CN101696027B - Cubic copper oxide nano particle and synthesizing method and application thereof - Google Patents
Cubic copper oxide nano particle and synthesizing method and application thereof Download PDFInfo
- Publication number
- CN101696027B CN101696027B CN2009102725461A CN200910272546A CN101696027B CN 101696027 B CN101696027 B CN 101696027B CN 2009102725461 A CN2009102725461 A CN 2009102725461A CN 200910272546 A CN200910272546 A CN 200910272546A CN 101696027 B CN101696027 B CN 101696027B
- Authority
- CN
- China
- Prior art keywords
- copper oxide
- nano particle
- oxide nano
- aqueous solution
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention relates to a cubic copper oxide nano particle and a preparation method and application thereof. The method comprises the following steps: uniformly mixing copper acetate aqueous solution, sodium hydroxide tetraglycol solution and polyvinylpyrrolidone aqueous solution by a microwave as a heating medium; heating by the microwave by stirring till the color of the solution is changed into transparent dark brown; and then obtaining the cubic copper oxide nano particle. The method has simple experiment process without complicated and rigorous process condition, and the obtained product can be used for preparing an air-sensitive element.
Description
One, technical field
The present invention relates to cubic copper oxide nano particle and its production and use.
Two, background technology
Common cupric oxide is a kind of broad-spectrum multi-functional meticulous inorganic materials, is mainly used in fields such as printing and dyeing, glass, pottery, medicine and catalysis.When the particle diameter of common copper oxide particle reaches nano level, will make its function unique more, use more extensive.Generally adopt at present liquid-phase precipitation technology, sonochemistry method, pressure-hydrothermal method, microemulsion method, the laser of solid reaction process, hydrothermal method, pure hot method, the precipitator method, spray pyrolysis, control dual-jet to steam the method for coagulating, microwave boiling reflux, electrochemical process, template etc., but all have a lot of problems to wait to solve.The first, synthesis condition is relatively harsher, and temperature requirement needs technologies such as calcining than higher.The second, be difficult to synthesize the clear and definite copper oxide nano particle of shape.
Three, summary of the invention
The objective of the invention is at above-mentioned present situation, it is simple to aim to provide a kind of synthesis technique, safe and reliable, and non-environmental-pollution, product are cubical copper oxide nano particle and uses thereof.
Technical scheme provided by the invention is: copper oxide nano particle, the pattern of described copper oxide nano particle is cubes.
The preparation method of above-mentioned copper oxide nano particle: with the microwave is that heating medium is even with the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution and polyvinylpyrrolidone (PVP) aqueous solution, stop microwave heating after microwave heating to solution colour becomes bright dark-brown under stirring, promptly obtain cubic copper oxide nano particle.
The concentration of the described neutralized verdigris aqueous solution is 0.01-0.08moldm
-3, the concentration of sodium hydroxide tetraethylene-glycol solution is 0.02-0.10moldm
-3, the concentration of the polyvinylpyrrolidone aqueous solution is 0.05-0.60moldm
-3, described microwave heating power is 300-500 watt, be 30-150s heat-up time.
Neutralized verdigris in the above-mentioned neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution and the polyvinylpyrrolidone aqueous solution: sodium hydroxide: the mol ratio of polyvinylpyrrolidone is 1～2: 2～4: 1～10.
Cubic copper oxide nano particle of the present invention can be used for preparing gas sensor.
The present invention has avoided using the reaction conditions of heat, reaction times was brought up to rapidly in 3 minutes, is not introduced any impurity, to reactant and product without any need for processing, synthesis technique is simple, safe and reliable, does not have any danger and environmental pollution.
Four, description of drawings
Fig. 1 is the x-ray diffraction pattern of product of the present invention;
Fig. 2 is the transmission electron microscope picture of product of the present invention; The transmission electron microscope picture of the single cubic copper oxide nano particle of transmission electron microscope picture (b) of (a) some cubic copper oxide nano particles wherein.
Five, embodiment
The present invention is according to mol ratio Cu (OAc) in the 50ml round-bottomed flask
2: NaOH: PVP is 1～2: 2～4: add the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution under 1～10 condition successively, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, the power with 500～1000 watts under stirring heats 30～150s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtain cubic copper oxide nano particle.
To obtain cubic copper oxide nano particle and place mortar, adding deionized water fully grinds, after becoming pasty state, be coated in (outside diameter d=1.35mm on the vitrified pipe that has gold electrode, length 1=4mm), sintering 2h under 500 ℃ of high temperature penetrates Ni-Cr alloy heater strip (d=0.5mm then in vitrified pipe in retort furnace, R=35 Ω), promptly be made into sintered type heater-type gas sensor.
The present invention with microwave for being heated to be supplementary means, prepare cubic copper oxide nano particle with the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, PVP aqueous solution and controlling reaction time, do not introduce any impurity, to reactant and product without any need for processing, synthesis technique is simple, reaction times shortens greatly, and safe and reliable, does not have any danger and environmental pollution.It is controlled that the present invention especially adopts sodium hydroxide tetraethylene-glycol solution and the PVP aqueous solution to make to be prepared into the copper oxide nano particle pattern.
With reference to Fig. 1,2, the applicant has made X-ray diffraction, TEM (transmission electron microscope) analysis with synthetic products C uO of the present invention, proves that the product that the present invention produces is copper oxide nano particle and is shaped as cubes.
Enumerate the specific embodiment of the invention below:
Example one, in the 50ml round-bottomed flask according to mol ratio Cu (CH
3COO)
2: NaOH: PVP condition under successively adds the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution at 1: 2: 10, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, stir down with 800 watts of power heating 20s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtain the cubic copper oxide nano particle that median size is 41nm.
Example two, in the 50ml round-bottomed flask according to mol ratio Cu (CH
3COO)
2: NaOH: PVP adds the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution under 1: 1: 5 the condition successively, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, stir down with 850 watts of power heating 65s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtain the cubic copper oxide nano particle that median size is 88nm.
Example three, in the 50ml round-bottomed flask according to mol ratio Cu (CH
3COO)
2: NaOH: PVP adds the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution under 2: 1: 10 the condition successively, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, stir down with 950 watts of power heating 120s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtain the cubic copper oxide nano particle that particle diameter is 140nm.
Example four, in the 50ml round-bottomed flask according to mol ratio Cu (CH
3COO)
2: NaOH: PVP condition under successively adds the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution at 1: 2: 10, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, stir down with 1000 watts of power heating 100s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtain the copper oxide nano particle that median size is a 110nm cubes pattern.
Example five, in the 50ml round-bottomed flask according to mol ratio Cu (CH
3COO)
2: NaOH: PVP condition under successively adds the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution, the PVP aqueous solution at 1: 2: 8, keep cumulative volume at 15ml, mix the back and form the light blue solution of homogeneous, insert then in the microwave oven, stir down with 900 watts of power heating 120s.Treat to stop microwave heating after solution colour becomes bright dark-brown.Promptly obtaining median size is the 92nm cubic copper oxide nano particle.
Example six, example one prepared cubic copper oxide nano particle is placed mortar, adding deionized water fully grinds, after becoming pasty state, be coated in (outside diameter d=1.35mm on the vitrified pipe that has gold electrode, length 1=4mm), sintering 2h under 500 ℃ of high temperature penetrates Ni-Cr alloy heater strip (d=0.5mm then in vitrified pipe in retort furnace, R=35 Ω), promptly be made into sintered type heater-type gas sensor. with the gas sensor characteristic tester air-sensitive performance of this element is tested.When working current was 180mA, the formaldehyde gas volume fraction was 300 * 10
-6The time, the sensitivity of element is 8.5, and the time of response is 10s, and be 12s time of recovery.
Example seven, example five prepared cubic copper oxide nano particles are placed mortar, adding deionized water fully grinds, after becoming pasty state, be coated in (outside diameter d=1.35mm on the vitrified pipe that has gold electrode, length 1=4mm), sintering 2h under 500 ℃ of high temperature penetrates Ni-Cr alloy heater strip (d=0.5mm then in vitrified pipe in retort furnace, R=35 Ω), promptly be made into sintered type heater-type gas sensor. with the gas sensor characteristic tester air-sensitive performance of this element is tested.When working current was 180mA, the formaldehyde gas volume fraction was 300 * 10
-6The time, the sensitivity of element is 7.4, and the time of response is 10s, and be 10s time of recovery.
Example eight, example one prepared cubic copper oxide nano particle is placed mortar, adding deionized water fully grinds, after becoming pasty state, be coated in (outside diameter d=1.35mm on the vitrified pipe that has gold electrode, length 1=4mm), sintering 2h under 500 ℃ of high temperature penetrates Ni-Cr alloy heater strip (d=0.5mm then in vitrified pipe in retort furnace, R=35 Ω), promptly be made into sintered type heater-type gas sensor. with the gas sensor characteristic tester air-sensitive performance of this element is tested.When working current was 180mA, the ammonia gas volume fraction was 300 * 10
-6The time, the sensitivity of element is 3.5, and the time of response is 11s, and be 10s time of recovery.
Example nine, example one prepared cubic copper oxide nano particle is placed mortar, adding deionized water fully grinds, after becoming pasty state, be coated in (outside diameter d=1.35mm on the vitrified pipe that has gold electrode, length 1=4mm), sintering 2h under 500 ℃ of high temperature penetrates Ni-Cr alloy heater strip (d=0.5mm then in vitrified pipe in retort furnace, R=35 Ω), promptly be made into sintered type heater-type gas sensor. with the gas sensor characteristic tester air-sensitive performance of this element is tested.When working current was 180mA, the CO (carbon monoxide converter) gas volume fraction was 300 * 10
-6The time, the sensitivity of element is 1.8, and the time of response is 13s, and be 9s time of recovery.
Claims (5)
1. copper oxide nano particle, it is characterized in that: the pattern of copper oxide nano particle is cubes, and make: be heating medium with the microwave by laxative remedy, the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution and polyvinylpyrrolidone aqueous solution is even, stop microwave heating after microwave heating to solution colour becomes bright dark-brown under stirring, promptly obtain cubic copper oxide nano particle.
2. the preparation method of the described copper oxide nano particle of claim 1, it is characterized in that: be heating medium with the microwave, the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution and polyvinylpyrrolidone aqueous solution is even, stop microwave heating after microwave heating to solution colour becomes bright dark-brown under stirring, promptly obtain cubic copper oxide nano particle.
3. preparation method according to claim 2 is characterized in that: the concentration of the described neutralized verdigris aqueous solution is 0.01-0.08moldm
-3, the concentration of sodium hydroxide tetraethylene-glycol solution is 0.02-0.10moldm
-3, the concentration of the polyvinylpyrrolidone aqueous solution is 0.05-0.60moldm
-3, described microwave heating power is 300-500 watt, be 30-150s heat-up time.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: neutralized verdigris in the neutralized verdigris aqueous solution, sodium hydroxide tetraethylene-glycol solution and the polyvinylpyrrolidone aqueous solution: sodium hydroxide: the mol ratio of polyvinylpyrrolidone is 1～2: 2～4: 1～10.
5. the described cubic copper oxide nano particle of claim 1 is used to prepare gas sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102725461A CN101696027B (en) | 2009-10-27 | 2009-10-27 | Cubic copper oxide nano particle and synthesizing method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102725461A CN101696027B (en) | 2009-10-27 | 2009-10-27 | Cubic copper oxide nano particle and synthesizing method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101696027A CN101696027A (en) | 2010-04-21 |
| CN101696027B true CN101696027B (en) | 2011-11-30 |
Family
ID=42141169
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102725461A Expired - Fee Related CN101696027B (en) | 2009-10-27 | 2009-10-27 | Cubic copper oxide nano particle and synthesizing method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101696027B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407343B (en) * | 2011-11-11 | 2013-05-22 | 华东师范大学 | Method for synthesizing copper nanoparticles |
| CN103232056B (en) * | 2013-04-10 | 2015-04-15 | 廖勇志 | Method of preparing copper oxide |
| CN105347382B (en) * | 2015-12-10 | 2017-06-23 | 济南大学 | A kind of preparation method of garland shape copper oxide nano material |
| CN107583648B (en) * | 2017-09-08 | 2020-12-22 | 华南理工大学 | Non-noble metal CoxCuyFezOH nanosphere electrocatalyst and preparation method thereof |
| CN107694571B (en) * | 2017-09-08 | 2020-07-28 | 华南理工大学 | Non-noble metal NixCuyFezO nanosphere electrocatalyst and preparation method thereof |
| CN109632894B (en) * | 2019-01-11 | 2021-05-14 | 东北大学 | Noble metal in-situ co-doped CuO-based NO2Preparation and application of gas-sensitive material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134245A (en) * | 2006-08-29 | 2008-03-05 | 三星电机株式会社 | Method for manufacturing cubic copper or copper oxide nanoparticles |
-
2009
- 2009-10-27 CN CN2009102725461A patent/CN101696027B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134245A (en) * | 2006-08-29 | 2008-03-05 | 三星电机株式会社 | Method for manufacturing cubic copper or copper oxide nanoparticles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101696027A (en) | 2010-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101696027B (en) | Cubic copper oxide nano particle and synthesizing method and application thereof | |
| Kitchen et al. | Modern microwave methods in solid-state inorganic materials chemistry: From fundamentals to manufacturing | |
| CN101956119B (en) | Preparation method of prealloying powder for dispersion strengthening metal by low-temperature combustion synthesis method | |
| CN102040203B (en) | Preparation method and application of nano nickel phosphide | |
| CN102892533A (en) | Process for production of nickel nanoparticles | |
| CN105727959A (en) | Method for preparing methanol synthesis catalyst by using microchannel reactor | |
| CN108580917B (en) | Method for preparing tungsten dispersion strengthening copper superfine powder by low-temperature combustion synthesis | |
| CN1443811A (en) | Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method | |
| CN101597472A (en) | A kind of method of utilizing copper iron tailings relieving haperacidity burning slag to prepare ferriferrous oxide microwave adsorbing material | |
| CN106082287A (en) | A kind of preparation method of magnesium oxide | |
| CN112745105B (en) | High-sintering-activity alumina ceramic powder and preparation method thereof | |
| CN110124678A (en) | The Fe prepared using waste silicon molybdenum rod2(MoO4)3/MoO3Catalysis material, method and its application | |
| CN104162682B (en) | The preparation method of a kind of silicon solar cell front silver electrode silver powder | |
| CN101224903A (en) | Method for preparing cerium dioxide nano cubic block | |
| CN107262095A (en) | The preparation method of Copper-cladding Aluminum Bar graphen catalyst | |
| CN101746826A (en) | Method for preparing niobium pentoxide hollow nanosphere | |
| CN101768015B (en) | Black nanophase ceramics pigment and preparation method thereof | |
| CN105693246B (en) | A kind of preparation method of yttrium oxide transparent ceramic | |
| CN106744741A (en) | A kind of Fe2O3 doping titanium nitride nano pipe and its preparation method and application | |
| CN110339852A (en) | A kind of CoO@nitrogen sulphur codope carbon material/CdS composite photocatalyst material, preparation method and applications | |
| CN101224883A (en) | Method for preparing hollow carbon balls | |
| CN100398453C (en) | Method of burning gel of stearic acid for preparing Nano LaCo03 in type of perovskite | |
| CN104760947B (en) | Carbon coated Fe3O4 composite material and preparation method thereof | |
| CN104743610B (en) | A kind of liquid-phase precipitation method prepares the method for nano bismuth oxide | |
| CN102513543A (en) | Microwave heating reduction technology for preparing superfine silver powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111130 Termination date: 20141027 |
|
| EXPY | Termination of patent right or utility model |