CN108144607B - Strontium iridate catalyst, preparation method and application thereof in aspect of producing oxygen by electrocatalytic cracking of acidic water - Google Patents
Strontium iridate catalyst, preparation method and application thereof in aspect of producing oxygen by electrocatalytic cracking of acidic water Download PDFInfo
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Abstract
A pure phase strontium iridate catalyst, a preparation method and application thereof in the aspect of high-efficiency electrocatalytic cracking of acidic water to produce oxygen, belonging to the field of inorganic functional materials. Mixing an iridium source, organic polyol, a strontium source, organic polyacid and water in different proportions, heating and evaporating to dryness, calcining the evaporated reactant for a period of time, and soaking the calcined product in 0.5-2 mol/L hydrochloric acid, sulfuric acid, perchloric acid and the like for 3-10 hours to obtain strontium iridate with different phases. Wherein the obtained monoclinic phase strontium iridate SrIrO3The iridium oxide has high crystallinity and is a regular hexagonal piece, and can replace the traditional iridium dioxide serving as an acid water oxidation catalyst, so that the dosage of noble metal iridium is reduced to a certain extent. The current density of the electrocatalytic water cracking oxygen evolution reaches 10mA/cm2The catalyst only needs over potential of 248mV, has the highest intrinsic activity in the currently reported water cracking oxygen evolution catalyst, is far better than the currently used noble metal catalyst in industry, has stable performance without attenuation, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of inorganic functional materials, and particularly relates to a series of pure-phase strontium iridate catalysts, a preparation method and application thereof in high-efficiency electrocatalytic cracking of acidic water to produce oxygen.
Background
With the rapid development of the economic society, the population is increased, and the energy problem is increasingly prominent. In the field of sustainable energy development, such as fuel cells and electrocatalytic hydrogen production, the electrochemical water splitting oxygen production reaction is crucial, but the kinetics of the oxygen production reaction limits the catalytic performance and commercial application thereof. In acidic water oxidation, the problem is more pronounced and most catalytic materials are difficult to stabilize at strong acids and oxygen-generating overpotentials. Conventional noble metal oxides (IrO)2，RuO2) The catalyst has high acidic water Oxidation (OER) activity, RuO2The performance is excellent in electrochemical acidic water oxidation catalysis, but the stability is poor. IrO2The performance in electrochemical water oxidation is good,but its large-scale application is limited by high price and lack of resources. Therefore, the key point of the acid water cracking oxygen production is to find a catalytic material which replaces the oxide of the noble metal iridium or reduces the dosage of the noble metal iridium and has better acid water oxidation oxygen production activity and stability.
In recent years, as related research advances, a series of acidic oxygen-generating catalysts have been developed. For example, IrO with high intrinsic acidic Water splitting oxygen production Activityx/SrIrO3(Science 2016: 353 volume 1011); iridium-based double perovskite type high-efficiency water oxidation catalyst (nat. Commun.2016, volume 7, page 12363) and hydrothermal method for synthesizing pyrochlore-structured Bi2Ir2O7Oxygen generating catalyst (chem. mater.2014 24 vol 4192). Although these catalysts have good properties in acidic oxygen generation, the synthesis methods are complicated, and most of them require a template-induced crystal phase synthesis method or a high-temperature high-pressure solid phase synthesis method. In order to solve the problems, the catalyst can be generated under normal pressure (101.325kPa) by a more general sol-gel method, and the product has more excellent and stable acidic water oxidation activity and can be used as a very excellent acidic water splitting water oxidation catalyst material.
Disclosure of Invention
The invention aims to synthesize a series of strontium iridate catalysts with different phases by taking the synthesis of a high-efficiency acidic water oxidation catalyst as an objective, wherein monoclinic strontium iridate SrIrO3The hexagonal tablet has the highest acidic oxygen generating activity and nano-micron-sized appearance and size, and realizes the application in the aspect of efficient acidic water oxidation; strontium orthorhombic Irate SrIrO3The acidic water oxidation activity has been reported, and the intrinsic activity is the highest in the reported acidic water oxidation catalyst, and the traditional synthesis method is difficult and needs high temperature and high pressure or crystalline phase induction. In the invention, the orthorhombic strontium iridate is synthesized by a normal pressure (101.325kPa) method, namely a sol-gel method; wherein the cubic phase Sr2Ir3O8Most of the reported synthetic methods in the literature are solid phase synthesis, and pure phase synthesis cannot be performed. The invention discovers a series of pure phase Sr synthesized by regulating the metering of the compound2Ir3O8And (b) and are successfully mixedPure nano-micron cubic phase Sr2Ir3O8Cubic block.
The strontium iridate catalyst provided by the invention is prepared by mixing an iridium source, organic polyol, a strontium source, organic polyacid and water in a certain proportion, heating and evaporating to dryness, then calcining the evaporated reactant for a period of time, and then soaking the calcined product in 0.5-2 mol/L hydrochloric acid, sulfuric acid, perchloric acid and the like for 3-10 hours to obtain a corresponding compound.
To obtain strontium iridate in different phases, we fix the molar amount of iridium source as naBy adjusting the molar amount n of the strontium sourcebAnd the molar amount n of organic polybasic acidcTo obtain a series of strontium iridate compounds with different phases; the specific operation steps are as follows:
monoclinic phase strontium iridium acid SrIrO3Preparation of the catalyst:
(1) preparation of mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naMolar source of iridium, wherein nc：nb：naWhen the ratio is 8: 4: 1. 8: 8: 1. 8: 16: 1 or 8: 24: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid, perchloric acid and the like for 6-10 h, cleaning with ethanol, and drying to obtain monoclinic phase strontium iridate SrIrO3A catalyst.
Strontium di-and orthorhombic Irate SrIrO3Preparation of the catalyst:
(1) preparation of mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naA molar source of iridium in the form of a source of iridium,wherein n isc：nb：na12-40: 8: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid, perchloric acid and the like for 6-10 h, cleaning with ethanol, and drying to obtain the orthorhombic strontium iridate SrIrO3A catalyst.
Three, cubic phase Sr2Ir3O8Preparation of cubic catalyst:
(1) preparation of mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naMolar source of iridium, wherein nc：nb：na0-4: 4-10: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid, perchloric acid and the like for 6-10 h, washing with ethanol, and drying to obtain cubic phase Sr2Ir3O8Cubic piece of catalyst.
In the above process, the iridium source includes, but is not limited to, potassium hexachloroiridium (IV), potassium hexachloroiridium (III), iridium chloride, chloroiridic acid, and the like or mixtures thereof.
In the above method, the strontium source includes, but is not limited to, strontium nitrate, strontium chloride, strontium hydroxide, strontium carbonate, and the like or a mixture thereof.
In the above method, the organic polyol solvent includes, but is not limited to, glycol, glycerol, and other polyol solvents.
In the above method, the organic polybasic acid includes, but is not limited to, a polycarboxylic acid compound such as citric acid, tartaric acid, oxalic acid, etc.
In the above process, nc：nb：naThe molar ratio of (A) is not limited to the listed ratio, and pure phases of the three substances can be synthesized by properly adjusting the relationship of the three.
Advantageous effects
1. The synthesis process is simple, the experimental procedures are convenient and controllable, the preparation period is short, the repeatability is good, and the method can be used for mass production.
2. The obtained monoclinic phase strontium iridate SrIrO3The material has high crystallinity and is a regular hexagonal sheet, and due to the specific iridium oxygen octahedral coplanar connection structure in the crystal structure, the defect of strong oxygen bonding capability of an iridium oxygen bond is optimized, so that the material has excellent oxidation activity and stability of acidic water cracking water. Can replace the iridium dioxide of the traditional acidic water oxidation catalyst, reduce the dosage of noble metal iridium to a certain extent, and has wide application prospect.
3. The obtained orthorhombic strontium Irate SrIrO3The method is a nano-micron powder material, and in the existing reports, the synthetic process of the method is the simplest and controllable, and the purity of a sample is high. Can be converted into IrO in the process of producing oxygen by acid water crackingx/SrIrO3Has higher oxidizing activity of the acid water cracking water.
4. The obtained cubic phase Sr2Ir3O8The cubic powder material has extremely high crystallinity and purity, uniform and adjustable appearance and size, and Sr can be realized by changing the type of the iridium source2Ir3O8The transition of cubic block size from micron-scale to nanometer-scale. In the existing reports, the invention synthesizes pure phase for the first time, and the method is simple and controllable.
Drawings
FIG. 1 sheet of example 1Oblique phase strontium Iridium SrIrO3X-ray diffraction (XRD) pattern of (panel a); strontium orthorhombic Irate SrIrO3X-ray diffraction (XRD) pattern of (panel B); cubic phase Sr2Ir3O8X-ray diffraction (XRD) pattern of (fig. C).
FIG. 2: example 1 monoclinic phase hexagonal strontium Iridium Irate SrIrO3Scanning Electron Microscope (SEM) photograph (fig. a); orthorhombic phase block strontium iridium (SrIrO)3Scanning Electron Microscope (SEM) photograph (fig. B); cubic block Sr2Ir3O8Scanning Electron Microscope (SEM) photograph (fig. C).
FIG. 3: the product of example 1 of the present invention was used as a water-splitting catalyst in an acidic buffer solution (0.5M H)2SO4) Polarization curve of water splitting Oxygen Evolution (OER); monoclinic phase strontium iridate SrIrO3Water splitting oxygen evolution polarization curve (panel a); strontium orthorhombic Irate SrIrO3Water splitting oxygen evolution polarization curve (panel B); cubic phase Sr2Ir3O8Water splitting oxygen evolution polarization curve (panel C).
FIG. 4: the product of example 1 of the present invention was used as a water-splitting catalyst in an acidic buffer solution (0.5M H)2SO4) Stability curve of water splitting Oxygen Evolution (OER). Monoclinic phase strontium iridate SrIrO3Water splitting oxygen evolution stability curve (panel a); strontium orthorhombic Irate SrIrO3Water splitting oxygen evolution stability curve (panel B); cubic phase Sr2Ir3O8Water splitting oxygen evolution stability curve (panel C).
Detailed Description
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited to the following examples. It will be apparent to those skilled in the art that variations or modifications of the present invention can be made without departing from the spirit and scope of the invention, and these variations or modifications are also within the scope of the invention.
Example 1
Monoclinic phase strontium iridate SrIrO3The preparation of (1): first, 80mg (0.166mmol) of potassium hexachloroiridium (IV) was put into 4mL of ethylene glycol and stirred at room temperature until the dissolution was completed to obtain a dark brown transparent solution, which was referred to as solution a. 280mg (1.332mmol)) Citric acid and 280mg (1.323mmol) strontium nitrate was dissolved in 5mL distilled water and stirred at room temperature to a colorless transparent solution, designated as solution b. Dropwise adding the solution b into the solution a, fully and uniformly stirring, and evaporating the mixed solution to dryness at 180 ℃ for 6 hours. In this example, nc：nb：naWhen the ratio is 8: 8: 1. the evaporated solid sample was then ground to a powder and heated at 200 ℃, 300 ℃, 500 ℃ and 700 ℃ at a rate of 1.7 ℃/min for 6h, 6h, 3h and 6h, respectively. After furnace cooling, soaking the black powder with 1mol/L hydrochloric acid for 6h, washing with ethanol, drying and collecting sample powder.
Strontium orthorhombic Irate SrIrO3The preparation of (1): first, 80mg (0.166mmol) of potassium hexachloroiridium (IV) was put into 4mL of ethylene glycol and stirred at room temperature until the dissolution was completed to obtain a dark brown transparent solution, which was referred to as solution a. 840mg (3.997mmol) of citric acid and 280mg (1.323mmol) of strontium nitrate are dissolved in 5mL of distilled water and stirred at room temperature to a colorless transparent solution, called solution b. Dropwise adding the solution b into the solution a, fully and uniformly stirring, and then evaporating the mixed solution to dryness at 180 ℃ for 6 hours. In this example, nc：nb：na24: 8: 1. the evaporated solid sample was then ground to a powder and heated at 200 ℃, 300 ℃, 500 ℃ and 700 ℃ at a rate of 1.7 ℃/min for 6h, 6h, 3h and 6h, respectively. After furnace cooling, soaking the black powder with 1mol/L hydrochloric acid for 6h, washing with ethanol, drying and collecting sample powder.
Cubic phase Sr2Ir3O8Preparation of cubes: first, 80mg (0.166mmol) of potassium hexachloroiridium (IV) was put into 4mL of ethylene glycol and stirred at room temperature until the dissolution was completed to obtain a dark brown transparent solution, which was referred to as solution a. 140mg (0.662mmol) of strontium nitrate was dissolved in 5mL of distilled water and stirred at room temperature to a colorless transparent solution, which was designated as solution b. Dropwise adding the solution b into the solution a, fully and uniformly stirring, and then evaporating the mixed solution to dryness at 180 ℃ for 6 hours. In this example, nc：nb：naWhen the ratio is 0: 4: 1 the evaporated solid sample is then ground to a powder and heated at 200 ℃, 300 ℃, 500 ℃ and 700 ℃ at a rate of 1.7 ℃/min for 6h, 6h, 3h and 6h, respectively. Followed byAfter the furnace and the like are cooled, the black powder is soaked for 6 hours by 1mol/L hydrochloric acid, washed by ethanol and dried, and then sample powder is collected.
Carrying out electrocatalytic water cracking Oxygen Evolution (OER) property test on the material prepared by the method in a standard three-electrode electrolytic cell; mixing the product of the invention in 10-50% naphthol isopropanol solution, and dropping the solution on a platinum-carbon electrode as a working electrode in an electrolytic cell; the reference electrode is a saturated calomel electrode, the counter electrode is a platinum wire, and the electrolyte is 0.5MH2SO4. It should be noted that all potentials obtained by taking saturated calomel as a reference electrode in an electrocatalysis test are converted into reversible hydrogen electrode potentials in a property diagram, and an external power supply is a main battery of an electrochemical working station.
Some structural and performance studies were performed on the materials prepared by the above methods. FIG. 1A shows the monoclinic strontium Irate obtained, SrIrO3X-ray diffraction (XRD) pattern; FIG. 1B shows the obtained strontium IrO orthorhombic salt3X-ray diffraction (XRD); FIG. 1C shows the obtained cubic phase Sr2Ir3O8Cubic block X-ray diffraction (XRD). As can be seen from FIG. 1, the strontium iridate compounds obtained by this method are all phase-pure.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the obtained strontium iridate compound, and FIG. 2A shows that the obtained monoclinic phase strontium iridate has a diameter of about 1 μm and a thickness of about 50nm in a hexagonal shape. Fig. 2B shows that the obtained orthorhombic strontium iridate is a bulk sample of micron size. FIG. 2C shows that cubic phase Sr is obtained2Ir3O8Cubes with cube sides of about 200 nm.
FIG. 3 shows that the product of the present invention is a water cracking catalyst in acidic sulfuric acid (0.5M H)2SO4) Polarization curve of water splitting Oxygen Evolution (OER) in solution. FIG. 3A shows monoclinic phase strontium Irate SrIrO3The polarization curve of water cracking oxygen evolution reaction reaches the current density of 10mA/cm at the overpotential of 248mV2. FIG. 3B shows the orthorhombic strontium Irate SrIrO3The polarization curve of water cracking oxygen evolution reaction reaches the current density of 10mA/cm at the overpotential of 270mV2. FIG. 3C is cubic phase Sr2Ir3O8Water splitting analysisOxygen reaction polarization curve, at an overpotential of 295mV, to a current density of 10mA/cm2. The three catalysts have better catalytic activity, and the monoclinic phase strontium iridate is the most excellent.
FIG. 4 shows that the product of the present invention is sulfuric acid (0.5M H) as an electrolyte of an acidic water cracking catalyst2SO4) Stability curve of water splitting Oxygen Evolution (OER) in solution. FIG. 4A shows monoclinic phase strontium Irate SrIrO3The current density is kept at 10mA/cm during the oxygen evolution by water cracking2The reaction overpotential and time profile of (a); FIG. 4B Quadrature phase strontium Irate SrIrO3The current density is kept at 10mA/cm during the oxygen evolution by water cracking2The reaction overpotential and time profile of (a); FIG. 4C is cubic phase Sr2Ir3O8The current density is kept at 10mA/cm during the oxygen evolution by water cracking2Overpotential and time profile of the reaction of (1). Under the test condition, in the oxygen evolution reaction environment of the three strontium iridate compounds, monoclinic phase strontium iridate SrIrO3Has the highest catalytic stability, the oxygen generating activity is not changed basically within 10h under the over-potential of oxygen evolution, and the orthorhombic strontium iridate SrIrO3And cubic phase Sr2Ir3O8The catalytic stability of (A) is poor, and the oxidation generation property is slightly reduced within 10 hours.
Example 2
Same as example 1, except that the monoclinic strontium Irite SrIrO3In the preparation of (1.323) reduce 280mg (1.323mmol) of strontium nitrate to 140mg (0.662mmol), when nc：nb：naWhen the ratio is 8: 4: 1, the amounts and conditions of the other reactants were unchanged.
Perovskite phase strontium iridium acid SrIrO3The amount of 840mg (3.997mmol) of citric acid was reduced to 420mg (1.999mmol) in the preparation, when nc：nb：na12: 8: 1, the amounts and conditions of the other reactants were unchanged.
Cubic phase Sr2Ir3O8The amount of 140mg (0.662mmol) of strontium nitrate was increased to 350mg (1.654mmol) in the preparation, when nc：nb：naWhen the ratio is 0: 10: 1, the amounts and conditions of the other reactants were unchanged.
Monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 3
Same as example 1, except that the monoclinic strontium Irite SrIrO3In the preparation of (1.332mmol) 280mg of strontium nitrate was increased to 560mg (2.646mmol), when nc：nb：naWhen the ratio is 8: 16: 1, the amounts and conditions of the other reactants were unchanged.
Perovskite phase strontium iridium acid SrIrO3The amount of 840mg (3.969mmol) of citric acid was increased to 1120mg (5.330mmol) in the preparation, when n isc：nb：na32: 8: 1, the amounts and conditions of the other reactants were unchanged.
Cubic phase Sr2Ir3O8140mg (0.666mmol) of citric acid are added, in this case nc：nb：na4: 4: 1, the amounts and conditions of the other reactants were unchanged.
Monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 4
Same as example 1, except that the monoclinic strontium Irite SrIrO3In the preparation of (1.323mmol) 280mg of strontium nitrate was increased to 560mg (2.646mmol), when nc：nb：naWhen the ratio is 8: 16: 1, the amounts and conditions of the other reactants were unchanged.
Perovskite phase strontium iridium acid SrIrO3The amount of 840mg (3.997mmol) of citric acid was increased to 1120mg (5.330mmol) in the preparation, when n isc：nb：na32: 8: 1, the amounts and conditions of the other reactants were unchanged.
Cubic phase Sr2Ir3O8140mg (0.666mmol) of citric acid are added, in this case nc：nb：na4: 4: 1, the amounts and conditions of the other reactants were unchanged.
Monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 5
Same as example 1, except that the monoclinic strontium Irite SrIrO3In the preparation of (1.323mmol) 280mg of strontium nitrate was increased to 840mg (3.969mmol), when nc：nb：naWhen the ratio is 8: 24: 1, the amounts and conditions of the other reactants were unchanged.
Perovskite phase strontium iridium acid SrIrO3The amount of 840mg (3.997mmol) of citric acid was increased to 1400mg (6.662mmol) in the preparation, when nc：nb：na40: 8: 1, the amounts and conditions of the other reactants were unchanged.
Cubic phase Sr2Ir3O8By adding 140mg (0.666mmol) of citric acid, the amount of 140mg (0.662mmol) of strontium nitrate is increased to 350mg (1.654mmol) of nc：nb：na4: 10: 1, the amounts and conditions of the other reactants were unchanged.
Monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 6
The same procedure as in example 1 was repeated except that potassium hexachloroiridium (IV) was changed to potassium hexachloroiridium (III) and the molar amount of the iridium source was changed to 0.166 mmol. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 7
Same as in example 1, except that potassium hexachloroiridium (IV) was changed to chloroiridate hydrate, the molar amount of the iridium source was 0.166mmol without changing. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 8
Same as example 1, except that the potassium hexachloroiridium (IV) in the preparation of the different phases was exchanged for iridium chloride, the moles of iridium source were unchanged at 0.166 mmol. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 9
The same as in example 1, except that the strontium nitrate was changed to strontium chloride in the preparation of the different phases, the molar amount of the strontium source was unchanged. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 10
The same as in example 1, except that strontium nitrate was replaced by strontium hydroxide in the preparation of the different phases, the molar amount of strontium source was unchanged. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 11
The same as in example 1, except that strontium nitrate was changed to strontium carbonate in the preparation of the different phases, the molar amount of strontium source was unchanged. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 12
The monoclinic strontium iridate SrIrO was prepared in the same manner as in example 1, except that citric acid was replaced by tartaric acid in the preparation of the different phases3The molar amount of tartaric acid was 1.332 mmol. Preparation of orthorhombic strontium Irate SrIrO3The molar weight of tartaric acid was 3.9996 mmol. Preparation of cubic phase Sr2Ir3O8The molar weight of cubic tartaric acid was 0.666 mmol. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 260mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When passing the currentWhen the potential is 295mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm when the overpotential was 310mV2。
Example 13
The same as in example 1, except that ethylene glycol was changed to glycerol, the volume of the fixed alcohol was 4 mL. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 250mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 275mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm when the overpotential was 305mV2。
Example 14
The same as in example 1 except that the calcination temperature was changed to 6h, 6h, 3h and 6h at a temperature rise rate of 2 ℃/min at 200 ℃, 300 ℃, 500 ℃ and 800 ℃ respectively. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 265mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 290mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm when the overpotential was 330mV2。
Example 15
The same as in example 1 except that the calcination temperature was changed to heat at 300 deg.C, 500 deg.C, 600 deg.C and 700 deg.C at a temperature-increasing rate of 1.7 deg.C/min for 6h, 6h, 3h and 6h, respectively. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 245mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 270mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 16
The same as in example 1 except that the calcination temperature was changed to heating at a temperature rise rate of 1.5 ℃/min at 500 ℃, 600 ℃ and 700 ℃ for 6 hours, respectively. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 245mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 270mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 17
The same as in example 1 except that the calcination temperature was changed to heating at 600 ℃ and 700 ℃ for 6 hours, respectively, at a temperature-increasing rate of 1 ℃/min. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 245mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 270mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 18
The same as in example 1 except that the calcination temperature was changed to be heated at a temperature rising rate of 1.7 ℃/min from room temperature to 700 ℃ for 6 hours. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 278mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm when the overpotential was 315mV2。
Example 19
Same as example 1 except that the acid-treated 1mol/L hydrochloric acid was changed to 0.5M H2SO4And (3) solution. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the overpotential is 245mV, theThe current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 270mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 20
Same as example 1 except that 1mol/L acid-treated hydrochloric acid was changed to 1M HClO4And (3) solution. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 245mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 270mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm at an overpotential of 300mV2。
Example 21
Same as example 1 except that the acid catalyst electrolyte sulfuric acid (0.5M H)2SO4) Solution was changed to 0.1M HClO4And (3) solution. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 255mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 278mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic block, the material current density reached 10mA/cm when the overpotential was 315mV2。
Example 22
Same as example 1 except that the acid catalyst sulfuric acid (0.5M H)2SO4) Solution was changed to 1M H2SO4And (3) solution. Electrocatalytic performance of the obtained samples: monoclinic phase strontium iridate SrIrO3When the over potential is 240mV, the current density of the material reaches 10mA/cm2(ii) a Strontium orthorhombic Irate SrIrO3When the over potential is 265mV, the current density of the material reaches 10mA/cm2(ii) a Cubic phase Sr2Ir3O8Cubic, when the over-potential is 290mV,the current density of the material reaches 10mA/cm2。
Claims (7)
1. A preparation method of a strontium iridate catalyst comprises the following steps:
(1) preparing a mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naMolar source of iridium, wherein nc：nb：naWhen the ratio is 8: 4: 1. 8: 8: 1. 8: 16: 1 or 8: 24: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid or perchloric acid for 6-10 h, washing with ethanol, and drying to obtain monoclinic phase strontium iridate SrIrO3A catalyst;
or the like, or, alternatively,
(1) preparing a mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naMolar source of iridium, wherein nc：nb：na12-40: 8: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid or perchloric acid for 6-10 h, washing with ethanol,drying to obtain the orthorhombic strontium iridium (SrIrO)3A catalyst;
or the like, or, alternatively,
(1) preparing a mixed solution: weighing ncMolar organic polybasic acid, nbMolar strontium source and naMolar source of iridium, wherein nc：nb：na0-4: 4-10: 1, then adding the mixture into a mixed solution of organic polyol and water, and uniformly mixing;
(2) drying and calcining: drying the mixed solution obtained in the step (1) at 120-200 ℃ for 5-10 h, grinding the dried solid sample into powder, heating at a heating rate of 0.5-5 ℃/min, heating at 120-220 ℃, 230-320 ℃, 330-520 ℃ and 620-720 ℃ for 1-10 h, 2-4 h and 1-10 h respectively, and naturally cooling to room temperature to obtain black powder;
(3) acid treatment: soaking the black powder finally obtained in the step (2) in 0.5-2 mol/L hydrochloric acid, sulfuric acid or perchloric acid for 6-10 h, washing with ethanol, and drying to obtain cubic phase Sr2Ir3O8Cubic piece of catalyst.
2. The method for preparing strontium iridate catalyst of claim 1, wherein: the iridium source is potassium hexachloroiridium (IV), potassium hexachloroiridium (III), iridium chloride, chloroiridic acid or mixtures thereof.
3. The method for preparing strontium iridate catalyst of claim 1, wherein: the strontium source is strontium nitrate, strontium chloride, strontium hydroxide, strontium carbonate or their mixture.
4. The method for preparing strontium iridate catalyst of claim 1, wherein: the organic polyol is ethylene glycol or glycerol.
5. The method for preparing strontium iridate catalyst of claim 1, wherein: the organic polybasic acid is citric acid, tartaric acid or oxalic acid.
6. A strontium iridate catalyst, which is characterized in that: is prepared by the method of any one of claims 1 to 5.
7. Use of the strontium iridate catalyst of claim 6 for the electrocatalytic cleavage of acidic water to produce oxygen.
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