CN102502766B - Method for preparing La2-xBaxCuO4 powder by sol-gel method - Google Patents
Method for preparing La2-xBaxCuO4 powder by sol-gel method Download PDFInfo
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- CN102502766B CN102502766B CN201110375498.6A CN201110375498A CN102502766B CN 102502766 B CN102502766 B CN 102502766B CN 201110375498 A CN201110375498 A CN 201110375498A CN 102502766 B CN102502766 B CN 102502766B
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Abstract
The invention relates to a method for preparing La2-xBaxCuO4 powder by a sol-gel method. The method comprises the steps that lanthanum nitrate, barium nitrate and copper nitrate are added into distilled water to obtain solution A, and citric acid is added into the solution A to obtain solution B; ammonia water is added into the solution B, and the pH is regulated to 1.5 to 4 to obtain solution C; the solution C is placed in a blowing drying box for constant-temperature drying to obtain dried gel; and the dried gel is ground into powder by a mortar, the powder is added in a crucible and is placed in a muffle furnace for heating reaction, then, the powder is cooled to the room temperature, substances in the powder are ground into the powder, and the La2-xBaxCuO4 powder is obtained. The low-cost sol-gel method in an inorganic system is adopted for preparing the La2-xBaxCuO4 powder, and the method has the advantages that the distribution of different components in the gel is uniform, the molecular level or the atomic level is reached, the reaction process is easy to control, the powder with larger specific surface area can be obtained, in addition, the equipment requirement is low, and the operation is simple. The obtained powder is the powder with the advantages that the grain diameter distribution is narrower, the appearance is controllable, and the component distribution is uniform. The method is an excellent method for preparing micron (nanometer)-level La2-xBaxCuO4 powder.
Description
Technical field
The present invention relates to a kind of La
2-xba
xcuO
4the preparation method of powder, is specifically related to a kind of sol-gel method and prepares La
2-xba
xcuO
4the method of powder.
Background technology
La
2-xm
xcuO
4the perovskite structure of oxygen vacancies such as (M=Ca, Sr, Ba) is widely studied at present.Since Bei Denuozi and Miao Le find first high temperature superconducting oxide La
2-xba
xcuO
4(LBCO) since, LBCO has obtained research extensively and profoundly, and people found gradually afterwards, at La
2-xba
xcuO
4in system, when x approaches 1/8, Tc is suppressed strongly, and its normal state physical properties is also with respect to La
2-xsr
xcuO
4occur abnormal behaviour, i.e. " 1/8 abnormal phenomena ", in LBCO system, when x is near 1/8, have the structural phase transition under a low temperature, i.e. the transformation (from high temperature to low temperature) from low temperature quadrature phase (LTO) to low temperature Tetragonal (LTT), at La
2-xba
xcuO
4in superconductor, when the replaced content of La is 0.125 (1/8), the repressed problem of superconducting transition temperature is the focus of a research always, but physical mechanism wherein does not still get across so far, necessaryly proceeds research.
At present, the preparation La of report
2-xba
xcuO
4method be mainly solid phase method [HU Baofu, WANG Yanwen.STUDY OF La
2-xba
xcuO
4sUPERCONDUCTOR BY PAT[J] .CHINESE JOURNAL OF LOW TEMPERATURE PHYSICS, 2005,27 (5): 555-558.], [ZHANG Heng, DONG Xinfa, LIN Weiming.Synthesis and Oxygen Permeability of La
2-xba
xcuO
4ceramic Membranes[J] .Chinese Rare earths, 2007,28 (2): 30-32.], but solid state reaction is in order to obtain the target product that purity is high, reactant powder should be enough thin, and need at high temperature long-time roasting and repeatedly middle grinding, the method expends time in, and in product, has more impurity phase.
Summary of the invention
The object of the present invention is to provide a kind of reaction to carry out at low temperatures, greatly reduce energy consumption, saved cost, and low for equipment requirements, sol-gel method simple to operate is prepared La
2-xba
xcuO
4the method of powder.
For achieving the above object, the technical solution used in the present invention is:
1) get 35ml～95ml distilled water and add in beaker, by La: Ba: Cu=2-x: x: 1 mol ratio is by analytically pure lanthanum nitrate (La (NO
3)
36H
2o), nitrate of baryta (Ba (NO
3)
2) and cupric nitrate (Cu (NO
3)
33H
2o) add magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.1-0.4mol/L, wherein x=0.02～0.3;
2) mol ratio of pressing citric acid and metallic cation summation is (0.5～2.5): 1 by analytically pure citric acid (C
6h
8o
7h
2o) add in solution A the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 3%～5% ammoniacal liquor, regulating pH is 1.5～4, obtains solution C;
4) solution C is inserted in air dry oven, in 60 ℃～110 ℃ freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 3～5 ℃/min, from room temperature, be warming up to 500 ℃～900 ℃, insulation 0.5h～7h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
Because sol-gel method is to prepare a kind of low temperature process of powder, have that goods purity is high, chemical uniformity good, particle is thin, synthesis temperature is low, an advantage such as easy control of components, processing unit are simple.The present invention adopts the sol-gel method of lower-cost inorganic system to prepare La
2-xba
xcuO
4powder, its advantage is that in gel, different group members are evenly distributed, and reaches molecular level or atom level, reaction process is easy to control, and can obtain the powder that specific surface area is larger, and equipment requirements is low, simple to operate.The diameter of particle narrow distribution obtaining, pattern is controlled, and the powder of uniform component distribution is preparation micro-(receiving) meter level La
2-xba
xcuO
4the excellent process of powder.
Accompanying drawing explanation
Fig. 1 is the prepared La of embodiment 1
2-xba
xcuO
4the X-ray diffraction of powder (XRD) collection of illustrative plates.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1) get 50ml distilled water and add in beaker, by La: Ba: Cu=1.9: within 0.1: 1, mol ratio is by analytically pure lanthanum nitrate (La (NO
3)
36H
2o), nitrate of baryta (Ba (NO
3)
2) and cupric nitrate (Cu (NO
3)
33H
2o) add magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.2mol/L;
2) by the mol ratio of citric acid and metallic cation summation be 1.2: 1 by analytically pure citric acid (C
6h
8o
7h
2o) add in solution A the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 4% ammoniacal liquor, regulating pH is 2.1, obtains solution C;
4) solution C is inserted in air dry oven, in 80 ℃ of freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 4 ℃/min, from room temperature, be warming up to 700 ℃, insulation 2h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
As seen from Figure 1, the product of preparing is the La of single-phase substantially
2-xba
xcuO
4.
Embodiment 2:
1) get 35ml distilled water and add in beaker, by La: Ba: Cu=1.98: within 0.02: 1, mol ratio is by analytically pure lanthanum nitrate (La (NO
3)
36H
2o), nitrate of baryta (Ba (NO
3)
2) and cupric nitrate (Cu (NO
3)
33H
2o) add magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.1mol/L;
2) by the mol ratio of citric acid and metallic cation summation be 2: 1 by analytically pure citric acid (C
6h
8o
7h
2o) add in solution A the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 3% ammoniacal liquor, regulating pH is 1.5, obtains solution C;
4) solution C is inserted in air dry oven, in 60 ℃ of freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 5 ℃/min, from room temperature, be warming up to 500 ℃, insulation 7h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
Embodiment 3:
1) get 70ml distilled water and add in beaker, by La: Ba: Cu=1.8: within 0.2: 1, mol ratio is by analytically pure lanthanum nitrate (La (NO
3)
36H
2o), nitrate of baryta (Ba (NO
3)
2) and cupric nitrate (Cu (NO
3)
33H
2o) add magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.3mol/L;
2) by the mol ratio of citric acid and metallic cation summation be 0.5: 1 by analytically pure citric acid (C
6h
8o
7h
2o) add in solution A the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 5% ammoniacal liquor, regulating pH is 4, obtains solution C;
4) solution C is inserted in air dry oven, in 110 ℃ of freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 3 ℃/min, from room temperature, be warming up to 900 ℃, insulation 0.5h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
Embodiment 4:
1) get 95ml distilled water and add in beaker, by La: Ba: Cu=1.7: within 0.3: 1, mol ratio is by analytically pure lanthanum nitrate (La (NO
3)
36H
2o), nitrate of baryta (Ba (NO
3)
2) and cupric nitrate (Cu (NO
3)
33H
2o) add magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.4mol/L;
2) by the mol ratio of citric acid and metallic cation summation be 2.5: 1 by analytically pure citric acid (C
6h
8o
7h
2o) add in solution A the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 3% ammoniacal liquor, regulating pH is 3, obtains solution C;
4) solution C is inserted in air dry oven, in 100 ℃ of freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 4 ℃/min, from room temperature, be warming up to 600 ℃, insulation 4h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
Claims (1)
1. sol-gel method is prepared La
2-xba
xcuO
4the method of powder, is characterized in that:
1) get 35ml～95ml distilled water and add in beaker, by La:Ba:Cu=2-x:x:1 mol ratio by analytically pure La (NO
3)
36H
2o, Ba (NO
3)
2and Cu (NO
3)
23H
2o adds magnetic agitation in beaker extremely completely to dissolve and be mixed with the solution A that lanthanum nitrate concentration is 0.1-0.4mol/L, wherein x=0.02～0.3;
2) mol ratio of pressing citric acid and metallic cation summation is (0.5～2.5): 1 by analytically pure C
6h
8o
7h
2o adds in solution A, the even solution B that obtains of stirring at normal temperature;
3) to dropwise adding mass percent in solution B, be 3%～5% ammoniacal liquor, regulating pH is 1.5～4, obtains solution C;
4) solution C is inserted in air dry oven, in 60 ℃～110 ℃ freeze-day with constant temperature, obtained xerogel;
5) xerogel is used to mortar grinding powder, added in crucible, insert in retort furnace, with the temperature rise rate of 3～5 ℃/min, from room temperature, be warming up to 500 ℃～900 ℃, insulation 0.5h～7h, is cooled to room temperature, takes out crucible, and wherein material grind into powder, obtains La
2-xba
xcuO
4powder.
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|---|---|---|---|
| CN201110375498.6A CN102502766B (en) | 2011-11-23 | 2011-11-23 | Method for preparing La2-xBaxCuO4 powder by sol-gel method |
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|---|---|---|---|
| CN201110375498.6A CN102502766B (en) | 2011-11-23 | 2011-11-23 | Method for preparing La2-xBaxCuO4 powder by sol-gel method |
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| CN102502766B true CN102502766B (en) | 2014-04-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347797A (en) * | 2015-10-10 | 2016-02-24 | 东北大学 | R2Cu2O5 oxide material used for low-temperature magnetic refrigeration and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112126250B (en) * | 2020-09-24 | 2022-05-13 | 中国科学院包头稀土研发中心 | Rare earth green pigment without cobalt and chromium, and preparation method and application thereof |
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2011
- 2011-11-23 CN CN201110375498.6A patent/CN102502766B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| La2CuO4微晶的溶胶–凝胶法制备及合成活化能;李意峰等;《硅酸盐学报》;20110930;第39卷(第9期);1418-1422 * |
| 李意峰等.La2CuO4微晶的溶胶–凝胶法制备及合成活化能.《硅酸盐学报》.2011,第39卷(第9期),1418-1422. |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347797A (en) * | 2015-10-10 | 2016-02-24 | 东北大学 | R2Cu2O5 oxide material used for low-temperature magnetic refrigeration and preparation method thereof |
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| CN102502766A (en) | 2012-06-20 |
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Effective date of registration: 20201117 Address after: 226200 Binjiang fine chemical industry park, Nantong, Jiangsu, Qidong Patentee after: Qidong Binhua water supply Co.,Ltd. Address before: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. Effective date of registration: 20201117 Address after: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |