CN107311220B - A kind of cupric oxide powder and preparation method thereof - Google Patents
A kind of cupric oxide powder and preparation method thereof Download PDFInfo
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- CN107311220B CN107311220B CN201710551347.9A CN201710551347A CN107311220B CN 107311220 B CN107311220 B CN 107311220B CN 201710551347 A CN201710551347 A CN 201710551347A CN 107311220 B CN107311220 B CN 107311220B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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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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Abstract
The invention discloses a kind of cupric oxide powders and preparation method thereof.The preparation method of the cupric oxide powder includes: directly to carry out atomization process to the copper of molten condition by pure copper smelting to molten condition, and in oxygen atmosphere, make copper and oxygen occur it is fully oxidized react, obtain cupric oxide powder.The preparation method of cupric oxide powder provided by the invention is when producing cupric oxide powder using atomization, it is passed through purity oxygen, aoxidizes fine copper and oxygen in atomization process high temperature, cupric oxide powder is made, production stage has been saved, the production method of cupric oxide powder has been widened；And obtained cupric oxide powder partial size is relatively concentrated, and is evenly distributed, is had excellent performance.
Description
Technical field
The present invention relates to a kind of preparation method of cupric oxide powder more particularly to a kind of cupric oxide powder and its preparation sides
Method belongs to technology of metal powder field.
Background technique
Gas atomization is the method for directly smashing liquid metals or alloy and powder being made, and application is relatively broad, production rule
Mould is only second to reduction method, can produce the metal powders such as lead, tin, aluminium, zinc, copper, iron, nickel, can also produce pre-alloyed powder.
It is had excellent performance by the metal powder that gas atomization is produced, even particle size distribution, powder apperance is subsphaeroidal, and tissue is thin
Small, ingredient is uniform.
Copper oxide has extensive purposes, in addition to as the raw material of mantoquita processed, is also widely used for other field, especially
In electronics and IT products, such as mobile phone, computer Related product integrated circuit connection is in great demand；And as enamel, ceramics
Consumption in terms of colorant also has preferable market manifestation, and demand is steady.Therefore, China for copper oxide demand size just by
Year expands.
Copper oxide is mainly produced by dry and wet at present, these methods are seriously polluted, and process is complex,
Produce that material required for copper oxide is more, and the uniformity of copper oxide and powder shape cannot be guaranteed, and influence whether oxygen
Change copper powders subsequent use.
Summary of the invention
The main purpose of the present invention is to provide a kind of cupric oxide powders and preparation method thereof, in the prior art to overcome
It is insufficient.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of preparation methods of cupric oxide powder comprising:
Atomization process is directly carried out to the copper of molten condition by pure copper smelting to molten condition, and in oxygen atmosphere, is made
Copper and oxygen occur it is fully oxidized react, obtain cupric oxide powder.
One of preferably, the temperature of the melting is 1400~1500 DEG C, and keeps the temperature 20~30min.
One of preferably, when carrying out atomization process, the pressure of the oxygen is 1.5~2.5MPa.
The embodiment of the invention also provides the cupric oxide powders prepared by preceding method.
One of preferably, the cupric oxide powder is regular shape or irregular shape.
Preferably, the regular shape includes round and/or ellipse.
Preferably, the partial size of the cupric oxide powder is less than 60 μm, and preferably 15~45 μm.
It is wherein preferred, in the cupric oxide powder partial size in 2~15 μm of accounting in 10~15wt%, partial size 20~
35 μm of accounting is in 20~25wt%, and partial size is in 45~60 μm of accounting in 20~25wt%.
Compared with prior art, advantages of the present invention at least that: the preparation method of cupric oxide powder provided by the invention
When producing cupric oxide powder using atomization, it is passed through purity oxygen, aoxidizes fine copper and oxygen in atomization process high temperature, is made
Cupric oxide powder.Present invention production is efficient and convenient quick, has saved production stage, has widened the production method of cupric oxide powder,
It is more competitive；And it is relatively concentrated, is evenly distributed by the obtained cupric oxide powder partial size of preparation method of the invention, object
Reason is had excellent performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the cupric oxide powder among a typical embodiments of the invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of the cupric oxide powder among another typical embodiments of the present invention.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention
Technical solution mainly directly fills pure oxygen with liquid copper using atomization and obtains cupric oxide powder.
The technical solution, its implementation process and principle etc. will be further explained as follows.
A kind of preparation method for cupric oxide powder that the one aspect of the embodiment of the present invention provides comprising:
Atomization process is directly carried out to the copper of molten condition by pure copper smelting to molten condition, and in oxygen atmosphere, is made
Copper and oxygen occur it is fully oxidized react, obtain cupric oxide powder.
One of preferably, the temperature of the melting is 1400~1500 DEG C, and keeps the temperature 20~30min.
One of preferably, when carrying out atomization process, the pressure of the oxygen is 1.5~2.5MPa.In certain model
In enclosing, pressure is bigger, and powder can be made broken more thoroughly, obtain more tiny powder.The oxygen pressure used in the production process
It is strong too low, it on the one hand may result in cupric oxide powder oxidation and be not thorough, it is also possible to it is too small to will lead to negative nozzle pressure area suction,
Increase the risk of stifled furnace.When the oxygen pressure used in the production process is excessive, atomization may result in a flash, in furnace body
Pressure moment become positive pressure, air-introduced machine has little time that safety accident will can be caused when gas is discharged in furnace body.In addition to safety with
Outside, when pressure is excessive, high speed oxygen stream is very big on the influence of the temperature of nozzle, may result in nozzle temperature reduction, is not achieved
Atomization temperature causes copper water to solidify in diversion pipe, leads to stifled furnace.
One of preferably, the mist droplet particle size that the atomization process uses is 15~53 μm.
Preferably, the cupric oxide powder is regular shape or irregular shape.
Further, the regular shape includes round and/or ellipse.
Preferably, the partial size of the cupric oxide powder is less than 60 μm, and preferably 15~45 μm.
It is wherein preferred, in the cupric oxide powder partial size in 2~15 μm of accounting in 10~15wt%, partial size 20~
35 μm of accounting is in 20~25wt%, and partial size is in 45~60 μm of accounting in 20~25wt%.
Wherein, in some more typical embodiments, the preparation method is specifically included:
(1) fine copper is placed in gas-atomized powder equipment, being warming up to 1400~1500 DEG C makes copper weld pool to molten condition, and
Keep the temperature 20~30min；
(2) it is passed through oxygen into gas-atomized powder equipment, to molten in the oxygen atmosphere that pressure is 1.5~2.5MPa
The copper of state carries out atomization process, make copper and oxygen occur it is fully oxidized react, cupric oxide powder is obtained, from powder collecting pot collection powder
?.
The cupric oxide powder prepared by preceding method that the other side of the embodiment of the present invention provides.
Preferably, the cupric oxide powder is regular shape or irregular shape.
Further, the regular shape includes round and/or ellipse, but not limited to this.
Preferably, the partial size of the cupric oxide powder is less than 60 μm, and preferably 15~45 μm.
It is wherein preferred, in the cupric oxide powder partial size in 2~15 μm of accounting in 10~15wt%, partial size 20~
35 μm of accounting is in 20~25wt%, and partial size is in 45~60 μm of accounting in 20~25wt%.
In conclusion the preparation method of cupric oxide powder provided by the invention exists by above-mentioned technical proposal of the invention
When producing cupric oxide powder using atomization, it is passed through purity oxygen, aoxidizes fine copper and oxygen in atomization process high temperature, oxygen is made
Change copper powders.Present invention production is efficient and convenient quick, has saved production stage, has widened the production method of cupric oxide powder, more
With competitiveness；And it is relatively concentrated, is evenly distributed by the obtained cupric oxide powder partial size of preparation method of the invention, physics
It has excellent performance.
Below by way of several embodiments technical solution that present invention be described in more detail.However, selected embodiment is only
For illustrating the present invention, and do not limit the scope of the invention.
Embodiment 1
The method for preparing cupric oxide powder of the present embodiment the following steps are included:
A. fine copper raw material is put into gas-atomized powder equipment, first by fine copper heating and thermal insulation, then in 1400 DEG C of meltings
To molten state, powder by atomization equipment is can be obtained by the approach such as commercially available, does not do excessive detailed description herein.
B. the pure copper material of molten state is atomized, is passed through pure oxygen gas, copper oxide is made in gas pressure intensity 1.5MPa
Powder, scanning electron microscope (SEM) photograph see Fig. 2, and partial size is 45~60 microns.
Embodiment 2
The method for preparing cupric oxide powder of the present embodiment the following steps are included:
A. fine copper raw material is put into gas-atomized powder equipment, first by fine copper heating and thermal insulation, then in 1500 DEG C of meltings
To molten state, powder by atomization equipment is can be obtained by the approach such as commercially available, does not do excessive detailed description herein.
B. the pure copper material of molten state is atomized, is passed through pure oxygen gas, cupric oxide powder is made in gas pressure intensity 2MPa
End, scanning electron microscope (SEM) photograph see Fig. 2, and partial size is 20~35 microns.
Embodiment 3
The method for preparing cupric oxide powder of the present embodiment the following steps are included:
A. fine copper raw material is put into gas-atomized powder equipment, first by fine copper heating and thermal insulation, then in 1450 DEG C of meltings
To molten state, powder by atomization equipment is can be obtained by the approach such as commercially available, does not do excessive detailed description herein.
B. the pure copper material of molten state is atomized, is passed through pure oxygen gas, copper oxide is made in gas pressure intensity 2.5MPa
Powder, scanning electron microscope (SEM) photograph see Fig. 1, and partial size is 2~15 microns.
Reference examples 1
This reference examples prepares cupric oxide powder, specific steps using chemical precipitation method are as follows: copper mixed with bases solution,
Kocide SD is generated, copper oxide is converted under certain temperature, the broken shortcake of machinery obtains cupric oxide powder later, the powder that this method obtains
Have to environment and centainly endangers and produce cumbersome.
Reference examples 2
This reference examples prepares cupric oxide powder, specific steps using electrochemical process are as follows: using copper sheet as anode, is put into hydrogen
In potassium oxide solution liquid, predecessor is generated, pyrolysis obtains copper oxide, obtains cupric oxide powder after broken, powder pair obtained by this method
Operate more demanding, step is relatively complicated.
Reference examples 3
This reference examples prepares cupric oxide powder, specific steps using hydro-thermal method are as follows: exists in cationic surfactant
Under the conditions of, using hexamethylenetetramine as precipitating reagent, thorniness shape star-like cupric oxide can be prepared using hydrothermal synthesis method.Powder obtained by this method
End, which is produced, to be not easy, and is not suitable for producing in enormous quantities.
Reference examples 4
The oxygen pressure that this reference examples uses in process of production is too low, and it is not thorough on the one hand to will lead to cupric oxide powder oxidation
Bottom, also will lead to that negative nozzle pressure area suction is too small, increase the risk of stifled furnace.
Reference examples 5
The oxygen pressure that this reference examples uses in process of production is excessive, will lead to atomization in a flash, the intracorporal pressure of furnace
Strong moment, which becomes positive pressure, can cause safety accident when air-introduced machine has little time for gas in furnace body to be discharged.Other than safety, when
When pressure is excessive, high speed oxygen stream is very big on the influence of the temperature of nozzle, may result in nozzle temperature reduction, and atomization temperature is not achieved
Degree, causes copper water to solidify in diversion pipe, leads to stifled furnace.
Pass through embodiment 1-3, it is found that by above-mentioned technical proposal of the invention, producing oxidation using atomization
When copper powders, it is passed through purity oxygen, aoxidizes fine copper and oxygen in atomization process high temperature, cupric oxide powder is made, production is efficient
It is convenient and efficient, production stage has been saved, the production method of cupric oxide powder has been widened；And it is obtained by preparation method of the invention
Cupric oxide powder particle diameter distribution is uniform, excellent physical properties.
In addition, inventor also refers to the mode of embodiment 1- embodiment 3, with the other conditions listed in this specification
It is tested, and the cupric oxide powder that partial size is relatively concentrated, is evenly distributed, haveing excellent performance equally has been made.
It should be appreciated that above-described is only some embodiments of the present invention, it is noted that for the common of this field
For technical staff, under the premise of not departing from concept of the invention, other modification and improvement can also be made, these are all
It belongs to the scope of protection of the present invention.
Claims (4)
1. a kind of preparation method of cupric oxide powder, characterized by comprising:
Atomization process is directly carried out to the copper of molten condition by pure copper smelting to molten condition, and in oxygen atmosphere, make copper with
Fully oxidized reaction occurs for oxygen, obtains cupric oxide powder, the partial size of the cupric oxide powder less than 60 μm, wherein partial size 2 ~
15 μm of accounting in 10 ~ 15wt%, partial size in 20 ~ 35 μm of accounting in 20 ~ 25wt%, partial size 45 ~ 60 μm of accounting 20 ~
25wt%；
The temperature of the melting is 1400 ~ 1500 DEG C, and keeps the temperature 20~30min, when carrying out atomization process, the pressure of the oxygen
For 1.5 ~ 2.5Mpa, the mist droplet particle size that the atomization process uses is 15 ~ 53 μm.
2. preparation method according to claim 1, it is characterised in that: the cupric oxide powder is for regular shape or irregularly
Shape.
3. preparation method according to claim 2, it is characterised in that: the regular shape includes round and/or ellipse.
4. preparation method according to any one of claim 1-3, it is characterised in that specifically include:
(1) fine copper is placed in gas-atomized powder equipment, being warming up to 1400 ~ 1500 DEG C makes copper weld pool to molten condition, and keeps the temperature
20~30min；
(2) it is passed through oxygen into gas-atomized powder equipment, to molten condition in the oxygen atmosphere that pressure is 1.5 ~ 2.5MPa
Copper carries out atomization process, make copper and oxygen occur it is fully oxidized react, acquisition cupric oxide powder.
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| CN107311220B true CN107311220B (en) | 2019-07-09 |
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| CN112723406A (en) * | 2021-01-07 | 2021-04-30 | 江苏智微新材料科技有限公司 | Device and method for quickly acquiring copper oxide powder special for semiconductor |
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| CN1824435A (en) * | 2006-04-07 | 2006-08-30 | 郭德林 | Spray method for preparing low apparent density bronze powder |
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