CN110937629A - Method for preparing Bi-2212 precursor powder by inclined rotary sintering method - Google Patents
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Abstract
The invention discloses a method for preparing Bi-2212 precursor powder by an inclined rotary sintering method, which comprises the following steps: first, Bi2O3、Ca(OH)2、SrCO3Preparing mixed powder or oxalate mixed powder with CuO; and secondly, loading the mixed powder or oxalate mixed powder into an inclined continuous rotating automatic sintering device, and carrying out continuous sectional heating sintering under the condition that furnace tubes of each sintering furnace are inclined and rotate to obtain the Bi-2212 precursor powder. The invention adopts the inclined continuous rotary sintering method to carry out the step-by-step temperature rise sintering, so that the corresponding processing powder is uniformly and continuously distributed in the furnace tube, the thickness of the processing powder in each sintering process is effectively reduced, andthe method is beneficial to the diffusion of external atmosphere into the treated powder, avoids the generation of impurity phases of the treated powder at the bottom or the center of the treated powder pile in the sintering process due to the low-oxygen atmosphere, and improves the quality of the Bi-2212 precursor powder.
Description
Technical Field
The invention belongs to the technical field of preparation of Bi-2212 superconducting wire strips, and particularly relates to a method for preparing Bi-2212 precursor powder by an inclined rotary sintering method.
Background
Bi-2212 high-temperature superconductor (Bi)2Sr2CaCu2Ox) Is the most important branch in high-temperature superconducting materials. Because of its easy processing and high current-carrying property, the Bi-2212 wire becomes one of the most promising high-temperature superconducting materials at present. The quality of the Bi-2212 precursor powder has a determining effect on the current-carrying performance of the Bi-2212 wire. The criteria for high quality Bi-2212 precursor powder are: high purity Bi-2212 phase powder, small and uniform particle size, as few as possible of impure phases and impurities. Height ofThe quality of Bi-2212 precursor powder puts high requirements on the powder preparation technology.
The reaction of the five-membered compound is complex, and the preparation of the high-purity phase five-membered compound is very difficult. The Bi-2212 powder is very sensitive not only to temperature but also to the sintering atmosphere. Different sintering atmospheres can obtain different phases at the same temperature, and even at the same temperature, high-purity Bi-2212 powder can be obtained by proper oxygen partial pressure, while the great accident that the powder is completely melted occurs under low-oxygen atmosphere, so that the sintering atmosphere of the powder must be strictly controlled to realize high-quality Bi-2212 precursor powder. But the conventional solid state sintering method is difficult to satisfy the requirements. Because when the conventional sintering is adopted, the amount of each sintering is larger and the thickness of the powder is higher in order to ensure the yield of the powder. During sintering, the atmosphere of the powder at the bottom or even at the center of the powder pile is difficult to ensure to meet the requirement. This is because the sintering process of the Bi-2212 powder is similar to the breathing process, the Bi-2212 powder absorbs oxygen during the temperature rise process of sintering, and the discharged part of easily decomposed impurities are decomposed to release part of gas, which results in an atmosphere with low oxygen partial pressure around each crystal grain of the Bi-2212 powder. This has little effect on the powder grains at the surface of the powder mass because, as the partial pressure of oxygen varies around these grains, oxygen in the ambient atmosphere can be replenished relatively quickly around these grains, ensuring a stable partial pressure of oxygen around these grains. However, for the powder grains at the bottom or the center of the powder pile, the problem of reduced oxygen partial pressure around the grains also occurs in the temperature rising process, but the powder is far away from the surface of the powder pile, and the external gas needs to supplement oxygen and needs to diffuse for a long time, so that the powder is in a low-oxygen atmosphere state for a long time, and the powder at the position has impurity phases, which greatly affects the powder quality.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing Bi-2212 precursor powder by inclined rotary sintering process, aiming at the defects of the prior art. The method adopts an inclined continuous rotary sintering method to carry out sectional heating sintering, so that the corresponding processing powder is uniformly and continuously distributed in the furnace tubes of each sintering furnace and sequentially and continuously moves, the thickness of the processing powder in each sintering process is effectively reduced, the external atmosphere is favorably diffused into the processing powder, the processing powder at the bottom or the center of a processing powder pile in the heating sintering process is prevented from generating impurity phases because the processing powder is in a low-oxygen atmosphere, and the quality of the Bi-2212 precursor powder is improved.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing Bi-2212 precursor powder by an inclined rotary sintering method is characterized by comprising the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3And CuO, wherein the CuO is prepared into mixed powder according to the atomic ratio of Bi, Sr, Ca, Cu, (1.95-2.2), (0.9-1) and (1.95-2.2);
or Bi2O3、Ca(OH)2、SrCO3And CuO are mixed according to the atomic ratio of Bi, Sr, Ca, Cu, (1.95-2.2), (0.9-1) and (1.95-2.2), then a nitrate mixed solution is prepared, and an oxalate coprecipitation method is adopted to prepare oxalate mixed powder;
step two, the mixed powder or oxalate mixed powder obtained in the step one is filled into a raw material powder storage tank of a primary sintering furnace in an inclined continuous rotary automatic sintering device to be used as raw material powder, the primary sintering furnace, a low-temperature sintering furnace, a medium-temperature sintering furnace, a high-temperature sintering furnace and a phase-forming sintering furnace are heated and kept warm for more than 30min, then furnace tubes of the primary sintering furnace, the low-temperature sintering furnace, the medium-temperature sintering furnace, the high-temperature sintering furnace and the phase-forming sintering furnace after heat preservation are inclined along the feeding direction to the discharging direction, the furnace tubes of the sintering furnaces are rotated, an air inlet switch of each sintering furnace is opened to introduce the sintering atmosphere, an induced draft fan of each sintering furnace is opened, a powder adding device of each sintering furnace is opened, the raw material powder in the raw material powder storage tank sequentially enters the primary sintering furnace, the low-temperature sintering furnace, the medium-temperature sintering furnace, the high-temperature sintering furnace and the phase-forming sintering furnace, obtaining Bi-2212 precursor powder.
The method comprises the steps of loading raw material powder for preparing Bi-2212 precursor powder into a raw material powder storage tank of an inclined continuous rotating automatic sintering device, then feeding and sequentially carrying out primary sintering, low-temperature sintering, medium-temperature sintering, high-temperature sintering and phase-forming sintering under the condition that furnace tubes of all sintering furnaces are in an inclined rotating state to obtain the Bi-2212 precursor powder, wherein when the furnace tubes of all sintering furnaces are in an inclined rotating state, under the action of gravity and the friction force of the furnace tubes, the powder adding speed, the included angle between the furnace tubes of all sintering furnaces and a horizontal ground and the rotating speed are controlled to uniformly and continuously distribute corresponding treated powder in the furnace tubes of all sintering furnaces, and the treated powder continuously moves from a feed inlet to a discharge outlet of each sintering furnace, so that accumulation and flow-off of the treated powder are avoided, the thickness of the treated powder in each sintering process is effectively reduced, and external atmosphere is facilitated to diffuse into the treated powder, the method avoids the phenomenon that the processing powder at the bottom or the center of the processing powder pile is in a low-oxygen atmosphere state in the heating and sintering process to cause impurity phases in the processing powder at the position, and improves the quality of the Bi-2212 precursor powder.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that in the second step, the temperature of the primary sintering furnace is increased to 450-500 ℃, the temperature of the low-temperature sintering furnace is increased to 600-650 ℃, the temperature of the medium-temperature sintering furnace is increased to 700-750 ℃, the temperature of the high-temperature sintering furnace is increased to 800-820 ℃, and the temperature of the phase-forming sintering furnace is increased to 830-850 ℃. Preferably, each sintering furnace is preheated to the sintering temperature of the subsequent raw materials in each sintering furnace in sequence, so that the stability of each sintering process is ensured, and the generation of adverse impurities caused by temperature difference in each sintering process is avoided.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that furnace tubes of the primary sintering furnace, the low-temperature sintering furnace, the medium-temperature sintering furnace, the high-temperature sintering furnace and the phase-forming sintering furnace in the step two are inclined along the feeding and discharging direction and form an included angle of 10-30 degrees with the horizontal ground.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that the rotation rate of the furnace tube of each sintering furnace in the step two is 3-5 circles/min.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that the introduction rate of the sintering atmosphere in the second step is 200 mL/min-500 mL/min.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that the powder adding speed of the powder adding device in the second step is 10 g/min-30 g/min.
The preferable included angle between the furnace tube of each sintering furnace and the horizontal ground, the rotation speed of the furnace tube, the introduction speed of the sintering atmosphere and the powder adding speed further ensure that the corresponding processed powder is uniformly and continuously distributed in the furnace tube of each sintering furnace, avoid the accumulation of the processed powder to generate an impurity phase and improve the quality of the Bi-2212 precursor powder.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that in the second step, the sintering atmosphere is formed by mixing high-purity nitrogen and oxygen, wherein the mass purity of the nitrogen is not less than 99.99%, the partial pressure of the oxygen is 20-22%, and the partial pressure of the impurity atmosphere is less than 100 ppm. The common sintering atmosphere is selected, so that the preparation difficulty of the invention is reduced, and the practical value of the invention is enlarged.
The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method is characterized in that furnace tube main bodies of a primary sintering furnace, a low-temperature sintering furnace, a medium-temperature sintering furnace, a high-temperature sintering furnace and a phase forming sintering furnace in the inclined continuous rotary automatic sintering equipment in the step two are all made of high-temperature alloy, wherein a silicon dioxide coating prepared by a thermal spraying method covers the inner surface of a high-temperature alloy furnace tube, and a pure silver lining layer prepared by an explosion cladding method covers the surface of the silicon dioxide coating. The preferable furnace tube adopts high-temperature alloy as the supporting material of the furnace tube, adopts the pure silver lining layer to avoid the pollution of sintering powder, adopts the silicon dioxide coating layer as the blocking layer, effectively inhibits the diffusion between the pure silver lining layer and the high-temperature alloy, and is beneficial to the smooth proceeding of each sintering process.
Compared with the prior art, the invention has the following advantages:
1. the method comprises the steps of sequentially carrying out primary sintering, low-temperature sintering, medium-temperature sintering, high-temperature sintering and phase-forming sintering on raw material powder by adopting an inclined continuous rotary sintering method to obtain Bi-2212 precursor powder, and controlling the powder feeding rate, the included angle between the furnace tube of each sintering furnace and the horizontal ground and the rotation rate to uniformly and continuously distribute the corresponding processed powder in the furnace tube of each sintering furnace and sequentially and continuously move, so that the thickness of the processed powder in each sintering process is effectively reduced (the thickness is 3-5 mm) and is lower than that of the powder in conventional static sintering (usually about 50 mm), external atmosphere diffusion is facilitated to enter the processed powder, impure phases are prevented from being generated in the processed powder at the bottom or the center of a processed powder pile in the heating sintering process due to the low-oxygen atmosphere, and the quality of the Bi-2212 precursor powder is improved.
2. In the preparation process of the inclined continuous rotary sintering method, the processing powder of each sintering furnace rotates along with the rotation of the furnace tube, so that the processing powder is stirred, the uniformity of the processing powder is improved, and the impurity phase caused by the fact that the processing powder at the bottom or the center of the processing powder is in a low-oxygen atmosphere for a long time is further avoided; in addition, the stirring process greatly accelerates the dispersion rate of the atmosphere in the sintering furnace, reduces the atmosphere difference of different parts of the treated powder, promotes the consistency of the oxygen partial pressure in the atmosphere of different parts of the treated powder and the oxygen partial pressure in the atmosphere of the sintering furnace, and further improves the quality of the Bi-2212 precursor powder.
3. The invention adopts a continuous dynamic sintering method, raw material powder sequentially enters each sintering furnace from the powder feeder and moves at the same speed and is sintered simultaneously, the consistency of the sintering process of all the raw material powder is ensured, the powder inlet and the powder outlet of each sintering furnace of the adopted inclined continuous rotation automatic sintering equipment are completely separated, the pollution of the processing powder added in each sintering furnace to the sintered processing powder is avoided, the preparation efficiency is improved, and the quality of the Bi-2212 precursor powder is further improved.
4. According to the invention, the gas outlet and the induced draft fan are arranged in each sintering furnace of the inclined continuous rotation automatic sintering equipment, and waste gas generated in the process of each sintering stage can be discharged to the external environment of the sintering furnace through the induced draft fan, so that adverse effects of the waste gas on the sintering process are avoided, and the improvement of the quality of the Bi-2212 precursor powder is facilitated.
5. The raw material powder is directly heated and sintered by a one-step sintering method in the prior art, and is rapidly decomposed into Bi2O3Bi after SrO2O3Compared with the method that the Bi which is not yet reacted with other elements and is melted to cause element segregation, the method adopts a sintering mode of temperature segmentation and gradually increases the temperature to decompose the raw material powder2O3Firstly, the high-temperature phase reacts with SrO, CaO and CuO completely to generate Bi-Sr-Cu-O or Bi-Sr-Cu-O and other high-temperature phases, and meanwhile, the sintering temperature of the next step is controlled to be lower than the melting point of the processed powder, so that the Bi-rich high-temperature phase cannot be melted, and the problem of powder segregation caused by powder melting is prevented.
6. The inclined continuous rotation automatic sintering equipment has the advantages of reasonable structure, easy realization, high automation degree, convenient operation and control, long-term continuous operation, great reduction of labor cost and suitability for industrial production of Bi-2212 precursor powder.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic structural view of an inclined continuous rotary automatic sintering apparatus used in the present invention.
Fig. 2 is a schematic structural diagram of each sintering furnace (primary sintering furnace, low-temperature sintering furnace, medium-temperature sintering furnace, high-temperature sintering furnace, phase-forming sintering furnace) in fig. 1.
Description of reference numerals:
1-primary sintering furnace; 1-raw material powder storage tank; 1-2-powder feeder;
1-3-a charging hopper; 1-4-dynamic sealing ring; 1-5-heating furnace;
1-6-synchronous belt; 1-7-motor; 1-8-induced draft fan;
1-9-a discharge funnel; 1-10 — a first bearing support; 1-11-synchronizing wheel;
1-12-fixed support; 1-13-lifting support; 1-14-second bearing support;
1-15-furnace tube; 1-16-air inlet; 2-low temperature sintering furnace;
3-medium temperature sintering furnace; 4-high temperature sintering furnace; 5-a phase forming sintering furnace;
6, a finished product powder storage tank.
Detailed Description
As shown in figure 1, the inclined continuous rotation automatic sintering equipment adopted by the invention comprises a primary sintering furnace 1, a low-temperature sintering furnace 2, a medium-temperature sintering furnace 3, a high-temperature sintering furnace 4 and a phase-forming sintering furnace 5 which are identical in structure and are sequentially connected, wherein the outlet of the phase-forming sintering furnace 5 is connected with a finished product powder storage tank 6.
As shown in figure 2, the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase-forming sintering furnace 5 have the same structure and respectively comprise furnace tubes 1-15 and heating furnaces 1-5 annularly arranged around the furnace tubes 1-15, the inlets of the furnace tubes 1-15 are connected with a raw material powder storage tank 1-1, a powder adding device 1-2 and a feeding funnel 1-3 are sequentially arranged between the raw material powder storage tank 1-1 and the inlets of the furnace tubes 1-15, the connecting part of the feeding funnel 1-3 and the furnace tubes 1-15 is provided with a dynamic sealing ring 1-4, the inlets of the furnace tubes 1-15 are also provided with air inlets 1-16, the outlets of the furnace tubes 1-15 are connected with a discharging funnel 1-9, the outlets of the furnace tubes 1-15 are connected with an induced draft fan 1-8 through pipelines, two ends of the furnace tubes 1-15 are respectively arranged on a support device through second bearing supports 1-14 and first bearing supports 1-10, the support device comprises fixed supports 1-12 and lifting supports 1-13, the outlet ends of the furnace tubes 1-15 are provided with synchronous wheels 1-11, and synchronous belts 1-6 arranged on the synchronous wheels 1-11 are connected with motors 1-7.
The furnace tube main bodies of the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase-forming sintering furnace 5 in the inclined continuous rotary automatic sintering equipment in the embodiments 1 to 8 of the invention are all made of high-temperature alloy, wherein the inner surface of the high-temperature alloy furnace tube is covered with a silica coating prepared by a thermal spraying method, and the surface of the silica coating is covered with a pure silver lining layer prepared by an explosion cladding method.
The details of the co-precipitation method for preparing the Bi-2212 precursor powder in the embodiments 1 to 8 of the present invention are described in the literature (huqing shore, preparation and performance research of high-current-carrying Bi-2212 high-temperature superconducting wire, northeast university, doctor academic thesis 2018), and the details of the spray thermal decomposition method for preparing the Bi-2212 precursor powder are described in the literature (the effect of the collection method on the spray thermal decomposition of the Bi-2223 precursor powder in heqing, huqing shore, and "low temperature and superconducting" 2018 st stage 1 59-63).
Example 1
The embodiment comprises the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3And CuO are prepared into mixed powder according to the atomic ratio of Bi, Sr, Ca and Cu of 1.95:1.95:0.9: 1.95;
or Bi2O3、Ca(OH)2、SrCO3And CuO are mixed according to the atomic ratio of Bi, Sr, Ca, Cu, (1.95-2.2), (0.9-1) and (1.95-2.2), then a nitrate mixed solution is prepared, and an oxalate coprecipitation method is adopted to prepare oxalate mixed powder;
step two, the mixed powder obtained in the step one is filled into a raw material powder storage tank 1-1 of a primary sintering furnace 1 in an inclined continuous rotary automatic sintering device to be used as raw material powder, the primary sintering furnace 1 is heated to 450 ℃, a low-temperature sintering furnace 2 is heated to 600 ℃, a medium-temperature sintering furnace 3 is heated to 700 ℃, a high-temperature sintering furnace 4 is heated to 800 ℃, a phase-forming sintering furnace 5 is heated to 830 ℃ and is kept warm for 30min, then the heat-preserved primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and furnace tubes 1-15 of the phase-forming sintering furnace 5 are inclined along the feeding and discharging direction and form 10-degree included angles with the horizontal ground in sequence, the furnace tubes 1-15 of each sintering furnace rotate at the speed of 3 circles/min, an air inlet switch of each sintering furnace is opened to introduce the sintering atmosphere at the air inlet speed of 200mL/min, an induced draft fan 1-8 of each sintering furnace, opening the powder adding devices 1-2 of the sintering furnaces to enable the raw material powder in the raw material powder storage tank 1-1 to sequentially enter the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase forming sintering furnace 5 for sintering at a powder adding rate of 10g/min and collect the raw material powder into a finished product powder storage tank 6, closing the powder adding devices 1-2 of the sintering furnaces for 1 hour, and taking down the finished product powder storage tank 6 to obtain Bi-2212 precursor powder; the sintering atmosphere is formed by mixing nitrogen and oxygen with the mass purity of 99.99%, wherein the partial pressure of the oxygen is 21%, and the partial pressure of the impurity atmosphere is lower than 100 ppm.
Comparing the Bi-2212 precursor powder prepared by the implementation with the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art by adopting a scanning electron microscope (multiplied by 100), wherein the result shows that the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the implementation is 1 per sheet, and the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art is 2 per sheet; under the same production period, the Bi-2212 precursor powder is prepared by respectively adopting the process of the embodiment and a coprecipitation method and a spray thermal decomposition method in the prior art, and the preparation efficiency of the embodiment is 700 kg/month by calculation, which is far higher than the preparation efficiency of the coprecipitation method in the prior art by 5 kg/month and the preparation efficiency of the spray thermal decomposition method by 20 kg/month, so that the preparation process reduces the generation of impurity phases, improves the quality of the Bi-2212 precursor powder, and simultaneously adopts a full-automatic inclined continuous rotary sintering method to greatly improve the preparation efficiency of the Bi-2212 precursor powder.
Example 2
The embodiment comprises the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3And CuO are prepared into mixed powder according to the atomic ratio of Bi, Sr, Ca and Cu being 2.2:2.2:1: 2.2;
step two, the mixed powder obtained in the step one is filled into a raw material powder storage tank 1-1 of a primary sintering furnace 1 in an inclined continuous rotary automatic sintering device to be used as raw material powder, the primary sintering furnace 1 is heated to 500 ℃, a low-temperature sintering furnace 2 is heated to 650 ℃, a medium-temperature sintering furnace 3 is heated to 750 ℃, a high-temperature sintering furnace 4 is heated to 820 ℃, a phase-forming sintering furnace 5 is heated to 850 ℃ and is kept warm for 30min, then the heat-preserved primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and furnace tubes 1-15 of the phase-forming sintering furnace 5 are inclined along the feeding and discharging direction and form 30-degree included angles with the horizontal ground, the furnace tubes 1-15 of each sintering furnace rotate at the speed of 5 circles/min, an air inlet switch of each sintering furnace is opened to introduce the sintering atmosphere at the air inlet speed of 500mL/min, an induced draft fan 1-8 of each sintering furnace is opened, opening the powder adding devices 1-2 of the sintering furnaces to enable the raw material powder in the raw material powder storage tank 1-1 to sequentially enter the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase forming sintering furnace 5 for sintering at the powder adding speed of 30g/min and collect the raw material powder into a finished product powder storage tank 6, closing the powder adding devices 1-2 of the sintering furnaces for 1 hour, and taking down the finished product powder storage tank 6 to obtain Bi-2212 precursor powder; the sintering atmosphere is formed by mixing nitrogen and oxygen with the mass purity of 99.995%, wherein the partial pressure of the oxygen is 20%, and the partial pressure of the impurity atmosphere is lower than 100 ppm.
Comparing the Bi-2212 precursor powder prepared by the implementation with the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art by adopting a scanning electron microscope (multiplied by 100), wherein the result shows that the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the implementation is 1 per sheet, and the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art is 2 per sheet; under the same production period, the Bi-2212 precursor powder is prepared by respectively adopting the process of the embodiment and a coprecipitation method and a spray thermal decomposition method in the prior art, and the preparation efficiency of the embodiment is 1000 kg/month and is far higher than the preparation efficiency of the coprecipitation method in the prior art by 5 kg/month and the preparation efficiency of the spray thermal decomposition method by 20 kg/month through calculation, which shows that the preparation process of the invention reduces the generation of impurity phases and improves the quality of the Bi-2212 precursor powder, and meanwhile, the preparation efficiency of the Bi-2212 precursor powder is greatly improved by adopting a full-automatic inclined continuous rotary sintering method.
Example 3
The embodiment comprises the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3Mixing CuO and Sr according to the atomic ratio of Bi to Sr to Ca to Cu of 2 to 0.95 to 2, preparing a nitrate mixed solution, and preparing oxalate mixed powder by adopting an oxalate coprecipitation method;
step two, filling the oxalate mixed powder obtained in the step one into a raw material powder storage tank 1-1 of a primary sintering furnace 1 in an inclined continuous rotary automatic sintering device as raw material powder, respectively heating the primary sintering furnace 1 to 470 ℃, a low-temperature sintering furnace 2 to 620 ℃, a medium-temperature sintering furnace 3 to 720 ℃, a high-temperature sintering furnace 4 to 810 ℃, and a phase-forming sintering furnace 5 to 840 ℃ and preserving heat for 30min, then sequentially inclining the furnace tubes 1-15 of the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase-forming sintering furnace 5 along the feeding and discharging direction and forming 20-degree included angles with the horizontal ground, rotating the furnace tubes 1-15 of each sintering furnace at the speed of 4 circles/min, opening an air inlet switch of each sintering furnace to introduce sintering atmosphere at the air inlet speed of 300mL/min, opening an induced draft fan 1-8 of each sintering furnace, opening a powder feeder 1-2 of each sintering furnace, feeding the raw material powder in a raw material powder storage tank 1-1 into a primary sintering furnace 1, a low-temperature sintering furnace 2, a medium-temperature sintering furnace 3, a high-temperature sintering furnace 4 and a phase sintering furnace 5 in sequence at a powder feeding rate of 25g/min, sintering and collecting the raw material powder into a finished product powder storage tank 6, closing the powder feeders 1-2 of each sintering furnace for 1 hour, and taking down the finished product powder storage tank 6 to obtain Bi-2212 precursor powder; the sintering atmosphere is formed by mixing nitrogen and oxygen with the mass purity of 99.99%, wherein the partial pressure of the oxygen is 22%, and the partial pressure of the impurity atmosphere is lower than 100 ppm.
Comparing the Bi-2212 precursor powder prepared by the implementation with the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art by adopting a scanning electron microscope (multiplied by 100), wherein the result shows that the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the implementation is 1 per sheet, and the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art is 2 per sheet; under the same production period, the Bi-2212 precursor powder is prepared by adopting the process of the embodiment and a coprecipitation method and a spray thermal decomposition method in the prior art respectively, and the preparation efficiency of the embodiment is 900 kg/month and is far higher than the preparation efficiency of the coprecipitation method in the prior art by 5 kg/month and the preparation efficiency of the spray thermal decomposition method by 20 kg/month through calculation, so that the preparation process reduces the generation of impurity phases, improves the quality of the Bi-2212 precursor powder, and simultaneously adopts a full-automatic inclined continuous rotary sintering method to greatly improve the preparation efficiency of the Bi-2212 precursor powder.
Example 4
The embodiment comprises the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3Mixing CuO and Sr with Ca with Cu in an atomic ratio of 2.1:2.1:0.95:2.1, preparing a nitrate mixed solution, and preparing oxalate mixed powder by adopting an oxalate coprecipitation method;
step two, the oxalate mixed powder obtained in the step one is loaded into a raw material powder storage tank 1-1 of a primary sintering furnace 1 in an inclined continuous rotary automatic sintering device to be used as raw material powder, the primary sintering furnace 1 is heated to 490 ℃, a low-temperature sintering furnace 2 is heated to 640 ℃, a medium-temperature sintering furnace 3 is heated to 740 ℃, a high-temperature sintering furnace 4 is heated to 810 ℃, a phase-forming sintering furnace 5 is heated to 840 ℃ and is subjected to heat preservation for 30min, then the furnace tubes 1-15 of the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase-forming sintering furnace 5 after heat preservation are inclined along the feeding and discharging direction and form an included angle of 30 degrees with the horizontal ground, the furnace tubes 1-15 of each sintering furnace rotate at the speed of 4 circles/min, an air inlet switch of each sintering furnace is opened to introduce the sintering atmosphere at the air inlet speed of 400mL/min, opening an induced draft fan 1-8 of each sintering furnace, opening a powder feeder 1-2 of each sintering furnace, feeding the raw material powder in a raw material powder storage tank 1-1 into a primary sintering furnace 1, a low-temperature sintering furnace 2, a medium-temperature sintering furnace 3, a high-temperature sintering furnace 4 and a phase sintering furnace 5 in sequence at a powder feeding rate of 20g/min, sintering and collecting the raw material powder into a finished product powder storage tank 6, closing the powder feeders 1-2 of each sintering furnace for 1 hour, and taking down the finished product powder storage tank 6 to obtain Bi-2212 precursor powder; the sintering atmosphere is formed by mixing nitrogen and oxygen with the mass purity of 99.99%, wherein the partial pressure of the oxygen is 21%, and the partial pressure of the impurity atmosphere is lower than 100 ppm.
Comparing the Bi-2212 precursor powder prepared by the implementation with the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art by adopting a scanning electron microscope (multiplied by 100), the result shows that the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the implementation is 0.75 per piece, and the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art is 2 per piece; under the same production period, the Bi-2212 precursor powder is prepared by respectively adopting the process of the embodiment and a coprecipitation method and a spray thermal decomposition method in the prior art, and the preparation efficiency of the embodiment is 1000 kg/month and is far higher than the preparation efficiency of the coprecipitation method in the prior art by 5 kg/month and the preparation efficiency of the spray thermal decomposition method by 20 kg/month through calculation, which shows that the preparation process of the invention reduces the generation of impurity phases and improves the quality of the Bi-2212 precursor powder, and meanwhile, the preparation efficiency of the Bi-2212 precursor powder is greatly improved by adopting a full-automatic inclined continuous rotary sintering method.
Example 5
The embodiment comprises the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3Mixing CuO and Sr according to the atomic ratio of Bi to Sr to Ca to Cu of 2 to 0.95 to 2, preparing a nitrate mixed solution, and preparing oxalate mixed powder by adopting an oxalate coprecipitation method;
step two, the oxalate mixed powder obtained in the step one is loaded into a raw material powder storage tank 1-1 of a primary sintering furnace 1 in an inclined continuous rotary automatic sintering device to be used as raw material powder, the primary sintering furnace 1 is heated to 480 ℃, a low-temperature sintering furnace 2 is heated to 630 ℃, a medium-temperature sintering furnace 3 is heated to 730 ℃, a high-temperature sintering furnace 4 is heated to 810 ℃ and a phase-forming sintering furnace 5 is heated to 840 ℃ and is insulated for 40min, then the furnace tubes 1-15 of the primary sintering furnace 1, the low-temperature sintering furnace 2, the medium-temperature sintering furnace 3, the high-temperature sintering furnace 4 and the phase-forming sintering furnace 5 which are insulated are inclined along the feeding and discharging direction and form an included angle of 20 degrees with the horizontal ground, the furnace tubes 1-15 of each sintering furnace are rotated at the speed of 4 circles/min, an air inlet switch of each sintering furnace is opened to introduce the sintering atmosphere at the air inlet speed of 300mL/min, opening an induced draft fan 1-8 of each sintering furnace, opening a powder feeder 1-2 of each sintering furnace, feeding the raw material powder in a raw material powder storage tank 1-1 into a primary sintering furnace 1, a low-temperature sintering furnace 2, a medium-temperature sintering furnace 3, a high-temperature sintering furnace 4 and a phase sintering furnace 5 in sequence at a powder feeding rate of 30g/min, sintering and collecting the raw material powder into a finished product powder storage tank 6, closing the powder feeders 1-2 of each sintering furnace for 1 hour, and taking down the finished product powder storage tank 6 to obtain Bi-2212 precursor powder; the sintering atmosphere is formed by mixing nitrogen and oxygen with the mass purity of 99.99%, wherein the partial pressure of the oxygen is 21%, and the partial pressure of the impurity atmosphere is lower than 100 ppm.
Comparing the Bi-2212 precursor powder prepared by the implementation with the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art by adopting a scanning electron microscope (multiplied by 100), the result shows that the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the implementation is 0.5 per piece, and the probability of one non-Bi-2212 phase particle appearing in the scanning electron microscope (multiplied by 100) picture of the Bi-2212 precursor powder prepared by the coprecipitation method in the prior art is 2 per piece; under the same production period, the Bi-2212 precursor powder is prepared by respectively adopting the process of the embodiment and a coprecipitation method and a spray thermal decomposition method in the prior art, and the preparation efficiency of the embodiment is 700 kg/month by calculation, which is far higher than the preparation efficiency of the coprecipitation method in the prior art by 5 kg/month and the preparation efficiency of the spray thermal decomposition method by 20 kg/month, so that the preparation process reduces the generation of impurity phases, improves the quality of the Bi-2212 precursor powder, and simultaneously adopts a full-automatic inclined continuous rotary sintering method to greatly improve the preparation efficiency of the Bi-2212 precursor powder.
Example 6
The present embodiment is different from embodiment 1 in that: adding Bi2O3、Ca(OH)2、SrCO3And CuO in an atomic ratio of Bi, Sr, Ca, Cu, 2:2:0.95:2.1 to prepare a mixed powder.
Example 7
The present embodiment is different from embodiment 2 in that: adding Bi2O3、Ca(OH)2、SrCO3And CuO are mixed according to the atomic ratio of Bi, Sr, Ca and Cu of 1.95:1.95:0.9:1.95, then nitrate mixed solution is prepared, and oxalate co-precipitation is adopted to prepare oxalate mixed powder.
Example 8
The present embodiment is different from embodiment 2 in that: adding Bi2O3、Ca(OH)2、SrCO3And CuO are mixed according to the atomic ratio of Bi, Sr, Ca and Cu being 2.2:2.2:1:2.2, then nitrate mixed solution is prepared, and oxalate coprecipitation method is adopted to prepare oxalate mixed powder.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (8)
1. A method for preparing Bi-2212 precursor powder by an inclined rotary sintering method is characterized by comprising the following steps:
step one, adding Bi2O3、Ca(OH)2、SrCO3And CuO, wherein the CuO is prepared into mixed powder according to the atomic ratio of Bi, Sr, Ca, Cu, (1.95-2.2), (0.9-1) and (1.95-2.2);
or Bi2O3、Ca(OH)2、SrCO3And CuO are mixed according to the atomic ratio of Bi, Sr, Ca, Cu, (1.95-2.2), (0.9-1) and (1.95-2.2), then a nitrate mixed solution is prepared, and an oxalate coprecipitation method is adopted to prepare oxalate mixed powder;
step two, the mixed powder or oxalate mixed powder obtained in the step one is filled into a raw material powder storage tank (1-1) of a primary sintering furnace (1) in an inclined continuous rotating automatic sintering device to be used as raw material powder, the primary sintering furnace (1), a low-temperature sintering furnace (2), a medium-temperature sintering furnace (3), a high-temperature sintering furnace (4) and a phase forming sintering furnace (5) are heated and insulated for more than 30min, then the furnace tubes (1-15) of the primary sintering furnace (1), the low-temperature sintering furnace (2), the medium-temperature sintering furnace (3), the high-temperature sintering furnace (4) and the phase forming sintering furnace (5) after heat insulation are inclined along the feeding and discharging direction in sequence, furnace tubes (1-15) of each sintering furnace are rotated, an air inlet switch of each sintering furnace is opened to introduce sintering atmosphere, an induced draft fan (1-8) of each sintering furnace is opened, a powder adding device (1-2) of each sintering furnace is opened, raw material powder in a raw material powder storage tank (1-1) sequentially enters a primary sintering furnace (1), a low-temperature sintering furnace (2), a medium-temperature sintering furnace (3), a high-temperature sintering furnace (4) and a phase forming sintering furnace (5) for sintering and is collected into a finished product powder storage tank (6), so that Bi-2212 precursor powder is obtained.
2. The method for preparing Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein in the second step, the primary sintering furnace (1) is heated to 450-500 ℃, the low-temperature sintering furnace (2) is heated to 600-650 ℃, the medium-temperature sintering furnace (3) is heated to 700-750 ℃, the high-temperature sintering furnace (4) is heated to 800-820 ℃, and the phase-forming sintering furnace (5) is heated to 830-850 ℃.
3. The method for preparing Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein in the step two, furnace tubes (1-15) of the primary sintering furnace (1), the low-temperature sintering furnace (2), the medium-temperature sintering furnace (3), the high-temperature sintering furnace (4) and the phase-forming sintering furnace (5) are inclined along the feeding and discharging direction and form an included angle of 10-30 degrees with the horizontal ground.
4. The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein the rotation rate of the furnace tube (1-15) of each sintering furnace in the second step is 3-5 circles/min.
5. The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method as claimed in claim 1, wherein the introduction rate of the sintering atmosphere in the second step is 200mL/min to 500 mL/min.
6. The method for preparing the Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein the powder adding speed of the powder adding device (1-2) in the second step is 10g/min to 30 g/min.
7. The method for preparing Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein the sintering atmosphere in the second step is formed by mixing high-purity nitrogen and oxygen, wherein the mass purity of the nitrogen is not less than 99.99%, the partial pressure of the oxygen is 20-22%, and the partial pressure of the impurity atmosphere is less than 100 ppm.
8. The method for preparing Bi-2212 precursor powder by the inclined rotary sintering method according to claim 1, wherein the furnace tubes (1-15) of the primary sintering furnace (1), the low-temperature sintering furnace (2), the medium-temperature sintering furnace (3), the high-temperature sintering furnace (4) and the phase-forming sintering furnace (5) in the inclined continuous rotary automatic sintering equipment in the step two are made of high-temperature alloy, wherein the inner surface of the high-temperature alloy furnace tube is covered with a silica coating prepared by a thermal spraying method, and the surface of the silica coating is covered with a pure silver inner lining layer prepared by an explosive cladding method.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445072A (en) * | 2010-10-05 | 2012-05-09 | 喻睿 | Continuous dynamic sintering kiln |
| CN203639169U (en) * | 2013-12-27 | 2014-06-11 | 萍乡宝海饲料添加剂有限公司 | Roasting furnace |
| CN104347280A (en) * | 2013-08-06 | 2015-02-11 | 三星电机株式会社 | Continuous heat treating device and method for heat treatment of chips by means of continuous heat treating device |
| CN104760994A (en) * | 2015-03-27 | 2015-07-08 | 成都德联微纳科技有限公司 | Dynamic continuous preparation method of Ti5O9 powder and dynamic continuous sintering device |
| CN104944955A (en) * | 2015-06-09 | 2015-09-30 | 四川大学 | M<y>(C<X>N<1-X>) powder rotary type dynamic continuous preparation method and sintering device |
-
2019
- 2019-12-07 CN CN201911245651.6A patent/CN110937629B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445072A (en) * | 2010-10-05 | 2012-05-09 | 喻睿 | Continuous dynamic sintering kiln |
| CN104347280A (en) * | 2013-08-06 | 2015-02-11 | 三星电机株式会社 | Continuous heat treating device and method for heat treatment of chips by means of continuous heat treating device |
| CN203639169U (en) * | 2013-12-27 | 2014-06-11 | 萍乡宝海饲料添加剂有限公司 | Roasting furnace |
| CN104760994A (en) * | 2015-03-27 | 2015-07-08 | 成都德联微纳科技有限公司 | Dynamic continuous preparation method of Ti5O9 powder and dynamic continuous sintering device |
| CN104944955A (en) * | 2015-06-09 | 2015-09-30 | 四川大学 | M<y>(C<X>N<1-X>) powder rotary type dynamic continuous preparation method and sintering device |
Non-Patent Citations (2)
| Title |
|---|
| 郝清滨 等: "Ag芯增强Bi-2212多芯线材的制备", 《稀有金属》 * |
| 郝清滨等: "共沉淀Bi-2212粉末与商用粉末的性能对比研究", 《低温物理学报》 * |
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