CN102320651A - Preparation method for strontium titanate nano powder - Google Patents
Preparation method for strontium titanate nano powder Download PDFInfo
- Publication number
- CN102320651A CN102320651A CN201110148088A CN201110148088A CN102320651A CN 102320651 A CN102320651 A CN 102320651A CN 201110148088 A CN201110148088 A CN 201110148088A CN 201110148088 A CN201110148088 A CN 201110148088A CN 102320651 A CN102320651 A CN 102320651A
- Authority
- CN
- China
- Prior art keywords
- powder
- strontium titanate
- preparation
- reaction vessel
- titanate nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method for strontium titanate nano powder, which is characterized by comprising the following steps: tetra-n-butyl titanate and strontium nitrate are weighed and added into a reaction vessel, sodium hydroxide solution is added into the reaction vessel, and a glass rod is used for stirring the mixture; the reaction vessel is placed in a microwave reaction instrument and is heated at a certain heating rate; and when being reduced to the room temperature, the solution is poured out, hydrochloric acid is added, the repeated washing, filtering and depositing are carried out through deionized water, obtained deposition is placed in a dryer and is dried at 70 DEG C, and the strontium titanate nano powder is obtained. Through the preparation method, the pure-phased strontium titanate nano powder is prepared at a lower temperature and within a shorter period through a microwave assisted hydrothermal method; and compared with the method adopted in the prior art, the pure-phased strontium titanate nano powder is obtained in the preparation method at the lower temperature, and the powder is more dispersive.
Description
Technical field
The present invention relates to a kind of preparation method of nano-powder, particularly a kind of preparation method of strontium titanate nano-powder.
Background technology
Strontium titanate is the important source material of electronic industry, is being widely used aspect the electronic devices and components such as thermistor and electrical condenser.In order to adapt to the microminiaturized development trend of electronic devices and components, the strontium titanate nano-powder that processability is good becomes new developing direction.At present, preparation strontium titanate nano-powder method has conventional solid-state method, oxalate coprecipitation method and organic method.And the strontium titanate particle diameter of nanometer powder of conventional solid-state method preparation is bigger and inhomogeneous, prepares strontium titanate nano-powder complex process through oxalate coprecipitation method, and cost is higher.
Document discloses " chemical coprecipitation of Cui Bin prepares strontium titanate nano-powder novel process; electronic component and material for Zhang Hao, smooth post state, 28 (6), 2009; 12-15 " a kind of preparation method of strontium titanate nano-powder, and document adopts coprecipitation method, through purification raw material metatitanic acid; To have made particle diameter be the Sr titanate powder of 60nm to other processing condition such as titanium strontium mol ratio, calcining temperature in the optimizing materials, but the preparation process is complicated, and influence factors such as material purity, dispersant concentration, calcining temperature are more; And in 800 ℃ of Sr titanate powders that calcining obtains down, still containing the Strontium carbonate powder dephasign, the purity of powder is not high.
Summary of the invention
The technical problem that solves
Weak point for fear of prior art; The present invention proposes a kind of preparation method of strontium titanate nano-powder; With tetra-n-butyl titanate, strontium nitrate, sodium hydroxide and deionized water is raw material, has just obtained the pure nano-powder of strontium titanate mutually through the microwave-assisted hydro-thermal reaction in lower temperature and short time.
Technical scheme
A kind of preparation method of strontium titanate nano-powder is characterized in that step is following:
Step 1: 1: 1 in molar ratio weighing tetra-n-butyl titanate and strontium nitrate, and it directly is added in the reaction vessel are the sodium hydroxide solution that 60% requirement adds 2～10mol/L by compactedness again, stir with glass stick simultaneously;
Step 2: reaction vessel is screwed, in the microwave reaction appearance of packing into, be heated to 100～200 ℃, insulation 1～2h with the temperature rise rate of 20 ℃/min;
Step 3: after waiting to reduce to room temperature, the solution in the reaction vessel is poured out, added 2～10ml hydrochloric acid, use deionized water repetitive scrubbing filtering-depositing again, the pH value of the deionized water after filtering is neutral;
Step 4: place baking oven in 70 ℃ of oven dry resulting deposition, obtain the strontium titanate nano-powder.
Beneficial effect
The preparation method of a kind of strontium titanate nano-powder that the present invention proposes; Adopt the microwave-assisted hydrothermal method to prepare pure strontium titanate nano-powder mutually in lower temperature and short time; Compare with the method that background technology is adopted; This method has obtained the strontium titanate nano-powder of pure phase in lower temperature, and powder has good dispersiveness.
Description of drawings
Fig. 1 is the X ray diffracting spectrum that adopts the Sr titanate powder of the inventive method preparation
Fig. 2 is the Sr titanate powder stereoscan photograph that adopts the inventive method preparation
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
Following examples are with reference to Fig. 1～2.
Embodiment 1, in reactor drum, adds 4ml tetra-n-butyl titanate and 2.739g strontium nitrate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1: 1.1; , add the sodium hydroxide solution of 40ml 4mol/L again, stir with glass stick simultaneously; Reaction vessel is screwed, in the microwave reaction appearance of packing into, be heated to 140 ℃, insulation 1h with the temperature rise rate of 20 ℃/min; After waiting to be cooled to room temperature, the solution in the reaction vessel is poured out, added small amount of hydrochloric acid, filter with the deionized water repetitive scrubbing, the pH value of the deionized water after filtering is neutral; Place baking oven in 70 ℃ of oven dry resulting deposition.
Embodiment 2, in reactor drum, add 4ml tetra-n-butyl titanate and 2.988g strontium nitrate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1: 1.2; , add the sodium hydroxide solution of 40ml 6mol/L again, stir with glass stick simultaneously; Reaction vessel is screwed, in the microwave reaction appearance of packing into, be heated to 160 ℃, insulation 1h with the temperature rise rate of 20 ℃/min; After waiting to be cooled to room temperature, the solution in the reaction vessel is poured out, added small amount of hydrochloric acid, filter with the deionized water repetitive scrubbing, the pH value of the deionized water after filtering is neutral; Place baking oven in 70 ℃ of oven dry resulting deposition.The X ray diffracting spectrum of the prepared powder of above-mentioned condition among Fig. 1, as can be seen from the figure, obtained powder is the strontium titanate of pure phase, does not have other dephasigns to exist; Fig. 2 is the stereoscan photograph according to the prepared Sr titanate powder of above-mentioned condition, as can be seen from the figure powder good dispersion, and particle diameter is approximately 100nm.
The Sr titanate powder purity that the present invention prepares is high, dispersiveness and good crystallinity, and particle diameter is approximately 100nm.
Claims (1)
1. the preparation method of a strontium titanate nano-powder is characterized in that step is following:
Step 1: 1: 1 in molar ratio weighing tetra-n-butyl titanate and strontium nitrate, and it directly is added in the reaction vessel are the sodium hydroxide solution that 60% requirement adds 2～10mol/L by compactedness again, stir with glass stick simultaneously;
Step 2: reaction vessel is screwed, in the microwave reaction appearance of packing into, be heated to 100～200 ℃, insulation 1～2h with the temperature rise rate of 20 ℃/min;
Step 3: after waiting to reduce to room temperature, the solution in the reaction vessel is poured out, added 2～10ml hydrochloric acid, use deionized water repetitive scrubbing filtering-depositing again, the pH value of the deionized water after filtering is neutral;
Step 4: place baking oven in 70 ℃ of oven dry resulting deposition, obtain the strontium titanate nano-powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110148088A CN102320651A (en) | 2011-06-02 | 2011-06-02 | Preparation method for strontium titanate nano powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110148088A CN102320651A (en) | 2011-06-02 | 2011-06-02 | Preparation method for strontium titanate nano powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102320651A true CN102320651A (en) | 2012-01-18 |
Family
ID=45448531
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110148088A Pending CN102320651A (en) | 2011-06-02 | 2011-06-02 | Preparation method for strontium titanate nano powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102320651A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674442A (en) * | 2012-04-28 | 2012-09-19 | 无锡隆傲电子有限公司 | Method for preparing strontium titanate nano powder through microwave hydrothermal method |
| JP2016041641A (en) * | 2014-08-19 | 2016-03-31 | 日本化学機械製造株式会社 | Fine particle of perovskite type titanium compound and production method of the same |
| CN105502480A (en) * | 2015-10-16 | 2016-04-20 | 浙江大学 | Hydrangea-like strontium titanate nano powder preparation method |
| CN107285374A (en) * | 2017-06-07 | 2017-10-24 | 广州天极电子科技有限公司 | A kind of hollow ball-shape Sr titanate powder and preparation method thereof |
| CN110203967A (en) * | 2019-07-05 | 2019-09-06 | 西安电子科技大学 | The preparation method of sheet strontium titanates nano crystal body |
| CN110952143A (en) * | 2019-12-03 | 2020-04-03 | 华东理工大学 | Synthesis method of mesoporous single-crystal strontium titanate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0558633A (en) * | 1991-09-03 | 1993-03-09 | Teika Corp | Production of strontium titanate |
| CN101311376A (en) * | 2008-02-26 | 2008-11-26 | 浙江大学 | Method for preparing strontium titanate nanometer powder of one-dimensional structure |
-
2011
- 2011-06-02 CN CN201110148088A patent/CN102320651A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0558633A (en) * | 1991-09-03 | 1993-03-09 | Teika Corp | Production of strontium titanate |
| CN101311376A (en) * | 2008-02-26 | 2008-11-26 | 浙江大学 | Method for preparing strontium titanate nanometer powder of one-dimensional structure |
Non-Patent Citations (3)
| Title |
|---|
| H. Y. HE ET AL.: "The effect of surfactant on SrTiO3 particles synthesized by a microwave hydrothermal method", 《JOURNAL OF CERAMIC PROCESSING RESEARCH》, vol. 11, no. 4, 31 December 2010 (2010-12-31), pages 485 - 489 * |
| 刘韩星 等: "微波合成SrTiO3的工艺、结构与性能研究", 《物理化学学报》, vol. 14, no. 7, 31 July 1998 (1998-07-31), pages 624 - 629 * |
| 邵义 等: "水热法制备钛酸锶纳米粉体的性能", 《沈阳工业大学学报》, vol. 30, no. 5, 31 October 2008 (2008-10-31), pages 535 - 538 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674442A (en) * | 2012-04-28 | 2012-09-19 | 无锡隆傲电子有限公司 | Method for preparing strontium titanate nano powder through microwave hydrothermal method |
| JP2016041641A (en) * | 2014-08-19 | 2016-03-31 | 日本化学機械製造株式会社 | Fine particle of perovskite type titanium compound and production method of the same |
| CN105502480A (en) * | 2015-10-16 | 2016-04-20 | 浙江大学 | Hydrangea-like strontium titanate nano powder preparation method |
| CN107285374A (en) * | 2017-06-07 | 2017-10-24 | 广州天极电子科技有限公司 | A kind of hollow ball-shape Sr titanate powder and preparation method thereof |
| CN110203967A (en) * | 2019-07-05 | 2019-09-06 | 西安电子科技大学 | The preparation method of sheet strontium titanates nano crystal body |
| CN110952143A (en) * | 2019-12-03 | 2020-04-03 | 华东理工大学 | Synthesis method of mesoporous single-crystal strontium titanate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102320651A (en) | Preparation method for strontium titanate nano powder | |
| CN101913853B (en) | Method for preparing bismuth titanate-barium titanate powder by hydrothermal method | |
| CN105271378A (en) | Preparation method of tetragonal barium titanate with high tetragonal rate | |
| CN101214990B (en) | Normal temperature synthesis method for nanometer zinc oxide | |
| CN103896335B (en) | The preparation method of high-ratio surface nano porous titanium dioxide | |
| CN105461311A (en) | Method for making NaNbO3 powder through sol-gel method and obtaining monocrystals through sintering | |
| CN101857430B (en) | Method for synthesizing titanate series electronic ceramic nano-crystalline materials | |
| CN104229874A (en) | Preparation method of strontium titanate nano-powder | |
| CN103693957B (en) | Method for preparing microwave dielectric ceramic material | |
| CN103395840A (en) | Method for preparing KNbWO6.H2O | |
| CN101928038B (en) | Preparation method of barium titanate hollow nanospheres | |
| CN102826606A (en) | Preparation method of negative thermal expansion rare earth tungstate Sc2W3O12 material | |
| JP5658295B2 (en) | Method for producing barium titanyl oxalate and method for producing barium titanate | |
| CN102674442A (en) | Method for preparing strontium titanate nano powder through microwave hydrothermal method | |
| CN105174309A (en) | Method for preparing perovskite-type flaky KNN (potassium sodium niobate) with hydrothermal method | |
| CN104446445A (en) | Preparation method of monodisperse nano-powdery barium titanate | |
| CN102030531B (en) | Method for preparing potassium sodium niobate nano powder | |
| CN104163627A (en) | Preparation method of KNbO3 nano solid solution with adjustable optical band gap | |
| CN102745747A (en) | Preparation method for rod-like Sc2W3O12 negative thermal expansion material | |
| CN103614139B (en) | Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body | |
| CN104671274A (en) | Preparation method of CuAlO<2> powder | |
| CN101851093B (en) | Method for preparing barium titanate nano powder | |
| CN105329938B (en) | A kind of oil-water interfaces method prepares BaTiO3The method of nano particle | |
| CN102584219A (en) | Method for quickly compounding barium titanate nano-powder | |
| CN105849049B (en) | The manufacture method of barium carbonate 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: 20120118 |