CN102476184A - Copper powder as well as manufacture method, manufacture device and heat radiation element thereof - Google Patents
Copper powder as well as manufacture method, manufacture device and heat radiation element thereof Download PDFInfo
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- CN102476184A CN102476184A CN2011103112772A CN201110311277A CN102476184A CN 102476184 A CN102476184 A CN 102476184A CN 2011103112772 A CN2011103112772 A CN 2011103112772A CN 201110311277 A CN201110311277 A CN 201110311277A CN 102476184 A CN102476184 A CN 102476184A
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Abstract
The invention discloses ultra-low-apparent density copper powder. The copper powder has the apparent density being 0.8g/cm<3> to 2.0g/cm<3> and is formed by single-particle copper powder with irregular shapes. The particles of the copper powder are rough and are provided with holes or cracks. Compared with the prior art, the copper powder has the ultra-low apparent density and is mainly formed by the single-particle copper powder with irregular shapes, the clotting phenomenon does not exist or hardly exists, the porosity of the copper powder after the compaction and the sintering is high, and good heat radiation performance is realized.
Description
Technical field
The present invention relates to the metal powder material field, relate in particular to a kind of apparent density and be lower than 2.0g/cm
3Copper powder and preparation method thereof, producing device and have the radiating piece of copper powder.
Background technology
Copper powder is the important raw and processed materials of electronics industry, machinery manufacturing industry and auto industry; The apparent density of copper powder then is the important parameter of copper powder performance; Different applications is different to the requirement of apparent density; Some field (like injection-molded product) requires the copper powder of high apparent density, and some field (like heat pipe in the scattering industry and hot plate) then requires the copper powder of low-apparent-density, and commercial at present its apparent density of copper powder is generally 2.8g/cm
3-3.8g/cm
3, enterprise of several family can produce 2.0g/cm
3-2.8g/cm
3Low-apparent-density copper powder, be lower than 2.0g/cm for apparent density
3Copper powder still belong to blank, bring restriction for the application of some high-order product and new product.
The method of producing low-apparent-density copper powder at present has: electrolysis, conventional water atomization, groupization method and ball-milling method.Said electrolysis is as anode with the blister copper slab; As electrolyte, can at negative electrode separate out copper powders may after the energising with sulfuric acid and copper sulphate mixed solution, but the copper powders may of electrolysis gained be shaped as dendritic structure; Flowability is extremely low, causes difficulty in the time of practical application, for operations such as filling out powder.And conventional water atomization is through adopting the copper flow of high speed pure water impact fusion; Quick cooling obtains the metallic copper powder after making the copper flow be broken into drop; But in the production technology atomized water press can and the cooldown rate of molten drop be difficult to control to optimum state; Very easily cause the nodularization of molten drop, thereby the apparent density that obtains all is higher than 2.0g/cm usually
3The groupization method is that thin copper powder is spread and sintering at high temperature, thereby obtains to change into oarse-grained copper powder by granule group, and this kind copper powder can be reduced to 2.0-3.0g/cm with apparent density according to the difference of a metallization processes
3, but every powder is made up of many fine powders, in screening, transportation or when using, is prone to cause the instability of quality and granularity.As for ball-milling method, it is the mode through mechanical ball milling, changes the shape of powder; Reduce the apparent density of powder, but the copper powder that adopts this kind method to obtain is shaped as laminar (thickness is less than 1 micron), does not have mobile; The mouldability extreme difference, and be prone to introduce impurity in process of production.
In view of the above problems, be necessary to provide a kind of preparation method of ultralow apparent-density copper powder newly to solve the problems referred to above.
Summary of the invention
The technical problem that the present invention solved is to provide a kind of ultralow apparent-density copper powder and preparation method thereof, and it can make apparent density and be lower than 2.0g/cm
3Copper powder.
For solving the problems of the technologies described above; The present invention adopts following technical scheme: a kind of preparation method of copper powder; It comprises that at least melting is handled and atomizing is handled, and it is under 1220 ℃ to 1350 ℃ temperature, fine copper to be carried out melting that said melting is handled, and oxygenation operation in fusion process; Said atomizing is handled after said melting is handled and is carried out, and is to utilize Conic nozzle that the copper melt of above-mentioned melting gained is atomized and obtain copper powder, and to be 30 degree spend to 55 the jet apex angle of said Conic nozzle.
Further, said Conic nozzle is made up of 4 to 45 nozzles that are arranged in annular, and the diameter of said nozzle is no more than 5.0mm greater than 2.0mm, and the water pressure in the nozzle is 2MPa to 10MPa.
Further, the mass percent of the oxygen content in the copper melt is 0.1% to 10% after the said oxygenation operation.
Further, the mass percent of said oxygen content is further defined to 0.2% to 5%.
Further, said oxygenation operation is oxygen blast or blow air in said copper melt in fusion process.
Further, the quantity of said nozzle is 21 to 60.
Further; After said melting processing and atomizing are handled; Again said copper powder is carried out dried and reduction processing; Said dried lets the mode of water evaporates or the mode that aforementioned dual mode carries out simultaneously through dewaterer drying mode or intensification, and it is under 300 ℃ to 600 ℃ temperature conditions, to utilize hydrogen or nitrogen hydrogen mixeding gas that copper powder is reduced that said reduction is handled.
The present invention also can adopt following technical scheme to realize: a kind of producing device of copper powder; Comprise the melting copper raw material smelting furnace, hold copper melt in the smelting furnace bottom pour ladle, an atomising device and the copper powder of handling that atomize of the copper melt in the said bottom pour ladle taken in bucket; The smelting temperature of said smelting furnace is 1220 ℃ to 1350 ℃; The bottom of said bottom pour ladle is provided with the small opening that an aperture is 4mm to 10mm; Said atomising device comprises a Conic nozzle, and this Conic nozzle comprises 4 to 45 nozzles that are arranged in annular, and the jet apex angle of said nozzle is that 30 degree are to 55 degree.
Further, be provided with the liquid pure water that sprays towards the copper melt that in small opening, flows out in the said nozzle, and the diameter of nozzle is for being no more than 5.0mm greater than 2.0mm, the water pressure in the nozzle is 2MPa to 10MPa.
Further, the quantity of said nozzle is 21 to 60.
The present invention also can adopt following technical scheme to realize: a kind of copper powder, the apparent density of this copper powder are 0.8g/cm
3To 2.0g/cm
3, and mainly form by non-dendroid individual particle copper powder in irregular shape, the rough surface of said copper powder particle also is provided with hole or the crack.
Further, the tap density of said copper powder is 1.2-2.5g/cm3, its through jolt ramming and in the porosity of 980 ℃ of sintering after 30 minutes greater than 63%.
Further, the granularity of said copper powder is 18 order to 500 orders.
The present invention also can adopt following technical scheme to realize: a kind of radiating piece; Comprise the heat radiation main body of metal material and be covered in the copper powder layer of said heat radiation main body; The thickness of said copper powder layer is 0.2mm-10mm, and this copper powder layer is the copper powder of 0.8g/cm3 to 2.0g/cm3 for apparent density, and copper powder mainly is made up of individual particle copper powder in irregular shape; The tap density of said copper powder is 1.2-2.5g/cm3, its through jolt ramming and in the porosity of 980 ℃ of sintering after 30 minutes greater than 63%.
Further, the granularity of said copper powder is 18 order to 500 orders.
Compared to prior art, copper powder preparation method of the present invention and producing device can make complex-shaped changeable copper powder, effectively reduce the apparent density of copper powder.
Description of drawings
Fig. 1 is the producing device sketch map of ultralow apparent-density copper powder according to the invention.
Fig. 2 utilizes the structural form of the present invention's prepared copper powder of ultralow apparent-density copper powder preparation method under electron microscope.
Fig. 3 is the configuration of surface of copper particle in the copper powder that utilizes preparation method of the present invention among Fig. 2 and make.
Fig. 4 is hole or the crack structural form under electron microscope on individual particle copper powder surface in the copper powder according to the invention.
Fig. 5 is a generalized section of utilizing a kind of radiating tube of copper powder of the present invention.
Fig. 6 is a generalized section of utilizing a kind of temperature uniforming heat radiation plate of copper powder of the present invention.
The specific embodiment
To shown in Figure 6, the present invention provides a kind of preparation method of ultralow apparent-density copper powder like Fig. 1, and it improves on the water atomization of routine, can make apparent density and be lower than 0.8-2.0g/cm
3Copper powder, this preparation method comprises following several steps at least: melting is handled, atomizing processing, dried, reduction processing and post-processed.
It is under 1150 ℃-1400 ℃ temperature (optimum temperature is 1220 ℃-1350 ℃) that said melting is handled; With solid-state fine copper raw material as in the smelting furnace 1 fusing; And in this fusion process, carry out oxygenation operation, this oxygenation operation is that oxygen is joined in the said smelting furnace 1, makes that the oxygen content of the molten copper liquid 2 after the oxygenation is 0.1%-10% (mass percent); Optimum value is 0.2%-5%, and said oxygenation operation can be that the molten metal copper in the smelting furnace 1 is carried out oxygen blast or blows air.Said melting is handled the liquid copper melt 2 of gained and is poured in the bottom pour ladle 11, and flows out from the small opening 3 of bottom pour ladle 11 bottoms, gets into the atomizing treatment process subsequently, and the aperture of said small opening 3 is 4mm to 10mm (optimum aperture is 6-8mm).
It is when liquid copper melt 2 flows out smelting furnace 1 that said atomizing is handled, and adopts atomising device (the present invention refers to shower nozzle 4) that said liquid copper melt 2 is sprayed aqueous water (being generally pure water), makes liquid copper melt 2 be cooled to graininess copper powder 6 fast.Said shower nozzle is Conic nozzle 4 and the below that places said smelting furnace small opening 3; See also shown in Figure 1; This shower nozzle 4 is formed (optimal number is 12 to 40) by 4 to 45 nozzles 5 that are arranged in annular; The quantity of nozzle 5 is merely signal among Fig. 1; Said each nozzle 5 all sprays towards the same spray site A that is positioned at said annular central lower, and the jet apex angle of said nozzle 5 (being the angle between injection direction M and the vertical direction) be 30 the degree to 55 the degree, so constituted said Conic nozzle 4.The diameter of said nozzle 5 is 1.0mm to 4.0mm (optimum diameter is 2.0mm-3.0mm); Water pressure in the nozzle 5 is 2MPa to 10MPa; Said liquid copper melt 2 is from the said spray site A that vertically flows through after said small opening 3 flows out; Under the effect of said Conic nozzle 4, liquid copper melt 2 can cool off rapidly and form copper powder 6, and contains in taking in bucket 7.
Said dried is resulting copper powder 6 to be handled in said atomizing carry out drying; Drying comprises the dry or heat treated of normal temperature centrifuge dewatering; This dual mode can carry out separately also can combining to carry out, and the heating-up temperature during heat treated is between 100 ℃ to 400 ℃.
Said reduction processing is that the copper powder after utilizing reducing gas to dried reduces, and said reducing gas comprises hydrogen or nitrogen hydrogen mixeding gas, and the reduction treatment temperature is between 200 ℃ to 800 ℃, and wherein, optimum temperature is between 300 ℃ to 600 ℃.
Said post-processed comprises carries out operations such as fragmentation, anti-oxidant and screening to copper powder; Obtaining apparent density is the finished product copper powder of 0.8-2.0g/cm3; Wherein, The composition of the anti-oxidant that said anti-oxidant operation is adopted contains C, H, O, N, Cl, F and Si, and its content is 0.001-0.2% (mass percent).
The present invention has changed the flowability and the surface tension of molten metal, especially oxygenation operational sequence because of adopting above-mentioned smelting technology; Oxygen has been circulated the inside of said copper melt; Increase the viscosity of metal liquid, better resisted the nodularization process of metallic copper drop when cooled and solidified, simultaneously; In the atomizing processing procedure; The parameter setting of said Conic nozzle 4 can effectively utilize the impact property of atomized water, can obtain optimum molten drop cooling velocity, thereby makes the copper particle A that forms copper powders may have changeable, irregular shape (only exist and be lower than 10% spherical or type spherical powder); Can join shown in Figure 2ly, so reduce the apparent density of copper powder effectively.In addition; Reduction of the present invention is handled can effectively remove the oxygen that contains in the copper powder; Make the hydrogen in the reducing gas combine to form water and at high temperature be evaporated with oxygen in the copper powder, the evaporation of moisture causes the surface of said copper particle A to form hole or crack B, can join shown in Figure 3.
Compared to prior art, preparation method of the present invention can make apparent density between 0.8-2.0g/cm
3Between copper powder; And said copper powder is made up of individual particle copper powder A, owing under 1220 ℃-1350 ℃ optimum temperature, copper melt is cooled off fast, makes not have or only exist very group's phenomenon of minority between the copper powder particle in the copper powder; And the granularity of copper powder is between 18 order to 500 orders; The rough surface of individual particle copper powder A is rough in the copper powder, and is provided with hole or the crack B that forms because of water evaporates, please cooperate and consult Fig. 4.Described hole, crack B produce in above-mentioned reducing process process; Because the oxygenation operation during melting makes a large amount of oxygen of dissolving in the copper liquid; Under reducing atmosphere, hydrogen atom is owing to its minimum atomic radius enters into copper powder inside, with oxygen water generation reaction steam; Water vapour goes out from the inner loss of copper powders may, forms a large amount of crackles and hole on the surface of copper powder particle thus.In addition, the copper powder that the present invention makes is behind the jolt ramming sintering, and porosity is greater than 63%; Wherein, the tap density of copper powder after jolt ramming is 1.2-2.5g/cm3,980 ℃ of sintering temperatures; Sintering time 30 minutes, so-called tap density are the comprehensive embodiments of the multiple physical property of powder, are meant the powder that is contained in the container (is undertaken by the GB5162 regulation) under defined terms by the density after the jolt ramming (being the quality of unit volume); As a rule; Tap density and bulk density, granule-morphology, size distribution etc. have relation, copper powder of the present invention mainly to be made up of the individual particle copper powder, and the shape of individual particle copper powder is extremely irregular; Therefore, make porosity between the copper powder particle than higher.
The copper powder of apparent density of the present invention between 0.8-2.0g/cm3 can be widely used in every field; Because its higher porosity (greater than 63%), individual particle copper powder is irregularly shaped; Make that space between the individual particle copper powder is big and space quantity is more, and form by the individual particle copper powder in the copper powder, do not have or exist group's phenomenon of only a few between the copper powder particle; The aforementioned structure characteristic has determined copper powder of the present invention can be widely used in very much the heat radiation field; As the computer innernal CPU with or the radiating piece used of VGA video card on, because of the microstructure of copper powder of the present invention can make heat eliminating mediums such as air, cooling water well through said hole, have good performance of heat dissipation; Can effectively improve the radiating effect of radiating piece, below illustrate.
Shown in Figure 6 for a kind of CPU with or the cross section view of the radiating tube used of VGA video card, the heat radiation main body 21 of this radiating tube 20 is processed for metal material, it is cylindrical and be provided with the inner chamber 22 of a circle; This inner chamber 22 is provided with an inner surface 23 and is covered in the copper powder layer 24 on the said inner surface 23; The thickness of this copper powder layer 24 is 0.2mm-10mm, and this copper powder layer has utilized the prepared apparent density of the present invention to be the copper powder between the 0.8-2.0g/cm3, because apparent density shape lower, copper powder particle is changeable; Increased the surface area of copper powder particle; And its higher porosity has also increased percent of pass, makes air or cooling medium (like cooling water) very easily to pass through, and has improved the radiating efficiency of radiating tube greatly; Compare copper powder of the prior art, utilize the radiating tube of copper powder according to the invention can improve radiating effect greatly.
In addition, except above-mentioned radiating tube, also has a kind of temperature uniforming heat radiation plate (vapor chamber on the said VGA video card; Also be the cavity soaking plate) 30, it is provided with the heat radiation main body 31 that is tabular and is positioned at chip (not shown) top, and this heat radiation main body 31 is a metal material; It is provided with an inner chamber 32, and the inner surface of this inner chamber 32 is coated with layer of copper bisque 33, and this copper powder layer 33 adopts copper powder of the present invention; (spherical copper powder particle is merely signal among Fig. 6 because this copper powder layer 33 contains a large amount of individual particle copper powders; Copper powder particle of the present invention is actual to be irregularly shaped), and have porosity behind its jolt ramming sintering greater than 63%, make the gap between the copper powder particle of flowing through that inner chamber 32 air or cooling water can be unobstructed; And the cooling that in inner chamber, circulates well; Improved the heat dispersion of heat radiation main body 31 surface of internal cavity greatly, heat can well be passed to heat on another outer surface 34 of temperature uniforming heat radiation plate through this main body 31 of dispelling the heat, thereby improves the radiating effect of temperature uniforming heat radiation plate.
The above only is a most preferred embodiment of the present invention, is not the present invention is done any pro forma restriction.Any those of ordinary skill in the art are not breaking away under the technical scheme scope situation of the present invention, utilize the method content of above-mentioned announcement that technical scheme of the present invention is made many possible changes and modification, all belong to the scope of claims protection.
Claims (15)
1. the preparation method of a copper powder, it comprises that at least melting is handled and atomizing is handled, it is characterized in that: it is under 1220 ℃ to 1350 ℃ temperature, fine copper to be carried out melting that said melting is handled, and oxygenation operation in fusion process; Said atomizing is handled after said melting is handled and is carried out, and is to utilize Conic nozzle that the copper melt of above-mentioned melting gained is atomized and obtain copper powder, and to be 30 degree spend to 55 the jet apex angle of said Conic nozzle.
2. the preparation method of copper powder as claimed in claim 1, it is characterized in that: said Conic nozzle is made up of 4 to 45 nozzles that are arranged in annular, and the diameter of said nozzle is no more than 5.0mm greater than 2.0mm, and the water pressure in the nozzle is 2MPa to 10MPa.
3. the preparation method of copper powder as claimed in claim 2 is characterized in that: the mass percent of the oxygen content in the copper melt of said oxygenation operation back is 0.1% to 10%.
4. the preparation method of copper powder as claimed in claim 3, it is characterized in that: the mass percent of said oxygen content is further defined to 0.2% to 5%.
5. the preparation method of copper powder as claimed in claim 4 is characterized in that: said oxygenation operation is oxygen blast or blow air in said copper melt in fusion process.
6. like the preparation method of any described copper powder in the claim 2 to 5, it is characterized in that: the quantity of said nozzle is 21 to 60.
7. the preparation method of copper powder as claimed in claim 6; It is characterized in that: after said melting processing and atomizing are handled; Again said copper powder is carried out dried and reduction processing; Said dried lets the mode of water evaporates or the mode that aforementioned dual mode carries out simultaneously through dewaterer drying mode or intensification, and it is under 300 ℃ to 600 ℃ temperature conditions, to utilize hydrogen or nitrogen hydrogen mixeding gas that copper powder is reduced that said reduction is handled.
8. the producing device of a copper powder; Comprise the melting copper raw material smelting furnace, hold copper melt in the smelting furnace bottom pour ladle, an atomising device and the copper powder of handling that atomize of the copper melt in the said bottom pour ladle taken in bucket; It is characterized in that: the smelting temperature of said smelting furnace is 1220 ℃ to 1350 ℃; The bottom of said bottom pour ladle is provided with the small opening that an aperture is 4mm to 10mm; Said atomising device comprises a Conic nozzle, and this Conic nozzle comprises 4 to 45 nozzles that are arranged in annular, and the jet apex angle of said nozzle is that 30 degree are to 55 degree.
9. the producing device of copper powder as claimed in claim 8; It is characterized in that: be provided with the liquid pure water that sprays towards the copper melt that in small opening, flows out in the said nozzle; And the diameter of nozzle is for being no more than 5.0mm greater than 2.0mm, and the water pressure in the nozzle is 2MPa to 10MPa.
10. the producing device of copper powder as claimed in claim 9, it is characterized in that: the quantity of said nozzle is 21 to 60.
11. a copper powder is characterized in that: the apparent density of this copper powder is 0.8g/cm
3To 2.0g/cm
3, and mainly form by non-dendroid individual particle copper powder in irregular shape, the rough surface of said copper powder particle also is provided with hole or the crack.
12. copper powder as claimed in claim 11 is characterized in that: the tap density of said copper powder is 1.2-2.5g/cm3, its through jolt ramming and in the porosity of 980 ℃ of sintering after 30 minutes greater than 63%.
13. copper powder as claimed in claim 12 is characterized in that: the granularity of said copper powder is 18 order to 500 orders.
14. radiating piece; Comprise the heat radiation main body of metal material and be covered in the copper powder layer of said heat radiation main body; It is characterized in that: the thickness of said copper powder layer is 0.2mm-10mm, and this copper powder layer is the copper powder of 0.8g/cm3 to 2.0g/cm3 for apparent density, and copper powder mainly is made up of individual particle copper powder in irregular shape; The tap density of said copper powder is 1.2-2.5g/cm3, its through jolt ramming and in the porosity of 980 ℃ of sintering after 30 minutes greater than 63%.
15. radiating piece as claimed in claim 14 is characterized in that: the granularity of said copper powder is 18 order to 500 orders.
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| CN103801704A (en) * | 2014-02-28 | 2014-05-21 | 昆山德泰新材料科技有限公司 | Forming copper powder suitable for 3D printing, and manufacturing method and purposes of forming copper powder |
| CN104028769A (en) * | 2014-06-10 | 2014-09-10 | 铜陵国传电子材料科技有限公司 | Manufacturing method of high-green-strength atomized copper powder |
| CN105108163A (en) * | 2015-09-09 | 2015-12-02 | 元磁新型材料(苏州)有限公司 | Copper powder used for ultrathin vapor chamber and manufacturing method thereof |
| CN105127412A (en) * | 2015-09-14 | 2015-12-09 | 宁波广博纳米新材料股份有限公司 | Preparation method of low-oxygen submicron copper and manganese alloy powder |
| CN108202144A (en) * | 2016-12-19 | 2018-06-26 | 天津艾博胜环保科技有限公司 | A kind of preparation method of conductive copper powder |
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| CN108202144A (en) * | 2016-12-19 | 2018-06-26 | 天津艾博胜环保科技有限公司 | A kind of preparation method of conductive copper powder |
| CN110216293A (en) * | 2019-07-01 | 2019-09-10 | 铜陵国传电子材料科技有限公司 | A kind of production technology of high desnity metal injection moulding copper powder |
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| CN111633216B (en) * | 2020-07-15 | 2021-03-16 | 湖南省天心博力科技有限公司 | Copper powder water atomization system and atomization structure thereof |
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| CN113894286B (en) * | 2021-04-15 | 2023-06-23 | 芜湖松合新材料科技有限公司 | Preparation method of high-quality copper powder |
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Application publication date: 20120530 |