CN107555473A - A kind of nanometer BaTiO3Raw powder's production technology - Google Patents
A kind of nanometer BaTiO3Raw powder's production technology Download PDFInfo
- Publication number
- CN107555473A CN107555473A CN201710898425.2A CN201710898425A CN107555473A CN 107555473 A CN107555473 A CN 107555473A CN 201710898425 A CN201710898425 A CN 201710898425A CN 107555473 A CN107555473 A CN 107555473A
- Authority
- CN
- China
- Prior art keywords
- barium
- powder
- batio
- solution
- nitrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of nanometer BaTiO3Raw powder's production technology, using titanyl nitrate solution as titanium source, barium nitrate or barium acetate are barium source, and deionized water is as solvent, first using barium titanium mol ratio as 0.8 1.2:1 prepares barium nitrate, titanyl nitrate solution, the two is uniformly mixed, mixed solution is slowly dropped into as in the ammonium hydrogen carbonate of precipitating reagent and the mixed liquor of ammoniacal liquor again afterwards, precipitating reagent is excessive, do not stop to stir, ammonium hydrogen carbonate and ammonia water mixture pH value are kept more than 8.5, after precipitation, by centrifuge precipitation and separation, drying, grinding, annealing, that is, obtain a nanometer BaTiO3Powder.The method of the present invention is easily operated, employs nitrate in preparation process, and the foreign ion remained during washing decomposes in sintering, volatilization, is easy to prepare high-purity BaTiO3Powder, contribute to the later stage to introduce the nitrate of rare earth element and prepare BaTiO3Base rare-earth-doped modification nano-powder.
Description
Technical field
The present invention relates to novel nano-material technical field, and in particular to a kind of nanometer BaTiO3Raw powder's production technology.
Background technology
Barium titanate is the basic parent stock of electrode component, be in electronic ceramics most popular material it
One, it is described as " pillar of electronic ceramics industry ".It is excellent ferroelectricity, piezoelectricity, pressure-resistant and exhausted because it has a high dielectric constant
Edge performance, it is widely used in multi-layer capacitor (MLCC), positive temperature coefficient (PTC) thermistor, piezoelectric ceramics etc..With electricity
Sub- ceramic industry develops rapidly, and the demand of barium titanate is increasing, for preparing barium phthalate base rare-earth-doped modification powder, height
The requirement of pure Super-fine Barium Titanate is also more and more urgent.
Traditional BaTiO3Ceramic powder preparation method is with BaCO3And TiO2For raw material, the high temperature bar more than 1150 DEG C
Obtained under part through solid phase reaction, the doping of traditional solid phase requires powder purity height, fine size, and technique has serious doping not
Uniform phenomenon, influence the dielectric properties of ceramics.Preparation method main at present has：Solid sintering technology, sol-gal process, hydro-thermal
The techniques such as method, oxalate coprecipitation method, hydrogen peroxide coprecipitation, hydro-thermal method.But the method that presently, there are also has the shortcomings that respective,
As sol-gal process process conditions are difficult to control, are difficult to heavy industrialization；Oxalate precipitation process barium titanium controls than difficult；It is double
Oxygen water coprecipitation is difficult to control doping when introducing rare earth ion progress alms giver, acceptor doping, substituting；Hydro-thermal method compares
It is suitable for preparing one pack system powder, it is big using difficulty for the modern functions ceramic powder of complicated components.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation method of nano barium carbonate powder, this method is easily operated, prepares
Barium nitrate or barium acetate are employed in journey, titanyl nitrate solution dissolves each other with barium nitrate or barium acetate in water, remains during washing
Foreign ion decomposes in sintering, volatilization, does not introduce foreign ion, is easy to prepare high-purity BaTiO3Powder, the later stage is contributed to draw
The nitrate for entering rare earth element prepares BaTiO3Base rare-earth-doped modification nano-powder.
The object of the invention to solve the technical problems is realized using following technical scheme.Itd is proposed according to the present invention
A kind of nanometer BaTiO3Raw powder's production technology, using titanyl nitrate solution as titanium source, barium nitrate or barium acetate are barium source, go from
Sub- water is as solvent, first using barium titanium mol ratio as 0.8-1.2：1 fills the solution of barium nitrate or barium acetate and titanyl nitrate solution
Point stirring, is well mixed, then will it is well mixed after solution be slowly dropped into as precipitating reagent ammonium hydrogen carbonate and ammoniacal liquor it is mixed
Closing in liquid, precipitating reagent is excessive, does not stop to stir, and keeps ammonium hydrogen carbonate and ammonia water mixture pH value after 8.5-11, precipitation,
By centrifuge precipitation and separation, upper strata settled solution is taken to be detected with pH meter or pH test paper, solution ph is a little in 8.5-11, instillation
Ba(OH)2Reagent (checking), there is precipitation to produce, illustrate that carbonate and hydroxyl are excessive in mixed solution, ensure Ba2+、TiO2+'s
Precipitation completely, can guarantee that the purity of final products；Precipitation after centrifuge is separated obtains nanometer through drying, grinding, annealing
BaTiO3Powder.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
Foregoing nanometer BaTiO3Raw powder's production technology, wherein, described barium titanium mol ratio is 1：1.
Foregoing nanometer BaTiO3Raw powder's production technology, wherein, the operation of centrifuge precipitation and separation is：3000 turns/
Centrifugation 5 minutes, described annealing operation are under point：Anneal 2-3h at 1100 DEG C.
Foregoing nanometer BaTiO3Raw powder's production technology, wherein, the preparation method of the titanyl nitrate solution is：With titanium
Acid butyl ester and concentrated nitric acid are raw material, and the butyl titanate refers to Ti (OC4H9)4AR reagents, the mass fraction of the concentrated nitric acid are
65%, by Ti (OC4H9)4：HNO3=1：3~5 mol ratio, a certain amount of butyl titanate is taken, adds deionization while stirring
Water, until thering is white precipitate to produce and being linked to be bulk, obtain Ti (OC4H9)4The reacted suspension of-deionized water；Take again corresponding
The concentrated nitric acid of amount, it is slowly dropped to above-mentioned Ti (OC4H9)4In the reacted suspension of-deionized water, stir 3~4 hours, precipitation
Constantly dissolving, obtains clear solution, stands, lower floor is titanyl nitrate, and the titanyl nitrate refers to TiO (NO3)2, upper strata has few
The butanol of amount, because organic matter decomposes during follow-up sintering, volatilizees, a small amount of butanol does not influence to test.Therefore, above-mentioned institute
Titanyl nitrate solution is obtained to be used directly for preparing BaTiO3。
The preparation method of foregoing titanyl nitrate solution, wherein, Ti (OC4H9)4With HNO3Mol ratio be 1：4.
The preparation method of foregoing titanyl nitrate solution, wherein, the preparation dosage of the titanyl nitrate solution is：
0.015molTi(OC4H9)4、0.06molHNO3, 100ml deionized waters.
Advantages of the present invention and effect are：
The method of the present invention is simple to operation, and all foreign ions volatilize in sintering process, therefore in preparation process,
It need not repeatedly be washed, not introduce foreign ion, the nano barium carbonate powder of high pure and ultra-fine can be obtained.Preparation process
In, titanyl nitrate solution dissolves each other with barium nitrate or barium acetate in water, is mixed solution and adds in precipitating reagent, through separating, forging
Burn and can obtain nano barium phthalate.Using this method and principle, rare earth doping elements can be added simultaneously, prepare rear-earth-doped change
The BaTiO of property3Nano-powder, such as rare earth ion (Nd3+、Y3+、Mn2+、ZrO2+Deng) nitrate can under aqueous solvent with nitric acid
Oxygen titanium, barium nitrate are molten altogether, and three is mixed, and carry out proper treatment, can prepare the BaTiO of rare-earth-doped modification3Powder.Utilize this
Method, it can accurately calculate BaTiO3And the initial component of adulterated powder, beneficial to the introducing and control of doping component, so that accurately,
Easily prepare rear-earth-doped BaTiO3Base nano-powder.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the present invention above-mentioned advantage and other purposes, feature and advantage
It can become apparent, below especially exemplified by preferred embodiment, describe in detail as follows.
Brief description of the drawings
Fig. 1 prepares BaTiO for the present invention3The flow chart of nano-powder；
Fig. 2 is gained BaTiO after annealing3The XRD diffraction maximums of powder and standard spectrum comparison diagram；
Fig. 3 is gained BaTiO after annealing3The SEM figures of powder.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Accompanying drawing and preferred embodiment, to according to a kind of nano-BaTiO_3 powder raw powder's production technology proposed by the present invention, its specific embodiment party
Formula, structure, feature and its effect, describe in detail as after.
1st, the preparation of titanyl nitrate solution
With butyl titanate (Ti (OC4H9)4AR reagents) and concentrated nitric acid (mass fraction 65%) be raw material, by Ti
(OC4H9)4：HNO3=1：4 mol ratio, appropriate deionized water, choose raw material.This patent uses 0.015mol Ti (OC4H9)4、
0.06molHNO3, 100ml deionized waters configuration titanyl nitrate solution.
Take a certain amount of butyl titanate (Ti (OC4H9)4AR reagents), appropriate amount of deionized water is added while stirring, has white heavy
Form sediment and produce and be linked to be bulk, the concentrated nitric acid of corresponding mol ratio is slowly added dropwise, is stirred vigorously 3~4 hours, precipitate constantly dissolving, obtain
To clear solution.Stand, there is a small amount of butanol on upper strata, and lower floor is titanyl nitrate TiO (NO3)2, because organic matter butanol is follow-up
Decompose, volatilize (a small amount of butanol does not influence to test) in sintering process, above-mentioned titanyl nitrate solution is used directly for preparing
BaTiO3。
2nd, nanometer BaTiO3The preparation of powder
Nanometer BaTiO3Preparation flow figure is as shown in figure 1, press Ba, Ti mol ratio 1：1 weighs raw material barium nitrate, takes respective amount
Butyl titanate, and configure titanyl nitrate solution.Barium nitrate is dissolved in appropriate amount of deionized water, magnetic stirrer is to completely molten
Solve (2 hours or so).The solution is mixed with titanyl nitrate solution, 4h is stirred, by the Ba after mixing fully2+、TiO2+Nitric acid
Salt mixed liquor is slowly dropped into the mixed liquor of precipitating reagent-ammoniacal liquor and ammonium hydrogen carbonate (precipitating reagent is suitably excessive, so that precipitation is abundant),
Do not stop to stir in precipitation process, while 8.5-11 is maintained at using ammoniacal liquor regulation pH value.After the completion of precipitation, slurry is loaded and centrifuged
Bottle, is centrifuged 5 minutes using centrifuge in the case of 3000 revs/min, takes upper strata settled solution to be detected with pH meter or pH test paper, solution
PH value instills a little Ba (OH) in 8.5-112Reagent (checking), there is precipitation to produce, illustrate carbonate and hydrogen-oxygen in mixed solution
Root is excessive, ensures Ba2+、TiO2+Complete precipitation, can guarantee that the purity of final products.Precipitation after centrifuge is separated is put in
Drying box is dried, and is ground 20 minutes using agate mortar after drying, and then anneal 2.5h in 1100 DEG C, and leads to a small amount of oxygen, i.e.,
Obtain nanometer BaTiO3Powder, powder is through XRD, SEM Scanning Detction after annealing.Nano-powder XRD diffraction patterns are shown in Fig. 2, SEM scanning figures
See Fig. 3.
The present invention operation principle be：Such as Fig. 1, when butyl titanate is added to deionized water, react such as equation
(1)；Reacted when adding enough nitric acid stirrings such as equation (2)；Ammonium hydrogen carbonate, ammoniacal liquor hybrid reaction such as equation (3),
The titanyl nitrate solution being prepared is mixed evenly with barium nitrate solution, mixed liquor instillation ammoniacal liquor-ammonium hydrogen carbonate is mixed
Close and chemical reaction such as (4), (5) occur in liquid.Because ionic level mixes under liquid-phase condition, barium carbonate and the TiO (OH) of gained2
Uniformly mixing, products therefrom is separated, ground, calcines and can prepare nano barium carbonate powder.
C16H36O4Ti+4H2O→Ti(OH)4↓+4C4H9OH (1)
Ti(OH)4+2HNO3→TiO(NO3)2+3H2O (2)
NH4HCO3+NH3·H2O→(NH4)2CO3+H2O (3)
TiO(NO3)2+2NH3·H2O→TiO(OH)2↓+2NH4NO3 (4)
Ba2++CO3 2-→BaCO3↓ (5)
Powder is through XRD, SEM Scanning Detction after annealing.Nano-powder XRD diffraction patterns are shown in Fig. 2, and SEM scanning figures are shown in Fig. 3.
Whole course of reaction does not introduce difficult volatility ion, and high-purity powder is easily obtained through calcining.
The above described is only a preferred embodiment of the present invention, not doing any formal limitation to the present invention, appoint
What those skilled in the art, without departing from the scope of the present invention, is made a little using above-mentioned technology contents
Change or the embodiment of modification, in the range of still falling within technical solution of the present invention.
Claims (6)
1. one kind nanometer BaTiO3Raw powder's production technology, it is characterised in that：Using titanyl nitrate solution as titanium source, barium nitrate or vinegar
Sour barium is barium source, and deionized water is as solvent, first using barium titanium mol ratio as 0.8-1.2：1 by the solution of barium nitrate or barium acetate with
Titanyl nitrate solution is sufficiently stirred, and is well mixed, then will it is well mixed after solution be slowly dropped into carbonic acid as precipitating reagent
In the mixed liquor of hydrogen ammonium and ammoniacal liquor, precipitating reagent is excessive, does not stop to stir, and keeps ammonium hydrogen carbonate and ammonia water mixture pH value in 8.5-
11, after precipitation, by centrifuge precipitation and separation, take upper strata settled solution to be detected with pH meter or pH test paper, solution ph exists
8.5-11, instill a little Ba (OH)2Reagent, there is precipitation to produce；Precipitation after centrifuge is separated is through drying, grinding, annealing, i.e.,
Obtain a nanometer BaTiO3Powder.
2. as claimed in claim 1 nanometer of BaTiO3Raw powder's production technology, it is characterised in that described barium titanium mol ratio is 1：
1。
3. as claimed in claim 1 nanometer of BaTiO3Raw powder's production technology, it is characterised in that the operation of centrifuge precipitation and separation
For：Centrifuged 5 minutes under 3000 revs/min, described annealing operation is：Anneal 2-3h at 1100 DEG C.
4. as claimed in claim 1 nanometer of BaTiO3Raw powder's production technology, it is characterised in that the system of the titanyl nitrate solution
Preparation Method is：Using butyl titanate and concentrated nitric acid as raw material, the butyl titanate refers to Ti (OC4H9)4AR reagents, the concentrated nitric acid
Mass fraction be 65%, by Ti (OC4H9)4：HNO3=1：3~5 mol ratio, a certain amount of butyl titanate is taken, while stirring
Deionized water is added, until having white precipitate to produce and being linked to be bulk, obtains Ti (OC4H9)4- deionized water is reacted suspended
Liquid；The concentrated nitric acid of respective amount is taken again, is slowly dropped to above-mentioned Ti (OC4H9)4In the reacted suspension of-deionized water, stirring 3
~4 hours, constantly dissolving is precipitated, obtains clear solution, is stood, lower floor is titanyl nitrate, and the titanyl nitrate refers to TiO
(NO3)2。
5. the preparation method of titanyl nitrate solution as claimed in claim 4, it is characterised in that Ti (OC4H9)4With HNO3Mole
Than for 1：4.
6. the preparation method of titanyl nitrate solution as claimed in claim 4, it is characterised in that the titanyl nitrate solution is matched somebody with somebody
Dosage processed is：0.015molTi(OC4H9)4、0.06mol HNO3, 100ml deionized waters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710898425.2A CN107555473A (en) | 2017-09-28 | 2017-09-28 | A kind of nanometer BaTiO3Raw powder's production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710898425.2A CN107555473A (en) | 2017-09-28 | 2017-09-28 | A kind of nanometer BaTiO3Raw powder's production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107555473A true CN107555473A (en) | 2018-01-09 |
Family
ID=60983384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710898425.2A Pending CN107555473A (en) | 2017-09-28 | 2017-09-28 | A kind of nanometer BaTiO3Raw powder's production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107555473A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019676A (en) * | 2018-10-10 | 2018-12-18 | 湖北天瓷电子材料有限公司 | A kind of method that the precipitation method prepare high-purity Nano-class barium titanate |
| CN114773882A (en) * | 2022-05-24 | 2022-07-22 | 天泰(福建)新材料科技有限公司 | Titanium dioxide for delustering chinlon chemical fibers and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190077A (en) * | 1997-02-05 | 1998-08-12 | 曾燮榕 | Technology for preparing hydrosol of superfine metal oxide powder |
| CN1390806A (en) * | 2002-07-10 | 2003-01-15 | 清华大学 | Process for preparing tetragonal nanoparticles of barium titanate |
| CN101239736A (en) * | 2008-03-12 | 2008-08-13 | 陕西师范大学 | Thin lobation strontium barium titanate |
| CN101708861A (en) * | 2009-11-09 | 2010-05-19 | 贵州红星发展股份有限公司 | Method for preparing barium titanate |
| CN102125834A (en) * | 2011-01-14 | 2011-07-20 | 上海交通大学 | Titanium-based nano-composite metal oxide catalyst and preparation method thereof |
-
2017
- 2017-09-28 CN CN201710898425.2A patent/CN107555473A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190077A (en) * | 1997-02-05 | 1998-08-12 | 曾燮榕 | Technology for preparing hydrosol of superfine metal oxide powder |
| CN1390806A (en) * | 2002-07-10 | 2003-01-15 | 清华大学 | Process for preparing tetragonal nanoparticles of barium titanate |
| CN101239736A (en) * | 2008-03-12 | 2008-08-13 | 陕西师范大学 | Thin lobation strontium barium titanate |
| CN101708861A (en) * | 2009-11-09 | 2010-05-19 | 贵州红星发展股份有限公司 | Method for preparing barium titanate |
| CN102125834A (en) * | 2011-01-14 | 2011-07-20 | 上海交通大学 | Titanium-based nano-composite metal oxide catalyst and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 李志强等: "超细钛酸钡粉体湿化学合成技术", 《山东陶瓷》 * |
| 杨峻等: "EDTA络合-微波法合成介电陶瓷钛酸钡", 《无机盐工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019676A (en) * | 2018-10-10 | 2018-12-18 | 湖北天瓷电子材料有限公司 | A kind of method that the precipitation method prepare high-purity Nano-class barium titanate |
| CN109019676B (en) * | 2018-10-10 | 2022-03-11 | 湖北天瓷电子材料有限公司 | Method for preparing high-purity nano-grade barium titanate by precipitation method |
| CN114773882A (en) * | 2022-05-24 | 2022-07-22 | 天泰(福建)新材料科技有限公司 | Titanium dioxide for delustering chinlon chemical fibers and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100310186B1 (en) | Process for the synthesis of crystalline ceramic powders of perovskite ccmpounds | |
| CN112499609A (en) | Method for preparing iron phosphate by using waste lithium iron phosphate anode powder lithium extraction slag and application | |
| US20050186133A1 (en) | Process for preparing a strontium titanate powder | |
| CN105271375A (en) | Method for preparing tetrabasic lead sulfate | |
| CN103189315A (en) | Production of high purity precipitated calcium carbonate | |
| CN102030352A (en) | Method for preparing nano material | |
| CN105293554B (en) | A kind of method that utilization strontium slag prepares high-purity strontium hydroxide | |
| CN103153871A (en) | Manganese oxide and method for producing same, and method for producing lithium manganese composite oxide using same | |
| CN102046562A (en) | Process for preparing advanced ceramic powder using onium dicarboxylates | |
| CN107555473A (en) | A kind of nanometer BaTiO3Raw powder's production technology | |
| JP2015525735A (en) | Method for producing lithium metal phosphate | |
| Chang et al. | Hydrothermal assisted sol–gel synthesis and multisite luminescent properties of anatase TiO 2: Eu 3+ nanorods | |
| CN109721096B (en) | Device and method for preparing high-purity barium titanate | |
| CN103833082B (en) | A kind of coprecipitation method prepares nanometer Ba (Fe 0.5nb 0.5) O 3the method of powder | |
| CN106082297B (en) | A kind of preparation method of 20~60 microns of gadolinium oxides of medium particle diameter | |
| CN104445341B (en) | A kind of preparation method of the nanometer yttrium aluminium garnet powder of pure YAG phase | |
| Yoshikawa et al. | Chemical Preparation of Lead‐Containing Niobate Powders | |
| KR100955802B1 (en) | Process for preparing fine barium titanate based composite oxide | |
| CN101591013B (en) | Organic phase back-extraction method for preparing cerium terbium lanthanum phosphate | |
| CN108529666A (en) | Method, product and the application of lithium titanate are prepared by inorganic ti sources | |
| CN1030308C (en) | Process for preparation of titanate | |
| CN107697893A (en) | Improve the method for calcium leaching efficiency and its product and application in phosphorus ore | |
| CN107903072B (en) | Method for preparing strontium barium niobate nano powder by two-step coprecipitation method | |
| CN1321901C (en) | Coprecipitation process of preparing relation base niobate ferroelectric powder | |
| Srisombat et al. | Chemical synthesis of magnesium niobate powders |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180109 |
|
| RJ01 | Rejection of invention patent application after publication |