 2 TiO 3 The core-shell structured lithium ceramic pellet with the shell layer has important significance for the development of the tritium proliferation field. However, li 4 SiO 4 And Li (lithium) 2 TiO 3 The crystal structure, the grain size, the sintering activity, the sintering temperature and the like of the ceramic material have larger differences, so that the two substances are difficult to keep consistent shrinkage rate in the high-temperature sintering process, and a larger challenge is brought to the stable preparation of the ceramic material with the core-shell structure. At present, no Li exists at home and abroad 4 SiO 4 -Li 2 TiO 3 Tritium proliferation ceramic pellet with core-shell structure (core: pure phase Li) 4 SiO 4 And (3) a shell: pure phase Li 2 TiO 3 ) Report of successful preparation.
Based on the above, the invention proposes to control Li after rotary granulation molding by using a powder presintering process 4 SiO 4 Inner core and Li 2 TiO 3 The sintering shrinkage of the shell biscuit is matched with the shrinkage of the core/shell structure by combining with the adjustment of sintering process parameters, and the purposes of designing and preparing Li with compact core-shell combination and controllable shell thickness are to 4 SiO 4 -Li 2 TiO 3 Ceramic pellets of core-shell structure.
Disclosure of Invention
The invention aims to overcome Li 4 SiO 4 And Li (lithium) 2 TiO 3 The ceramic sintering shrinkage rate is not matched, and Li with simple process is provided 4 SiO 4 -Li 2 TiO 3 Preparation method of ceramic pellets with core-shell structure, wherein Li is as follows 4 SiO 4 -Li 2 TiO 3 Core-shell structure ceramic pellet shell thickness is controllable, operabilityStrong.
The preparation method of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet for tritium proliferation comprises the following steps:
(1) Synthesis of lithium orthosilicate precursor powder
By LiOH H 2 O powder and H 2 SiO 3 The powder is used as a raw material, the raw material powder is added into a nylon ball milling tank according to the mol ratio of 4:1, deionized water and agate balls are added into the nylon ball milling tank, and mechanical ball milling mixing is carried out;
transferring the mixed suspension into a blast drying oven, preserving heat for 10-24 hours at 80-110 ℃, transferring into a muffle furnace, adjusting a furnace body heater to 400-500 ℃ for powder pre-sintering heat treatment, and preserving heat for 1-2 hours;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium orthosilicate precursor powder.
(2) Synthesis of lithium titanate precursor powder
By LiOH H 2 O powder and H 2 TiO 3 Adding the raw materials into a nylon ball milling tank according to the molar ratio of 2:1, adding deionized water and agate balls into the nylon ball milling tank, and mechanically ball milling and mixing;
transferring the mixed suspension into a blast drying oven, preserving heat for 10-24 hours at 80-110 ℃, transferring into a muffle furnace, adjusting a furnace body heater to 600-700 ℃ for powder pre-sintering heat treatment, and preserving heat for 3-4 hours;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium titanate precursor powder.
(3) Adhesive coating
Dissolving polyvinyl butyral (PVB) powder in absolute ethyl alcohol at 50 ℃, and magnetically stirring for 4-6 hours to obtain a polyvinyl butyral solution;
fully mixing PVB solution and lithium orthosilicate precursor powder prepared in the step (1) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat for 10-24 hours at 80-110 ℃ to finally obtain PVB coated lithium orthosilicate precursor powder;
fully mixing PVB solution and the lithium titanate precursor powder prepared in the step (2) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat for 10-24 hours at 80-110 ℃ to finally obtain the PVB lithium titanate precursor powder coated;
the adding amount of the PVB powder is 0.5% -1% of the mass of the precursor powder prepared in the step (1) and the step (2) respectively.
(4) Preparation of core-shell structured pellet biscuit
According to different requirements of the yield, adding the PVB coated lithium orthosilicate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 1-3 hours at a rotating speed of 160-200rads by a planetary ball mill to obtain a plurality of spherical lithium orthosilicate biscuits with diameters of 1.0-1.4 mm;
continuously adding the PVB-coated lithium titanate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 2-4 hours at the rotating speed of 200-220rads by a planetary ball mill to obtain a plurality of lithium orthosilicate-lithium titanate core-shell structure biscuit pellets with the diameter of 1.2-1.6 mm.
(5) High temperature sintering
Placing the lithium orthosilicate-lithium titanate core-shell structure biscuit pellets into a muffle furnace, heating to 500 ℃ at the heating rate of 3-5 ℃/min, preserving heat for 2-4 hours to remove PVB adhesive, heating to 1000 ℃ at the heating rate of 5-8 ℃/min, and preserving heat for 1-2 hours to obtain the lithium orthosilicate-lithium titanate core-shell structure ceramic pellets with controllable diameter of 1-1.4 mm and shell thickness of 50-200 mm.
In the method, the ball-material ratio in the mechanical ball milling is controlled to be 1:1-1:5, wherein the ball-material ratio is the mass ratio of grinding balls to the ground materials, and the volume occupied by the grinding balls and the materials is not more than 2/3 of the total volume of the ball milling tank.
In the method, the heat treatment and sintering atmosphere in the steps (1), (2) and (5) are all air.
In the above method, the diameter of the planetary ball mill was 60cm.
In the method, the inner diameter of the nylon ball milling tank is 12cm.
The invention has the following beneficial effects:
1. the method provided by the invention overcomes the problem of mismatching of sintering shrinkage rates of lithium orthosilicate and lithium titanate ceramic, and can be used for obtaining the ceramic pellet with the core-shell combined tightly and adopting the lithium orthosilicate-lithium titanate core-shell structure, wherein the spherical core is prepared from the lithium orthosilicate precursor powder subjected to presintering treatment at 400-500 ℃ and the spherical shell is prepared from the lithium titanate precursor powder subjected to presintering treatment at 600-700 ℃.
2. According to the method, the thickness of the core-shell structure ceramic pellet can be controlled by adjusting the adding amount of the lithium titanate precursor powder, so that the performance requirements of different scenes can be met.
3. The method combines the advantages of rapid molding and ceramic sintering technology, has short preparation period and is easy for batch production.
Drawings
FIG. 1 is a schematic diagram of a preparation flow of a ceramic pellet with a lithium orthosilicate-lithium titanate core-shell structure
Fig. 2 is a cross-sectional SEM image of the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 1.
FIG. 3 is an XRD pattern of lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 1.
FIG. 4a is a graph showing the Si element distribution of the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 1.
FIG. 4b is a graph showing the Ti element profile of the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 1.
Fig. 5 is a cross-sectional SEM image of the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 2.
FIG. 6a is a graph of the Si/Ti elemental distribution of lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 2.
FIG. 6b is a graph of the Si/Ti elemental distribution of lithium orthosilicate-lithium titanate core-shell structured ceramic pellets prepared in example 2.
Detailed Description
The following is a further description of the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets for tritium proliferation and the preparation method thereof by way of example and with reference to the accompanying drawings. In the examples below, the raw materials were purchased from Chengdu Kelong chemical reagent plant.
Example 1
In this embodiment, as shown in fig. 1, the preparation method of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet is as follows:
(1) Synthesis of lithium orthosilicate precursor powder
41.96g of LiOH H having a purity of 99.99% 2 O powder and 18.52g of H with purity of 99.9% 2 SiO 3 Adding the raw material powder into a nylon ball milling tank with the diameter of 12cm according to the molar ratio of 4:1, adding 300ml of deionized water and agate ball milling, and mechanically ball milling for 6 hours at the rotating speed of 200rads for mixing;
transferring the mixed suspension into a blast drying oven, preserving heat at 100 ℃ for 24 hours, filling the dried powder into a corundum crucible, transferring into a muffle furnace, heating to 400 ℃ at a heating rate of 3 ℃/min, and preserving heat for 1 hour to perform presintering heat treatment on the powder;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium orthosilicate precursor powder.
(2) Synthesis of lithium titanate precursor powder
20.98g of LiOH H having a purity of 99.99% 2 O powder and 24.47g of H with purity of 99.99 percent 2 TiO 3 Adding the raw material powder into a nylon ball milling tank according to a molar ratio of 2:1, adding 200ml of deionized water and agate balls into the nylon ball milling tank, and mechanically ball milling for 3 hours at a rotating speed of 160rads for mixing;
transferring the mixed suspension into a blast drying oven, preserving heat at 100 ℃ for 24 hours, filling the dried powder into a corundum crucible, transferring into a muffle furnace, heating to 600 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours to perform presintering heat treatment on the powder;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium titanate precursor powder.
(3) Adhesive coating
5g of polyvinyl butyral (PVB) powder is dissolved in 200ml of absolute ethyl alcohol and heated to 50 ℃, and after magnetic stirring for 6 hours, polyvinyl butyral solution is obtained;
fully mixing 100ml of PVB solution and the lithium orthosilicate precursor powder prepared in the step (1) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat at 90 ℃ for 24 hours to finally obtain the PVB coated lithium orthosilicate precursor powder;
fully mixing 50ml of PVB solution and the lithium titanate precursor powder prepared in the step (2) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat at 90 ℃ for 124 hours to finally obtain PVB-coated lithium titanate precursor powder;
(4) Preparation of core-shell structured pellet biscuit
Adding the PVB-coated lithium orthosilicate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 2 hours at a rotating speed of 160rads by a planetary ball mill to obtain a plurality of spherical lithium orthosilicate blanks with diameters of 1.2 mm;
continuously adding the PVB-coated lithium titanate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 2 hours at a rotating speed of 200rads by a planetary ball mill to obtain a plurality of lithium orthosilicate-lithium titanate core-shell structure biscuit pellets with the diameter of 1.6 mm.
(5) High temperature sintering
Placing the lithium orthosilicate-lithium titanate core-shell structure biscuit pellets into a muffle furnace, heating to 500 ℃ at a heating rate of 5 ℃/min, preserving heat for 2 hours to remove PVB adhesive, heating to 1000 ℃ at a heating rate of 8 ℃/min, and preserving heat for 1 hour to obtain the lithium orthosilicate-lithium titanate core-shell structure ceramic pellets.
The cross-sectional SEM diagram of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet prepared in the embodiment is shown in FIG. 2, and it can be seen from the diagram that the core-shell structure pellet has a core of 1050 μm directly and a shell layer of 170 μm thick, and the core-shell is tightly combined, and no obvious defect structure is found; the XRD pattern of fig. 3 shows that the core-shell ceramic pellet consists of only lithium orthosilicate and lithium titanate, with no other impurity phases; further Si/Ti element profiles in FIGS. 4a and 4b indicate that lithium orthosilicate is present only in the core and lithium titanate is present only in the shell.
Example 2
In this embodiment, the preparation method of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet is as follows:
(1) Synthesis of lithium orthosilicate precursor powder
62.94g of LiOH H having a purity of 99.99% 2 O powder and 27.78g of H with purity of 99.9% 2 SiO 3 Adding the raw material powder into a nylon ball milling tank with the diameter of 12cm according to the molar ratio of 4:1, adding 500ml of deionized water and agate ball milling, and mechanically ball milling for 8 hours at the rotating speed of 180rads for mixing;
transferring the mixed suspension into a blast drying oven, preserving heat at 100 ℃ for 24 hours, filling the dried powder into a corundum crucible, transferring into a muffle furnace, heating to 400 ℃ at a heating rate of 3 ℃/min, and preserving heat for 1 hour to perform presintering heat treatment on the powder;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium orthosilicate precursor powder.
(2) Synthesis of lithium titanate precursor powder
25.18g of LiOH H having a purity of 99.99% are reacted 2 O powder and 29.36g of H with purity of 99.99% 2 TiO 3 Adding the raw material powder into a nylon ball milling tank according to a molar ratio of 2:1, adding 300ml of deionized water and agate balls into the nylon ball milling tank, and mechanically ball milling for 2 hours at a rotating speed of 200rads for mixing;
transferring the mixed suspension into a blast drying oven, preserving heat at 100 ℃ for 24 hours, filling the dried powder into a corundum crucible, transferring into a muffle furnace, heating to 600 ℃ at a heating rate of 4 ℃/min, and preserving heat for 4 hours to perform presintering heat treatment on the powder;
and after the heat preservation is finished, naturally cooling to room temperature, and finishing the preparation of the lithium titanate precursor powder.
(3) Adhesive coating
10g of polyvinyl butyral (PVB) powder is dissolved in 400ml of absolute ethyl alcohol and heated to 50 ℃, and after magnetic stirring for 6 hours, a polyvinyl butyral solution is obtained;
fully mixing 150ml of PVB solution and the lithium orthosilicate precursor powder prepared in the step (1) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat at 100 ℃ for 24 hours to finally obtain the PVB coated lithium orthosilicate precursor powder;
fully mixing 100ml of PVB solution and the lithium titanate precursor powder prepared in the step (2) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat at 100 ℃ for 124 hours to finally obtain PVB-coated lithium titanate precursor powder;
(4) Preparation of core-shell structured pellet biscuit
Adding the PVB-coated lithium orthosilicate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 3 hours at a rotating speed of 180rads through a planetary ball mill to obtain a plurality of spherical lithium orthosilicate blanks with diameters of 1.4 mm;
continuously adding the PVB-coated lithium titanate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 2 hours at the rotating speed of 210rads by a planetary ball mill to obtain a plurality of lithium orthosilicate-lithium titanate core-shell structure biscuit pellets with the diameter of 1.6 mm.
(5) High temperature sintering
Placing the lithium orthosilicate-lithium titanate core-shell structure biscuit pellets into a muffle furnace, heating to 500 ℃ at a heating rate of 3 ℃/min, preserving heat for 4 hours to remove PVB adhesive, heating to 1000 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours to obtain the lithium orthosilicate-lithium titanate core-shell structure ceramic pellets.
The cross-sectional SEM image of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet prepared in the embodiment is shown in FIG. 5, and as can be seen from the image, the core-shell structure pellet has an inner core of 1220 μm directly and a shell layer of 75 μm thick, and the core-shell is tightly combined, and no obvious defect structure is found; the Si/Ti element profiles in FIGS. 6a and 6b show that lithium orthosilicate is present only in the core and lithium titanate is present only in the shell.
Claims (6)
1. The preparation method of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet for tritium proliferation is characterized in that the diameter of the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet for tritium proliferation is 1-1.4 mm, and the thickness of a shell layer is 50-200 microns controllable; the preparation method comprises the following steps:
(1) Synthesis of lithium orthosilicate precursor powder
By LiOH H 2 O powder and H 2 SiO 3 The powder is the raw material LiOH H 2 O powder and H 2 SiO 3 Adding the powder into a nylon ball milling tank according to the molar ratio of 4:1, adding deionized water and agate balls into the nylon ball milling tank, and carrying out mechanical ball milling and mixing;
transferring the mixed suspension into a blast drying oven, preserving heat for 10-24 hours at 80-110 ℃, transferring into a muffle furnace, adjusting a furnace body heater to 400-500 ℃ for powder pre-sintering heat treatment, and preserving heat for 1-2 hours;
after the heat preservation is completed, naturally cooling to room temperature, and completing the preparation of lithium orthosilicate precursor powder;
(2) Synthesis of lithium titanate precursor powder
By LiOH H 2 O powder and H 2 TiO 3 The powder is the raw material LiOH H 2 O powder and H 2 TiO 3 Adding the powder into a nylon ball milling tank according to the mol ratio of 2:1, adding deionized water and agate balls into the nylon ball milling tank, and carrying out mechanical ball milling and mixing;
transferring the mixed suspension into a blast drying oven, preserving heat for 10-24 hours at 80-110 ℃, transferring into a muffle furnace, adjusting a furnace body heater to 600-700 ℃ for powder pre-sintering heat treatment, and preserving heat for 3-4 hours;
after the heat preservation is completed, naturally cooling to room temperature, and completing the preparation of lithium titanate precursor powder;
(3) Adhesive coating
Dissolving polyvinyl butyral PVB powder in absolute ethyl alcohol at 50 ℃, and magnetically stirring for 4-6 hours to obtain a polyvinyl butyral solution;
fully mixing PVB solution and lithium orthosilicate precursor powder prepared in the step (1) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat for 10-24 hours at 80-110 ℃ to finally obtain PVB coated lithium orthosilicate precursor powder;
fully mixing PVB solution and the lithium titanate precursor powder prepared in the step (2) at room temperature through a magnetic stirrer, then placing the suspension in a blast drying box, and preserving heat for 10-24 hours at 80-110 ℃ to finally obtain the PVB lithium titanate precursor powder coated;
(4) Preparation of core-shell structured pellet biscuit
According to different requirements of the yield, adding the PVB coated lithium orthosilicate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 1-3 hours at a rotating speed of 160-200rads by a planetary ball mill to obtain a plurality of spherical lithium orthosilicate biscuits with diameters of 1.0-1.4 mm;
continuously adding the PVB-coated lithium titanate precursor powder obtained in the step (3) into a nylon ball milling tank, and rotating for 2-4 hours at a rotating speed of 200-220rads by a planetary ball mill to obtain a plurality of lithium orthosilicate-lithium titanate core-shell structure biscuit pellets with the diameter of 1.2-1.6 mm;
(5) High temperature sintering
The green pellets of the lithium orthosilicate-lithium titanate core-shell structure are placed in a muffle furnace, and the sintering curve is as follows: heating to 500 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 2-4 hours to remove PVB adhesive, heating to 1000 ℃ at a heating rate of 5-8 ℃/min, preserving heat for 1-2 hours, and sintering to obtain the lithium orthosilicate-lithium titanate core-shell structure ceramic pellet, wherein the core: pure phase Li 4 SiO 4 And (3) a shell: pure phase Li 2 TiO 3 。
2. The method for preparing the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets according to claim 1, wherein in the step (3), the adding amount of PVB powder is 0.5% -1% of the mass of the precursor powder prepared in the steps (1) and (2), respectively.
3. The method for preparing the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets, according to claim 1, is characterized in that in the preparation process of the precursor powder in the step (1) and the step (2), the ball-material ratio in the mechanical ball milling process is controlled to be 1:1-1:5, and the ball-material ratio is the mass ratio of grinding balls to materials to be ground, and the volume occupied by the grinding balls and the materials is not more than 2/3 of the total volume of a ball milling tank.
4. The method for preparing the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets according to claim 1, wherein the purity of the polyvinyl butyral in the step (3) is m.w.40,000-70,000.
5. The method for preparing the lithium orthosilicate-lithium titanate core-shell structured ceramic pellets according to claim 1, which is characterized in that: in the process of preparing the biscuit pellets with the core-shell structure by rotary granulation in the step (4), the diameter of the planetary ball mill is 60cm, and the inner diameter of the nylon ball milling tank is 12cm.
6. Ceramic pellets of lithium orthosilicate-lithium titanate core-shell structure, obtainable by the process according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310035630.1A CN116041052B (en) | 2023-01-10 | 2023-01-10 | Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310035630.1A CN116041052B (en) | 2023-01-10 | 2023-01-10 | Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116041052A CN116041052A (en) | 2023-05-02 |
| CN116041052B true CN116041052B (en) | 2023-11-28 |
Family
ID=86114385
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310035630.1A Active CN116041052B (en) | 2023-01-10 | 2023-01-10 | Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116041052B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11228130A (en) * | 1998-02-04 | 1999-08-24 | Nuclear Fuel Ind Ltd | Lithium ceramic granule and its production |
| JP2009249216A (en) * | 2008-04-04 | 2009-10-29 | Japan Atomic Energy Agency | Method for producing powder for producing lithium granulated body, lithium ceramics microsphere produced by using the method, and rolling granulation device for producing lithium ceramics microsphere |
| WO2012047657A2 (en) * | 2010-09-27 | 2012-04-12 | Purdue Research Foundation | Ceramic-ceramic composites and process therefor, nuclear fuels formed thereby, and nuclear reactor systems and processes operated therewith |
| CN106630985A (en) * | 2016-12-16 | 2017-05-10 | 四川大学 | Nanostructured lithium orthosilicate ceramic spheres used for tritium propagation and preparation method thereof |
| CN106747435A (en) * | 2017-03-03 | 2017-05-31 | 河南科技大学 | A kind of preparation method of the core shell structure microwave-medium ceramics of temperature stabilization |
| CN111018557A (en) * | 2019-12-26 | 2020-04-17 | 广州赛隆增材制造有限责任公司 | Preparation method of lithium orthosilicate spherical shell for tritium breeding |
| CN112725716A (en) * | 2020-12-23 | 2021-04-30 | 中国兵器工业第五九研究所 | Core-shell structure ceramic composite powder for thermal spraying and preparation method thereof |
| CN114477964A (en) * | 2022-01-28 | 2022-05-13 | 中国科学院近代物理研究所 | High-wear-resistance beryllium oxide-zirconium oxide core-shell structure ceramic ball and preparation method and application thereof |
-
2023
- 2023-01-10 CN CN202310035630.1A patent/CN116041052B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11228130A (en) * | 1998-02-04 | 1999-08-24 | Nuclear Fuel Ind Ltd | Lithium ceramic granule and its production |
| JP2009249216A (en) * | 2008-04-04 | 2009-10-29 | Japan Atomic Energy Agency | Method for producing powder for producing lithium granulated body, lithium ceramics microsphere produced by using the method, and rolling granulation device for producing lithium ceramics microsphere |
| WO2012047657A2 (en) * | 2010-09-27 | 2012-04-12 | Purdue Research Foundation | Ceramic-ceramic composites and process therefor, nuclear fuels formed thereby, and nuclear reactor systems and processes operated therewith |
| CN103299375A (en) * | 2010-09-27 | 2013-09-11 | 普渡研究基金会 | Ceramic-ceramic composites and process therefor, nuclear fuels formed thereby, and nuclear reactor systems and processes operated therewith |
| CN106630985A (en) * | 2016-12-16 | 2017-05-10 | 四川大学 | Nanostructured lithium orthosilicate ceramic spheres used for tritium propagation and preparation method thereof |
| CN106747435A (en) * | 2017-03-03 | 2017-05-31 | 河南科技大学 | A kind of preparation method of the core shell structure microwave-medium ceramics of temperature stabilization |
| CN111018557A (en) * | 2019-12-26 | 2020-04-17 | 广州赛隆增材制造有限责任公司 | Preparation method of lithium orthosilicate spherical shell for tritium breeding |
| CN112725716A (en) * | 2020-12-23 | 2021-04-30 | 中国兵器工业第五九研究所 | Core-shell structure ceramic composite powder for thermal spraying and preparation method thereof |
| CN114477964A (en) * | 2022-01-28 | 2022-05-13 | 中国科学院近代物理研究所 | High-wear-resistance beryllium oxide-zirconium oxide core-shell structure ceramic ball and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| Preparation of Li2TiO3eLi4SiO4 coreeshell ceramic pebbles with enhanced crush load by graphite bed process;Maoqiao Xiang et al.;Journal of Nuclear Materials;466;477-483 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116041052A (en) | 2023-05-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109354075B (en) | Preparation method of small-particle-size uniformly-aluminum-doped spherical cobaltosic oxide | |
| CN106630985B (en) | A kind of positive lithium metasilicate ceramic bead of tritium proliferation nanostructure and preparation method thereof | |
| CN101698609B (en) | Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder | |
| CN110157934B (en) | Manufacturing method of tungsten or molybdenum-based uranium dioxide fuel pellet | |
| CN110746186B (en) | Al (aluminum)3+Doped semiconductor ceramic material with low infrared and low thermal conductivity and preparation method thereof | |
| CN108565032A (en) | UO2Metal fuel pellet and its manufacturing method | |
| CN114105156B (en) | Nickel-cobalt-boron precursor material, preparation method thereof and nickel-cobalt-boron positive electrode material | |
| CN108039210A (en) | Fuel pellet and its manufacture method | |
| CN102219230A (en) | Method for preparing ferrous silicate lithium of anode material of lithium ion battery | |
| WO2023000594A1 (en) | High-entropy ceramic inert matrix dispersion fuel pellet and preparation method therefor | |
| CN116041052B (en) | Ceramic pellet with lithium orthosilicate-lithium titanate core-shell structure for tritium proliferation and preparation method thereof | |
| CN106084902B (en) | A kind of high infrared radiation powder and preparation method thereof | |
| CN114620774A (en) | Preparation method and application of core-shell structure high-nickel ternary precursor | |
| CN107565123B (en) | Nickel, cobalt and lithium manganate core-shell material gel and preparation method thereof | |
| CN1319848A (en) | Method for preparing Gd2O3-UO2 flammable poison fuel core block by using U3O8 powder | |
| CN105565810A (en) | Preparation method of rare-earth-doped yttrium oxide laser ceramic optical fiber | |
| CN105552354B (en) | A kind of preparation method of lithium ion battery negative material | |
| CN111146435A (en) | Spherical-like lithium manganate material and preparation method of raw material manganese dioxide thereof | |
| CN103183509A (en) | Lithium titanate ceramic ball tritium propagation material and preparation method thereof | |
| CN112694331B (en) | Method for preparing uranium dioxide composite fuel pellet by doping graphene oxide | |
| CN104134793B (en) | A kind of preparation method of lithium cell anode material lithium manganate and products thereof | |
| CN108002839A (en) | A kind of ZrC1-xThe preparation method of-SiC complex phase ceramics | |
| CN115676798A (en) | Preparation method of spherical titanium-doped high-compaction lithium iron phosphate cathode material | |
| CN115084516B (en) | Preparation method of boron-based multi-element composite material | |
| CN112537958B (en) | Lanthanum lithium zirconate solid electrolyte and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |