CN108610048A - It is a kind of to prepare sintering temperature and low corundum type Mg4Ta2O9The method of microwave dielectric ceramic materials - Google Patents
It is a kind of to prepare sintering temperature and low corundum type Mg4Ta2O9The method of microwave dielectric ceramic materials Download PDFInfo
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- 238000005245 sintering Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 27
- 239000010431 corundum Substances 0.000 title claims abstract description 27
- 229910010293 ceramic material Inorganic materials 0.000 title claims description 41
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 253
- 239000011777 magnesium Substances 0.000 claims abstract description 203
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 200
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 150
- 239000000843 powder Substances 0.000 claims abstract description 114
- 238000003756 stirring Methods 0.000 claims abstract description 67
- 238000007873 sieving Methods 0.000 claims abstract description 65
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 40
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 40
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 39
- 238000001354 calcination Methods 0.000 claims abstract description 36
- 238000005469 granulation Methods 0.000 claims abstract description 33
- 230000003179 granulation Effects 0.000 claims abstract description 33
- 238000000465 moulding Methods 0.000 claims abstract description 33
- 238000004321 preservation Methods 0.000 claims description 53
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 37
- 238000012545 processing Methods 0.000 claims description 35
- 239000001993 wax Substances 0.000 claims description 35
- 239000012188 paraffin wax Substances 0.000 claims description 33
- 238000002360 preparation method Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 12
- 229910052715 tantalum Inorganic materials 0.000 claims description 8
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 206010001497 Agitation Diseases 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 39
- 229910052573 porcelain Inorganic materials 0.000 abstract description 31
- 239000003989 dielectric material Substances 0.000 abstract description 21
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 229910004537 TaCl5 Inorganic materials 0.000 description 58
- 229910052799 carbon Inorganic materials 0.000 description 54
- 239000002245 particle Substances 0.000 description 35
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 29
- 239000003513 alkali Substances 0.000 description 29
- 229910052749 magnesium Inorganic materials 0.000 description 29
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 description 29
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical compound O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002253 acid Substances 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- 235000007686 potassium Nutrition 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 4
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 150000004682 monohydrates Chemical class 0.000 description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910001460 tantalum ion Inorganic materials 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- UVULZYXRKRXQGT-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;tantalum Chemical compound [Ta].OC(=O)CC(O)(C(O)=O)CC(O)=O UVULZYXRKRXQGT-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 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
- 230000005540 biological transmission Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 tantalum-citric acid compound Chemical class 0.000 description 1
Classifications
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- 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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
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- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- 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
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Abstract
The present invention provides a kind of corundum type Mg of the synthesis with sintering temperature and low4Ta2O9The method of microwave dielectric material.This method prepares citric acid, ethylene glycol and TaCl first using methanol as solvent, by certain mol proportion5Mixed solution, after stirring to clarify, be added basic magnesium carbonate, be allowed to fully react under a certain concentration, and Mg is obtained after cracking and calcining4Ta2O9Above-mentioned powder is finally carried out stir-fry wax, sieving, granulation and molding by material powder, into the porcelain of sintering under 1150 degree.The method and process of the present invention is simple, process is easy to control, instrument and equipment requirement is low.
Description
Technical field
The invention belongs to electronic ceramics preparation and applied technical fields, and in particular to a kind of to prepare sintering temperature and low corundum type
Mg4Ta2O9The method of microwave dielectric ceramic materials.
Background technology
With the fast development of microwave communication cause, mobile communication, automobile telephone, satellite television, military radar, the whole world are fixed
Demand of the position fields such as system and portable phone to miniaturization, high performance microwave circuit and microwave device increasingly increases,
Demand to the microwave dielectric material of novel superior performance is also more and more urgent.
Corundum type Mg4Ta2O9Ceramics show preferable microwave property due to its specific crystal structure.It is domestic at present
Outside about the research of the system mostly based on traditional solid phase method technique.Prepared Mg4Ta2O9Ceramics sintering temperature be
1400-1500 degree.It is high for low-temperature co-fired ceramics (Low Temperature Co-fired Ceramic, LTCC) technology
Sintering temperature can cause the decline of transmission speed and the delay of signal transmission, so reduce Mg4Ta2O9The sintering temperature of ceramics
It is extremely important.
Currently, the most common method for reducing sintering temperature mainly has：1) suitable Refractory oxides or low softening are mixed
Glass is put to reduce sintering temperature；2) wet chemical synthesis is used.It is complicated by the method and process for mixing fluxing agent, it is difficult to control
System, and be often to sacrifice the dielectric properties of ceramic material as cost, this is because passing through the ceramic powder that Mechanical Method mixes
And fluxing agent, the two mixing can be caused uneven, to increase the dosage of fluxing agent.
In conclusion corundum type Mg4Ta2O9Ceramic material has preferable microwave property, but is limited to higher sintering temperature
Degree, has seriously affected its practical value, therefore, its sintering temperature how is effectively reduced under the premise of not introducing impurity to pass
It is important.
Invention content
In view of the above-mentioned problems, it is an object of the present invention to provide more simple and easy to operate to prepare the rigid of sintering temperature and low
Beautiful type Mg4Ta2O9The method of microwave-medium ceramics.This method has simple for process, preparation process easy to control and high income etc. is excellent
Point, it is even more important that this method, can effectively will be pure under the premise of not sacrificing dielectric properties, ensureing microwave property
Mg4Ta2O9Sintering temperature be reduced to 950 degree.
In order to achieve the above-mentioned object of the invention, present invention employs the following technical solutions：
Present invention offer is a kind of to prepare sintering temperature and low corundum type Mg4Ta2O9The method of microwave dielectric ceramic materials, the party
Method includes：Using tantalic chloride and basic magnesium carbonate Mg is prepared as raw material4Ta2O9Powder, and further prepared through ceramic sintering process
Obtain Mg4Ta2O9The step of microwave dielectric ceramic materials.
Preferably, the Mg4Ta2O9The preparation of powder includes the following steps：Tantalic chloride is added in the first lower alcohol,
Obtain the alcoholic solution of tantalic chloride；It is added in above-mentioned solution after citric acid and the second lower alcohol are sufficiently mixed, stirs for the first time
Clear solution is obtained after mixing；Basic magnesium carbonate is added in above-mentioned clear solution, then second of stirring, isothermal holding exists
It is heated in air, obtains Mg4Ta2O9Powder.
Preferably, first lower alcohol is methanol or ethyl alcohol, preferably methanol；
Preferably, second lower alcohol is one or more in ethylene glycol, glycerine and 1,2-PD, preferably
For ethylene glycol.
Preferably, the first time stirring carries out 10-40 minutes, preferably 30 minutes；
Preferably, second of stirring be not less than 30 minutes.
Preferably, the molar ratio of tantalic chloride, citric acid and the second lower alcohol is 0.5~2:10~20：20~100, it is excellent
Select 0.5~1：15~20：60~80, more preferably 1：15：60.
Preferably, the molar ratio of the basic magnesium carbonate and tantalic chloride is 1：1~5, preferably 1:2.5.
Preferably, the isothermal holding is to keep the temperature 4-20 hours at 150-500 DEG C；
Preferably, the isothermal holding carries out stage by stage, is included at 150-300 DEG C and keeps the temperature 2-10 hours, then exists
2-10 hours are kept the temperature at 300-500 DEG C；
Preferably, the isothermal holding carries out stage by stage, is included at 200 DEG C and keeps the temperature 5 hours, is then protected at 450 DEG C
Temperature 5 hours.
Preferably, it after isothermal holding, is heated 10-20 hours in air at 900-1000 DEG C；
Preferably, it after isothermal holding, is heated 15 hours in air at 950 DEG C.
Preferably, the ceramic sintering process includes to Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcining
The step of processing.
Preferably, the stir-fry wax is that Mg is added4Ta2O9The paraffin of the 5-20% of powder quality carries out frying, it is preferable that institute
The addition for stating paraffin is Mg4Ta2O9The 10% of powder quality；
Preferably, the sieving was 30-80 mesh sieve, preferably crossed 60 mesh sieve；
Preferably, the briquetting pressure is 2.5-5MPa, preferably 4MPa；
Preferably, the calcination processing is carried out in Muffle furnace, and 800- is warming up to the heating rate of 3-15 DEG C/min
It 1200 DEG C, calcines 3-10 hours；It is preferred that being warming up to 950 DEG C with the heating rate of 3-5 DEG C/min, calcine 3 hours.
Preferably, the Mg4Ta2O9The particle size range of powder is 1-6 μm, preferably 1-5 μm, more preferably 1-3 μm.
Preferably, the Mg4Ta2O9The dielectric constant of microwave dielectric ceramic materials is between 10.0-12.2, more preferably
Between 10.8-12.0, further preferably between 10.8-11.5, quality factor q f preferably exists between 80000-86000
Between 83000-85900, more preferably between 84000-85900.
Compared with prior art, this patent has technique effect beneficial below：
1, the tantalum pentoxide that the tantalum source that uses of the present invention generally uses for tantalic chloride rather than the prior art, advantage exist
Can form complex with methanol or ethyl alcohol in tantalic chloride, the complex during subsequent reactions by slow release tantalum from
Son achievees the purpose that control reaction rate, can preferably control prepared Mg in this way4Ta2O9The particle size range of powder and crystallization
Degree is conducive to the physical and chemical performance for improving material.
In addition, present invention discover that the molar ratio of tantalic chloride, citric acid and the second lower alcohol (such as ethylene glycol) is limited
For 0.5-2：10‐20：20-100, especially 0.5-1：15‐20：60-80, more particularly 1：15：Best results when 60, reason
May be：Foregoing tantalic chloride forms tantalum -ol complex with methanol or ethyl alcohol first, and the alcohol liquid of citric acid is added
Afterwards, the coordination ability of citric acid and tantalum ion is stronger, can capture tantalum ion from tantalum -ol complex, forms tantalum-citric acid cooperation
Object, the two category competitive relation.The concentration of tantalum-citric acid compound is to influence subsequent reactions rate and Mg4Ta2O9Material materialization
An important factor for performance.In addition, present invention discover that the addition sequence of the second lower alcohol (such as ethylene glycol) can generate shadow to result
It rings, present invention discover that after being first sufficiently mixed citric acid and the second lower alcohol, then add it to the alcoholic solution of tantalic chloride
Middle best results, thus it is speculated that so operation is conducive to the full and uniform contact with tantalum ion.
2, present invention effectively prevents the strong acid (such as nitric acid) during material preparation or strong corrosive acid (such as hydrogen fluorine
Acid) use, greatly reduce the requirement to Preparation equipment, and reduce production cost, and be conducive to environmental protection.
3, compared with prior art, the present invention flow is short, easy to operate.
Description of the drawings
Hereinafter, carry out the embodiment that the present invention will be described in detail in conjunction with attached drawing, wherein：
Fig. 1 is Mg prepared by the embodiment of the present invention 14Ta2O9The XRD diagram of powder body material；
Fig. 2 is Mg prepared by the embodiment of the present invention 14Ta2O9The SEM of powder body material schemes.
Specific implementation mode
The present invention is described below with reference to specific embodiments.It will be appreciated by those skilled in the art that these embodiments are only
For illustrating the present invention, do not limit the scope of the invention in any way.
Experimental method in following embodiments is unless otherwise specified conventional method.Medicine as used in the following examples
Material raw material, reagent material etc. are commercially available products unless otherwise specified.
Embodiment 1Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm, Mg4Ta2O9The XRD diagram of powder body material such as Fig. 1 institutes
Show, SEM figures are as shown in Figure 2；Mg after tested4Ta2O9The microwave property of ceramic material is ε r=10.8, Qf=85900GHz.
Embodiment 2Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 2.5g TaCl5, it is dissolved into methanol；It weighs
44g monohydrate potassiums, measure 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein
The molar ratio of the tantalic chloride, citric acid and ethylene glycol is 0.5：15：60, stir about 30 minutes to solution is clarified；Weigh alkali
Formula magnesium carbonate (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes,
200 DEG C keep the temperature 5 hours, then continue heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain
Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-6 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.0, Qf=83100GHz.
Embodiment 3Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 10g TaCl5, it is dissolved into methanol；It weighs
44g monohydrate potassiums, measure 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein
The molar ratio of the tantalic chloride, citric acid and ethylene glycol is 2：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula
Magnesium carbonate (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, 200
DEG C heat preservation 5 hours, then continue at 450 DEG C heat preservation 5 hours；At 950 DEG C, in air, heats 15 hours, obtain
Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.2, Qf=80900GHz.
Embodiment 4Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 30g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：10：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.2, Qf=80000GHz.
Embodiment 5Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 66g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：20：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.2, Qf=84900GHz.
Embodiment 6Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 66g
Monohydrate potassium, measures 15.52ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：20, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-6 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.2, Qf=8000GHz.
Embodiment 7Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 66g
Monohydrate potassium, measures 62.11ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：80, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.2, Qf=83000GHz.
Embodiment 8Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 66g
Monohydrate potassium, measures 77.63ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：100, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-6 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.2, Qf=81950GH.
Embodiment 9Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 10g TaCl5, it is dissolved into methanol；It weighs
44g monohydrate potassiums, measure 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein
The molar ratio of the tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula
Magnesium carbonate (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, 200
5 hours are kept the temperature at DEG C, then continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain
Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 8Mpa；Calcined using Muffle furnace, heating rate be 10 DEG C/
Min is sintered 3 hours at 1200 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.7, Qf=82300GHz.
Embodiment 10Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Lower heat preservation 5 hours, then continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain
Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 15%, 80 mesh of sieving are granulated, briquetting pressure 5Mpa；Calcined using Muffle furnace, heating rate be 15 DEG C/
Min is sintered 5 hours at 800 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.0, Qf=80200GHz.
Embodiment 11Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 150 DEG C
Then heat preservation 2 hours continues heat preservation 10 hours at 500 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-6 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.9, Qf=83500GHz.
Embodiment 12Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 300 DEG C
Then heat preservation 10 hours continues heat preservation 2 hours at 300 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.8, Qf=84600GHz.
Embodiment 13Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 1000 DEG C, in air, heats 10 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.2, Qf=84300GHz.
Embodiment 14Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 900 DEG C, in air, heats 20 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-5 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.3, Qf=84710GHz.
Embodiment 15Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 20%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.0, Qf=84800GHz.
Embodiment 16Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 5%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；It is calcined using Muffle furnace, heating rate is 5 DEG C/min,
It is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.1, Qf=85000GHz.
Embodiment 17Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 3 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=10.9, Qf=85500GHz.
Embodiment 18Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：1) it, is added in clear solution, stir about 30 minutes, is protected at 200 DEG C
Then temperature 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9Powder
Body.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.2, Qf=80000GHz.
Embodiment 19Sintering temperature and low corundum type Mg4Ta2O9The preparation of microwave dielectric material
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：5) it, is added in clear solution, stir about 30 minutes, is protected at 200 DEG C
Then temperature 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9Powder
Body.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=11.9, Qf=82950GHz.
Comparative example 1
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 0.2：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula
Magnesium carbonate (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, 200
DEG C heat preservation 5 hours, then continue at 450 DEG C heat preservation 5 hours；At 950 DEG C, in air, heats 15 hours, obtain
Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-8 μm；Mg after tested4Ta2O9Ceramic material microwave performance is
ε r=12.3, Qf=82000GHz.
Comparative example 2
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 3：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 2-7 μm；Mg after tested4Ta2O9The microwave property of ceramic material
For ε r=12.3, Qf=80500GHz.
Comparative example 3
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 450 DEG C
Lower heat preservation 10 hours；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 3-8 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.5, Qf=77800GHz.
Comparative example 4
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 850 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 3-8 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.9, Qf=79900GHz.
Comparative example 5
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 1200 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 2-7 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.1, Qf=78000GHz.
Comparative example 6
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 2 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.4, Qf=80500GHz.
Comparative example 7
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder,
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 18 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.6, Qf=80100GHz.
Comparative example 8
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 700 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.4, Qf=80010GHz.
Comparative example 9
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, stir about 30 minutes, at 200 DEG C
Then heat preservation 5 hours continues heat preservation 5 hours at 450 DEG C；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9
Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 1350 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 1-3 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=12.8, Qf=83200GHz.
Comparative example 10
15ml methanol is measured, is placed in the beaker that volume is 50ml, weighs 5g TaCl5, it is dissolved into methanol；Weigh 44g
Monohydrate potassium, measures 46.58ml ethylene glycol, and the two is added to TaCl after being sufficiently mixed5Methanol solution in, wherein institute
The molar ratio for stating tantalic chloride, citric acid and ethylene glycol is 1：15：60, stir about 30 minutes to solution is clarified；Weigh alkali formula carbon
Sour magnesium (basic magnesium carbonate and TaCl5Molar ratio be 1：2.5) it, is added in clear solution, adulterates H3BO3(doping 5%
Mg4Ta2O9Theoretical weight), stir about 30 minutes keeps the temperature 5 hours at 200 DEG C, and it is 5 small then to continue heat preservation at 450 DEG C
When；At 950 DEG C, in air, heats 15 hours, obtain Mg4Ta2O9Powder.
By above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, and the quality of wherein paraffin accounts for
Than being 10%, 60 mesh of sieving are granulated, briquetting pressure 4Mpa；Calcined using Muffle furnace, heating rate be 5 DEG C/
Min is sintered 3 hours at 950 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 2-8 μm；After tested, Mg4Ta2O9The microwave of ceramic material
Can be ε r=10.9, Qf=82900GHz.
Comparative example 11
(1) aqueous citric acid solution of tantalum is prepared
(a) it is 1: 5 dispensing according to the molar ratio of tantalum pentoxide and potassium carbonate, weighs tantalum pentoxide powder respectively
5.326 grams, 13.819 grams of cosolvent potassium carbonate；Tantalum pentoxide powder is uniformly mixed with potassium carbonate powder, is packed into high alumina crucible
It is interior, 2h is melted in 1000 degree, obtains potassium tantalate；
(b) potassium tantalate of step (a) is dissolved in 500ml deionized waters, nitric acid is added, it is 3 to adjust its pH value, it is ensured that complete
Portion generates tantalic acid precipitation；
(c) 15.3712 grams of citric acid is weighed, 500ml deionized waters are added, forms aqueous citric acid solution；By above-mentioned steps
(b) tantalic acid precipitation is centrifuged, washs, and then the tantalic acid is added in aqueous citric acid solution, and in 80 DEG C of water-bath
Heating, makes tantalic acid be completely dissolved, forms the aqueous citric acid solution of tantalum.
(2) aqueous citric acid solution of magnesium is prepared
(a) 20.513 grams of magnesium nitrate hexahydrate is weighed, 100ml deionized waters are dissolved in；
(b) and then 76.856 grams of citric acid is weighed, and be added to above-mentioned solution, ensure mole of citric acid and magnesium nitrate
Than being 5: 1, ensure that dissolving is abundant, it is 3 to adjust its pH value；
(c) 80 DEG C of heating of water-bath, are stirred continuously, and ensure the aqueous citric acid solution for forming magnesium.
(3) acquisition of Mg-Ta precursor solutions, xerogel and nano-powder
(a) aqueous citric acid solution of the aqueous citric acid solution of tantalum prepared by above-mentioned (1), (2), magnesium is uniformly mixed, then
Ethylene glycol is added as esterifying agent, the addition mole of ethylene glycol is 4 times of citric acid；By 80 DEG C of heating of water-bath, constantly stir
It mixes, ensures uniform, acquisition Mg-Ta precursor solutions；
(b) the Mg-Ta precursor solutions of preparation are placed in 100 DEG C of baking oven to dry, form xerogel；
(c) it uses under 550 DEG C of oxygen atmospheres of chamber type electric resistance furnace and xerogel is subjected to calcination processing；By further grinding,
Can obtain uniformly, the tiny nanoscale tantalic acid magnesium (Mg of particle4Ta2O9) powder；Using field emission scanning electron microscope (JEOL JSM-
7600F, Japan) average particle size distribution of the nano-powder particle is tested as 40-50nm.
(4) by above-mentioned Mg4Ta2O9Powder carries out stir-fry wax, sieving, granulation, molding and calcination processing, the wherein matter of paraffin
It is 10% to measure accounting, and 60 mesh of sieving are granulated, briquetting pressure 4Mpa；It is calcined using Muffle furnace, heating rate 5
DEG C/min, it is sintered 3 hours at 1150 DEG C and sinters porcelain into.
Wherein, Mg4Ta2O9The particle size range of powder body material is 50-80nm；After tested, Mg4Ta2O9The microwave of ceramic material
Performance is ε r=12.9, Qf=82200GHz.
Specific description of embodiments of the present invention above is not intended to limit the present invention, and those skilled in the art can be according to this
Invention is variously modified or deforms, and without departing from the spirit of the present invention, should all belong to the model of appended claims of the present invention
It encloses.
Claims (10)
1. a kind of preparing sintering temperature and low corundum type Mg4Ta2O9The method of microwave dielectric ceramic materials, this method include：With pentachloro-
It is that raw material prepares Mg to change tantalum and basic magnesium carbonate4Ta2O9Powder, and Mg further is prepared through ceramic sintering process4Ta2O9It is micro-
The step of wave medium ceramic material.
2. according to the method described in claim 1, it is characterized in that, the Mg4Ta2O9The preparation of powder includes the following steps：It will
Tantalic chloride is added in the first lower alcohol, obtains the alcoholic solution of tantalic chloride；After citric acid and the second lower alcohol are sufficiently mixed
It is added in above-mentioned solution, clear solution is obtained after stirring for the first time；Basic magnesium carbonate is added in above-mentioned clear solution, the
Then secondary agitation, isothermal holding heat in air, obtain Mg4Ta2O9Powder.
3. according to the method described in claim 2, it is characterized in that, first lower alcohol is methanol or ethyl alcohol, preferably methanol；
Preferably, second lower alcohol is one or more in ethylene glycol, glycerine and 1,2-PD, preferably second
Glycol.
4. according to the method described in claim 2, it is characterized in that, first time stirring carries out 10-40 minutes, preferably 30 points
Clock；
Preferably, second of stirring be not less than 30 minutes.
5. according to the method described in claim 2, it is characterized in that, the molar ratio of tantalic chloride, citric acid and the second lower alcohol
For 0.5-2：10‐20：20-100, preferably 0.5-1：15‐20：60‐80:, more preferably 1：15：60.
6. method according to claim 1 or 2, which is characterized in that the molar ratio of the basic magnesium carbonate and tantalic chloride
It is 1:1-5, preferably 1:2.5.
7. according to the method described in claim 2, it is characterized in that, the isothermal holding is to keep the temperature 4-20 at 150-500 DEG C
Hour；
Preferably, the isothermal holding carries out stage by stage, is included at 150-300 DEG C and keeps the temperature 2-10 hours, then in 300-500
2-10 hours are kept the temperature at DEG C；
Preferably, the isothermal holding carries out stage by stage, is included at 200 DEG C and keeps the temperature 5 hours, and then heat preservation 5 is small at 450 DEG C
When.
8. according to the method described in claim 2, it is characterized in that, after isothermal holding, add in air at 900-1000 DEG C
It is 10-20 hours hot；
Preferably, it after isothermal holding, is heated 15 hours in air at 950 DEG C.
9. method according to claim 1 or 2, which is characterized in that the ceramic sintering process includes to Mg4Ta2O9Powder
The step of carrying out stir-fry wax, sieving, granulation, molding and calcination processing；
Preferably, the stir-fry wax is that Mg is added4Ta2O9The paraffin of the 5-20% of powder quality carries out frying, it is preferable that the stone
The addition of wax is Mg4Ta2O9The 10% of powder quality；
Preferably, the sieving was 30-80 mesh sieve, preferably crossed 60 mesh sieve；
Preferably, the briquetting pressure is 2.5-5MPa, preferably 4MPa；
Preferably, the calcination processing is carried out in Muffle furnace, and 800-1200 is warming up to the heating rate of 3-15 DEG C/min
DEG C, it calcines 3-10 hours；It is preferred that being warming up to 950 DEG C with the heating rate of 3-5 DEG C/min, calcine 3 hours.
10. method according to any one of claim 1 to 9, which is characterized in that the Mg4Ta2O9The grain size model of powder
Enclose is 1-6 μm, preferably 1-5 μm, more preferably 1-3 μm；
Preferably, the Mg4Ta2O9The dielectric constant of microwave dielectric ceramic materials is between 10.0-12.2, preferably in 10.8-
Between 12.0, more preferably between 10.8-11.5, quality factor q f is between 80000-86000, preferably in 83000-85900
Between, more preferably between 84000-85900.
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| CN112979311A (en) * | 2021-04-30 | 2021-06-18 | 昆明理工大学 | Nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and method thereof |
| CN113105237A (en) * | 2021-04-30 | 2021-07-13 | 昆明理工大学 | AB2O6 type tantalate ceramic and preparation method thereof |
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| CN101774812A (en) * | 2010-02-02 | 2010-07-14 | 天津大学 | Method for preparing magnesium tantalate microwave ceramic powder by sol-gel technique |
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| CN101774812A (en) * | 2010-02-02 | 2010-07-14 | 天津大学 | Method for preparing magnesium tantalate microwave ceramic powder by sol-gel technique |
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| JUDIT SZANICS等: "Preparation of LiTaO3 powders at reduced temperatures by a polymerized complex method", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112979311A (en) * | 2021-04-30 | 2021-06-18 | 昆明理工大学 | Nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and method thereof |
| CN113105237A (en) * | 2021-04-30 | 2021-07-13 | 昆明理工大学 | AB2O6 type tantalate ceramic and preparation method thereof |
| CN113105237B (en) * | 2021-04-30 | 2023-02-17 | 昆明理工大学 | AB2O6 type tantalate ceramic and preparation method thereof |
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