CN109727720A - A kind of preparation method of Bi2212 high-temperature superconductor powder - Google Patents
A kind of preparation method of Bi2212 high-temperature superconductor powder Download PDFInfo
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- CN109727720A CN109727720A CN201910179619.6A CN201910179619A CN109727720A CN 109727720 A CN109727720 A CN 109727720A CN 201910179619 A CN201910179619 A CN 201910179619A CN 109727720 A CN109727720 A CN 109727720A
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Abstract
The invention discloses a kind of preparation method of Bi2212 high-temperature superconductor powder, this method comprises: one, by Bi2O3、CaCO3、SrCO3It is dissolved with Cu, obtains corresponding salting liquid, then mix to obtain mixing salt solution, then adjust mixing salt solution concentration with deionized water；Two, it will be thermally decomposed after the mixing salt solution atomization after deionized water is adjusted using ultrasonic atomizatio method, oxide powder obtained using Electrostatic；Three, oxide powder is carried out obtaining Bi2212 high-temperature superconductor powder at being mutually heat-treated.The present invention is from raw material control, Bi2212 high-temperature superconductor powder is prepared at mutually heat treatment in conjunction with ultrasonic atomizatio method, thermal decomposition, Electrostatic, avoid element segregation, improve the uniformity of each element in Bi2212 high-temperature superconductor powder, reduce into the step of being mutually heat-treated, so as to avoid the generation of the second phase of bulky grain, the performance of Bi2212 high-temperature superconductor powder is improved.
Description
Technical field
The invention belongs to high-temperature superconductor powder preparation technical fields, and in particular to a kind of system of Bi2212 high-temperature superconductor powder
Preparation Method.
Background technique
Bi2212(Bi2Sr2CaCu2Ox) have relatively high superconducting transition temperature (85K), relatively high upper critical field, than
Higher current-carrying performance and relatively good processing performance are one of the high temperature superconducting materias of Bi most future.Bi2212 superconducting line
Material generally uses powder-in-tube technique (PIT) to prepare, and first prepares Bi2212 superconductive powder, and superconductive powder is then packed into silver-colored pipe and is drawn
It pulls out and prepares single-core line, prepare split conductor using assembling and drawing, obtain Bi2212 finally by part fusing heat treatment
Superconducting wire, wherein Bi2212 powder is the key that prepare wire rod.
The preparation method of Bi2212 high-temperature superconductor powder mainly has solid reaction process and coprecipitation.Solid reaction process will be golden
Belong to oxide or metal salt passes through multiple mixed grinding and sintering, the Bi2212 high-temperature superconductor powder granularity of preparation is big, member
Element is easy segregation；Coprecipitation generally uses oxalate coprecipitation, and needs by up to ten sintering and grinding several times, preparation
Bi2212 high-temperature superconductor powder granularity it is big, element is easy segregation, and carbon content is high, when preparing superconducting wire, in oxygen
Handle CO easy to form2It is bubbled wire rod.Other methods are quickly cooled down the Bi2212 high-temperature superconductor of polishing preparation such as melting
Powder size is big, is unfavorable for Multi-core wire preparation；There is flammable body to participate in reaction, system in the preparation process of flame atomizing thermal decomposition method
Standby Bi2212 high-temperature superconductor powder carbon content is higher.
Since Bi2212 high-temperature superconductor powder includes Determination of multiple metal elements, changed using traditional solid phase reaction and co-precipitation etc.
Method preparation be easy to cause element segregation, influences the performance of Bi2212 superconducting wire, and the powder of coprecipitation method preparation
Need multistep at being mutually heat-treated, the second phase that will form bulky grain is made to influence the processing uniformity of subsequent superconducting wire
At the decline of wire rod part current-carrying performance.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of Bi2212 high temperature
The preparation method of superconductive powder.This method is from raw material control, in conjunction with ultrasonic atomizatio method, thermal decomposition, Electrostatic and at phase
Heat treatment, is prepared Bi2212 high-temperature superconductor powder, avoids element segregation, improves each in Bi2212 high-temperature superconductor powder
The uniformity of element, reduces into the step of being mutually heat-treated, and so as to avoid the generation of the second phase of bulky grain, improves
The performance of Bi2212 high-temperature superconductor powder.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of system of Bi2212 high-temperature superconductor powder
Preparation Method, which is characterized in that method includes the following steps:
Step 1: using nitric acid respectively to Bi2O3、CaCO3、SrCO3It is dissolved with Cu, it is molten to obtain Bi salting liquid, Ca salt
Then above-mentioned four kinds of salting liquids are uniformly mixed and obtain mixing salt solution, then use deionized water by liquid, Sr salting liquid and Cu salting liquid
Mixing salt solution concentration is adjusted, metal ion total concentration 0.5mol/L~1.0mol/L in mixing salt solution is made；It is described
Bi2O3、CaCO3、SrCO3Mass ratio with Cu is 3.67:1.58:1.16:1；
Step 2: the mixing salt solution in step 1 after deionized water is adjusted is atomized into liquid using ultrasonic atomizatio method
Drop, then drop is brought into high temperature pipe furnace thermally decompose by gas, then is trapped using electrostatic, and oxidate powder is obtained
End；
It carries out obtaining Bi2212 at being mutually heat-treated Step 3: oxide powder obtained in step 2 is placed in electric furnace
High-temperature superconductor powder.
The present invention uses nitric acid to be completely dissolved four kinds of raw materials first and is configured to certain density mixing salt solution, usually adopts
Guaranteed to be completely dissolved and prevent the precipitation of metal salt with excessive concentrated nitric acid, since the performance of above-mentioned four kinds of raw materials is stable and without knot
Brilliant water controls the ratio of each metal ion in mixing salt solution by the mass ratio of considered critical four kinds of raw materials, to control
Four kinds of metallic element ratios in Bi2212 high-temperature superconductor powder have been made, the quality of Bi2212 high-temperature superconductor powder has been improved, avoids
The nitrate comprising the crystallization water for directlying adopt corresponding four kinds of metallic elements leads to deviation occur during weighing as raw material, into
Caused by element ratio deviation in Bi2212 high-temperature superconductor powder, in addition, four kinds of raw materials of the invention are easy to get, cost compared with
It is low, and solubility property is preferable；Then the mixing salt solution after deionized water is adjusted is converted to by liquid using ultrasonic atomizatio method
It drips and is thermally decomposed, the mixing salt solution comprising four metal ion species is formed by ultrasonic atomizatio having a size of micron-sized liquid
Drop, the size droplet diameter is small, is readily decomposed to phase, and drop is thermally decomposed under floating state, and obtaining main phase is Bi2Sr2CaCu2Ox
(i.e. Bi2212 phase), Bi2Sr2CuOx(i.e. Bi2201 phase), Ca2CuO3With the oxide powder of CuO, reduce element loss, keeps away
Element segregation is exempted from；Again through once at being mutually heat-treated, removing the moisture adsorbed in oxide powder, and make to wrap in oxide powder
The Bi contained2Sr2CuOx、Ca2CuO3With CuO the reaction was continued generate Bi2Sr2CaCu2Ox, improve in Bi2212 high-temperature superconductor powder
The content of Bi2212 phase.Method of the invention effectively prevents element segregation, improves each member in Bi2212 high-temperature superconductor powder
The uniformity of element, reduces into the step of being mutually heat-treated, so as to avoid the generation of the second phase of bulky grain, promotes Bi2212
The performance of high-temperature superconductor powder.
The preparation method of above-mentioned a kind of Bi2212 high-temperature superconductor powder, which is characterized in that Cu described in step 1 is nothing
Oxygen copper.The quality purity of copper is higher in oxygen-free copper, and the proportional jitter of four kinds of metallic elements is further reduced from raw material, improves
The quality of Bi2212 high-temperature superconductor powder.
A kind of preparation method of above-mentioned Bi2212 high-temperature superconductor powder, which is characterized in that drop described in step 2
Granularity is 1 μm~10 μm.The granularity for the drop that control ultrasonic atomizatio method obtains is 1 μm~10 μm, thus after ensure that thermal decomposition
Oxide powder granularity be 1 μm~5 μm, be conducive to subsequent Electrostatic, reduce oxide powder loss, improve
The yield of Bi2212 high-temperature superconductor powder, while the size distribution of Bi2212 high-temperature superconductor powder is controlled in relatively narrow range,
Further avoid the element segregation in Bi2212 high-temperature superconductor powder.
The preparation method of above-mentioned a kind of Bi2212 high-temperature superconductor powder, which is characterized in that thermally decomposed described in step 2
Temperature be 800 DEG C~900 DEG C.The temperature of above-mentioned thermal decomposition advantageously reduces Bi2Sr2CuOxThe formation of (i.e. Bi2201 phase), together
When promote Bi2Sr2CaCu2OxA large amount of formation of (i.e. Bi2212 phase), improve the content of Bi2201 phase in oxide powder,
In turn avoid temperature it is excessively high cause oxide powder formed hard aggregation, improve the powder characteristic of Bi2212 high-temperature superconductor powder.
A kind of preparation method of above-mentioned Bi2212 high-temperature superconductor powder, which is characterized in that Cheng Xiangre described in step 3
The temperature of processing is 800 DEG C~865 DEG C, and the time is 30min~60min.It is above-mentioned to be conducive at the temperature and time being mutually heat-treated
The Bi for including in oxide powder2Sr2CuOx、Ca2CuO3With CuO the reaction was continued generate Bi2Sr2CaCu2Ox, further improve
The content of Bi2212 phase in Bi2212 high-temperature superconductor powder.
Compared with the prior art, the present invention has the following advantages:
1, the present invention is prepared in conjunction with ultrasonic atomizatio method, thermal decomposition, Electrostatic at mutually heat treatment from raw material control
Bi2212 high-temperature superconductor powder is obtained, element segregation is avoided, improves the uniform of each element in Bi2212 high-temperature superconductor powder
Property, reduce into the step of being mutually heat-treated, so as to avoid the generation of the second phase of bulky grain, improves Bi2212 high-temperature superconductor
The performance of powder.
2, the present invention can make the size distribution of Bi2212 high-temperature superconductor powder in relatively narrow model by controlling the granularity of drop
In enclosing, reduces oxide powder loss, improve the yield of Bi2212 high-temperature superconductor powder, while it is super to control Bi2212 high temperature
The size distribution of powder is led in relatively narrow range, the uniformity of Bi2212 high-temperature superconductor powder is further improved, avoids
Element segregation in Bi2212 high-temperature superconductor powder.
3, the Bi2212 high-temperature superconductor powder uniformity that the present invention is prepared is preferable, Bi2212 phase (Bi2Sr2CaCu2Ox)
Content is high, and since Bi2212 is layer structure structure, c-axis direction atomic distance is big in lattice, is easy sliding, high-content Bi2212
The Bi2212 high-temperature superconductor powder of phase powder in superconducting wire drawing process is easy flowing, is conducive to multi-core superconducting wire rod system
It is standby；Meanwhile preparation process of the invention does not have C element introducing, and powder carbon content is low, and superconducting wire will not be caused to be bubbled, and
Bi2212 high-temperature superconductor powder partial size is small, large specific surface area, has relatively high activity, is conducive to the raising of superconducting wire performance,
To improve the current-carrying performance of Bi2212 hts tape.
4, preparation process of the invention is simple, and preparation efficiency is high, easy to spread.
Technical solution of the present invention is described in further detail below by embodiment.
Specific embodiment
Embodiment 1
The preparation method of the present embodiment the following steps are included:
Step 1: using nitric acid respectively to the Bi of 7.34g2O3, 3.16g CaCO3, 2.32g SrCO3With the Cu of 2g into
Row dissolution, obtains Bi salting liquid, Ca salting liquid, Sr salting liquid and Cu salting liquid, is then uniformly mixed above-mentioned four kinds of salting liquids
Mixing salt solution is obtained, then adjusts mixing salt solution concentration with deionized water, makes the metal ion total concentration in mixing salt solution
For 1.0mol/L；
Step 2: the mixing salt solution in step 1 after deionized water is adjusted is atomized into granularity using ultrasonic atomizatio method
For 1 μm~10 μm of drop, then drop is brought into high temperature pipe furnace by gas and is thermally decomposed at 850 DEG C, then used
Electrostatic is trapped, and oxide powder is obtained；
Step 3: oxide powder obtained in step 2 is placed in electric furnace, in air atmosphere, temperature be 850 DEG C
Under conditions of at 45min is mutually heat-treated, obtain Bi2212 high-temperature superconductor powder.
Embodiment 2
The preparation method of the present embodiment the following steps are included:
Step 1: using nitric acid respectively to the Bi of 3.67g2O3, 1.58g CaCO3, 1.16g SrCO3With the anaerobic of 1g
Copper is dissolved, and Bi salting liquid, Ca salting liquid, Sr salting liquid and Cu salting liquid are obtained, and then mixes above-mentioned four kinds of salting liquids
Mixing salt solution is uniformly obtained, then adjusts mixing salt solution concentration with deionized water, keeps the metal ion in mixing salt solution total
Concentration is 0.5mol/L；
Step 2: the mixing salt solution in step 1 after deionized water is adjusted is atomized into granularity using ultrasonic atomizatio method
For 1 μm~10 μm of drop, then drop is brought into high temperature pipe furnace by gas and is thermally decomposed at 800 DEG C, then used
Electrostatic is trapped, and oxide powder is obtained；
Step 3: oxide powder obtained in step 2 is placed in electric furnace, in air atmosphere, temperature be 800 DEG C
Under conditions of at 30min is mutually heat-treated, obtain Bi2212 high-temperature superconductor powder.
Embodiment 3
The preparation method of the present embodiment the following steps are included:
Step 1: using nitric acid respectively to the Bi of 11.01g2O3, 4.74g CaCO3, 3.48g SrCO3With the Cu of 3g into
Row dissolution, obtains Bi salting liquid, Ca salting liquid, Sr salting liquid and Cu salting liquid, is then uniformly mixed above-mentioned four kinds of salting liquids
Mixing salt solution is obtained, then adjusts mixing salt solution concentration with deionized water, makes the metal ion total concentration in mixing salt solution
For 0.80mol/L；
Step 2: the mixing salt solution in step 1 after deionized water is adjusted is atomized into granularity using ultrasonic atomizatio method
For 1 μm~10 μm of drop, then drop is brought into high temperature pipe furnace by gas and is thermally decomposed at 900 DEG C, then used
Electrostatic is trapped, and oxide powder is obtained；
Step 3: oxide powder obtained in step 2 is placed in electric furnace, in air atmosphere, temperature be 865 DEG C
Under conditions of at 60min is mutually heat-treated, obtain Bi2212 high-temperature superconductor powder.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (5)
1. a kind of preparation method of Bi2212 high-temperature superconductor powder, which is characterized in that method includes the following steps:
Step 1: using nitric acid respectively to Bi2O3、CaCO3、SrCO3It is dissolved with Cu, obtains Bi salting liquid, Ca salting liquid, Sr
Then above-mentioned four kinds of salting liquids are uniformly mixed and obtain mixing salt solution, then adjusted with deionized water by salting liquid and Cu salting liquid
Mixing salt solution concentration makes metal ion total concentration 0.5mol/L~1.0mol/L in mixing salt solution；The Bi2O3、
CaCO3、SrCO3Mass ratio with Cu is 3.67:1.58:1.16:1；
Step 2: the mixing salt solution in step 1 after deionized water is adjusted is atomized into drop using ultrasonic atomizatio method, so
Drop is brought into high temperature pipe furnace by gas afterwards and is thermally decomposed, then is trapped using electrostatic, oxide powder is obtained；
Step 3: oxide powder obtained in step 2 is placed in electric furnace, carries out into being mutually heat-treated in air atmosphere, obtains
To Bi2212 high-temperature superconductor powder.
2. a kind of preparation method of Bi2212 high-temperature superconductor powder according to claim 1, which is characterized in that in step 1
The Cu is oxygen-free copper.
3. a kind of preparation method of Bi2212 high-temperature superconductor powder according to claim 1, which is characterized in that in step 2
The granularity of the drop is 1 μm~10 μm.
4. a kind of preparation method of Bi2212 high-temperature superconductor powder according to claim 1, which is characterized in that in step 2
The temperature of the thermal decomposition is 800 DEG C~900 DEG C.
5. a kind of preparation method of Bi2212 high-temperature superconductor powder according to claim 1, which is characterized in that in step 3
It is described at the temperature being mutually heat-treated be 800 DEG C~865 DEG C, the time be 30min~60min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110817956A (en) * | 2019-12-07 | 2020-02-21 | 西北有色金属研究院 | Preparation method of nano Bi-2212 precursor powder |
| CN110817957A (en) * | 2019-12-07 | 2020-02-21 | 西北有色金属研究院 | Method for preparing Bi-2212 precursor powder by suspension sintering method |
| CN110853830A (en) * | 2019-11-21 | 2020-02-28 | 西北有色金属研究院 | Preparation method of Bi-2212 multi-core superconducting wire |
| CN113603138A (en) * | 2021-09-08 | 2021-11-05 | 西北有色金属研究院 | Method for preparing Bi2212 micro-nano powder by chemical combustion |
| CN114093568A (en) * | 2021-11-26 | 2022-02-25 | 西北有色金属研究院 | Heat treatment method of Bi-2223 high-temperature superconducting strip |
| CN114920291A (en) * | 2022-07-04 | 2022-08-19 | 西北有色金属研究院 | Method for preparing Bi-2212 superconducting powder by alternately feeding liquid |
| CN114974723A (en) * | 2022-07-04 | 2022-08-30 | 西北有色金属研究院 | Preparation method of Bi-2212 superconducting powder with controllable second phase |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110853830A (en) * | 2019-11-21 | 2020-02-28 | 西北有色金属研究院 | Preparation method of Bi-2212 multi-core superconducting wire |
| CN110817956A (en) * | 2019-12-07 | 2020-02-21 | 西北有色金属研究院 | Preparation method of nano Bi-2212 precursor powder |
| CN110817957A (en) * | 2019-12-07 | 2020-02-21 | 西北有色金属研究院 | Method for preparing Bi-2212 precursor powder by suspension sintering method |
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| CN114093568A (en) * | 2021-11-26 | 2022-02-25 | 西北有色金属研究院 | Heat treatment method of Bi-2223 high-temperature superconducting strip |
| CN114093568B (en) * | 2021-11-26 | 2023-01-31 | 西北有色金属研究院 | Heat treatment method of Bi-2223 high-temperature superconducting strip |
| CN114920291A (en) * | 2022-07-04 | 2022-08-19 | 西北有色金属研究院 | Method for preparing Bi-2212 superconducting powder by alternately feeding liquid |
| CN114974723A (en) * | 2022-07-04 | 2022-08-30 | 西北有色金属研究院 | Preparation method of Bi-2212 superconducting powder with controllable second phase |
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Application publication date: 20190507 |