CN114604889A - Copper-based oxide La2CuO4Method for preparing powder material - Google Patents
Copper-based oxide La2CuO4Method for preparing powder material Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 67
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 27
- 239000010949 copper Substances 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 53
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011858 nanopowder Substances 0.000 claims abstract description 30
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 24
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 238000009837 dry grinding Methods 0.000 claims abstract description 21
- 238000001238 wet grinding Methods 0.000 claims abstract description 21
- 229910002282 La2CuO4 Inorganic materials 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 239000005751 Copper oxide Substances 0.000 claims abstract description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 3
- 238000002347 injection Methods 0.000 claims abstract description 3
- 239000007924 injection Substances 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000003746 solid phase reaction Methods 0.000 description 6
- 238000010671 solid-state reaction Methods 0.000 description 6
- 238000005429 filling process Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002260 LaCuO3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a copper-based oxide La2CuO4The preparation method of the powder material comprises adopting lanthanum oxide La2O3Mixing with copper oxide CuO and then putting into a ball milling tank; carrying out vacuum treatment on the ball milling tank to ensure that the vacuum degree is less than 6Pa, then filling argon into the ball milling tank, repeating the steps for at least three times, and carrying out dry milling; after the dry grinding is finished, simultaneously injecting argon and absolute ethyl alcohol into the air inlet and the air outlet of the ball milling tank respectively, and closing the air outlet and the air inlet in sequence after the injection is finished to carry out wet grinding; drying the wet-milled mixture to obtain nano powder, placing the nano powder in a die, pressing the nano powder into a flaky sample by using an electric powder tablet press, and placing the flaky sample in a crucible; putting the crucible into a resistance furnace for heating and heat preservation, and then cooling the crucible to room temperature along with the resistance furnace; taking out the flaky sample in the crucible, grinding and sieving to obtain the nano-powder of the copper-based oxide2CuO4Simple preparation of powder, low cost, short time, controllable particle sizeLarge-scale industrial production is carried out.
Description
Technical Field
The invention relates to the technical field of copper-based oxides, in particular to a copper-based oxide La2CuO4A method for preparing powder material.
Background
Copper-based oxide La2CuO4Is made of perovskite layer (LaCuO)3) And a salt formation (LaO) in a c-axis direction at a ratio of 1: 1 in a ratio of 1 to overlap each other to form a layered perovskite-like (La)2CuO4) A composite oxide. In this layered structure, the LaO layer is in contact with LaCuO3The layer interface has strong scattering effect on phonons, so La2CuO4The composite oxide with the structure has lower thermal conductivity, is easy to form an oxygen-deficient non-stoichiometric compound, and has better oxygen exchange and diffusion capacity, so that the composite oxide can be used as a novel oxygen-sensitive material with development prospect. In recent years, La has been found2CuO4The thermoelectric material has a large Seebeck coefficient, and the Seebeck coefficient at room temperature can reach 340uV/K according to literature records, and a good ZT value can be obtained in a strongly related electronic system by optimizing the electrical property and reducing the thermal conductivity, so that the thermoelectric material becomes a potential thermoelectric material. Further, La2CuO4The catalyst has good application potential in the aspects of catalytic oxidation of organic matters, catalytic purification of automobile exhaust, catalytic elimination of nitrogen oxides and the like.
In the preparation process of the perovskite type composite oxide, different preparation methods have great influence on physical and chemical properties of a sample, such as structure, shape, particle size, specific surface and even catalytic activity on reaction, such as a solid-state reaction method, a self-propagating combustion method, a sol-gel method and the like, most of the chemical methods for synthesizing nano materials adopt a sol-gel method, the yield is low, the polymerization reaction can not be carried out for a long time, and when metal ions can not be completely complexed, the process is limited in practical application.
Disclosure of Invention
The invention aims to provide a copper-based oxide La2CuO4A preparation method of powder material.
The technical solution for realizing the purpose of the invention is as follows: copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
1) adopting lanthanum oxide La2O3Mixing with copper oxide CuO, and ball millingIn a tank;
2) carrying out vacuum treatment on the ball milling tank to ensure that the vacuum degree is less than 6Pa, then filling argon into the ball milling tank, repeating the steps for at least three times, and carrying out dry milling;
3) after the dry milling is finished, simultaneously injecting argon and absolute ethyl alcohol into the air inlet and the air outlet of the ball milling tank respectively, and closing the air outlet and the air inlet in sequence after the injection is finished to carry out wet milling;
4) placing the nano powder obtained by drying the mixture after wet grinding in a mould, pressing the nano powder into a flaky sample by an electric powder tablet press, and placing the flaky sample in a crucible with 99% of alumina;
5) putting the crucible into a resistance furnace for heating and heat preservation, and then cooling the crucible to room temperature along with the resistance furnace;
6) and taking out the flaky sample in the crucible, grinding and sieving to obtain the copper-based oxide nano powder.
Further, the rotation speed of the dry grinding is 100-500 rpm, and the time is 15 min-96 h.
Furthermore, the rotation speed of the wet grinding is 50-300 rpm, and the time is 15 min-12 h.
Further, the drying temperature is 20-200 ℃, and the time is 4-20 h.
Further, the pressure of the electric powder tablet press is 10-50 MPa;
further, the sheet sample is a cylindrical sheet body with the diameter of 12.5mm and the height of 3-15 mm.
Further, the heating and heat preservation in the resistance furnace are carried out by firstly heating to 750-900 ℃ at a speed of 50-150 ℃/h, then heating to 800-950 ℃ at a speed of 20-50 ℃/h, and carrying out heat preservation for 5-24 h.
Compared with the prior art, the invention has the beneficial effects that:
the invention realizes that2CuO4The powder is simple to prepare, low in cost, short in time, controllable in particle size (the ball milling speed, the ball milling time and the sieve aperture are adjusted), and capable of being used for large-scale industrial production.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the copper-based oxide powders prepared in examples 3, 4 and 5 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) image of the copper-based oxide powder material of the present invention;
FIG. 3 is an enlarged view of a Transmission Electron Microscope (TEM) of the copper-based oxide powder material of the present invention.
Detailed Description
A preferred embodiment of the present invention will be described in detail below with reference to the accompanying drawings.
La used in the following examples2O3: 1, CuO: 1 is the conventional stoichiometric proportion, and single La can be synthesized according to the proportion2CuO4A phase.
Example 1
Copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
step one, adopting high-purity La2O3And CuO oxide as a starting material, as La2O3: 1, CuO: 1, proportioning and mixing into powder;
step two, putting the mixed powder into a ball milling tank, performing vacuum treatment on the ball milling tank filled with the powder to ensure that the vacuum degree is less than 6Pa in order to prevent the powder from deteriorating in air, filling argon into the ball milling tank after vacuumizing is finished, performing the vacuum treatment and argon filling process for more than three times in order to remove the air in the tank body, controlling the rotating speed of the ball milling tank to be 100rpm, and performing dry milling for 15 min;
during dry grinding operation, the mutual grinding and rubbing action among the powder particles is larger, the rounding of the particle shape is facilitated, and the compaction density is higher;
step three, in order to prevent the powder from caking and enable the ball milling to be more uniform, after the dry milling is finished, injecting argon gas into an air inlet of a ball milling tank, simultaneously injecting absolute ethyl alcohol into an air outlet of the ball milling tank through a needle tube, and after the absolute ethyl alcohol is injected, firstly closing the air outlet and then closing the air inlet; controlling the rotation speed of the ball milling tank to be 50rpm for 15min, and carrying out wet milling;
in the wet grinding process, the absolute ethyl alcohol is added, the agglomeration of powder is limited, and the particle refinement is promoted, so that the refinement efficiency of the wet grinding is higher, the dry grinding and the wet grinding are combined, and the required particle size can be obtained by adjusting the time and the rotating speed of the dry grinding and the wet grinding;
step four, drying the mixture after wet grinding at the drying temperature of 20 ℃ for 4 hours to finally obtain the La2O3Nano powder fully and uniformly mixed with CuO;
putting the nano powder into a die with the diameter of 12.5mm, pressing the nano powder into a cylindrical sheet with the diameter of 12.5mm and the height of 15mm under the pressure of 10MPa of an electric powder tablet press, uniformly putting the cylindrical sheet into a crucible of 99% alumina, and covering the crucible cover;
step six, uniformly placing the crucible filled with the sheet sample into a box-type resistance furnace, wherein the temperature control program of the box-type resistance furnace is as follows: heating to 750 ℃ at the speed of 50 ℃/h, heating to 800 ℃ at the speed of 20 ℃/h, preserving heat for 5h, and then cooling to room temperature along with the furnace;
step six, taking the flaky sample obtained after the solid-state reaction in the step five out of the crucible, grinding the flaky sample into powder by using a mortar, and sieving the powder by using a 200-mesh sieve to finally obtain the La2CuO4And (3) nano powder.
Example 2
Copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
step one, adopting high-purity La2O3And CuO oxide as a starting material, as La2O3: 1, CuO: 1, proportioning and mixing into powder;
step two, putting the mixed powder into a ball milling tank, performing vacuum treatment on the ball milling tank filled with the powder to ensure that the vacuum degree is less than 6Pa in order to prevent the powder from being oxidized and changing valence, filling argon into the ball milling tank after vacuumizing is finished, circularly performing the vacuum treatment and argon filling processes for more than three times in order to remove air in the tank body, controlling the rotating speed of the ball milling tank to be 500rpm, and performing dry milling for 96 hours;
step three, in order to prevent the powder from caking and enable the ball milling to be more uniform, after the dry milling is finished, injecting argon gas into an air inlet of a ball milling tank, simultaneously injecting absolute ethyl alcohol into an air outlet of the ball milling tank through a needle tube, and after the absolute ethyl alcohol is injected, firstly closing the air outlet and then closing the air inlet; controlling the rotation speed of the ball milling tank to be 300rpm for 12 hours, and carrying out wet milling;
step four, drying the mixture after wet grinding at the drying temperature of 200 ℃ for 20 hours to finally obtain the La2O3Nano powder fully and uniformly mixed with CuO;
putting the nano powder into a die with the diameter of 12.5mm, pressing the nano powder into cylindrical sheets with the diameter of 12.5mm and the height of 3mm under the pressure of 50MPa of an electric powder tablet press, uniformly putting the cylindrical sheets into a crucible of 99% alumina, and covering the crucible cover;
step six, uniformly placing the crucible filled with the sheet sample into a box-type resistance furnace, wherein the temperature control program of the box-type resistance furnace is as follows: heating to 900 ℃ at the speed of 150 ℃/h, heating to 950 ℃ at the speed of 50 ℃/h, preserving heat for 24h, and then cooling to room temperature along with the furnace;
step six, taking the flaky sample obtained after the solid-state reaction in the step five out of the crucible, grinding the flaky sample into powder by using a mortar, and sieving the powder by using a 500-mesh sieve to finally obtain the La2CuO4And (3) nano powder.
Example 3
Copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
step one, adopting high-purity La2O3And CuO oxide as a starting material, as La2O3: 1, CuO: 1, proportioning and mixing into powder;
step two, putting the mixed powder into a ball milling tank, performing vacuum treatment on the ball milling tank filled with the powder to ensure that the vacuum degree is less than 6Pa in order to prevent the powder from being oxidized and changing valence, filling argon into the ball milling tank after vacuumizing is finished, circularly performing the vacuum treatment and argon filling processes for more than three times in order to remove air in the tank body, controlling the rotating speed of the ball milling tank to be 300rpm and the time to be 300min, and performing dry milling;
step three, in order to prevent powder from caking and enable the ball milling to be more uniform, after the dry milling is finished, argon is injected into an air inlet of a ball milling tank, absolute ethyl alcohol is injected into an air outlet of the ball milling tank through a needle tube, and after the absolute ethyl alcohol is injected, the air outlet is closed firstly and then the air inlet is closed; controlling the rotation speed of the ball milling tank to be 300rpm and the time to be 300min, and carrying out wet milling;
step four, drying the mixture after wet grinding at 50 ℃ for 10 hours to finally obtain the La2O3Nano powder fully and uniformly mixed with CuO;
putting the nano powder into a die with the diameter of 12.5mm, pressing the nano powder into cylindrical sheets with the diameter of 12.5mm and the height of 3mm under the pressure of 50MPa of an electric powder tablet press, uniformly putting the cylindrical sheets into a crucible of 99% alumina, and covering the crucible cover;
step six, uniformly placing the crucible filled with the sheet sample into a box-type resistance furnace, wherein the temperature control program of the box-type resistance furnace is as follows: heating to 800 ℃ at the speed of 100 ℃/h, heating to 850 ℃ at the speed of 20 ℃/h, preserving heat for 12h, and then cooling to room temperature along with the furnace;
step six, taking the flaky sample obtained after the solid-state reaction in the step five out of the crucible, grinding the flaky sample into powder by using a mortar, and sieving the powder by using a 200-mesh sieve to finally obtain the La2CuO4And (3) nano powder.
Example 4
Copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
step one, adopting high-purity La2O3And CuO oxide as a starting material, as La2O3: 1, CuO: 1, proportioning and mixing into powder;
step two, putting the mixed powder into a ball milling tank, performing vacuum treatment on the ball milling tank filled with the powder to ensure that the vacuum degree is less than 6Pa in order to prevent the powder from being oxidized and changing valence, filling argon into the ball milling tank after vacuumizing is finished, circularly performing the vacuum treatment and argon filling processes for more than three times in order to remove air in the tank body, controlling the rotating speed of the ball milling tank to be 300rpm and the time to be 300min, and performing dry milling;
step three, in order to prevent powder from caking and enable the ball milling to be more uniform, after the dry milling is finished, argon is injected into an air inlet of a ball milling tank, absolute ethyl alcohol is injected into an air outlet of the ball milling tank through a needle tube, and after the absolute ethyl alcohol is injected, the air outlet is closed firstly and then the air inlet is closed; controlling the rotation speed of the ball milling tank to be 300rpm and the time to be 300min, and carrying out wet milling;
step four, drying the mixture after wet grinding at 50 ℃ for 10 hours to finally obtain the La2O3Nano powder fully and uniformly mixed with CuO;
putting the nano powder into a die with the diameter of 12.5mm, pressing the nano powder into cylindrical sheets with the diameter of 12.5mm and the height of 3mm under the pressure of 50MPa of an electric powder tablet press, uniformly putting the cylindrical sheets into a crucible of 99% alumina, and covering the crucible cover;
step six, uniformly placing the crucible filled with the sheet sample into a box-type resistance furnace, wherein the temperature control program of the box-type resistance furnace is as follows: heating to 850 ℃ at the speed of 100 ℃/h, heating to 900 ℃ at the speed of 20 ℃/h, preserving heat for 12h, and then cooling to room temperature along with the furnace;
step six, taking the flaky sample obtained after the solid-state reaction in the step five out of the crucible, grinding the flaky sample into powder by using a mortar, and sieving the powder by using a 200-mesh sieve to finally obtain the La2CuO4And (3) nano powder.
Example 5
Copper-based oxide La2CuO4The preparation method of the powder material comprises the following steps:
step one, adopting high-purity La2O3And CuO oxide as a starting material, as La2O3: 1, CuO: 1, proportioning and mixing into powder;
step two, putting the mixed powder into a ball milling tank, performing vacuum treatment on the ball milling tank filled with the powder to ensure that the vacuum degree is less than 6Pa in order to prevent the powder from being oxidized and changing valence, filling argon into the ball milling tank after vacuumizing is finished, circularly performing the vacuum treatment and argon filling processes for more than three times in order to remove air in the tank body, controlling the rotating speed of the ball milling tank to be 300rpm and the time to be 300min, and performing dry milling;
step three, in order to prevent powder from caking and enable the ball milling to be more uniform, after the dry milling is finished, argon is injected into an air inlet of a ball milling tank, absolute ethyl alcohol is injected into an air outlet of the ball milling tank through a needle tube, and after the absolute ethyl alcohol is injected, the air outlet is closed firstly and then the air inlet is closed; controlling the rotation speed of the ball milling tank to be 300rpm and the time to be 300min, and carrying out wet milling;
step four, drying the mixture after wet grinding at 50 ℃ for 10 hours to finally obtain the La2O3Nano powder fully and uniformly mixed with CuO;
putting the nano powder into a die with the diameter of 12.5mm, pressing the nano powder into cylindrical sheets with the diameter of 12.5mm and the height of 3mm under the pressure of 50MPa of an electric powder tablet press, uniformly putting the cylindrical sheets into a crucible of 99% alumina, and covering the crucible cover;
step six, uniformly placing the crucible filled with the sheet sample into a box-type resistance furnace, wherein the temperature control program of the box-type resistance furnace is as follows: heating to 900 ℃ at the speed of 100 ℃/h, heating to 950 ℃ at the speed of 20 ℃/h, preserving heat for 12h, and then cooling to room temperature along with the furnace;
step six, taking the flaky sample obtained after the solid-state reaction in the step five out of the crucible, grinding the flaky sample into powder by using a mortar, and sieving the powder by using a-200-mesh sieve to finally obtain the La2CuO4And (3) nano powder.
In FIG. 1, a, b and c are X-ray diffraction (XRD) patterns of the copper-based oxide powders prepared in examples 3, 4 and 5, respectively, and it can be seen from FIG. 1 that all the characteristic peaks of the powders are La2CuO4Characteristic spectral line (PDF # 38-0709).
The above examples are only for describing the present invention in detail, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (7)
1. Copper-based oxide La2CuO4The preparation method of the powder material is characterized by comprising the following steps:
1) adopting lanthanum oxide La2O3Mixing the raw materials with copper oxide CuO, and putting the mixture into a ball milling tank;
2) carrying out vacuum treatment on the ball milling tank to ensure that the vacuum degree is less than 6Pa, then filling argon into the ball milling tank, repeating the steps for at least three times, and then carrying out dry milling;
3) after the dry milling is finished, simultaneously injecting argon and absolute ethyl alcohol into the air inlet and the air outlet of the ball milling tank respectively, and closing the air outlet and the air inlet in sequence after the injection is finished to carry out wet milling;
4) placing the nano powder obtained by drying the mixture after wet grinding in a mould, pressing the nano powder into a flaky sample by an electric powder tablet press, and placing the flaky sample in a crucible with 99% of alumina;
5) putting the crucible into a resistance furnace for heating and heat preservation, and then cooling the crucible to room temperature along with the resistance furnace;
6) and taking out the flaky sample in the crucible, grinding and sieving to obtain the copper-based oxide nano powder.
2. Copper-based oxide La according to claim 12CuO4The preparation method of the powder material is characterized in that the dry grinding speed is 100-500 rpm, and the time is 15 min-96 h.
3. Copper-based oxide La according to claim 12CuO4The preparation method of the powder material is characterized in that the rotation speed of wet grinding is 50-300 rpm, and the time is 15 min-12 h.
4. Copper-based oxide La according to claim 12CuO4The preparation method of the powder material is characterized in that the drying temperature is 20-200 ℃ and the time is 4-20 h.
5. According to claim 1The copper-based oxide La2CuO4The preparation method of the powder material is characterized in that the pressure of the electric powder tablet press is 10-50 MPa.
6. Copper-based oxide La according to claim 12CuO4The preparation method of the powder material is characterized in that the flaky sample is a cylindrical sheet with the diameter of 12.5mm and the height of 3-15 mm.
7. Copper-based oxide La according to claim 12CuO4The preparation method of the powder material is characterized in that the heating and heat preservation in the resistance furnace are carried out by firstly heating to 750-900 ℃ at the speed of 50-150 ℃/h, then heating to 800-950 ℃ at the speed of 20-50 ℃/h, and carrying out heat preservation for 5-24 h.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8804810D0 (en) * | 1988-03-01 | 1988-03-30 | Chancellor Masters & Scholars | Synthesising inorganic compounds using microwave radiation |
| CN102502763A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing lanthanum copper oxide (La2CuO4) powder by sol gel-ultrasonic chemical method |
| CN104291279A (en) * | 2014-09-26 | 2015-01-21 | 北京航空航天大学 | Preparation method of SnS3 nano powder |
| CN107857289A (en) * | 2017-11-13 | 2018-03-30 | 东北大学 | A kind of preparation method of copper acid lanthanum nano adsorption material |
| CN108671927A (en) * | 2018-04-28 | 2018-10-19 | 中国科学院工程热物理研究所 | Composite catalyst and preparation method, the hydrogen production process of hydrogen production from methanol-steam reforming |
| CN111867726A (en) * | 2018-03-19 | 2020-10-30 | 富士胶片株式会社 | Photocatalyst for water splitting, electrode, and water splitting apparatus |
-
2022
- 2022-03-09 CN CN202210224940.3A patent/CN114604889A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8804810D0 (en) * | 1988-03-01 | 1988-03-30 | Chancellor Masters & Scholars | Synthesising inorganic compounds using microwave radiation |
| CN102502763A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing lanthanum copper oxide (La2CuO4) powder by sol gel-ultrasonic chemical method |
| CN104291279A (en) * | 2014-09-26 | 2015-01-21 | 北京航空航天大学 | Preparation method of SnS3 nano powder |
| CN107857289A (en) * | 2017-11-13 | 2018-03-30 | 东北大学 | A kind of preparation method of copper acid lanthanum nano adsorption material |
| CN111867726A (en) * | 2018-03-19 | 2020-10-30 | 富士胶片株式会社 | Photocatalyst for water splitting, electrode, and water splitting apparatus |
| CN108671927A (en) * | 2018-04-28 | 2018-10-19 | 中国科学院工程热物理研究所 | Composite catalyst and preparation method, the hydrogen production process of hydrogen production from methanol-steam reforming |
Non-Patent Citations (4)
| Title |
|---|
| CHUNHUI ZHU ET AL.: ""Investigation of the thermoelectric properties of La2CuO4 ceramics with the addition of Ag"", 《PHYSICA B》 * |
| 方俊飞等: "钙钛矿型La2CuO4亚微米材料的制备及性能研究", 《重庆理工大学学报(自然科学)》 * |
| 曲远方: "《现代陶瓷材料及技术》", 31 May 2008, 华东理工大学出版社 * |
| 顾立德 等, 中南工业大学出版社 * |
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