CN110217835A - A kind of PtO2The preparation method of tapered nano-particle material - Google Patents
A kind of PtO2The preparation method of tapered nano-particle material Download PDFInfo
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- CN110217835A CN110217835A CN201910615508.5A CN201910615508A CN110217835A CN 110217835 A CN110217835 A CN 110217835A CN 201910615508 A CN201910615508 A CN 201910615508A CN 110217835 A CN110217835 A CN 110217835A
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 25
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000011591 potassium Substances 0.000 claims abstract description 44
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 44
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 230000007062 hydrolysis Effects 0.000 claims abstract description 18
- 229910019020 PtO2 Inorganic materials 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 230000001788 irregular Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 123
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 35
- 239000007789 gas Substances 0.000 claims description 32
- 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
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 13
- 239000010931 gold Substances 0.000 claims description 13
- 229910052737 gold Inorganic materials 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003556 assay Methods 0.000 claims description 12
- 238000012790 confirmation Methods 0.000 claims description 12
- 239000001103 potassium chloride Substances 0.000 claims description 12
- 235000011164 potassium chloride Nutrition 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 235000013339 cereals Nutrition 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 238000003912 environmental pollution Methods 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 241000416536 Euproctis pseudoconspersa Species 0.000 claims 1
- 240000007594 Oryza sativa Species 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 84
- 238000004458 analytical method Methods 0.000 description 30
- 238000007789 sealing Methods 0.000 description 21
- 238000002347 injection Methods 0.000 description 20
- 239000007924 injection Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 20
- 238000003786 synthesis reaction Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 13
- 238000012545 processing Methods 0.000 description 12
- 238000001069 Raman spectroscopy Methods 0.000 description 11
- 239000005457 ice water Substances 0.000 description 11
- 239000002131 composite material Substances 0.000 description 10
- 238000002386 leaching Methods 0.000 description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- 239000013589 supplement Substances 0.000 description 10
- 238000009423 ventilation Methods 0.000 description 10
- 238000002203 pretreatment Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 241000209094 Oryza Species 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
- 230000035484 reaction time Effects 0.000 description 3
- 229910020437 K2PtCl6 Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 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
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910003446 platinum oxide Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000002322 conducting polymer 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
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 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
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of PtO2The preparation method of tapered nano-particle material, potassium chloroplatinate weak solution is prepared, potassium chloroplatinate weak solution is placed in golden pipe and is sealed, then golden pipe is placed in hydrothermal reaction kettle and is sealed, under the conditions of the temperature and pressure of setting, PtO is prepared by itself hydrolysis2Tapered nano particle, wherein temperature is 200 DEG C~600 DEG C, and pressure is 100Mpa~200Mpa, itself hydrolysis time is 1~48h.The preparation method raw material is easy to get, and at low cost, experimentation is rigorously efficient, and energy consumption is small, the PtO of preparation2Nano particle diameter is dozens to a few hundred nanometers, and has irregular tapered structure, and crystal form is intact.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of PtO2The preparation side of tapered nano-particle material
Method.
Background technique
PtO2As a kind of catalyst material with high activity, obtained in battery electrode, the reaction of various chemical catalysis
Extensive utilization.With the synthesis technology raising and the functional development of nanocomposite of nanocomposite, nanometer-
The route of synthesis and technique of micron order platinum dioxide are more and more paid attention to.
PtO at present2General synthesis technology is to utilize chloroplatinic acid or ammonium chloroplatinate and sodium nitrate the congruent melting system at 500 DEG C
It is standby.This preparation process is prepared by Luo Jie Adams and his student V.Voorhees earliest.Its specific preparation method is
Sodium nitrate is added in 50mL beaker, adds 10% chloroplatinic acid or ammonium chloroplatinate solution, is evaporated to dryness, while constantly stirring
It mixes to avoid mixture partial melting, and sodium nitrate is heated to 500 DEG C in evaporating dish, then disposably add evaporation residue
Enter in sodium nitrate, stops heating, the brownish black platinum oxide finally obtained.It is utilized in the patent of 101712493 A of Publication No. CN
Purified ammonium chloroplatinate with purified sodium nitrate is finely ground respectively remixes, be placed in high temperature furnace and be slowly warming up to 340-360
DEG C, and kept when the temperature constant temperature 1-1.5 hours, it is then cooling to obtain platinum dioxide material.Publication No. CN104900891
The PtO of sub-micron is utilized in the patent of A2Powder and conducting polymer organic carrier are mixed in a certain ratio, grinding prepares platinum guaze
Support platinum oxide electrode material.But current various synthesis PtO2The process is more complicated for material, PtO at high cost, obtained2
Purity is lower.This constrains PtO to a certain extent2Utilization and popularization of the nano-particle material in various industrial catalyst.
Summary of the invention
The purpose of the present invention is to provide a kind of PtO2The preparation method of tapered nano-particle material, the preparation method
Raw material is easy to get, at low cost, and experimentation is rigorously efficient, and energy consumption is small, the PtO of preparation2Nano particle diameter arrives several hundred for tens
Nanometer, and there is irregular tapered structure, crystal form is intact.
Above-mentioned purpose of the invention is achieved by the following technical solution: a kind of PtO2Tapered nano-particle material
Preparation method prepares potassium chloroplatinate weak solution, potassium chloroplatinate weak solution is placed in golden pipe and is sealed, golden pipe is then placed in water
It in thermal response kettle and seals, under the conditions of the temperature and pressure of setting, PtO is prepared by itself hydrolysis2It is tapered to receive
Rice grain, wherein temperature is 200 DEG C~600 DEG C, and pressure is 100Mpa~200Mpa, itself hydrolysis time is 1~48h.
In the PtO2In the preparation method of tapered nano-particle material:
Preferably, itself hydrolysis time is 1~48h, can be effectively observed PtO in the time range2It is tapered to receive
Rice grain crystallization rate and the influence of temperature (200 DEG C~600 DEG C) and pressure (100Mpa~200Mpa) to crystal morphology.
More preferably, when itself hydrolysis, temperature be 400 DEG C~600 DEG C, use argon gas adjust pressure for 100Mpa~
150Mpa, itself hydrolysis time are 20~28h, available partial size and the better PtO of crystal form2Tapered nano particle；Its
Described in itself hydrolysis time do not include heating and cooling time, refer to and carried out under the conditions of the temperature and pressure of setting
Itself hydrolysis time.
Preferably, the potassium chloroplatinate weak solution is by potassium chloroplatinate (K2PtCl6) powder be dissolved in deionized water be made,
Wherein the potassium chloroplatinate powder is purity assay reagent, the concentration of the potassium chloroplatinate weak solution be 0.002mol/L~
0.01mol/L；The 40~50% of the volume Zhan Jinguan total volume of the potassium chloroplatinate weak solution.
Preferably, the PtO2The partial size of tapered nano particle is dozens to a few hundred nanometers, has irregular tapered knot
Structure, crystal form are intact.
Preferably, the gold Guan Jing is boiled, washs and is quenched including truncation, acid, it is ensured that without other impurity shadows in gold pipe
Ring experiment, and the complete seal of guarantee fund's pipe.
Preferably, the golden pipe can be commercially available high-purity gold pipe (purity is about 99.9%).
Preferably, potassium chloroplatinate weak solution is placed in golden pipe and carries out welded seal, then carry out drying weighing, drying is
2h or more is dried in 110 DEG C of drying boxes, is then weighed, it is ensured that front and back quality error is less than 0.001g, with the complete of guarantee fund's pipe
Hermetically sealed and experiment validity.
Preferably, cooling after itself hydrolysis, hydrothermal reaction kettle is then opened, the gold pipe after taking out reaction is broken
Karat gold pipe takes out residual reaction solution in kettle, collects sample, obtains tapered PtO after dry2Nano particle.
Preferably, cooling using ice water is to reaction kettle progress fast cooling cooling or constant pressure cooling is cooled to room temperature or room
Temperature.
Preferably, the gold pipe after taking-up reaction weighs confirmation after clean to pipe progress golden after reaction, dry again and reacted
Whether journey seals completely, and ensures to test the validity carried out.
Preferably, the residual reaction solution includes potassium chloroplatinate, hydrochloric acid and potassium chloride, takes out residual reaction solution in kettle
It is recycled to mitigate environmental pollution.
Residual reaction solution composition is simple, and processing can be recycled, and environmental pollution is smaller.
Preferably, when collecting sample, golden inside pipe wall is respectively impregnated with deionized water and dehydrated alcohol, is washed 2~3 times, is made
It is attached to the PtO of golden inside pipe wall2Sample is clean, then will be attached to the PtO of golden inside pipe wall2Take out simultaneously natural air drying or using baking
Up to tapered PtO after dry ware drying2Nano particle.
A kind of PtO of the invention2The core of the preparation method of tapered nano-particle material is single using potassium chloroplatinate
Hydrolysis of the reagent under different Temperature-pressure Conditions generates PtO2Nano particle, sole agent used are that potassium chloroplatinate is dilute molten
Following hydrolysis occurs for liquid, under hydrothermal conditions, potassium chloroplatinate and water:
K2PtCl6+2H2O=2KCl+PtO2↓+4HCl
Compared with prior art, the present invention has the advantage that
(1) the method for the present invention carries out itself hydrolysis, operating process technique using single agents potassium chloroplatinate weak solution
Succinctly, it is easily manipulated；
(2) the method for the present invention, which makees housing using proof gold pipe, can guarantee that reactant is not reacted with other materials, and can guarantee
The leakproofness and validity of reaction process；
(3) present invention carries out itself hydrolysis using hydrothermal reaction kettle, and at low cost, energy consumption is small；
(4) present invention observes PtO using time series2Nanoparticle growth state change, residual reaction solution composition
Simply, processing can be recycled, environmental pollution is smaller；
(5) the entire process safety of the method for the present invention, environmental protection, and the tapered PtO prepared2Nano-particle material crystal form is complete
It is whole.
Detailed description of the invention
Fig. 1 is to prepare PtO in 1-10 of the embodiment of the present invention2Tapered nano-particle material LR laser raman map；
Fig. 2 is to prepare PtO in 1-5 of the embodiment of the present invention2The stereoscan photograph of tapered nano particle, (a) are real
It applies and prepares unformed PtO in example 12Nano particle (b) is to prepare unformed PtO in embodiment 22Nano particle, (c)
To prepare tapered PtO in embodiment 32Nano particle (d) is to prepare tapered PtO in embodiment 42Nano particle, (e-
It f) is to prepare tapered PtO in embodiment 52Nano particle；
Fig. 3 is to prepare PtO in 6-10 of the embodiment of the present invention2The stereoscan photograph of tapered nano particle, (a) are real
It applies and prepares unformed PtO in example 62Nano particle (b) is to prepare tapered PtO in embodiment 72Nano particle (c) is
Tapered PtO is prepared in embodiment 82Nano particle (d) is to prepare tapered PtO in embodiment 92Nano particle, (e-f)
To prepare tapered PtO in embodiment 102Nano particle.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is further illustrated, but the scope of protection of present invention is for example anti-
Device and the volume of reaction temperature, reaction time and reaction liquid is answered to be not limited to the embodiment and lifted.
Embodiment 1
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) by diameter be 4mm high-purity gold pipe be truncated into experiment needed for length and carry out acid boil, wash, quench with
And one end shifts to an earlier date the pre-processings such as sealing, it is ensured that gold manages interior free from admixture and crack；
(2) by the potassium chloroplatinate (K of 0.486g purity assay2PtCl6) powder is dissolved in 100mL deionized water, sufficiently dissolve
0.01mol/L K is made2PtCl6The reaction solution of preparation is taken about 0.1mL to put into golden pipe by solution, and compactedness control is 40%
~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry case 2h or more, after weighed again, it is ensured that front and back weigh quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and carry out reaction 1h under Temperature-pressure Conditions, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the unformed PtO of Fig. 2 (a) stereoscan photograph display synthesis2Nanometer
Particle, nucleus are begun to show, and crystal form is imperfect；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 2
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.486g purity assay2PtCl6) powder is dissolved in 100mL deionized water, sufficiently dissolve
0.01mol/L K is made2PtCl6The reaction solution of preparation is taken about 0.1mL to put into golden pipe by solution, and compactedness control is 40%
~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry case 2h or more, after weighed again, it is ensured that front and back weigh quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and carry out reaction 6h under Temperature-pressure Conditions, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the unformed PtO of Fig. 2 (b) stereoscan photograph display synthesis2Nanometer
Particle, crystal form is imperfect, and particle is in chain-like growth；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 3
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.486g purity assay2PtCl6) powder is dissolved in 100mL deionized water, sufficiently dissolve
0.01mol/L K is made2PtCl6The reaction solution of preparation is taken about 0.1mL to put into golden pipe by solution, and compactedness control is 40%
~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry case 2h or more, after weighed again, it is ensured that front and back weigh quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and carry out reaction 9h under Temperature-pressure Conditions, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the preliminary tapered PtO of Fig. 2 (c) stereoscan photograph display synthesis2It receives
Rice grain, crystal form are more complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 4
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.486g purity assay2PtCl6) powder is dissolved in 100mL deionized water, sufficiently dissolve
0.01mol/L K is made2PtCl6The reaction solution of preparation is taken about 0.1mL to put into golden pipe by solution, and compactedness control is 40%
~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry case 2h or more, after weighed again, it is ensured that front and back weigh quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 2 (d) stereoscan photograph display synthesis2Nanometer
Grain, crystal form are complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 5
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.486g purity assay2PtCl6) powder is dissolved in 100mL deionized water, sufficiently dissolve
0.01mol/L K is made2PtCl6The reaction solution of preparation is taken about 0.1mL to put into golden pipe by solution, and compactedness control is 40%
~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry case 2h or more, after weighed again, it is ensured that front and back weigh quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and carry out reaction 48h under Temperature-pressure Conditions, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 2 (e-f) stereoscan photograph display synthesis2Nanometer
Particle, crystal form are complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 6
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.0972g purity assay2PtCl6) powder is dissolved in 100mL deionized water, it is sufficiently molten
It solves and 0.002mol/L K is made2PtCl6Solution, takes about 0.1mL to put into golden pipe the reaction solution of preparation, and compactedness control is
40%~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110
DEG C drying box 2h or more, after weighed again, it is ensured that front and back weighs quality error and is less than 0.001g, illustrates that golden composite pipe tightness is complete
It is good；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (b) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the unformed PtO of Fig. 3 (a) stereoscan photograph display synthesis2Nanometer
Particle, nucleus are begun to show, and crystal form is imperfect；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 7
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.0972g purity assay2PtCl6) powder is dissolved in 100mL deionized water, it is sufficiently molten
It solves and 0.002mol/L K is made2PtCl6Solution, takes about 0.1mL to put into golden pipe the reaction solution of preparation, and compactedness control is
40%~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110
DEG C drying box 2h or more, after weighed again, it is ensured that front and back weighs quality error and is less than 0.001g, illustrates that golden composite pipe tightness is complete
It is good；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 300 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (c) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 3 (b) stereoscan photograph display synthesis2Nanometer
Grain, crystal form are more complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 8
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.0972g purity assay2PtCl6) powder is dissolved in 100ml deionized water, it is sufficiently molten
It solves and 0.002mol/L K is made2PtCl6Solution, takes about 0.1ml to put into golden pipe the reaction solution of preparation, and compactedness control is
40%~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110
DEG C drying box 2h or more, after weighed again, it is ensured that front and back weighs quality error and is less than 0.001g, illustrates that golden composite pipe tightness is complete
It is good；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 400 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (d) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 3 (c) stereoscan photograph display synthesis2Nanometer
Grain, crystal form are more complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 9
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.0972g purity assay2PtCl6) powder is dissolved in 100mL deionized water, it is sufficiently molten
It solves and 0.002mol/L K is made2PtCl6Solution, takes about 0.1mL to put into golden pipe the reaction solution of preparation, and compactedness control is
40%~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110
DEG C drying box 2h or more, after weighed again, it is ensured that front and back weighs quality error and is less than 0.001g, illustrates that golden composite pipe tightness is complete
It is good；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 500 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (e) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 3 (d) stereoscan photograph display synthesis2Nanometer
Grain, crystal form are complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
Embodiment 10
PtO provided in this embodiment2The preparation method of tapered nano particle, comprising the following steps:
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium chloroplatinate (K of 0.0972g purity assay2PtCl6) powder is dissolved in 100mL deionized water, it is sufficiently molten
It solves and 0.002mol/L K is made2PtCl6Solution, takes about 0.1mL to put into golden pipe the reaction solution of preparation, and compactedness control is
40%~50% or so, and sealing is carried out, weighing record is carried out after sealing, and the golden pipe equipped with solution example is then put into 110
DEG C drying box 2h or more, after weighed again, it is ensured that front and back weighs quality error and is less than 0.001g, illustrates that golden composite pipe tightness is complete
It is good；
(3) will confirm that the intact and golden pipe equipped with solution example of leakproofness puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water is as medium, after tightening reaction kettle, checks the leakproofness of reaction kettle, confirms that the errorless rear ventilation pipe that passes through is injected into kettle
Argon gas closes shut-off valve and stops gas injection, heated by heating furnace to reaction kettle to pressure 60MPa as initial pressure, if
Setting reaction temperature is 200 DEG C；
(4) temperature rises to after 600 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, reaction kettle in leaching step (3), which is poured, using ice water after the reaction was completed carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (3) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes the PtO for being attached to golden inside pipe wall2Sample is clean, then deposit sample air-dried with natural wind or
Tapered PtO can be obtained after drying ware drying in person2Nano particle；
(6) by the tapered PtO of acquisition2Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (f) is laser drawing
It is graceful analysis shows that tapered PtO obtained2Nano particle, the tapered PtO of Fig. 3 (e-f) stereoscan photograph display synthesis2Nanometer
Particle, crystal form are complete；
(7) residual solution this be mainly potassium chloroplatinate, hydrochloric acid and potassium chloride, all recyclable processing of this solution, and to environment
Less pollution.
From above embodiments, it can be deduced that obtain preferable PtO2The experimental temperature of tapered nano particle diameter and crystal form is
400 DEG C~600 DEG C, pressure is 100Mpa~150Mpa and the reaction time is 20~28h.The above preferred temperature, pressure and reaction
Time obtains according only to the above-mentioned experiment of the application, if you need to advanced optimize experiment condition and inquire into the PtO under different experimental conditions2
Nano particle crystal form variation, it is also necessary to which further refinement experiment condition is discussed.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included in protection scope of the present invention.
Claims (10)
1. a kind of PtO2The preparation method of tapered nano-particle material, it is characterized in that: potassium chloroplatinate weak solution is prepared, by chloroplatinic acid
Potassium weak solution is placed in golden pipe and seals, and then golden pipe is placed in hydrothermal reaction kettle and is sealed, in the temperature and pressure of setting
Under the conditions of, PtO is prepared by itself hydrolysis2Tapered nano particle, wherein temperature is 200 DEG C~600 DEG C, and pressure is
100Mpa~200Mpa, itself hydrolysis time are 1~48h.
2. PtO according to claim 12The preparation method of tapered nano-particle material, it is characterized in that: when itself hydrolysis,
Temperature is 400 DEG C~600 DEG C, and argon gas is used to adjust pressure as 100Mpa~150Mpa, itself hydrolysis time for 20~
28h；Wherein itself hydrolysis time does not include the time of heating and cooling, refers to the temperature and pressure condition in setting
Lower itself hydrolysis time of progress.
3. PtO according to claim 1 or claim 22The preparation method of tapered nano-particle material, it is characterized in that: the potassium chloroplatinate
Weak solution be potassium chloroplatinate powder is dissolved in deionized water be made, wherein the potassium chloroplatinate powder be purity assay reagent,
The concentration of the potassium chloroplatinate weak solution is 0.002mol/L~0.01mol/L；The volume of the potassium chloroplatinate weak solution accounts for gold
The 40~50% of pipe total volume.
4. PtO according to claim 32The preparation method of tapered nano-particle material, it is characterized in that: the PtO2It is tapered to receive
The partial size of rice grain is dozens to a few hundred nanometers, and with irregular tapered structure, crystal form is intact.
5. PtO according to claim 12The preparation method of tapered nano-particle material, it is characterized in that: the gold Guan Jing includes
It truncates, acid is boiled, washs and is quenched, it is ensured that tested in gold pipe without other impurity effects, and the complete seal of guarantee fund's pipe.
6. PtO according to claim 12The preparation method of tapered nano-particle material, it is characterized in that: potassium chloroplatinate is dilute molten
Liquid, which is placed in golden pipe, carries out welded seal, then carries out drying weighing, and drying is the drying 2h or more in 110 DEG C of drying boxes, so
After weigh, it is ensured that front and back quality error be less than 0.001g, with the validity for being fully sealed and testing of guarantee fund's pipe.
7. PtO according to claim 12The preparation method of tapered nano-particle material, it is characterized in that: itself hydrolysis knot
It is cooling after beam, hydrothermal reaction kettle is then opened, the gold pipe after taking out reaction breaks golden pipe, takes out residual reaction solution in kettle, receives
Collect sample, obtains tapered PtO after dry2Nano particle.
8. PtO according to claim 72The preparation method of tapered nano-particle material, it is characterized in that: taking out the gold after reaction
Pipe weighs whether confirmation reaction process seals completely after carrying out clean, drying to pipe golden after reaction again, and ensures to test to carry out
Validity.
9. PtO according to claim 72The preparation method of tapered nano-particle material, it is characterized in that: the residual reaction is molten
Liquid includes potassium chloroplatinate, hydrochloric acid and potassium chloride, takes out residual reaction solution in kettle and is recycled to mitigate environmental pollution.
10. PtO according to claim 72The preparation method of tapered nano-particle material, it is characterized in that: being used when collecting sample
Golden inside pipe wall is respectively impregnated, is washed 2~3 times by deionized water and dehydrated alcohol, makes the PtO for being attached to golden inside pipe wall2Sample is clean,
Then the PtO of golden inside pipe wall will be attached to2Up to tapered PtO after taking out simultaneously natural air drying or being dried using drying ware2Nanometer
Grain.
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| 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 |
| CN113697871A (en) * | 2021-08-04 | 2021-11-26 | 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 |
| 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 |
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