CN109056076A - A kind of preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material - Google Patents
A kind of preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material Download PDFInfo
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- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 39
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 30
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 28
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 22
- 150000007524 organic acids Chemical class 0.000 claims description 21
- 150000002500 ions Chemical class 0.000 claims description 16
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 7
- 238000007710 freezing Methods 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 239000002270 dispersing agent Substances 0.000 abstract description 9
- 238000003837 high-temperature calcination Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 20
- 229910002804 graphite Inorganic materials 0.000 description 11
- 239000010439 graphite Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 7
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 229910003327 LiNbO3 Inorganic materials 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000012286 potassium permanganate Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002525 ultrasonication Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000138 intercalating agent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000004317 sodium nitrate Substances 0.000 description 3
- 235000010344 sodium nitrate Nutrition 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- -1 Graphite alkene Chemical class 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to field of inorganic material preparing technology, more particularly to the preparation method of a kind of doped lithium columbate presoma and doped polycrystalline lithium niobate material, the method is using graphene oxide solution as dispersing agent, the doped lithium columbate presoma containing graphene oxide is obtained by liquid phase synthesis, high-temperature calcination removes graphene oxide again, obtained doped polycrystalline lithium niobate material is high-purity and uniformly mixed, and method is simple, is suitble to industrialized mass production.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, and in particular to a kind of doped lithium columbate presoma and doped lithium columbate are more
The preparation method of crystalline substance material.
Background technique
Lithium niobate (LiNbO3, abbreviation LN) crystal be it is a kind of collect the functions such as non-linear, electric light, piezoelectricity, photoelastic, Preset grating in
The multi-functional crystal of one, it not only has good thermal stability, chemical stability and mechanical stability, but also is easy to add
Work, cost of material are in contrast also relatively cheap.Therefore LN is with crystal as, is that minority is lasting and do not turn off and ward off application
The critical function material of frontier.
LN crystal is a kind of typical non-stoichiometric crystal, and czochralski method or Bridgman-Stockbarger method can be used from congruent
Growth obtains congruent lithium columbate crystal (CLN) in LN melt.Missing in CLN crystal due to lithium ion causes to deposit in crystal
In a large amount of vacancy defect and antistructure defect intrinsic defect, some important physicals of LN crystal and optical property are affected.Crystal
In Li/Nb be stoichiometric ratio lithium columbate crystal be known as stoichiometric ratio lithium niobate crystal (SLN), to reach complete chemistry
Metering is difficult than (Li/Nb=50/50 molar ratio), and by improving crystal technique, people can be obtained close to stoichiometry
Than lithium columbate crystal, therefore sometimes referred to as lithium niobate crysal near stoichiometric ratio (NSLN), SLN or NSLN crystal it is some important
Physical property and optical property are apparently higher than CLN crystal.
The preparation method of traditional doped crystal growth raw material is by by doped chemical oxide, niobium oxide, lithium carbonate
Powder mixing forms polycrystalline lithium niobate material in 1150 DEG C of high-temperature calcinations.Although the method can largely prepare polycrystal material,
Since the fusing point of doping oxide particle is very high, and nano-oxide itself is easy to reunite, it is not easy to be evenly mixed in oxidation
In niobium and lithium carbonate mixed powder, it is not easy Uniform Doped in polycrystal material so as to cause oxide, in crystal growing process
It can not be completely melt, cause the inclusion enclave for occurring oxide concentration in doped crystal.Therefore, exploitation can make doping oxide
It is dispersed in polycrystal material and the preparation method for being able to batch generation is very necessary.
Summary of the invention
Non-uniform technical problem is adulterated for existing solid phase method, it is an object of the present invention to provide a kind of doping niobic acids
The preparation method of lithium presoma, the method are obtained by liquid phase synthesis containing oxidation using graphene oxide solution as dispersing agent
The doped lithium columbate presoma of graphene, then high-temperature calcination remove graphene oxide, and obtained doped polycrystalline lithium niobate material is high-purity
And be uniformly mixed, and method is simple, it is suitble to industrialized mass production.
It is a further object to provide a kind of preparation methods of doped polycrystalline lithium niobate material, and the method is to adulterate
Lithium niobate presoma is raw material, and the doped polycrystalline lithium niobate material being prepared is not only with high purity, uniformly mixed, and fusing point reduces,
, not only can be energy saving during growing lithium columbate crystal as raw material using doped polycrystalline lithium niobate material, and for even
For continuous charging growth technique, it can prevent from floating crystalline substance phenomenon caused by the addition of polycrystal material during the growth process.
For achieving the above object, the present invention the following technical schemes are provided:
A kind of preparation method of doped lithium columbate presoma, comprising the following steps:
Step (1): Doped ions oxide is added in organic acid, and it is rear cold to being completely dissolved to be heated to 50~80 DEG C of stirrings
But to room temperature, the dosage of the organic acid contains 1 in terms of the quality of lithium carbonate, by above-mentioned organic acid dilute to every 4~8ml organic acid
~5 grams of lithium carbonates, with the molar amount of niobium pentaoxide, Doped ions oxide rubs the dosage of the Doped ions oxide
Your amount is the 0.1%~7% of niobium pentaoxide mole；
Step (2): being added graphene oxide solution into step (1) acquired solution, adjusts pH value of solution >=7, institute with ammonium hydroxide
The dosage of graphene oxide solution is stated in terms of the quality of lithium carbonate, the volume mass ratio of graphene oxide solution and lithium carbonate is
1ml:20g~1ml:50g；
Step (3): niobium pentaoxide and lithium carbonate being added into step (2) acquired solution, and ultrasonic agitation divides it completely
It dissipates, forms uniformly mixed suspension, the molar ratio of the niobium pentaoxide and lithium carbonate is 41.5:58.5；
Step (4): it by the freezing of suspension obtained by step (3), is dried in vacuo up to doped lithium columbate presoma.
Second aspect, the present invention provide a kind of preparation method of doped polycrystalline lithium niobate material, including by doping of the invention
Lithium niobate presoma 1100 DEG C temperature lower calcination 10h to obtain the final product.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (1)
Doped ions oxide is in magnesia, zinc oxide, indium oxide, iron oxide, copper oxide, manganese oxide, erbium oxide, chromium oxide
It is at least one.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (1)
Organic acid is selected from citric acid and malic acid.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (1)
Organic acid dilute to 4ml organic acid contains 1 gram of lithium carbonate.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (1)
The dosage of Doped ions oxide is niobium pentaoxide with the molar amount of niobium pentaoxide, the mole of Doped ions oxide
The 0.1%~3% of mole.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (2)
PH value of solution is adjusted to 7-9.
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (2)
For the dosage of graphene oxide solution in terms of the quality of lithium carbonate, the volume mass ratio of graphene oxide solution and lithium carbonate is 1ml:
20g。
The preparation method of doped lithium columbate presoma and doped polycrystalline lithium niobate material according to the present invention, described in step (2)
Graphene oxide solution be by least one in potassium permanganate and the concentrated sulfuric acid, concentrated nitric acid or the concentrated sulfuric acid and sodium nitrate mixture
After graphite oxide is prepared with Hummers method in kind, ultrasonic disperse is made in water；Specifically, oxygen described in step (2)
Graphite alkene solution is using crystalline flake graphite as raw material, at least one in the concentrated sulfuric acid, concentrated nitric acid or the concentrated sulfuric acid and sodium nitrate mixture
Kind is intercalator, and potassium permanganate is acid oxidant, graphite oxide is prepared with Hummers method, then take above-mentioned graphite oxide
It is added to the water and carries out the clear liquid of ultrasonication, standing, centrifugation.
The inventors discovered that dispersing agent and its dosage doped polycrystalline lithium niobate material quality obtained is influenced it is very big, when making
With other dispersing agents, such as Tween 80, oxide ion dispersion is uneven in doped polycrystalline lithium niobate material obtained, and uses oxidation stone
Black alkene as dispersing agent, inventors have found that when the volume mass of graphene oxide solution and lithium carbonate ratio be greater than 1ml:20g when,
Mixed effect is not improved；When the volume mass of graphene oxide solution and lithium carbonate ratio is less than 1ml:50g, mixed effect
It is bad；When the volume mass of graphene oxide solution and lithium carbonate ratio is 1ml:20g~1ml:50g, oxide is enabled to
Ion, niobium pentaoxide and lithium carbonate are uniformly adsorbed on the surface of graphene oxide, mix them thoroughly uniformly simultaneous oxidation
Graphene is easy to remove, and will not introduce other impurities pollution raw material.
The method provided by the invention for preparing doped lithium columbate presoma passes through using graphene oxide solution as dispersing agent
The method of liquid phase synthesis, so that oxide ion, niobium pentaoxide and lithium carbonate are uniformly adsorbed on the surface of graphene oxide,
It is uniformly mixed it, then by freezing, vacuum drying method, it is obtained containing graphene oxide doped lithium niobate presoma,
Graphene oxide is removed by high-temperature calcination, high-purity, uniformly mixed doped polycrystalline lithium niobate material can be obtained, be very suitable to niobium
The preparation of sour crystalline lithium.
Specific embodiment
The preparation of 1 graphene oxide solution of embodiment
Using crystalline flake graphite 10g as raw material, using concentrated sulfuric acid 250mL and sodium nitrate 10g as intercalator, potassium permanganate 40g is acid
Oxidant, oxidation reaction 5 hours.30% aqueous hydrogen peroxide solution 30mL is poured into again, is reacted 1 hour, is then used deionized water
Being washed till filtrate pH is 7, filtering, 80 DEG C of drying, i.e. acquisition graphite oxide.Above-mentioned graphite oxide 30mg is taken, the burning of 250mL is added to
In cup, add water to carry out ultrasonication to 100mL, the ultrasonication time is set to 30 minutes, takes out and stand, existed with centrifuge
It is centrifuged 20min under conditions of 12000 revs/min, the clear liquid after taking centrifugation, i.e. acquisition graphene oxide solution.
The preparation of 2 graphene oxide solution of embodiment
Using crystalline flake graphite 10g as raw material, using concentrated sulfuric acid 250mL and nitric acid 50mL as intercalator, potassium permanganate 40g is sour oxygen
Agent is reacted 5 hours, then pours into 30% aqueous hydrogen peroxide solution 30mL, is reacted 1 hour, is then washed with deionized water to filtrate
PH is 7, filtering, 80 DEG C of drying, i.e. acquisition graphite oxide, takes above-mentioned graphite oxide 30mg, is added in the beaker of 250mL, adds
Water carries out ultrasonication 30 minutes to 100mL, takes out and stands, and is centrifuged 20min with centrifuge, the revolving speed of centrifugation is 12000 revs/min
Clock.Clear liquid after taking centrifugation, i.e. acquisition graphene oxide solution.
The preparation of 3 doped polycrystalline lithium niobate material of embodiment
According to 2LiCO3+Nb2O5+ 0.1%MgO=MgO:LiNbO3Proportion weighed, weigh 0.0768gMgO addition
Into the organic acid of 10ml, heating stirring is settled to 800ml to being completely dissolved, and graphene oxide dispersing agent 4ml is added, and is added dropwise
Ammonium hydroxide adjusts pH >=7 of solution, and 510.4g niobium pentaoxide and 200g lithium carbonate are added into solution, and ultrasonic agitation keeps its complete
Full dispersion, suspends in the solution, forms uniformly mixed suspension, and freezing, vacuum drying obtain mixing containing graphene oxide
Miscellaneous lithium niobate presoma.The uniform doped polycrystalline lithium niobate material of ingredient is obtained using 1100 DEG C of high-temperature calcination 10h.
The preparation of 4 doped polycrystalline lithium niobate material of embodiment
According to 2LiCO3+Nb2O5+ 7%ZnO=ZnO:LiNbO3Proportion weighed, weigh 10.94gZnO and be added to
In the organic acid of 800ml, heating stirring is settled to 800ml to being completely dissolved, and graphene oxide dispersing agent 10ml is added, and is added dropwise
Ammonium hydroxide adjusts pH >=7 of solution, and 510.4g niobium pentaoxide and 200g lithium carbonate are added into solution, and ultrasonic agitation keeps its complete
Full dispersion, suspends in the solution, forms uniformly mixed suspension, and freezing, vacuum drying obtain mixing containing graphene oxide
Miscellaneous lithium niobate presoma.The uniform doped polycrystalline lithium niobate material of ingredient is obtained using 1100 DEG C of high-temperature calcination 10h.
The preparation of 5 doped polycrystalline lithium niobate material of embodiment
According to 2LiCO3+Nb2O5+ 3%Fe2O3=Fe2O3:LiNbO3Proportion weighed, weigh 15.36gFe2O3Add
Entering into the organic acid of 500ml, heating stirring is settled to 800ml to being completely dissolved, graphene oxide dispersing agent 10ml is added,
PH >=7 that ammonium hydroxide adjusts solution are added dropwise, 510.4g niobium pentaoxide and 200g lithium carbonate are added into solution, ultrasonic agitation makes
It is completely dispersed, and suspends in the solution, forms uniformly mixed suspension, and freezing, vacuum drying are obtained containing graphene oxide
Doped lithium columbate presoma.The uniform doped polycrystalline lithium niobate material of ingredient is obtained using 1100 DEG C of high-temperature calcination 10h.
Claims (8)
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