CN110217835B - PtO (PtO)2Preparation method of tapered nano-particle material - Google Patents
PtO (PtO)2Preparation method of tapered nano-particle material Download PDFInfo
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- CN110217835B CN110217835B CN201910615508.5A CN201910615508A CN110217835B CN 110217835 B CN110217835 B CN 110217835B CN 201910615508 A CN201910615508 A CN 201910615508A CN 110217835 B CN110217835 B CN 110217835B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 100
- 239000000463 material Substances 0.000 title claims description 24
- 238000000034 method Methods 0.000 title abstract description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000010931 gold Substances 0.000 claims abstract description 127
- 229910052737 gold Inorganic materials 0.000 claims abstract description 127
- 229910019020 PtO2 Inorganic materials 0.000 claims abstract description 54
- 238000007789 sealing Methods 0.000 claims abstract description 53
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 44
- 239000011591 potassium Substances 0.000 claims abstract description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- 239000013078 crystal Substances 0.000 claims abstract description 21
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 18
- 230000035484 reaction time Effects 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 230000001788 irregular Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 129
- 238000005303 weighing Methods 0.000 claims description 46
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- 238000001035 drying Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 23
- 238000003466 welding Methods 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 15
- 238000003912 environmental pollution Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000001103 potassium chloride Substances 0.000 claims description 12
- 235000011164 potassium chloride Nutrition 0.000 claims description 12
- 238000002474 experimental method Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 85
- 238000004458 analytical method Methods 0.000 description 30
- 238000010438 heat treatment Methods 0.000 description 21
- 238000001069 Raman spectroscopy Methods 0.000 description 20
- 238000011049 filling Methods 0.000 description 18
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- 229910020437 K2PtCl6 Inorganic materials 0.000 description 11
- 239000005457 ice water Substances 0.000 description 11
- 239000002244 precipitate Substances 0.000 description 11
- 238000007605 air drying Methods 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 238000002347 injection Methods 0.000 description 10
- 239000007924 injection Substances 0.000 description 10
- 238000000643 oven drying Methods 0.000 description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- 230000001502 supplementing effect Effects 0.000 description 10
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- YKIOKAURTKXMSB-UHFFFAOYSA-N adams's catalyst Chemical compound O=[Pt]=O YKIOKAURTKXMSB-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 2
- 229910003446 platinum oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/004—Oxides; Hydroxides
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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
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- 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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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a PtO2Preparing dilute potassium chloroplatinate solution, placing the dilute potassium chloroplatinate solution in a gold tube, sealing, placing the gold tube in a hydrothermal reaction kettle, sealing, and preparing to obtain PtO through self-hydrolysis reaction under the conditions of set temperature and pressure2The conical nano-particles have the temperature of 200-600 ℃, the pressure of 100-200 Mpa and the self-hydrolysis reaction time of 1-48 h. The preparation method has the advantages of easily-obtained raw materials, low cost, rigorous and efficient experimental process and low energy consumption, and the prepared PtO is2The grain diameter of the nano-particles is dozens of to hundreds of nanometers, and the nano-particles have irregular cone-shaped structures and complete crystal forms.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to PtO2A preparation method of a tapered nano-particle material.
Background
PtO2As a catalyst material having high activity, it has been widely used in battery electrodes and various chemical catalytic reactions. With the improvement of the synthesis process of the nano composite material and the development of the function of the nano composite material, the synthesis path and the process of the nano-micron platinum dioxide are more and more emphasized.
Current PtO2A general synthetic process is that chloroplatinic acid or ammonium chloroplatinate and sodium nitrate are co-melted at 500 ℃, which is prepared by the first one by the student V.Voorhees of Roger Adam and others, the specific preparation method is that sodium nitrate is added into a 50m L beaker, 10% chloroplatinic acid or ammonium chloroplatinate solution is added, the mixture is evaporated to dryness while continuously stirring to avoid partial melting of the mixture, the sodium nitrate is heated to 500 ℃ in an evaporating dish, then the evaporation residue is added into the sodium nitrate once, the heating is stopped, finally, brownish black platinum oxide is obtained, the purified ammonium chloroplatinate and the purified sodium nitrate are respectively ground and mixed in the patent with the publication No. CN 101712493A, the mixture is placed in a high-temperature furnace and slowly heated to 340 ℃ for 360 ℃, and the temperature is kept constant for 1-1.5 hours, and then the temperature is kept for 1-1.5 hours, and then the temperature is adjusted to the temperatureAnd cooling to obtain the platinum dioxide material. The use of submicron PtO in patent publication No. CN104900891A2The powder and the conductive polymer organic carrier are mixed and ground according to a certain proportion to prepare the platinum-mesh-supported platinum oxide electrode material. However, various synthetic PtO's are currently available2The process of the material is complex, the cost is high, and the obtained PtO2The purity is lower. This limits the PtO to some extent2The application and popularization of the nano-particle material in various industrial catalysts.
Disclosure of Invention
The invention aims to provide a PtO2The preparation method of the conical nano-particle material has the advantages of easily obtained raw materials, low cost, rigorous and efficient experimental process and low energy consumption, and the prepared PtO2The grain diameter of the nano-particles is dozens of to hundreds of nanometers, and the nano-particles have irregular cone-shaped structures and complete crystal forms.
The above object of the present invention is achieved by the following technical solutions: PtO (PtO)2Preparing dilute potassium chloroplatinate solution, placing the dilute potassium chloroplatinate solution in a gold tube, sealing, placing the gold tube in a hydrothermal reaction kettle, sealing, and preparing to obtain PtO through self-hydrolysis reaction under the conditions of set temperature and pressure2The conical nano-particles have the temperature of 200-600 ℃, the pressure of 100-200 Mpa and the self-hydrolysis reaction time of 1-48 h.
In the PtO2The preparation method of the tapered nano-particle material comprises the following steps:
preferably, the autohydrolysis reaction time is 1-48 h, and PtO can be effectively observed in the time range2The crystallization speed, temperature (200-600 ℃) and pressure (100-200 MPa) of the conical nano-particles influence the appearance of the crystals.
Preferably, the temperature is 400-600 ℃ during the self-hydrolysis reaction, the pressure is adjusted to be 100-150 Mpa by adopting argon, the self-hydrolysis reaction time is 20-28 h, and PtO with better grain diameter and crystal form can be obtained2Tapered nanoparticles; wherein the autohydrolysis reaction time does not include the time of temperature rise and temperature drop, and refers to the conditions of set temperature and pressureThe autohydrolysis reaction time is carried out.
Preferably, the dilute solution of potassium chloroplatinate is potassium chloroplatinate (K)2PtCl6) The powder is dissolved in deionized water to prepare the gold tube, wherein the potassium chloroplatinate powder is an analytical purity reagent, the concentration of the dilute potassium chloroplatinate solution is 0.002 mol/L-0.01 mol/L, and the volume of the dilute potassium chloroplatinate solution accounts for 40-50% of the total volume of the gold tube.
Preferably, the PtO2The particle size of the conical nano-particles is dozens to hundreds of nanometers, the conical nano-particles have irregular conical structures, and the crystal forms are intact.
Preferably, the gold tube is subjected to truncation, acid boiling, washing and quenching treatment, so that the experiment is ensured to be free from other impurities in the gold tube, and the complete sealing property of the gold tube is ensured.
Preferably, the gold tube can be a commercially available high-purity gold tube (purity about 99.9%).
Preferably, the diluted potassium chloroplatinate solution is placed in a gold tube for welding and sealing, then drying and weighing are carried out, the drying is carried out for more than 2 hours in a drying box at the temperature of 110 ℃, then weighing is carried out, and the mass error before and after the drying is ensured to be less than 0.001g, so that the complete sealing of the gold tube and the effectiveness of an experiment are ensured.
Preferably, after the self-hydrolysis reaction is finished, cooling is carried out, then the hydrothermal reaction kettle is opened, the gold tube after the reaction is taken out, the gold tube is broken, the residual reaction solution in the kettle is taken out, the sample is collected and dried to obtain the conical PtO2And (3) nanoparticles.
Preferably, the reaction kettle is cooled by ice water at a high speed or at a constant pressure to room temperature or room temperature.
Preferably, the reacted gold tube is taken out, cleaned and dried, and weighed again to confirm whether the reaction process is completely sealed, and to ensure the effectiveness of the experiment.
Preferably, the residual reaction solution comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the residual reaction solution in the kettle is taken out for recycling to reduce environmental pollution.
The residual reaction solution has simple components, can be recycled and has less environmental pollution.
Preferably, when collecting the sample, the inner wall of the gold tube is soaked and washed 2-3 times respectively by deionized water and absolute ethyl alcohol, so that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and then attaching PtO attached to the inner wall of the gold tube2Taking out and naturally drying or drying by adopting a drying dish to obtain the conical PtO2And (3) nanoparticles.
A PtO of the present invention2The core of the preparation method of the conical nano-particle material lies in that the hydrolysis reaction of potassium chloroplatinate single reagent under different temperature and pressure conditions is utilized to generate PtO2The nano-particles use only potassium chloroplatinate as a dilute solution, and the potassium chloroplatinate and water have the following hydrolysis reaction under the hydrothermal condition:
K2PtCl6+2H2O＝2KCl+PtO2↓+4HCl
compared with the prior art, the invention has the following advantages:
(1) the method adopts a single reagent of potassium chloroplatinate dilute solution to carry out the self-hydrolysis reaction, and has simple operation process and easy operation and control;
(2) the method of the invention adopts the pure gold tube as the outer sleeve, which can ensure that the reactant does not react with other substances and can ensure the sealing property and the effectiveness in the reaction process;
(3) the invention adopts the hydrothermal reaction kettle to carry out the hydrolysis reaction, the cost is low, and the energy consumption is low;
(4) the invention uses time series to observe PtO2The growth state of the nano particles is changed, the components of the residual reaction solution are simple, the reaction solution can be recycled, and the environmental pollution is less;
(5) the method has the advantages of safe and environment-friendly whole process, and the prepared conical PtO2The crystal form of the nano-particle material is complete.
Drawings
FIG. 1 shows PtO prepared in examples 1 to 10 of the present invention2Laser Raman spectrum of the tapered nano-particle material;
FIG. 2 shows PtO prepared in examples 1 to 5 of the present invention2Scanning electron micrograph of tapered nanoparticles (a) prepared in example 1Amorphous PtO2Nanoparticles, (b) amorphous PtO prepared as in example 22Nanoparticles, (c) tapered PtO prepared in example 32Nanoparticles, (d) preparation of example 4 to obtain the tapered PtO2Nanoparticles, (e-f) preparation of example 5 to obtain the tapered PtO2A nanoparticle;
FIG. 3 shows PtO prepared in examples 6 to 10 of the present invention2Scanning electron micrograph of tapered nanoparticles, (a) amorphous PtO prepared in example 62Nanoparticles, (b) preparation of example 7 to obtain the tapered PtO2Nanoparticles, (c) preparation of example 8 to obtain the tapered PtO2Nanoparticles, (d) PtO in the form of a cone prepared as described in example 92Nanoparticles, (e-f) preparation of example 10 to obtain the tapered PtO2And (3) nanoparticles.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings, but the scope of the present invention as claimed is not limited to the examples, as the reaction apparatus and the reaction temperature, the reaction time and the volume of the reaction liquid.
Example 1
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) cutting a high-purity gold tube with the diameter of 4mm into a length required by an experiment, performing early-stage treatment such as acid boiling, washing, quenching, welding and sealing one end in advance and the like to ensure that no impurities or cracks exist in the gold tube;
(2) 0.486g of potassium chloroplatinate (K) of analytical purity was added2PtCl6) Dissolving the powder in 100m L deionized water, and dissolving to obtain 0.01 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 200MPa, keeping the temperature and pressure stable, reacting for 1h, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapidly cooling or cooling to normal temperature at constant pressure;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(a) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 2(a) scanning Electron micrograph showing the synthesized amorphous PtO2The crystal nucleus of the nano-particles is just appeared, and the crystal form is incomplete;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 2
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.486g of potassium chloroplatinate (K) of analytical purity was added2PtCl6) Dissolving the powder in 100m L deionized water, and dissolving to obtain 0.01 mol/L K2PtCl6The prepared reaction solution was taken to be about 0.1m L and containedFeeding the gold tube into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and weighing again after that, ensuring that the mass error before and after weighing is less than 0.001g, and indicating that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 200MPa, keeping the temperature and pressure stable, reacting for 6 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapidly cooling or cooling to normal temperature at constant pressure;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(a) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 2(b) scanning Electron micrograph showing the synthesized amorphous PtO2Nanoparticles, the crystal form is incomplete, and the particles grow in a chain shape;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 3
PtO provided in the present embodiment2Preparation of tapered nanoparticlesThe method comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.486g of potassium chloroplatinate (K) of analytical purity was added2PtCl6) Dissolving the powder in 100m L deionized water, and dissolving to obtain 0.01 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 200MPa, keeping the temperature and pressure stable, reacting for 9 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant-pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(a) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 2(c) SEM image shows the preliminary synthesized tapered PtO2NanoparticlesThe crystal form is relatively complete;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 4
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.486g of potassium chloroplatinate (K) of analytical purity was added2PtCl6) Dissolving the powder in 100m L deionized water, and dissolving to obtain 0.01 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 200MPa, keeping the temperature and pressure stable, reacting for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant-pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying the precipitate sample to obtainConical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(a) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 2(d) scanning Electron micrograph showing the synthetic tapered PtO2Nanoparticles, complete in crystal form;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 5
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.486g of potassium chloroplatinate (K) of analytical purity was added2PtCl6) Dissolving the powder in 100m L deionized water, and dissolving to obtain 0.01 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 200MPa, keeping the temperature and pressure stable, reacting for 48 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapidly cooling or cooling to normal temperature at constant pressure;
(5) opening the reaction kettle in the step (3), taking out the gold tube in the reaction kettle,Cleaning, drying and weighing to ensure the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming no errors, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol for 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(a) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 2(e-f) scanning Electron micrograph showing the synthetic pyramidal PtO2Nanoparticles, complete in crystal form;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 6
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.0972g of potassium chloroplatinate (K) of analytical purity2PtCl6) The powder is dissolved in 100m L deionized water and fully dissolved to obtain 0.002 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 200 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 100MPa, keeping the temperature and pressure stable, reacting for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant-pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(b) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 3(a) scanning Electron micrograph showing the synthesized amorphous PtO2The crystal nucleus of the nano-particles is just appeared, and the crystal form is incomplete;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 7
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.0972g of potassium chloroplatinate (K) of analytical purity2PtCl6) The powder is dissolved in 100m L deionized water and fully dissolved to obtain 0.002 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 300 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 100MPa, keeping the stable temperature and pressure condition for reaction for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(c) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 3(b) scanning Electron micrograph showing the synthetic tapered PtO2The crystal form of the nano-particles is complete;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 8
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.0972g of potassium chloroplatinate (K) of analytical purity2PtCl6) The powder is dissolved in 100ml deionized water and fully dissolved to obtain 0.002 mol/L K2PtCl6Solution, about 0.1ml of prepared reaction solution is filled into a gold tube, the filling degree is controlled to be about 40-50%, welding and sealing are carried out, and weighing is carried out after welding and sealingRecording, then placing the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error of the previous weighing and the next weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 400 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 100MPa, keeping the stable temperature and pressure condition for reaction for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(d) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 3(c) scanning Electron micrograph showing the synthetic tapered PtO2The crystal form of the nano-particles is complete;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 9
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.0972g of potassium chloroplatinate (K) of analytical purity2PtCl6) The powder is dissolved in 100m L deionized water and fully dissolved to obtain 0.002 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 500 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 100MPa, keeping the temperature and pressure stable, reacting for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapid cooling or constant-pressure cooling to normal temperature;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2The nanoparticle sample was subjected to Raman analysis and morphology analysis, and FIG. 1(e) shows the obtained tapered PtO by laser Raman analysis2Nanoparticles, FIG. 3(d) scanning Electron micrograph showing the synthetic tapered PtO2Nanoparticles, complete in crystal form;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
Example 10
PtO provided in the present embodiment2The preparation method of the tapered nano-particles comprises the following steps:
(1) pretreatment of the gold tube was the same as in example 1;
(2) 0.0972g of potassium chloroplatinate (K) of analytical purity2PtCl6) The powder is dissolved in 100m L deionized water and fully dissolved to obtain 0.002 mol/L K2PtCl6Solution, namely filling the prepared reaction solution with about 0.1m L into a gold tube, controlling the filling degree to be about 40-50%, performing welding sealing, performing weighing recording after welding sealing, then putting the gold tube filled with the solution sample into a drying box at 110 ℃ for more than 2h, and then weighing again, wherein the mass error before and after weighing is ensured to be less than 0.001g, which indicates that the gold tube is complete in sealing property;
(3) placing a gold tube which is confirmed to have perfect tightness and is filled with a solution sample into a high-temperature high-pressure reaction kettle, injecting deionized water as a medium, screwing down the reaction kettle, checking the tightness of the reaction kettle, confirming that no error exists, injecting argon into the kettle to the pressure of 60MPa through a vent pipeline to serve as an initial pressure, closing a stop valve to stop gas injection, heating the reaction kettle through a heating furnace, and setting the reaction temperature to be 200 ℃;
(4) after the temperature is increased to 600 ℃, opening the stop valve in the step (3), continuously supplementing and injecting argon to the pressure of 100MPa, keeping the temperature and pressure stable, reacting for 24 hours, and after the reaction is finished, using ice water to pour the reaction kettle in the step (3) for rapidly cooling or cooling to normal temperature at constant pressure;
(5) opening the reaction kettle in the step (3), taking out, cleaning, drying and weighing the gold tube in the reaction kettle, ensuring the sealing property and effectiveness of the reaction process, breaking the gold tube after confirming that no error exists, recovering the residual solution, washing the inner wall of the gold tube with deionized water and alcohol 2-3 times respectively to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and air-drying the precipitate sample with natural wind or oven-drying to obtain the conical PtO2A nanoparticle;
(6) the obtained conical PtO2Nanoparticle sample introductionPerforming Raman analysis and morphology analysis, and FIG. 1(f) shows the obtained conical PtO by laser Raman analysis2Nanoparticles, FIG. 3(e-f) scanning Electron micrograph showing the synthetic pyramidal PtO2Nanoparticles, complete in crystal form;
(7) the residual solution mainly comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the solution can be recycled and has small environmental pollution.
From the above examples, it can be seen that better PtO is obtained2The experimental temperature of the particle size and the crystal form of the conical nano particles is 400-600 ℃, the pressure is 100-150 Mpa, and the reaction time is 20-28 h. The above preferred temperatures, pressures and reaction times are obtained only from the above experiments of the present application, if further optimization of experimental conditions and discussion of PtO under different experimental conditions is required2The crystal form of the nano particles is changed, and the experimental conditions need to be further refined for discussion.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (10)
1. PtO (PtO)2The preparation method of the tapered nano-particle material is characterized by comprising the following steps: preparing a dilute solution of potassium chloroplatinate, placing the dilute solution of potassium chloroplatinate in a gold tube and sealing, then placing the gold tube in a hydrothermal reaction kettle and sealing, and preparing the PtO by self-hydrolysis reaction under the conditions of set temperature and pressure2The conical nanoparticles have the temperature of 300-600 ℃, the pressure of 100-200 Mpa and the self-hydrolysis reaction time of 24-48 h.
2. The PtO of claim 12The preparation method of the tapered nano-particle material is characterized by comprising the following steps: during the self-hydrolysis reaction, the temperature is 400-600 ℃, the pressure is regulated to be 100-150 Mpa by adopting argon, and the self-hydrolysis reaction time is 20-28 h; wherein the autohydrolysis reaction time does not include the time of temperature rise and temperature decreaseThe term "hydrolysis" means a reaction time for which the hydrolysis is carried out under the conditions of a predetermined temperature and pressure.
3. The PtO of claim 1 or 22The preparation method of the tapered nano-particle material is characterized in that the dilute potassium chloroplatinate solution is prepared by dissolving potassium chloroplatinate powder in deionized water, wherein the potassium chloroplatinate powder is an analytical purity reagent, the concentration of the dilute potassium chloroplatinate solution is 0.002 mol/L-0.01 mol/L, and the volume of the dilute potassium chloroplatinate solution accounts for 40-50% of the total volume of a gold tube.
4. The PtO of claim 32The preparation method of the tapered nano-particle material is characterized by comprising the following steps: the PtO2The particle size of the conical nano-particles is dozens to hundreds of nanometers, the conical nano-particles have irregular conical structures, and the crystal forms are intact.
5. The PtO of claim 12The preparation method of the tapered nano-particle material is characterized by comprising the following steps: the gold tube is subjected to truncation, acid boiling, washing and quenching treatment, so that the experiment is ensured to be free from other impurities in the gold tube, and the complete sealing property of the gold tube is ensured.
6. The PtO of claim 12The preparation method of the tapered nano-particle material is characterized by comprising the following steps: and (2) placing the potassium chloroplatinate dilute solution into a gold tube for welding and sealing, then drying and weighing, wherein the drying is carried out for more than 2h in a drying box at the temperature of 110 ℃, and then weighing is carried out, so that the mass error before and after the drying is ensured to be less than 0.001g, and the complete sealing of the gold tube and the effectiveness of an experiment are ensured.
7. The PtO of claim 12The preparation method of the tapered nano-particle material is characterized by comprising the following steps: cooling after the self-hydrolysis reaction is finished, opening the hydrothermal reaction kettle, taking out a gold tube after the reaction, breaking the gold tube, taking out residual reaction solution in the kettle, collecting a sample, and drying to obtain the conical PtO2And (3) nanoparticles.
8. The PtO of claim 72The preparation method of the tapered nano-particle material is characterized by comprising the following steps: and taking out the reacted gold tube, cleaning and drying the reacted gold tube, weighing again to confirm whether the reaction process is completely sealed, and ensuring the effectiveness of the experiment.
9. The PtO of claim 72The preparation method of the tapered nano-particle material is characterized by comprising the following steps: the residual reaction solution comprises potassium chloroplatinate, hydrochloric acid and potassium chloride, and the residual reaction solution in the kettle is taken out for recycling to reduce environmental pollution.
10. The PtO of claim 72The preparation method of the tapered nano-particle material is characterized by comprising the following steps: when collecting the sample, soaking and washing the inner wall of the gold tube for 2-3 times respectively by using deionized water and absolute ethyl alcohol to ensure that the PtO attached to the inner wall of the gold tube2Cleaning the sample, and then attaching PtO attached to the inner wall of the gold tube2Taking out and naturally drying or drying by adopting a drying dish to obtain the conical PtO2And (3) nanoparticles.
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| CN113620357B (en) * | 2021-08-04 | 2022-05-27 | 中国科学院广州地球化学研究所 | OsO (OsO)2Preparation method of spherical nano-particle material |
| CN113772752A (en) * | 2021-08-04 | 2021-12-10 | 中国科学院广州地球化学研究所 | PdO2Preparation method of irregular conical nano-particle material |
| CN113697871B (en) * | 2021-08-04 | 2022-06-10 | 中国科学院广州地球化学研究所 | Preparation of short columnar PdO based on hydrolysis reaction2Method for producing nanoparticle material |
| CN113620358A (en) * | 2021-08-04 | 2021-11-09 | 中国科学院广州地球化学研究所 | Hydrolysis method based cluster IrO preparation2Method for preparing nano material |
| CN113603162B (en) * | 2021-08-04 | 2023-05-16 | 中国科学院广州地球化学研究所 | Nearly spherical Rh 2 O 3 Method for preparing nano material |
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| CN104724764A (en) * | 2015-02-14 | 2015-06-24 | 溧阳市超强链条制造有限公司 | Platinum oxide nano powder and preparation method thereof |
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