CN117602674A - Yttrium iron garnet nano powder and its preparing method and use - Google Patents
Yttrium iron garnet nano powder and its preparing method and use Download PDFInfo
- Publication number
- CN117602674A CN117602674A CN202311596032.8A CN202311596032A CN117602674A CN 117602674 A CN117602674 A CN 117602674A CN 202311596032 A CN202311596032 A CN 202311596032A CN 117602674 A CN117602674 A CN 117602674A
- Authority
- CN
- China
- Prior art keywords
- powder
- iron garnet
- heat treatment
- yttrium iron
- garnet nano
- 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.)
- Pending
Links
- 239000002223 garnet Substances 0.000 title claims abstract description 39
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000011858 nanopowder Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 72
- 239000000446 fuel Substances 0.000 claims abstract description 21
- 239000008139 complexing agent Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- YBHYYFYQHRADCQ-UHFFFAOYSA-N 2-aminoacetic acid;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound NCC(O)=O.OC(=O)CC(O)(C(O)=O)CC(O)=O YBHYYFYQHRADCQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 230000005415 magnetization Effects 0.000 claims abstract description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 71
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 51
- 239000004471 Glycine Substances 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 claims description 10
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000009841 combustion method Methods 0.000 claims description 3
- 230000005587 bubbling Effects 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 54
- 230000008569 process Effects 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 description 79
- 239000012071 phase Substances 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 25
- 239000013078 crystal Substances 0.000 description 22
- 229910000859 α-Fe Inorganic materials 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 238000003746 solid phase reaction Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 241001337814 Erysiphe glycines Species 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- ROBFUDYVXSDBQM-UHFFFAOYSA-N hydroxymalonic acid Chemical compound OC(=O)C(O)C(O)=O ROBFUDYVXSDBQM-UHFFFAOYSA-N 0.000 description 2
- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0054—Mixed oxides or hydroxides containing one rare earth metal, yttrium or scandium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C04B35/26—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 ferrites
- C04B35/2675—Other ferrites containing rare earth metals, e.g. rare earth ferrite garnets
-
- 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
-
- 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
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/32—Non-reciprocal transmission devices
- H01P1/38—Circulators
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Geology (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses yttrium iron garnet nano-powder and a preparation method and application thereof. The invention adopts a glycine-citric acid composite fuel/complexing agent system, and can reduce the heat treatment temperature of YIG powder with higher purity. The method for preparing YIG powder has the advantages of simple process, high repeatability and low heat treatment temperature of 900 ℃, thereby saving energy sources; the YIG powder prepared by the method has higher purity, good crystallinity and higher saturation magnetization. The method is used for preparing ceramics by sintering yttrium iron garnet nano-powder and then applying the ceramics in a microwave circulator.
Description
Technical Field
The invention relates to the technical field of Yttrium Iron Garnet (YIG) preparation, in particular to Yttrium Iron Garnet (YIG) nano-powder and a preparation method and application thereof.
Background
Yttrium iron garnet (Y) 3 Fe 5 O 12 YIG for short) has the advantages of small electromagnetic loss, high resistivity, high dielectric constant, excellent magneto-optical performance and the like, meets the requirements of miniaturization, integration and high frequency of electromagnetic elements, and is widely applied to the field of microwave communication, such as isolators, phase shifters, circulators, oscillators and the like.
The powder is a raw material for preparing ceramic components, and therefore, preparation of YIG powder with excellent performance is one of key factors for obtaining YIG components with excellent performance. Nanomaterials impart unique properties to nanomaterials that differ from conventional materials due to the specificity of structure and properties. Thus, the preparation method of the nano YIG powder is of great interest.
Common preparation methods of nano YIG powder include a traditional solid phase reaction method, a microemulsion method, a hydrothermal method, a coprecipitation method and the like. Wherein, the temperature for preparing pure YIG powder by the traditional solid phase reaction method is higher and is generally not lower than 1300 ℃; the preparation conditions of the microemulsion method, the coprecipitation method, the hydrothermal method and the like are harsh, the process control is complex, and the repeatability is poor. The YIG nano powder with higher purity and excellent performance can be obtained by the combustion method at a lower temperature, and the preparation method has the advantages of simple process and high repeatability.
Disclosure of Invention
The purpose of the present invention is to obtain YIG powder with high purity and good crystallinity at a low temperature.
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a method for preparing yttrium iron garnet nano-powder, which comprises using yttrium nitrate hexahydrate, ferric nitrate nonahydrate, and glycine-citric acid composite fuel/complexing agent system as raw materials, generating a fluffy product by a combustion method, and performing a heat-insulating heat treatment on the fluffy product to obtain high-purity yttrium iron garnet nano-powder.
Preferably, yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid and glycine are added with water to prepare a mixed solution, the mixed solution is heated to enable the mixed solution to be in a micro-boiling state, and as the heating is carried out, the reaction system becomes viscous and starts to bubble, and then a fluffy product is generated by burning.
Preferably, the amounts of yttrium nitrate hexahydrate, iron nitrate nonahydrate and citric acid are calculated according to the following formulas: 3Y (NO) 3 ) 3 .6H 2 O+5Fe(NO 3 ) 3 .9H 2 O+8C 6 H 8 O 7 →3YC 6 H 5 O 7 +5FeC 6 H 5 O 7 +24HNO 3 +63H 2 O↑。
Preferably, the glycine is used in an amount of 0.5 to 2 times the theoretical amount calculated according to the following chemical formula;
9Y(NO 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 ↑。
preferably, fe in the mixed solution 3+ The concentration of (C) is 0.2-0.4 mol/L.
Preferably, the heating is performed by a universal furnace with a power of 300W-600W.
Preferably, the temperature of the heat preservation and heat treatment is 900-1100 ℃; the heat preservation and heat treatment time is 1-3 hours.
Preferably, the temperature of the heat preservation and heat treatment is 900 ℃; the time of the heat preservation and heat treatment is 2 hours.
The invention also provides the yttrium iron garnet nano-powder prepared by the preparation method, and when the heat preservation and heat treatment temperature is increased from 900 ℃ to 1100 ℃, the average grain size of the yttrium iron garnet nano-powder is increased from 41.1-42.2 nm to 71-81 nm.
Preferably, when the heat preservation and heat treatment temperature is 900 ℃, the average grain size of the yttrium iron garnet nano-powder is 41.1-42.2 nm, and the saturation magnetization Ms of the yttrium iron garnet nano-powder is 25.1emu/g; when the heat preservation and heat treatment temperature is 1000 ℃, the average grain size of the yttrium iron garnet nano-powder is 51-54.3 nm; when the heat preservation and heat treatment temperature is 1100 ℃, the average grain size of the yttrium iron garnet nano-powder is 71-81 nm.
The invention also provides application of the yttrium iron garnet nano-powder prepared by the preparation method in a microwave circulator, wherein the yttrium iron garnet nano-powder is sintered to prepare ceramic, and the ceramic prepared by sintering is applied in the microwave circulator.
The invention at least comprises the following beneficial effects:
(1) Glycine or citric acid is generally used as a fuel/complexing agent in the preparation of YIG powder by combustion in the literature; the invention adopts a glycine-citric acid composite fuel/complexing agent system, and can reduce the heat treatment temperature of YIG powder with higher purity.
(2) The method for preparing YIG powder has the advantages of simple process, high repeatability and low heat treatment temperature of 900 ℃, thereby saving energy sources; the YIG powder prepared by the method has higher purity, good crystallinity and higher saturation magnetization.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is an XRD pattern of the combustion products and their subsequent heat treated products in a citric acid-glycine combustion system when glycine is used in varying amounts;
FIG. 2 is an SEM image of the powder product at various heat treatment temperatures for a citric acid-glycine combustion system;
FIG. 3 is an XRD pattern of the combustion products of a glycine combustion system and products at different subsequent heat treatment temperatures;
FIG. 4 is an XRD pattern of the combustion products of the citric acid combustion system and the different subsequent heat treatment temperature products thereof;
FIG. 5 shows hysteresis loops of YIG powder prepared by different combustion systems.
The specific embodiment is as follows:
the present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Raw material citric acid for experiment (C) 6 H 8 O 7 ) Glycine (C) 2 H 5 NO 2 ) Yttrium nitrate (Y (NO) 3 ) 3 .6H 2 O), ferric nitrate (Fe (NO) 3 ) 3 .9H 2 O) are all analytically pure grades. Wherein, the citric acid and the glycine have the functions of fuel and complexing agent, and the yttrium nitrate and the ferric nitrate are target products Y 3 Fe 5 O 12 (abbreviated as YIG). The dosage of yttrium nitrate and ferric nitrate is Y 3 Fe 5 O 12 Stoichiometric ratio.
X-ray diffraction (XRD) characterization is carried out on the combustion products and the powder thermally treated at different temperatures, the phase composition and the reaction mechanism in the powder preparation process are analyzed, and the average grain size of the nano powder is estimated. The morphology of the powder product was observed by Scanning Electron Microscopy (SEM). The hysteresis loop of the sample was tested using a Vibrating Sample Magnetometer (VSM) to obtain the static magnetic properties of the product.
Example 1:
a preparation method of yttrium iron garnet nano-powder (YIG powder prepared by taking citric acid-glycine as fuel/complexing agent) comprises the following steps:
6.89g of yttrium nitrate hexahydrate (0.018 mol), 12.12g of ferric nitrate nonahydrate (0.030 mol) were weighed and mixed with citric acid (9.22 g) and glycine (3.00 g) in water to prepare 100mL of a clear mixed solution, and Fe in the mixed solution 3+ The concentration of (2) is 0.3mol/L; heating the mixed solution in a universal furnace, and controlling the power (300W-600W) of the universal furnace to enable the mixed solution to be in a micro-boiling state; as the heating proceeds, the reaction system becomes viscous and begins to bubble, followed by combustion to produce a fluffy product; heat-preserving the fluffy combustion products at 900 ℃ for 2 hours for heat treatment, and carrying out manual preliminary grinding on the heat-treated products to obtain yttrium iron garnet nano-powder;
the amounts of yttrium nitrate hexahydrate, iron nitrate nonahydrate and citric acid were calculated according to the following chemical formulas:
3Y(NO 3 ) 3 .6H 2 O+5Fe(NO 3 ) 3 .9H 2 O+8C 6 H 8 O 7 →3YC 6 H 5 O 7 +5FeC 6 H 5 O 7 +24HNO 3 +63H 2 O↑；
the amount of glycine is 0.5 times the theoretical amount calculated according to the following chemical formula; 9Y (NO) 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 ↑。
Example 2:
the difference from example 1 is that the glycine is used in an amount 1 times the theoretical amount calculated according to the following formula, i.e. glycine (6.01 g); the rest of the procedure is exactly the same as in example 1; 9Y (NO) 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 ↑。
Example 3:
the difference from example 1 is that the glycine is used in an amount 2 times the theoretical amount calculated according to the following formula, i.e. glycine (12.02 g); the rest of the procedure is exactly the same as in example 1; 9Y (NO) 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 ↑。
Example 4:
the difference from example 1 is that the fluffy combustion product is heat-treated at 1000 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 1;
example 5:
the difference from example 2 is that the fluffy combustion product is heat-treated at 1000 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 2;
example 6:
the difference from example 3 is that the fluffy combustion product is heat-treated at 1000 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 3;
example 7:
the difference from example 1 is that the fluffy combustion product is heat-treated at 1100 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 1;
example 8:
the difference from example 2 is that the fluffy combustion product is heat-treated at 1100 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 2;
example 9:
the difference from example 3 is that the fluffy combustion product is heat-treated at 1100 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 3;
comparative example 1:
the difference from example 1 is that the fluffy combustion product is heat-treated at 650 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 1;
comparative example 2:
the difference from example 2 is that the fluffy combustion product is heat-treated at 650 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 2;
comparative example 3:
the difference from example 3 is that the fluffy combustion product is heat-treated at 650 ℃ for 2 hours; the rest of the procedure is exactly the same as in example 3;
as can be seen from the above examples 1 to 9 and comparative examples 1 to 3, as the amount of glycine increases, the brightness of flame and the flame propagation speed at the time of combustion of the reaction system gradually decrease, and the XRD patterns of the combustion products and the products at different subsequent heat treatment temperatures are shown in FIG. 1; as can be seen from FIG. 1, the crystallinity of the combustion products and the products heat-treated at 650℃were low for the reaction systems with different glycine amounts, but the crystallinity of the products gradually decreased with increasing glycine content.
For a reaction system in which the amount of glycine was 0.5 times the theoretical amount calculated according to the chemical formulaAfter heat treatment of the combustion products at 900 ℃, the main crystal phase of the products is YIG, and secondary crystal phases YIP and alpha-Fe are also present in the XRD pattern of the products (figure 1 a) 2 O 3 A stronger diffraction peak indicates that more secondary crystal phase is still present in the product, at which time the average grain size of YIG is 41.1nm; when the subsequent heat treatment temperature of the combustion product is raised to 1000 ℃, the primary crystal phase of the product is YIG, and the secondary crystal phases YIP and alpha-Fe in the XRD pattern of the product 2 O 3 The diffraction peak of (2) is very weak, which indicates that the purity of YIG powder product is very high, and the average grain size of YIG powder is estimated to be 54.3nm according to X-ray diffraction data and a Shelle formula. As the subsequent heat treatment temperature continued to rise to 1100 ℃, the phase composition of the product and the relative intensities of the diffraction peaks of the phases did not change significantly, and the average grain size of the YIG powder increased to 71.0nm。
The dosage of glycine is 1 times and 2 times of the theoretical dosage calculated according to the chemical formulaAnd) After the combustion products are subjected to heat treatment at 900 ℃, the main crystal phase of the powder products is YIG, and the purity is higher (as shown in figures 1a and 1 b). When the subsequent heat treatment temperature was continuously increased, the product was still YIG powder of higher purity, except that the average grain size of the powder was increased, as shown in table 1.
TABLE 1 average grain size of powders after heat treatment of combustion products at different temperatures
According to the analysis, when the dosage of glycine in the citric acid-glycine composite fuel/complexing agent system is different, the subsequent heat treatment temperature of the obtained high-purity YIG powder is different. This is because, in a combustion system in which citric acid is used as a complexing agent, the addition of a small amount of glycine (fuel) can promote the combustion of the reaction system, and when the amount of glycine added is large, heat is required for decomposition of glycine during the combustion process, which in turn lowers the temperature at which the system burns. When the temperature of the combustion system is different, the crystallinity and the composition of the combustion products are inevitably different, and the performance of the subsequent heat treatment products is affected. For a reaction system in which the amount of glycine was 0.5 times the theoretical amount calculated according to the chemical formulaThe crystal grain size of the obtained oxide obtained by combustion is relatively large and the activity is low due to the high combustion temperature, and then the solid phase reaction between the oxides can be carried out at a higher temperature (1000 ℃) to generate the target phase YIG. For glycine, the amount is calculated according to the chemical formula1-fold and 2-fold reaction system (+.>And->) Since glycine is used in a large amount, it is thermally decomposed in the combustion process to absorb a large amount of heat, so that the temperature is low in the combustion of the system, the amorphous degree of the oxide in the product is high, the lattice defect is large and the chemical activity is high, and therefore, the solid phase reaction between the oxides can be generated at a low subsequent heat treatment temperature (900 ℃) to generate the target phase YIG. When the YIG powder product with higher purity is obtained, if the subsequent heat treatment temperature is continuously increased, YIG grains will continue to grow. In the present invention, the highest temperature of the subsequent heat treatment of the combustion products is 1100 ℃, and the average grain size of the YIG powder obtained at this time is still on the nanometer scale.
In the combustion system with glycine-citric acid as fuel/complexing agent, the reaction system with glycine in an amount 1 times of the theoretical amount calculated according to the chemical formula is taken into considerationPreferably.
When glycine-citric acid is used as fuel/complexing agent, the dosage of glycine is 1 times of theoretical dosage calculated according to chemical formulaDuring this time, the combustion products were subjected to SEM images of the powder after heat treatment at 900 ℃, 1000 ℃ and 1100 ℃, respectively (as shown in fig. 2). As can be seen from fig. 2, the product morphology is porous and the voids and particles of the porous product gradually increase as the heat treatment temperature increases. This is because the reaction system generates a large amount of gas during combustion, which prevents particle agglomeration during discharge of the reaction system, while leaving holes in the sample. When the heat treatment temperature of the combustion products is raised, the sample particles are gradually made to be in accordance with the increase of mass transfer powerThe reticulate veins of the product become thicker and the loose holes become larger.
Comparative example 4:
glycine is used as fuel to prepare YIG powder phase composition:
6.89g of yttrium nitrate hexahydrate (0.018 mol), 12.12g of ferric nitrate nonahydrate (0.030 mol) were weighed and water was added to prepare a 100mL clear mixed solution of glycine (6.01 g), at which time Fe in the mixed solution 3+ The concentration of (2) is 0.3mol/L; heating the mixed solution in a universal furnace, and controlling the power (300W-600W) of the universal furnace to enable the mixed solution to be in a micro-boiling state; as the heating proceeds, the reaction system becomes viscous and begins to bubble, followed by combustion to produce a fluffy product; heat-preserving the fluffy combustion products at 650 ℃ for 2 hours for heat treatment, and carrying out manual preliminary grinding on the heat-treated products to obtain YIG powder;
comparative example 5:
the difference from comparative example 4 is that the fluffy combustion product was heat-treated at 900 ℃ for 2 hours; the remainder was identical to comparative example 4;
comparative example 6:
the difference from comparative example 4 is that the fluffy combustion product was heat-treated at 1000 ℃ for 2 hours; the remainder was identical to comparative example 4;
comparative example 7:
the difference from comparative example 4 is that the fluffy combustion product was heat-treated at 1100 ℃ for 2 hours; the remainder was identical to comparative example 4;
according to the chemical propellant theory, when the total reduction value of each reducing agent (fuel) and the total oxidation value of each oxidizing agent (nitrate) in the reaction raw materials are equal, the raw materials can be theoretically combusted without providing oxygen from the outside; in the present invention, when glycine is used as fuel (comparative examples 4 to 7), the amounts of the respective raw materials are calculated as follows: 9Y (NO) 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 E, -; the reaction system is burntWhen burned, the product after quick combustion emits bright flame, and the XRD patterns of the product after subsequent heat treatment at different temperatures are shown in figure 3:
as can be seen from FIG. 3, the main crystal phase of the combustion product of the glycine combustion system is YFeO 3 (abbreviated as YIP, PDF#39-1489), the secondary crystal phase is alpha-Fe 2 O 3 (PDF # 33-0664) with a small amount of tartronic acid (C) 3 H 4 O 5 PDF # 18-1911). Carrying out subsequent heat treatment on the combustion product at 650 ℃, wherein the main crystal phase of the product is YIP, and the secondary crystal phase is alpha-Fe 2 O 3 At this time C 3 H 4 O 5 And vanishes. YIG (PDF#43-0507) appears in the combustion product when it is heat treated at 900 ℃, but the main crystal phase is still YIP, and the secondary crystal phase alpha-Fe is also present 2 O 3 . When the temperature of the subsequent heat treatment is increased to 1000 ℃, the diffraction peak intensities of YIG phase and YIP phase in the powder product are equivalent, and the secondary crystal phase is alpha-Fe 2 O 3 . When the subsequent heat treatment temperature is raised to 1100 ℃, YIG phase becomes the main crystal phase of the powder product, YIP and alpha-Fe 2 O 3 Becomes a secondary crystal phase. From the above analysis, the reaction occurring at the time of combustion in the glycine combustion system is shown as follows:
6Y(NO 3 ) 3 .6H 2 O+10C 2 H 5 NO 2 →3Y 2 O 3 +20CO 2 ↑+61H 2 O↑+14N 2 ↑
6Fe(NO 3 ) 3 .9H 2 O+10C 2 H 5 NO 2 →3Fe 2 O 3 +20CO 2 ↑+79H 2 O↑+14N 2 ↑
Y 2 O 3 +Fe 2 O 3 →2YFeO 3
i.e. during combustion of the system, Y is first formed 2 O 3 And Fe (Fe) 2 O 3 And part Y 2 O 3 And Fe (Fe) 2 O 3 The reaction produces YIP, and at the same time, small amount of C generated by insufficient combustion of fuel is also present in the combustion products 3 H 4 O 5 . For combustion productsSubsequent heat treatment at 650 deg.c, the oxide has insufficient power to react in solid phase due to lower heat treatment temperature, and Y in the combustion product 2 O 3 、Fe 2 O 3 And YIP, with only a small amount of C in the combustion products 3 H 4 O 5 The decomposition reaction occurs as shown in the following formula:
2C 3 H 4 O 5 +3O 2 →4H 2 O↑+6CO 2 ↑
when the subsequent heat treatment temperature of the combustion products reaches 900 ℃, Y 2 O 3 And Fe (Fe) 2 O 3 Continuing the reaction to form YIP (e.g. Y 2 O 3 +Fe 2 O 3 →2YFeO 3 Shown), and YIP and Fe 2 O 3 The solid phase reaction starts to take place to generate YIG, which is shown in the following formula:
3YFeO 3 +Fe 2 O 3 →Y 3 Fe 5 O 12
with the subsequent heat treatment temperature rising, YIP and Fe in the product 2 O 3 Continuing as in 3YFeO 3 +Fe 2 O 3 →Y 3 Fe 5 O 12 A solid phase reaction occurs. When the subsequent heat treatment temperature reaches 1100 ℃, the main crystal phase of the powder product has become the target product YIG, but still has a small amount of secondary crystal phase YIP and alpha-Fe 2 O 3 Is present.
Comparative example 8:
the phase composition of YIG powder prepared by using citric acid as fuel/complexing agent comprises:
6.89g of yttrium nitrate hexahydrate (0.018 mol), 12.12g of ferric nitrate nonahydrate (0.030 mol) were weighed and water was added to prepare 100mL of a clear mixed solution of citric acid (9.22 g) together with Fe in the mixed solution 3+ The concentration of (2) is 0.3mol/L; heating the mixed solution in a universal furnace, and controlling the power (300W-600W) of the universal furnace to enable the mixed solution to be in a micro-boiling state; as the heating proceeds, the reaction system becomes viscous and begins to bubble, followed by combustion to produce a fluffy product; the fluffy combustion products are heat-treated by heat preservation for 2 hours at 650 ℃,carrying out manual preliminary grinding on the heat-treated product to obtain YIG powder;
comparative example 9:
the difference from comparative example 8 is that the fluffy combustion product was heat-treated at 900 ℃ for 2 hours; the remainder was identical to comparative example 8;
comparative example 10:
the difference from comparative example 8 is that the fluffy combustion product was heat-treated at 1000 ℃ for 2 hours; the remainder was identical to comparative example 8;
comparative example 11:
the difference from comparative example 8 is that the fluffy combustion product was heat-treated at 1100 ℃ for 2 hours; the remainder was identical to comparative example 8;
preparing YIG powder by taking citric acid as fuel and a complexing agent, and calculating the consumption of raw materials according to the following formula; 3Y (NO) 3 ) 3 .6H 2 O+5Fe(NO 3 ) 3 .9H 2 O+8C 6 H 8 O 7 →3YC 6 H 5 O 7 +5FeC 6 H 5 O 7 +24HNO 3 +63H 2 O↑
The XRD patterns of the combustion products and the products with different subsequent heat treatment temperatures are shown in figure 4.
As can be seen from fig. 4, the combustion products of this system and their subsequent heat treatment at 650 ℃ are less crystalline, almost amorphous. When the subsequent heat treatment temperature is 650 ℃, the main crystal phase of the powder product is YIG (PDF#43-0507), and the secondary crystal phase is YIP (PDF#39-1489) and alpha-Fe 2 O 3 (PDF # 33-0664). When the subsequent treatment temperature is more than or equal to 1000 ℃, the diffraction peak intensity of YIG in the powder product is enhanced, and the paracrystalline phase YIP and alpha-Fe 2 O 3 The diffraction peak of (C) is very weak, which indicates that the YIG crystallinity in the product is improved and the purity is higher when the subsequent heat treatment is more than or equal to 1000 ℃.
From the combustion phenomenon of the reaction system and the phase composition analysis of the product, the reaction of the following formula occurs in the combustion process;
3Y(NO 3 ) 3 .6H 2 O+5Fe(NO 3 ) 3 .9H 2 O+8C 6 H 8 O 7 →3YC 6 H 5 O 7 +5FeC 6 H 5 O 7 +24HNO 3 +63H 2 O↑
YC 6 H 5 O 7 +FeC 6 H 5 O 7 +9O 2 →YFeO 3 +5H 2 O+12CO 2 ↑
2YC 6 H 5 O 7 +9O 2 →Y 2 O 3 +5H 2 O↑+12CO 2 ↑
2FeC 6 H 5 O 7 +9O 2 →Fe 2 O 3 +5H 2 O↑+12CO 2 ↑
meanwhile, no obvious flame appears during combustion, which means that the combustion temperature is low, and the combustion products are not fully crystallized and are almost amorphous.
When the subsequent heat treatment temperature reaches 900 ℃, the crystallinity of the combustion products is low, the activity is high, and most of the activity is high 2 O 3 And alpha-Fe 2 O 3 The solid phase reaction can quickly generate YIP (such as Y) 2 O 3 +Fe 2 O 3 →2YFeO 3 Represented by the formula), followed by YIP and alpha-Fe 2 O 3 Generating YIG (such as 3 YFeO) through solid phase reaction 3 +Fe 2 O 3 →Y 3 Fe 5 O 12 Shown in the formula), and becomes a main crystal phase of the powder product, and the average grain size of the YIG powder product is estimated to be 40.9nm according to the Shelle formula. When the subsequent heat treatment temperature of the combustion products is raised to 1000 ℃, 3YFeO continues to occur 3 +Fe 2 O 3 →Y 3 Fe 5 O 12 The reaction is shown to generate YIG, the relative content of YIG in the powder product is continuously increased, and YIG powder with higher purity is obtained, and the average grain size of YIG powder is 53.5nm. The subsequent heat treatment of the combustion products was continued to raise the temperature to 1100 ℃, the phase composition of the products did not change, but the average grain size increased to 67.2nm.
When glycine, citric acid and glycine-citric acid are used as fuel/complexing agent to prepare YIG powder with higher purity, the lowest subsequent heat treatment temperature is 1100 ℃, 1000 ℃ and 900 ℃ respectively.
Hysteresis loop tests were performed on YIG powder prepared with higher purity when glycine, citric acid, and glycine-citric acid were used as fuel/complexing agent, respectively, and the results are shown in FIG. 5. As can be seen from FIG. 5, the powder obtained by heat treatment of glycine as fuel and combustion product at 1100deg.C has the lowest saturation magnetization (Ms) of 22.7emu/g, since the product under the preparation conditions contains more YIP and α -Fe of weakly magnetic secondary crystal phase 2 O 3 Thereby reducing the Ms value of the sample. Powder obtained by heat treatment of combustion products at 1000 ℃ with citric acid as complexing agent and reaction system with glycine-citric acid as fuel/complexing agent and glycine in an amount 1 times of theoretical amount calculated according to chemical formulaThe Ms of the powder after heat treatment at 900 ℃ of the combustion products are higher, and the Ms are not greatly different, namely 24.8emu/g and 25.1emu/g, which is caused by the fact that the purity of the two YIG powder products is higher, the average grain size is close, and the Ms are similar.
Application example 1:
sintering the yttrium iron garnet nano-powder prepared in the embodiment 1 to prepare ceramic, and applying the ceramic prepared by sintering in a microwave circulator; because the yttrium iron garnet powder is nano-scale powder, the sintering activity is high, and the compact YIG ceramic can be obtained at a lower temperature, so that the microwave loss is smaller when the yttrium iron garnet powder is used as a ceramic component.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (10)
1. The preparation method of yttrium iron garnet nano-powder is characterized in that yttrium nitrate hexahydrate, ferric nitrate nonahydrate and glycine-citric acid composite fuel/complexing agent system are used as raw materials, a combustion method is adopted to generate fluffy products, and the fluffy products are subjected to heat preservation and heat treatment to obtain high-purity yttrium iron garnet nano-powder.
2. The method for preparing yttrium iron garnet nano-powder according to claim 1, wherein,
adding water into yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid and glycine to prepare a mixed solution, heating the mixed solution to enable the mixed solution to be in a micro-boiling state, enabling a reaction system to become viscous and start bubbling along with the heating, and then burning to generate a fluffy product.
3. The method of preparing yttrium iron garnet nano-powder according to claim 2, wherein the amounts of yttrium nitrate hexahydrate, ferric nitrate nonahydrate and citric acid are calculated according to the following chemical formula: 3Y (NO) 3 ) 3 .6H 2 O+5Fe(NO 3 ) 3 .9H 2 O+8C 6 H 8 O 7 →3YC 6 H 5 O 7 +5FeC 6 H 5 O 7 +24HNO 3 +63H 2 O↑。
4. The method for preparing yttrium iron garnet nano-powder according to claim 2, wherein the amount of glycine is 0.5 to 2 times of the theoretical amount calculated according to the following chemical formula;
9Y(NO 3 ) 3 .6H 2 O+15Fe(NO 3 ) 3 .9H 2 O+40C 2 H 5 NO 2 →3Y 3 Fe 5 O 12 +80CO 2 ↑+289H 2 O↑+56N 2 ↑。
5. the method for preparing yttrium-iron garnet nano-powder according to claim 2, wherein Fe in the mixed solution 3+ The concentration of (2) is 0.2-0.4 mol/L; the heating adopts a universal furnace, and the power of the universal furnace is 300W-600W.
6. The method for preparing yttrium iron garnet nano-powder according to claim 1, wherein the temperature of the thermal insulation heat treatment is 900-1100 ℃; the heat preservation and heat treatment time is 1-3 hours.
7. The method for preparing yttrium-iron garnet nano-powder according to claim 1, wherein the temperature of the heat-preserving heat treatment is 900 ℃; the time of the heat preservation and heat treatment is 2 hours.
8. The yttrium iron garnet nano-powder prepared by the method according to any one of claims 1 to 7, wherein the average grain size of the yttrium iron garnet nano-powder increases from 41.1 to 42.2nm to 71 to 81nm when the soaking heat treatment temperature is increased from 900 ℃ to 1100 ℃.
9. The yttrium iron garnet nano-powder according to claim 8, wherein the average grain size of the yttrium iron garnet nano-powder is 41.1-42.2 nm and the saturation magnetization Ms of the yttrium iron garnet nano-powder is 25.1emu/g when the heat-insulating treatment temperature is 900 ℃; when the heat preservation and heat treatment temperature is 1000 ℃, the average grain size of the yttrium iron garnet nano-powder is 51-54.3 nm; when the heat preservation and heat treatment temperature is 1100 ℃, the average grain size of the yttrium iron garnet nano-powder is 71-81 nm.
10. Use of yttrium iron garnet nano-powder prepared by the preparation method according to any one of claims 1 to 7 in a microwave circulator, wherein the yttrium iron garnet nano-powder is sintered to prepare ceramic, and the ceramic prepared by sintering is used in the microwave circulator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311596032.8A CN117602674A (en) | 2023-11-28 | 2023-11-28 | Yttrium iron garnet nano powder and its preparing method and use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311596032.8A CN117602674A (en) | 2023-11-28 | 2023-11-28 | Yttrium iron garnet nano powder and its preparing method and use |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117602674A true CN117602674A (en) | 2024-02-27 |
Family
ID=89943807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311596032.8A Pending CN117602674A (en) | 2023-11-28 | 2023-11-28 | Yttrium iron garnet nano powder and its preparing method and use |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117602674A (en) |
-
2023
- 2023-11-28 CN CN202311596032.8A patent/CN117602674A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Peng et al. | Fe-based soft magnetic composites coated with NiZn ferrite prepared by a co-precipitation method | |
| Junliang et al. | One-step synthesis of barium hexaferrite nano-powders via microwave-assisted sol–gel auto-combustion | |
| Chen et al. | Synthesis of nickel ferrite nanoparticles by sol-gel method | |
| Fu et al. | Fe/Sr ratio effect on magnetic properties of strontium ferrite powders synthesized by microwave-induced combustion process | |
| Rao et al. | Controlled phase evolution and the occurrence of single domain CoFe2O4 nanoparticles synthesized by PVA assisted sol-gel method | |
| Costa et al. | Effect of urea and glycine fuels on the combustion reaction synthesis of Mn–Zn ferrites: evaluation of morphology and magnetic properties | |
| JP5105503B2 (en) | ε Iron oxide production method | |
| Hwang et al. | Combustion synthesis of Ni–Zn ferrite powder—influence of oxygen balance value | |
| Thomas et al. | Comparative study of the structural and magnetic properties of alpha and beta phases of lithium ferrite nanoparticles synthesized by solution combustion method | |
| Rashad et al. | Controlling the composition, microstructure, electrical and magnetic properties of LiFe5O8 powders synthesized by sol gel auto-combustion method using urea as a fuel | |
| Fu et al. | Microwave-induced combustion synthesis of Ni0. 25Cu0. 25Zn0. 5 ferrite powders and their characterizations | |
| Gabal et al. | Structural, magnetic and electrical properties of Ga-substituted NiCuZn nanocrystalline ferrite | |
| Fu et al. | Microwave-induced combustion synthesis of Ni–Zn ferrite powder and its characterization | |
| Roohani et al. | Effect of annealing temperature on structural and magnetic properties of strontium hexaferrite nanoparticles synthesized by sol–gel auto-combustion method | |
| Cernea et al. | Magnetic properties of BaNixFe12–xO19 (x= 0.0–1.0) hexaferrites, synthesized by citrate–gel auto-combustion and sintered by conventional and spark plasma methods | |
| Fu et al. | Li0. 5Fe2. 5− xMnxO4 ferrite sintered from microwave-induced combustion | |
| Liu et al. | Microstructure and magnetic properties of Ni0· 75Zn0· 25Fe2O4 ferrite prepared using an electric current-assisted sintering method | |
| Harikrishnan et al. | Temperature-dependent phase transition: Structural and magnetic properties of Ba0. 5Sr0. 5Fe12O19-CoFe2O4 nanocomposites | |
| Parkin et al. | Self‐propagating high temperature synthesis of hexagonal ferrites MFe12O19 (M= Sr, Ba) | |
| Lai et al. | Enhanced soft magnetic properties and high-frequency stability of FeNiMo powder cores by coating SiO 2 insulation layer | |
| Khan et al. | Low-temperature Griffiths phase in chemically synthesized CoMn2O4 spinel oxide | |
| Li et al. | Combustion synthesis and characterization of NiCuZn ferrite powders | |
| Naik et al. | Tailoring magnetic and dielectric properties of Co0. 9Cu0. 1Fe2O4 with substitution of small fractions of Gd3+ ions | |
| Liu et al. | Synthesis of nanocrystalline Zn0. 5Mn0. 5Fe2O4 via in situ polymerization technique | |
| CN117602674A (en) | Yttrium iron garnet nano powder and its preparing method and use |
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 |