CN113697852B - Preparation method of coralline semiconductive strontium titanate powder - Google Patents
Preparation method of coralline semiconductive strontium titanate powder Download PDFInfo
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Abstract
The invention discloses a preparation method of coralline semiconducting strontium titanate powder, which comprises the following steps: preparing dry gel by adopting a strontium source, a titanium source and glucose; placing the xerogel in a crucible to perform self-propagating reaction to obtain black powder; mixing the black powder with starch and polyvinyl alcohol (PVA), ball-milling, and performing heat treatment and cooling to obtain black powder; washing and filtering the black powder to obtain the semi-conductive nano SrTiO 3 And (3) powder. The invention can obtain SrTiO with coral-shaped appearance characteristics and the resistivity of 50-250 omega cm 3 And (3) powder.
Description
Technical Field
The invention belongs to the technical field of electronic information semiconductor material preparation, and particularly relates to a preparation method of coralline semiconducting strontium titanate powder.
Background
Materials having perovskite structure, e.g. SrTiO such as strontium titanate 3 Barium titanate BaTiO 3 Because of its various excellent electrical, optical and magnetic properties, it is widely used in various electronic functional materials and devices.
SrTiO 3 Is prepared from SrO and TiO 2 Intercrossed, and the crystal structure of the crystal is formed by strontium Sr in divalent oxidation state 2+ Titanium Ti in tetravalent oxidation state 4+ And oxygen O in a divalent reduced state 2- Composition of Ti 4+ At the body center position of the cubic unit cell, O 2- In the face center of the unit cell, sr 2+ At the apex position of the cell; ti (titanium) 4+ And O 2- Constituting TiO 6 Octahedron, sr 2+ Is coated with 4 TiO 6 And (4) octahedron surrounding. Ti 4+ And 6O 2- Coordination of Sr 2+ And 12O 2- Coordinated to TiO 6 The octahedral Ti-3d orbital and O-2p orbital hybridize to form a covalent bond, O 2- And Sr 2+ Form an ionic bond, and thus, srTiO 3 The material has the properties of covalent bonds and ionic bonds, the indirect forbidden band width is 3.25eV, and the direct forbidden band width is 3.75eV. Lattice-completed SrTiO 3 Is a good insulator and has poor conductivity, but in the application of electronic functional materials, it is generally necessary to make it semiconductive in order to improve its conductivity.
Preparation of SrTiO in general 3 The powder method mainly comprises a sol-gel method, a hydrothermal method, a high-temperature solid phase method and the like. Semiconducting SrTiO 3 The method mainly comprises two methods, one is that the impurity defect ionization is formed by doping the heterovalent metal ions, and the carrier concentration is increased; the other is by vacuum or reducing atmosphere (such as CO and H) 2 Etc.), however, these methods have problems of long flow path, high temperature, complicated equipment, and the like.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a method for preparing a coral-like semiconducting strontium titanate powder.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the embodiment of the invention provides a preparation method of coralline semiconducting strontium titanate powder, which comprises the following steps:
preparing dry gel from a strontium source, a titanium source and glucose;
placing the xerogel in a crucible to perform self-propagating reaction to obtain black powder;
mixing the black powder with starch and polyvinyl alcohol (PVA), ball-milling, and performing heat treatment and cooling to obtain black powder;
washing and filtering the black powder to obtain the semi-conductive nano SrTiO 3 And (3) powder.
In the above scheme, the xerogel prepared from a strontium source, a titanium source and glucose specifically comprises: dissolving a strontium source, a titanium source and glucose in a mixed solution of ethanol and water, and strongly stirring to form a transparent solution; glucose was added to the clear solution and a viscous gel was formed under water bath conditions, which dried to obtain a xerogel.
In the above scheme, the xerogel prepared by adopting the strontium source, the titanium source and the glucose is specifically realized by the following steps:
step (ii) of1.1 strontium Source adopts Sr (NO) 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 1.2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.95-1:1;
step 1.3, preparing a mixed solution of ethanol and water according to a volume ratio of 1.5-4.5;
step 1.4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into the mixed solution of 250-750 ml, stirring for 30-60 min at room temperature until the Ti is completely dissolved to obtain a transparent solution;
step 1.5, adding glucose into the transparent solution, and magnetically stirring for 1-2 hours at the speed of 600-700 r/min to form viscous gel;
and step 1.6, drying the viscous gel at the temperature of between 70 and 90 ℃ for 12 to 16 hours to obtain dry gel.
In the scheme, the xerogel is placed in a crucible to carry out self-propagating reaction to obtain black powder, and the method is realized by the following steps:
2.1, putting the xerogel into an alumina crucible with a cover, and compacting;
step 2.2, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 2.3, putting the crucible into a muffle furnace, rapidly heating to 400-800 ℃ at a heating rate of 20-25 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1-2 h, and cooling to obtain black powder.
In the scheme, the black powder is mixed with starch and polyvinyl alcohol (PVA) for ball milling, and after heat treatment and cooling, the black powder is obtained, and the method is specifically realized through the following steps:
step 3.1, mixing the black powder with starch and PVA, and ball-milling;
and 3.2, adding 150-200 wt% of starch and 2-5 wt% of PVA.
Step 3.3, the ball milling rotating speed is 200-300 r/min, and the time is 2-4 h;
and 3.4, placing the mixture obtained in the step 3.1 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 500-800 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 1-3 h, cooling to room temperature, and grinding to obtain black powder.
In the scheme, the semi-conductive nano SrTiO is obtained after the black powder is washed and filtered 3 The powder is specifically as follows: washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
Compared with the prior art, the method can obtain SrTiO with coral-shaped appearance characteristics and resistivity of 50-250 omega cm 3 And (3) powder.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a schematic diagram of coral-shaped semiconducting strontium titanate powder prepared by a method for preparing coral-shaped semiconducting strontium titanate powder according to embodiment 1 of the present invention;
FIG. 2 is a morphology diagram of coral-shaped semiconducting strontium titanate powder prepared by the method for preparing coral-shaped semiconducting strontium titanate powder provided in embodiment 2 of the present invention;
FIG. 3 is a morphology chart of coral-shaped semiconducting strontium titanate powder prepared by the method for preparing coral-shaped semiconducting strontium titanate powder according to embodiment 3 of the present invention;
fig. 4 is a morphology diagram of coral-shaped semiconducting strontium titanate powder prepared by the method for preparing coral-shaped semiconducting strontium titanate powder provided in embodiment 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, article, or apparatus that comprises the element.
The embodiment of the invention provides a preparation method of coralline semiconducting strontium titanate powder, which is realized by the following steps:
step 1, preparing xerogel by adopting a strontium source, a titanium source and glucose;
specifically, a strontium source, a titanium source and glucose are dissolved in a mixed solution of ethanol and water, and a transparent solution is formed by strong stirring; glucose was added to the clear solution and a viscous gel was formed under water bath conditions, which dried to obtain a xerogel.
Further, the xerogel prepared by adopting the strontium source, the titanium source and the glucose is specifically realized by the following steps:
step 1.1, sr (NO) is adopted as strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 1.2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.95-1:1;
step 1.3, preparing a mixed solution of ethanol and water according to a volume ratio of 1.5-4.5;
step 1.4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into the mixed solution of 250-750 ml, stirring for 30-60 min at room temperature until the Ti is completely dissolved to obtain a transparent solution;
step 1.5, adding glucose into the transparent solution, and magnetically stirring for 1-2 hours at the speed of 600-700 r/min to form viscous gel;
and step 1.6, drying the viscous gel at 70-90 ℃ for 12-16 h to obtain dry gel.
Step 2, placing the xerogel in a crucible to perform self-propagating reaction to obtain black powder;
the method is realized by the following steps:
2.1, putting the xerogel into an alumina crucible with a cover, and compacting;
step 2.2, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 2.3, putting the crucible into a muffle furnace, rapidly heating to 400-800 ℃ at a heating rate of 20-25 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1-2 h, and cooling to obtain black powder.
Step 3, mixing and ball-milling the black powder with starch and polyvinyl alcohol (PVA), and performing heat treatment and cooling to obtain black powder;
the method is realized by the following steps:
step 3.1, mixing the black powder with starch and PVA, and ball-milling;
and 3.2, adding 150-200 wt% of starch and 2-5 wt% of PVA.
Step 3.3, the ball milling rotating speed is 200-300 r/min, and the time is 2-4 h;
and 3.4, placing the mixture obtained in the step 3.1 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 500-800 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 2 hours, cooling to room temperature, and grinding to obtain black powder.
Step 4, washing and filtering the black powder to obtain the semi-conductive nano SrTiO 3 And (3) powder.
Specifically, the black powder is washed and dried in deionized water, and is sieved by a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
In the preparation method, glucose is used as a dispersing agent and a combustion improver, and a simple and easily-realized self-propagating reaction is adopted to synthesize SrTiO 3 Further, by burying and burning in starch, oxygen escape is realized, oxygen vacancy is formed, and semiconducting SrT is obtainediO 3 And (3) powder.
SrTiO prepared by the preparation method of the invention 3 Has a nano-grade coral-shaped structure, thus not only maintaining SrTiO 3 The nano-scale of the powder has good fluidity and activity, and well ensures SrTiO 3 The particles are well electrically connected, the conductivity of the particles can be effectively enhanced, and the SrTiO is obviously improved 3 Electrical conductivity of, srTiO prepared 3 The resistivity is 50-250 omega cm, and the material is a raw material for preparing electronic functional materials with excellent performance.
Example 1
Embodiment 1 of the present invention provides a method for preparing coral-shaped semiconducting strontium titanate powder, which is implemented by the following steps:
step 1, sr (NO) is adopted as a strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.95;
step 3, preparing a mixed solution of ethanol and water according to the volume ratio of 1.5;
step 4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into 250ml of mixed solution, and stirring for 30min at room temperature until the Ti is completely dissolved to obtain transparent solution;
step 5, adding glucose into the transparent solution, and magnetically stirring for 1h at the speed of 600r/min to form viscous gel;
step 6, drying the viscous gel at 70 ℃ for 12h to obtain a xerogel.
Step 7, putting the xerogel into an alumina crucible with a cover, and compacting;
step 8, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 9, putting the crucible into a muffle furnace, rapidly heating to 600 ℃ at a heating rate of 20 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1h, and cooling to obtain black powder.
Step 10, mixing the black powder with starch and PVA, and ball-milling;
step 11, the amount of starch added was 150wt%, and the amount of PVA added was 2 wt%.
Step 12, ball milling at the rotating speed of 200r/min for 2h;
and step 13, placing the mixture obtained in the step 10 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 500 ℃ at the speed of 3 ℃/min, preserving the heat for 1h, cooling to room temperature, and grinding to obtain black powder.
Step 14, washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
As shown in FIG. 1, it can be seen that the nano SrTiO semiconductor prepared by the embodiment of the invention 3 The powder has coral-shaped appearance characteristics.
Example 2
Embodiment 2 of the present invention provides a method for preparing coralline semiconducting strontium titanate powder, which is implemented by the following steps:
step 1, sr (NO) is adopted as a strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 1:1;
step 3, preparing a mixed solution of ethanol and water according to a volume ratio of 4.5;
step 4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into the mixed solution of 250-750 ml, stirring for 60min at room temperature until the Ti is completely dissolved to obtain a transparent solution;
step 5, adding glucose into the transparent solution, and magnetically stirring for 2 hours at the speed of 700r/min to form viscous gel;
step 6, drying the viscous gel at 90 ℃ for 16h to obtain dry gel.
Step 7, putting the xerogel into an alumina crucible with a cover, and compacting;
step 8, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 9, putting the crucible into a muffle furnace, rapidly heating to 800 ℃ at a heating rate of 25 ℃/min, carrying out self-propagating reaction, keeping the temperature for 2h, and cooling to obtain black powder.
Step 10, mixing the black powder with starch and PVA, and ball-milling;
and 11, adding 200wt% of starch and 5wt% of PVA.
Step 12, ball milling rotation speed is 300r/min, and time is 4h;
and step 13, placing the mixture obtained in the step 10 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 800 ℃ at the speed of 5 ℃/min, preserving the temperature for 3h, cooling to room temperature, and grinding to obtain black powder.
Step 14, washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
As shown in FIG. 2, it can be seen that the nano SrTiO semiconductor prepared by the embodiment of the invention 3 The powder has coral-shaped appearance characteristics.
Example 3
Embodiment 3 of the present invention provides a method for preparing coralline semiconducting strontium titanate powder, which is implemented by the following steps:
step 1, sr (NO) is adopted as a strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, the purity requirement is analytically pure AR;
step 2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.96;
step 3, preparing a mixed solution of ethanol and water according to a volume ratio of 3:1;
step 4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into the mixed solution of 250-750 ml, stirring for 30-60 min at room temperature until the Ti is completely dissolved to obtain a transparent solution;
step 5, adding glucose into the transparent solution, and magnetically stirring at the speed of 500r/min for 1.5 hours to form viscous gel;
step 6, drying the viscous gel at 80 ℃ for 14h to obtain a dry gel.
Step 7, putting the xerogel into an alumina crucible with a cover, and compacting;
step 8, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 9, putting the crucible into a muffle furnace, rapidly heating to 600 ℃ at a heating rate of 23 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1.5h, and cooling to obtain black powder.
Step 10, mixing the black powder with starch and PVA, and ball-milling;
and 11, adding 180wt% of starch and 3wt% of PVA.
Step 12, ball milling rotation speed is 250r/min, and time is 3h;
and step 13, placing the mixture obtained in the step 10 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 600 ℃ at the speed of 4 ℃/min, preserving the temperature for 2h, cooling to room temperature, and grinding to obtain black powder.
Step 14, washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
As shown in FIG. 3, it can be seen that the nano SrTiO semiconductor prepared by the embodiment of the invention 3 The powder has coral-shaped appearance characteristics.
Example 4
Embodiment 4 of the present invention provides a method for preparing coralline semiconducting strontium titanate powder, which is implemented by the following steps:
step 1, sr (NO) is adopted as a strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.97;
step 3, preparing a mixed solution of ethanol and water according to a volume ratio of 4.2;
step 4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into 650ml of mixed solution, and stirring for 50min at room temperature until the Ti is completely dissolved to obtain transparent solution;
step 5, adding glucose into the transparent solution, and magnetically stirring for 2 hours at the speed of 500r/min to form viscous gel;
step 6, drying the viscous gel at 80 ℃ for 13h to obtain a xerogel.
Step 7, putting the xerogel into an alumina crucible with a cover, and compacting;
step 8, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 9, putting the crucible into a muffle furnace, rapidly heating to 600 ℃ at a heating rate of 24 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1.8h, and cooling to obtain black powder.
Step 10, mixing the black powder with starch and PVA, and ball-milling;
and 11, adding 190wt% of starch and 3.3wt% of PVA.
Step 12, ball milling rotation speed is 280r/min, and time is 3.5h;
and step 13, placing the mixture obtained in the step 10 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 650 ℃ at the speed of 4 ℃/min, preserving the temperature for 2.5 hours, cooling to room temperature, and grinding to obtain black powder.
Step 14, washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
As shown in FIG. 4, it can be seen that the semiconducting nano SrTiO prepared by the embodiment of the invention 3 The powder has coral-shaped appearance characteristics.
Semiconducting nanosSrTiO from examples 1-4, respectively 3 The powder was subjected to resistivity test, and the specific resistivity is shown in table 1:
it can be seen that the semiconducting nano SrTiO prepared by the method of the invention 3 The powder has a nano-grade coralline structure, the resistivity of the powder is 50-250 omega cm, and the SrTiO is obviously improved 3 The conductivity of (2) is a raw material for preparing electronic functional materials with excellent performance.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (5)
1. A preparation method of coral-shaped semiconducting strontium titanate powder is characterized by comprising the following steps:
preparing dry gel by adopting a strontium source, a titanium source and glucose;
the method specifically comprises the following steps: dissolving a strontium source, a titanium source and glucose in a mixed solution of ethanol and water, and strongly stirring to form a transparent solution; adding glucose into the transparent solution, forming viscous gel under the condition of water bath, and drying to obtain xerogel;
placing the xerogel in a crucible, heating to 400-800 ℃ to perform self-propagating reaction, and keeping the temperature for 1-2 hours to obtain black powder;
mixing and ball-milling the black powder with starch and polyvinyl alcohol, and performing heat treatment and cooling to obtain black powder;
wherein the heat treatment comprises the following steps: heating to 500-800 deg.c and maintaining for 1-3 hr;
washing and filtering the black powder to obtain the semi-conductive nano SrTiO 3 And (3) powder.
2. The method for preparing coral-shaped semiconducting strontium titanate powder according to claim 1, wherein the xerogel is prepared by adopting a strontium source, a titanium source and glucose, and the method comprises the following steps:
step 1.1, sr (NO) is adopted as a strontium source 3 ) 2 The titanium source adopts C 16 H 36 O 4 Ti, purity requirement is analytically pure AR;
step 1.2, sr (NO) 3 ) 2 And C 16 H 36 O 4 The molar ratio of Ti is 0.95-1:1;
step 1.3, preparing a mixed solution of ethanol and water according to a volume ratio of 1.5-4.5;
step 1.4, sr (NO) 3 ) 2 And C 16 H 36 O 4 Adding Ti into the mixed solution of 250-750 ml, stirring for 30-60 min at room temperature until the Ti is completely dissolved to obtain a transparent solution;
step 1.5, adding glucose into the transparent solution, and magnetically stirring at the speed of 600-700 r/min for 1-2 h to form viscous gel;
and step 1.6, drying the viscous gel at the temperature of between 70 and 90 ℃ for 12 to 16 hours to obtain dry gel.
3. The method for preparing coral-shaped semiconducting strontium titanate powder according to any one of claims 1 to 2, wherein the xerogel is placed in a crucible to undergo a self-propagating reaction to obtain black powder, and the method is specifically realized by the following steps:
2.1, putting the xerogel into an alumina crucible with a cover, and compacting;
step 2.2, the amount of the xerogel is less than 1/3 of the crucible capacity;
and 2.3, putting the crucible into a muffle furnace, rapidly heating to 400-800 ℃ at a heating rate of 20-25 ℃/min, carrying out self-propagating reaction, keeping the temperature for 1-2 h, and cooling to obtain black powder.
4. The method for preparing coral-shaped semiconducting strontium titanate powder according to claim 3, wherein the black powder is mixed with starch and polyvinyl alcohol, ball-milled, heat-treated and cooled to obtain black powder, and the method is specifically realized by the following steps:
step 3.1, mixing and ball-milling the black powder, starch and polyvinyl alcohol;
step 3.2, adding 150-200 wt% of starch and 2-5 wt% of polyvinyl alcohol;
step 3.3, the ball milling rotating speed is 200-300 r/min, and the time is 2-4 h;
and 3.4, placing the ball-milled mixture obtained in the step 3.1 into a crucible and placing the crucible into a muffle furnace, heating the muffle furnace to 500-800 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 1-3 h, cooling to room temperature, and grinding to obtain black powder.
5. The method of claim 4, wherein the black powder is washed and filtered to obtain semiconducting nano-SrTiO powder 3 The powder is specifically as follows: washing and drying the black powder in deionized water, and sieving with a 300-mesh sieve to obtain the semi-conductive nano SrTiO 3 And (3) powder.
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