CN102050485A - Preparation method of high-density spherical barium titanate powder particles - Google Patents
Preparation method of high-density spherical barium titanate powder particles Download PDFInfo
- Publication number
- CN102050485A CN102050485A CN 201010609800 CN201010609800A CN102050485A CN 102050485 A CN102050485 A CN 102050485A CN 201010609800 CN201010609800 CN 201010609800 CN 201010609800 A CN201010609800 A CN 201010609800A CN 102050485 A CN102050485 A CN 102050485A
- Authority
- CN
- China
- Prior art keywords
- preparation
- concentration
- barium titanate
- powder particles
- titanate powder
- 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
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of high-density spherical barium titanate powder particles, which comprises the following steps: using titanium tetraisopropanolate (TTIP) and barium acetate as precursors, adding organic acid or urea, and adopting an ultrasonic spray pyrolytic process to prepare the barium titanate powder particles. Thus, in the invention the phenomena of fragmenting, shell breaking, porousness, hollowness and the like in the powder particles in the spray pyrolytic process in the prior art and effectively overcome. The particle sizes of the high-density spherical barium titanate powder particles are small and uniformly distributed; and the high-density spherical barium titanate powder particles have the advantages of high purity and no aggregation, and are compact spheres.
Description
Technical field
The present invention relates to a kind of preparing barium titanate powder.
Technical background
Barium titanate has good dielectric, ferroelectric, piezoelectric property, is a kind of electron ceramic material with widespread use field.As the raw materials for sintering of electron ceramic material, it is little and be evenly distributed that the barium carbonate powder particle need satisfy particle diameter usually, and the purity height does not have and reunites, and is requirements such as dense spherical.
In preparing barium titanate powder, exercise question is document (the TAKASHI OGIHARA of " Synthesisand sinteringof barium titanate fine powders by ultrasonic spray pyrolysis ", HITOSHI AIKIYO, NOBUOOGATA, NOBUYASU MIZUTANI.Advanced Powder Technol.VOl.10, No.1,1999:37-50) provide a kind of technology of spray heating decomposition, with titanium isopropylate, barium acetate is a presoma, can realize that its product is the sphere of non-reunion shape usually by the one-step synthesis of precursor solution to powder particle.This technology has certain controllability for product particle grain size, pattern, density, thing phase composite and distribution, but exists prepared BaTiO
3Be prone to fragment, broken shell and porous hollow particle in the powder granule.These particles with bad shape characteristic can cause the low tap density of crystalline overgrowth and electron ceramic material behind sintering, thereby influence the performance of final electronic ceramic device.
Summary of the invention
The objective of the invention is,, provide a kind of preparation method that can improve obtained barium carbonate powder granule-morphology at the deficiencies in the prior art.
Method of the present invention is, is 0.1～0.3molL with concentration
-1Titanium isopropylate and barium acetate be presoma, adding organic acid to concentration is 0.2～0.5molL
-1Or to add urea to concentration be 0.5～1.5molL
-1, be 1～4mlmin at the mixing solutions flow
-1, the carrier gas flux scope is 1～4Lmin
-1, temperature range is to adopt the ullrasonic spraying mode to prepare barium titanate particles under 700～1000 ℃ the condition.
Organic acid comprises that citric acid, oxalic acid, tartrate, oxysuccinic acid, xitix etc. do not form sedimentary aliphatic carboxylic acid with titanium isopropylate and barium acetate.
The advantage of the inventive method is to produce phenomenons such as fragment, broken shell and porous hollow by changing the character of solution, overcome effectively the powder granule that exists in the prior art of spray heating decomposition; Raw material mixes under solution state, can accurately control stoichiometric ratio, has guaranteed uniform component distribution, the purity height; Technological process is simple, and a step promptly obtains finished product, and the component loss is few, does not have filtration, washing, dry, crushing process, and easy and simple to handle, production process is continuous, non-pollution discharge.
Description of drawings
Fig. 1 is the ullrasonic spraying thermolysis experimental installation synoptic diagram of the inventive method;
The SEM photo of the powder granule that Fig. 2 makes during for 0.3M for citric acid concentration in the inventive method;
Fig. 3 makes particulate XRD figure spectrum when citric acid concentration is for 0.3M in the inventive method;
Fig. 4 makes particulate SEM photo during for 0.4M for the inventive method mesoxalic acid concentration;
Fig. 5 makes particulate XRD figure spectrum during for 0.4M for the inventive method mesoxalic acid concentration;
Fig. 6 makes particulate SEM photo during for 0.5M for the inventive method unresolvable tartaric acid concentration;
Fig. 7 makes particulate XRD figure spectrum during for 0.5M for the inventive method unresolvable tartaric acid concentration;
The SEM photo of the powder granule that Fig. 8 makes during for 1.0M for urea concentration in the inventive method;
The XRD figure spectrum of the powder granule that Fig. 9 makes during for 1.0M for urea concentration in the inventive method.
Embodiment
Measure the titanium isopropylate (TTIP) of doses, and dropwise add rare 0.1～0.5M HNO
3In the solution, violent stirring is 1～3 hour under 300r/min, treat solution becomes pure clear and do not have visible precipitate after, volumetric molar concentration (mol ratio 1: 1) such as press and add Ba (CH
3COO)
2, gentle agitation mixing solutions under 200r/min, and the adding deionized water is diluted to desired concn.Under the normal condition, precursor solution concentration is set at 0.1～0.3molL usually
-1, with 0.1～0.2molL
-1For good.
Organic acid or urea is added to by the concentration range of various dose respectively makes mixing solutions in the precursor solution.
The concentration range of citric acid even can be 0.1～0.5molL in the mixing solutions
-1, when the concentration of citric acid is 0.3～0.5molL
-1The time be the pattern optimal state, when the concentration that adds citric acid further increased, the gained particle was expanded ghost shape.
The concentration range of solution mesoxalic acid even can be 0.1～0.6molL
-1, the best is 0.3～0.5molL
-1
The concentration range of solution unresolvable tartaric acid even can be 0.2～0.8molL
-1, the best is 0.3～0.6molL
-1
The concentration of urea is 0.5～1.5molL in the solution
-1, the best is 0.8～1.2molL
-1
The mixing solutions flow control is at 1～4mlmin
-1, the best is 2～3mlmin
-1The carrier gas flux scope is 1～4Lmin
-1, the best is 2～3Lmin
-1Temperature range is 700～1000 ℃, and the best is 900～1000 ℃.
The equipment that this experiment is adopted as shown in Figure 1, wherein 1 is nitrogengas cylinder, 2 is oxygen cylinder, 3 is Reaktionsofen, 4 is container for storing liquid, 5 is under meter, 6 is ultrasonic atomizing nozzle, 7 is ultra-sonic generator, 8 is thermopair, 9 is powder catcher.
Mixing solutions is a droplet by the atomizing of 60HZ ultrasonic atomizer; Droplet is subsequently with air or use N
2And O
2The mixed gas that is made into is as carrier gas (vol%N
2: O
2=3: 1～4: 1) bring in the cylindrical reaction boiler tube (internal diameter 95mm, long 1400mm); Reaction boiler tube carries out indirect heating by resistance furnace, and the temperature of reaction boiler tube center is set at preset temperature; The bottom of equipment used is provided with and is used to collect product particulate collector
In the spraying thermal decomposition process, solution is pressed the following formula reaction:
Below be specific embodiment:
Table 1 adds the condition and the result of citric acid
Table 2 adds the condition and the result of oxalic acid
Table 3 adds tartaric condition and result
Table 4 adds the condition and the result of urea
Citric acid concentration makes particulate SEM photo as shown in Figure 2 during for 0.3M, and XRD figure is composed as shown in Figure 3, and as can be seen from the figure its size-grade distribution is more even, the degree of crystallinity height, and good sphericity, hollow broken shell is few.
Concentration of oxalic acid makes particulate SEM photo as shown in Figure 4 during for 0.4M, and XRD figure is composed as shown in Figure 5, and as can be seen from the figure its size-grade distribution is more even, the degree of crystallinity height, and good sphericity, hollow broken shell is few.
Tartaric acid concentration makes particulate SEM photo as shown in Figure 6 during for 0.5M, and XRD figure is composed as shown in Figure 7, and as can be seen from the figure its size-grade distribution is more even, the degree of crystallinity height, and good sphericity, hollow broken shell is few.
Urea concentration makes particulate SEM photo as shown in Figure 8 during for 1.0M, and XRD figure is composed as shown in Figure 9, and as can be seen from the figure its size-grade distribution is more even, the degree of crystallinity height, and good sphericity, hollow broken shell is few.
Claims (10)
1. a high-density spherical barium carbonate powder particulate preparation method is characterized in that, is 0.1～0.3molL with concentration
-1Titanium isopropylate and barium acetate be presoma, adding organic acid to concentration is 0.2～0.5molL
-1Or interpolation urea to concentration is 0.5～1.5molL
-1Make mixing solutions, with air or with N
2: O
2The mixed gas of volume ratio=3: 1～4: 1 is carrier gas; At the mixing solutions flow is 1～4mlmin
-1, carrier gas flux is 1～4Lmin
-1, temperature is to adopt the ullrasonic spraying mode to prepare barium titanate particles under 700～1000 ℃ the condition.
2. preparation method according to claim 1 is characterized in that, the concentration of described presoma is 0.1～0.2molL
-1
3. preparation method according to claim 1 and 2 is characterized in that, described organic acid is citric acid or oxalic acid or tartrate.
4. preparation method according to claim 1 and 2 is characterized in that, described mixing solutions flow is 2～3mlmin
-1
5. preparation method according to claim 1 and 2 is characterized in that, described carrier gas flux is 2～3Lmin
-1
6. preparation method according to claim 1 and 2 is characterized in that, described temperature range is 900～1000 ℃
7. preparation method according to claim 1 and 2 is characterized in that, described urea concentration is 0.8～1.2molL
-1
8. preparation method according to claim 3 is characterized in that, the concentration of described citric acid is 0.3～0.5molL
-1
9. preparation method according to claim 3 is characterized in that, the concentration of described oxalic acid is 0.3～0.5molL
-1
10. preparation method according to claim 3 is characterized in that, described tartaric concentration is 0.3～0.6molL
-1
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010609800 CN102050485A (en) | 2010-12-29 | 2010-12-29 | Preparation method of high-density spherical barium titanate powder particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010609800 CN102050485A (en) | 2010-12-29 | 2010-12-29 | Preparation method of high-density spherical barium titanate powder particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102050485A true CN102050485A (en) | 2011-05-11 |
Family
ID=43955354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010609800 Pending CN102050485A (en) | 2010-12-29 | 2010-12-29 | Preparation method of high-density spherical barium titanate powder particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102050485A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145199A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Preparation method of cobalt oxide/graphene composite nano material |
| CN103880066A (en) * | 2014-02-19 | 2014-06-25 | 陕西科技大学 | Preparation method of cubic phase BaTiO3 hollow nanospheres |
| CN106315667A (en) * | 2016-08-07 | 2017-01-11 | 淮安新能源材料技术研究院 | Solid phase preparation method of multihole barium-titanate micro-nano particle ball |
-
2010
- 2010-12-29 CN CN 201010609800 patent/CN102050485A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of European Ceramic Society》 20081231 Yoshitake Terashi et al. Role of urea addition in the preparation of tetragonal BaTiO3 nanoparticles using flame-assisted spray pyrolysis 第2573-2580页 1-10 第28卷, * |
| 《功能材料》 20081231 李启厚等 超声雾化热分解法制备超细SnO2粉体及其形貌和粒度控制 第1450-1457页 1-10 第39卷, 第9期 * |
| 《粉末冶金技术》 20100831 李启厚等 喷雾热分解法合成BaTiO3超细粉末及其形貌控制 第292-301页 1-10 第28卷, 第4期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145199A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Preparation method of cobalt oxide/graphene composite nano material |
| CN103880066A (en) * | 2014-02-19 | 2014-06-25 | 陕西科技大学 | Preparation method of cubic phase BaTiO3 hollow nanospheres |
| CN103880066B (en) * | 2014-02-19 | 2015-05-20 | 陕西科技大学 | Preparation method of cubic phase BaTiO3 hollow nanospheres |
| CN106315667A (en) * | 2016-08-07 | 2017-01-11 | 淮安新能源材料技术研究院 | Solid phase preparation method of multihole barium-titanate micro-nano particle ball |
| CN106315667B (en) * | 2016-08-07 | 2018-08-14 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous barium titanate micro-nano particle ball |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101397317B1 (en) | Pulverulent compounds, processes for the preparation thereof and the use thereof in electrochemical applications | |
| EP2465821B1 (en) | Method for producing nanoscale lithium titanate particles | |
| KR100753773B1 (en) | Method for preparing perovskite oxide nanopowders | |
| EP2969170A1 (en) | Method for the use of slurries in spray pyrolysis for the production of non-hollow, porous particles | |
| WO2023024591A1 (en) | Crystal-transformed precursor and preparation method therefor | |
| CN102050485A (en) | Preparation method of high-density spherical barium titanate powder particles | |
| CN103570083A (en) | Preparation method of nickel-cobalt-aluminum spherical precursor of positive material of lithium ion battery | |
| CN103214235A (en) | Preparation method of microwave dielectric ceramic material | |
| CN110697789A (en) | Preparation method of spinel type magnetic aerogel material | |
| CN105502480B (en) | Hydrangea-like strontium titanate nano powder preparation method | |
| CN105693243A (en) | Preparation method of medium-dielectric-constant high-performance microwave dielectric ceramic | |
| JP2011113924A (en) | Method of manufacturing lithium titanate negative electrode material | |
| CN103303961B (en) | Preparation method of spherical electroplating-level copper oxide powder | |
| US6409983B1 (en) | Process for preparing crystalline barium titanate powder | |
| CN101100310A (en) | Preparation method for nanometer barium titanate | |
| CN103626223A (en) | Barium titanate production process | |
| JP6961428B2 (en) | Porous alumina sintered body and its manufacturing method | |
| JP4578428B2 (en) | Barium titanate powder and production method thereof | |
| JPH0950811A (en) | Production of lithium battery active material | |
| CN102617120B (en) | Method for producing beta''-aluminum oxide ceramic membrane | |
| CN106431389B (en) | A kind of CaCu3Ti4O12Preparation method | |
| JP4711744B2 (en) | Method for producing barium titanate powder and barium titanate powder | |
| CN101333005A (en) | Method for low-temperature preparing K0.5Na0.5NbO3 super fines | |
| CN105948109A (en) | Preparation method of mesoporous barium titanate particles | |
| JP2002029745A (en) | Method for producing crystalline barium titanate powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110511 |