CN106086510A - A kind of preparation method of nanoporous copper radiating rib - Google Patents
A kind of preparation method of nanoporous copper radiating rib Download PDFInfo
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- CN106086510A CN106086510A CN201610462165.XA CN201610462165A CN106086510A CN 106086510 A CN106086510 A CN 106086510A CN 201610462165 A CN201610462165 A CN 201610462165A CN 106086510 A CN106086510 A CN 106086510A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1103—Making porous workpieces or articles with particular physical characteristics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to the preparation method of a kind of nanoporous copper radiating rib, belong to metal material field.The most powerful to the function along with computer, requirement to fin heat radiation is more and more higher, existing alloy heat-sink sheet is difficult to meet the requirement of computer heat radiation, it is excessive to there is weight in fine copper fin, the shortcoming that difficulty of processing is big, and easily more than the CPU problem to fin heavily quantitative limitation, the invention provides the preparation method of a kind of nanoporous copper radiating rib, the present invention uses copper nitrate to be raw material, with succinic acid, tetraethylammonium bromide, copper nanoparticle is prepared in hydrazine hydrate reaction, and the graphite-structure carbonitride prepared by tripolycyanamide is as pore-creating agent, copper fiber is blended as reinforcing agent, extrusion forming in radiating fin die, prepare green compact, and high temperature sintering molding, again with abrasive paper for metallograph to Porous Cu surface rubbing extremely light no marking, after polishing, prepare nanoporous copper radiating rib.
Description
Technical field
The present invention relates to the preparation method of a kind of nanoporous copper radiating rib, belong to metal material field.
Background technology
Along with the development of science and technology, the kind that porous metal material range of application is increasingly wider, function is more and more stronger, new
Also continue to bring out.So-called porous metals, refer to that artificial metal's material of a large amount of three-dimensional pore space structure, porous gold are contained in a kind of inside
Belong to and have function and structure double grading concurrently, mostly inherit original advantage of parent metal, such as the excellent conductive heat conductivility of copper,
The good anticorrosion candle performance of silver, the bio-compatibility etc. of titanium.Simultaneously as there is a large amount of pore space structure in inside makes again this material
Possesses the plurality of advantages not available for its parent metal.Porous metal material physical property, chemical property and mechanical performance are excellent
Good, the feature presented is: the specific surface area that proportion is little, specific strength is big, big, good energy absorption, good sound-deadening and noise-reducing
Energy and excellent capability of electromagnetic shielding.In architectural engineering, mechanical engineering, metallurgical engineering, petrochemical industry, energy environment protection, national defence
It is used widely in the field such as military project, Electrochemical Engineering.The porous material preparation method of domestic more system further investigation includes
The methods such as powder metallurgic method, THROUGH METHOD, solution foaming, spark plasma sintering method, solid-gas eutectic freezing method, it is already possible to
Preparing porosity 50% ~ 95%, aperture is only 0.5 millimeter of multiple porous metal material to several millimeters.
In addition to silver, the heat conductivility of copper is best in metal, and it is preferable that it makes fin radiating effect, but fine copper dissipates
It is excessive to there is weight in backing, the shortcoming that difficulty of processing is big, and easily more than CPU to fin heavily quantitative limitation.Fin also can be adopted
Forming with aluminium alloy extruded, but the function being as computer is the most powerful, the requirement to fin heat radiation is more and more higher, existing
Alloy heat-sink sheet is difficult to meet the requirement of computer heat radiation.
Summary of the invention
The technical problem to be solved: the most powerful for the function along with computer, to fin heat radiation
Requiring more and more higher, existing alloy heat-sink sheet is difficult to meet the requirement of computer heat radiation, and it is excessive that fine copper fin exists weight, processing
The shortcoming that difficulty is big, and easily more than the CPU problem to fin heavily quantitative limitation, the invention provides a kind of nano porous copper and dissipate
The preparation method of backing, the present invention uses copper nitrate to be raw material, and with succinic acid, tetraethylammonium bromide, hydrazine hydrate reaction preparation is received
Rice copper powder, and the graphite-structure carbonitride prepared by tripolycyanamide is as pore-creating agent, copper fiber is blended as reinforcing agent,
Extrusion forming in radiating fin die, prepares green compact, and high temperature sintering molding, then with abrasive paper for metallograph to Porous Cu surface rubbing to light
Bright no marking, after polishing, prepares nanoporous copper radiating rib.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) weigh 30 ~ 50g succinic acid, 30 ~ 50g tetraethylammonium bromide, 50 ~ 80g copper nitrate respectively, add grinding machine for grinding
To transparence, adding 250 ~ 300mL mass fraction is 80% hydrazine hydrate, is heated to 160 ~ 180 DEG C, is incubated 4 ~ 5h, filters, uses matter
Amount mark is that 50% ethanol solution washs 3 ~ 5 times, is placed in 100 ~ 105 DEG C of drying baker and is dried to constant weight, obtains copper nanoparticle, standby；
(2) weigh 40 ~ 60g tripolycyanamide to be placed in batch-type furnace, under nitrogen atmosphere, with 2.0 ~ 2.5 DEG C/min be heated to 580 ~
600 DEG C of reaction 3 ~ 4h, are cooled to room temperature, take out, obtain graphite-structure carbonitride；
(3) copper nanoparticle prepared by above-mentioned graphite-structure carbonitride and above-mentioned steps (1) is added in planetary ball mill, with
200 ~ 300r/min ball milling 6 ~ 8h, crosses 200 mesh sieves by mixed powder, the mixed powder after sieving and 2 ~ 3g a diameter of 80 ~ 100
μm copper fiber mixes, and loads in radiating fin die, and is 180 ~ 200MPa with pressure, and the press time is 1 ~ 2min, after molding
Green compact；
(4) mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace, first opens pumped vacuum systems, is evacuated to by sintering furnace
In furnace chamber, working vacuum degree is 0.03 ~ 0.05Pa, then is warming up to 800 DEG C with 10 DEG C/min, and after keeping temperature 40 ~ 50min, with
5 DEG C/min is warming up to 1000 DEG C, is passed through high pure nitrogen, is 0.12 ~ 0.15MPa to stove internal gas pressure, and keeps temperature 50 ~ 60min,
Cool to room temperature with the furnace, take out, obtain porous copper product；
(5) by above-mentioned Porous Cu material abrasive paper for metallograph to its surface rubbing to light no marking, and with 2.5mm diamond and going
After ionized water is to going to be polished, soak 2 ~ 3h in deionized water, take out, be placed in 105 ~ 110 DEG C of drying baker and be dried to perseverance
Weight, obtains nanoporous copper radiating rib.
The application process of the present invention is: nanoporous copper radiating rib prepared by the present invention as computer CPU radiator, than
Like product heat dispersion improves 15 ~ 18%, and rate of heat dispation is fast, and nano porous copper heat sink mass prepared by the present invention is light,
It is prone to processing.
The method have the benefit that:
(1) the nanoporous copper radiating rib heat radiation heart infarction that prepared by the present invention is good, rapid heat dissipation；
(2) the nano porous copper heat sink mass that prepared by the present invention is light, it is easy to processing；
(3) preparation process of the present invention is simple, it is easy to operation.
Detailed description of the invention
Weigh 30 ~ 50g succinic acid, 30 ~ 50g tetraethylammonium bromide, 50 ~ 80g copper nitrate respectively, add grinding machine for grinding
To transparence, adding 250 ~ 300mL mass fraction is 80% hydrazine hydrate, is heated to 160 ~ 180 DEG C, is incubated 4 ~ 5h, filters, uses matter
Amount mark is that 50% ethanol solution washs 3 ~ 5 times, is placed in 100 ~ 105 DEG C of drying baker and is dried to constant weight, obtains copper nanoparticle；Weigh
40 ~ 60g tripolycyanamide is placed in batch-type furnace, under nitrogen atmosphere, with 2.0 ~ 2.5 DEG C/min be heated to 580 ~ 600 DEG C reaction 3 ~
4h, is cooled to room temperature, takes out, obtains graphite-structure carbonitride；Above-mentioned graphite-structure carbonitride is added with above-mentioned copper nanoparticle and enters a profession
In planetary ball mill, with 200 ~ 300r/min ball milling 6 ~ 8h, mixed powder is crossed 200 mesh sieves, the mixed powder after sieving and 2
A diameter of 80 ~ 100 μm copper fiber mixing of ~ 3g, load in radiating fin die, and are 180 ~ 200MPa with pressure, and the press time is 1
~ 2min, obtains green compact after molding；The mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace, first opens pumped vacuum systems, will burn
It is 0.03 ~ 0.05Pa that freezing of a furnace is evacuated to working vacuum degree in furnace chamber, then is warming up to 800 DEG C with 10 DEG C/min, and keeps temperature
After 40 ~ 50min, it is warming up to 1000 DEG C with 5 DEG C/min, is passed through high pure nitrogen, be 0.12 ~ 0.15MPa to stove internal gas pressure, and keep
Temperature 50 ~ 60min, cools to room temperature with the furnace, takes out, obtains porous copper product；By above-mentioned Porous Cu material abrasive paper for metallograph to it
Surface rubbing to light no marking, and with 2.5mm diamond and deionized water to going to be polished after, soak in deionized water
2 ~ 3h, takes out, is placed in 105 ~ 110 DEG C of drying baker and is dried to constant weight, obtain nanoporous copper radiating rib.
Example 1
Weigh 30g succinic acid, 30g tetraethylammonium bromide, 50g copper nitrate respectively, add grinding machine for grinding to transparence, addition
250mL mass fraction is 80% hydrazine hydrate, is heated to 160 DEG C, is incubated 4h, filters, and is 50% ethanol solution washing 3 with mass fraction
Secondary, it is placed in 100 DEG C of drying baker and is dried to constant weight, obtain copper nanoparticle；Weigh 40g tripolycyanamide to be placed in batch-type furnace, at nitrogen
Under atmosphere, it is heated to 580 DEG C of reaction 3h with 2.0 DEG C/min, is cooled to room temperature, takes out, obtain graphite-structure carbonitride；By above-mentioned stone
Ink structure carbonitride adds in planetary ball mill with above-mentioned copper nanoparticle, with 200r/min ball milling 6h, mixed powder is crossed 200
Mesh sieve, the 80 μm copper fibers a diameter of with 2g of the mixed powder after sieving mix, and load in radiating fin die, and with pressure are
180MPa, the press time is 1min, obtains green compact after molding；The mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace, first beats
Opening pumped vacuum systems, it is 0.03Pa that sintering furnace is evacuated to working vacuum degree in furnace chamber, then is warming up to 800 with 10 DEG C/min
DEG C, and after keeping temperature 40min, be warming up to 1000 DEG C with 5 DEG C/min, be passed through high pure nitrogen, be 0.12MPa to stove internal gas pressure,
And keep temperature 50min, cool to room temperature with the furnace, take out, obtain porous copper product；By above-mentioned Porous Cu material abrasive paper for metallograph pair
Its surface rubbing to light no marking, and with 2.5mm diamond and deionized water to going to be polished after, be immersed in deionized water
Middle 2h, takes out, is placed in 105 DEG C of drying baker and is dried to constant weight, obtain nanoporous copper radiating rib.
The application process of the present invention is: nanoporous copper radiating rib prepared by the present invention as computer CPU radiator, than
Like product heat dispersion improves 15%, and rate of heat dispation is fast, and nano porous copper heat sink mass prepared by the present invention is light, easily
In processing.
Example 2
Weigh 40g succinic acid, 40g tetraethylammonium bromide, 70g copper nitrate respectively, add grinding machine for grinding to transparence, addition
280mL mass fraction is 80% hydrazine hydrate, is heated to 170 DEG C, is incubated 4.5h, filters, is that 50% ethanol solution is washed with mass fraction
Wash 4 times, be placed in 102 DEG C of drying baker and be dried to constant weight, obtain copper nanoparticle；Weigh 50g tripolycyanamide to be placed in batch-type furnace, at nitrogen
Under atmosphere is enclosed, it is heated to 590 DEG C of reaction 3.5h with 2.2 DEG C/min, is cooled to room temperature, takes out, obtain graphite-structure carbonitride；By upper
State graphite-structure carbonitride and add in planetary ball mill with above-mentioned copper nanoparticle, with 250r/min ball milling 7h, by mixed powder
Crossing 200 mesh sieves, the 90 μm copper fibers a diameter of with 2.5g of the mixed powder after sieving mix, and load in radiating fin die, and use
Pressure is 190MPa, and the press time is 1.5min, obtains green compact after molding；The mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace
In, first open pumped vacuum systems, it is 0.04Pa that sintering furnace is evacuated to working vacuum degree in furnace chamber, then heats up with 10 DEG C/min
To 800 DEG C, and after keeping temperature 45min, it is warming up to 1000 DEG C with 5 DEG C/min, is passed through high pure nitrogen, to stove internal gas pressure be
0.13MPa, and keep temperature 55min, cool to room temperature with the furnace, take out, obtain porous copper product；By above-mentioned Porous Cu material gold
Phase sand paper to its surface rubbing to light no marking, and with 2.5mm diamond and deionized water to going to be polished after, be immersed in
2.5h in deionized water, takes out, is placed in 108 DEG C of drying baker and is dried to constant weight, obtain nanoporous copper radiating rib.
The application process of the present invention is: nanoporous copper radiating rib prepared by the present invention as computer CPU radiator, than
Like product heat dispersion improves 16%, and rate of heat dispation is fast, and nano porous copper heat sink mass prepared by the present invention is light, easily
In processing.
Example 3
Weigh 50g succinic acid, 50g tetraethylammonium bromide, 80g copper nitrate respectively, add grinding machine for grinding to transparence, addition
300mL mass fraction is 80% hydrazine hydrate, is heated to 180 DEG C, is incubated 5h, filters, and is 50% ethanol solution washing 5 with mass fraction
Secondary, it is placed in 105 DEG C of drying baker and is dried to constant weight, obtain copper nanoparticle；Weigh 60g tripolycyanamide to be placed in batch-type furnace, at nitrogen
Under atmosphere, it is heated to 600 DEG C of reaction 4h with 2.5 DEG C/min, is cooled to room temperature, takes out, obtain graphite-structure carbonitride；By above-mentioned stone
Ink structure carbonitride adds in planetary ball mill with above-mentioned copper nanoparticle, with 300r/min ball milling 8h, mixed powder is crossed 200
Mesh sieve, the 100 μm copper fibers a diameter of with 3g of the mixed powder after sieving mix, and load in radiating fin die, and with pressure are
200MPa, the press time is 2min, obtains green compact after molding；The mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace, first beats
Opening pumped vacuum systems, it is 0.05Pa that sintering furnace is evacuated to working vacuum degree in furnace chamber, then is warming up to 800 with 10 DEG C/min
DEG C, and after keeping temperature 50min, be warming up to 1000 DEG C with 5 DEG C/min, be passed through high pure nitrogen, be 0.15MPa to stove internal gas pressure,
And keep temperature 60min, cool to room temperature with the furnace, take out, obtain porous copper product；By above-mentioned Porous Cu material abrasive paper for metallograph pair
Its surface rubbing to light no marking, and with 2.5mm diamond and deionized water to going to be polished after, be immersed in deionized water
Middle 3h, takes out, is placed in 110 DEG C of drying baker and is dried to constant weight, obtain nanoporous copper radiating rib.
The application process of the present invention is: nanoporous copper radiating rib prepared by the present invention as computer CPU radiator, than
Like product heat dispersion improves 18%, and rate of heat dispation is fast, and nano porous copper heat sink mass prepared by the present invention is light, easily
In processing.
Claims (1)
1. the preparation method of a nanoporous copper radiating rib, it is characterised in that concrete preparation process is:
(1) weigh 30 ~ 50g succinic acid, 30 ~ 50g tetraethylammonium bromide, 50 ~ 80g copper nitrate respectively, add grinding machine for grinding
To transparence, adding 250 ~ 300mL mass fraction is 80% hydrazine hydrate, is heated to 160 ~ 180 DEG C, is incubated 4 ~ 5h, filters, uses matter
Amount mark is that 50% ethanol solution washs 3 ~ 5 times, is placed in 100 ~ 105 DEG C of drying baker and is dried to constant weight, obtains copper nanoparticle, standby；
(2) weigh 40 ~ 60g tripolycyanamide to be placed in batch-type furnace, under nitrogen atmosphere, with 2.0 ~ 2.5 DEG C/min be heated to 580 ~
600 DEG C of reaction 3 ~ 4h, are cooled to room temperature, take out, obtain graphite-structure carbonitride；
(3) copper nanoparticle prepared by above-mentioned graphite-structure carbonitride and above-mentioned steps (1) is added in planetary ball mill, with
200 ~ 300r/min ball milling 6 ~ 8h, crosses 200 mesh sieves by mixed powder, the mixed powder after sieving and 2 ~ 3g a diameter of 80 ~ 100
μm copper fiber mixes, and loads in radiating fin die, and is 180 ~ 200MPa with pressure, and the press time is 1 ~ 2min, after molding
Green compact；
(4) mould that will be equipped with above-mentioned green compact is placed in vacuum sintering furnace, first opens pumped vacuum systems, is evacuated to by sintering furnace
In furnace chamber, working vacuum degree is 0.03 ~ 0.05Pa, then is warming up to 800 DEG C with 10 DEG C/min, and after keeping temperature 40 ~ 50min, with
5 DEG C/min is warming up to 1000 DEG C, is passed through high pure nitrogen, is 0.12 ~ 0.15MPa to stove internal gas pressure, and keeps temperature 50 ~ 60min,
Cool to room temperature with the furnace, take out, obtain porous copper product；
(5) by above-mentioned Porous Cu material abrasive paper for metallograph to its surface rubbing to light no marking, and with 2.5mm diamond and going
After ionized water is to going to be polished, soak 2 ~ 3h in deionized water, take out, be placed in 105 ~ 110 DEG C of drying baker and be dried to perseverance
Weight, obtains nanoporous copper radiating rib.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195559A (en) * | 2017-04-27 | 2017-09-22 | 华中科技大学 | A kind of method for covering tin nano porous copper low-temperature bonding |
| CN110364498A (en) * | 2019-05-28 | 2019-10-22 | 广东省智能制造研究所 | A kind of porous flat plate formula radiator, system and manufacturing method |
| CN111020260A (en) * | 2019-12-13 | 2020-04-17 | 昆明理工大学 | Preparation method of layered copper-based composite material |
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| CN102618745A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Preparation method of copper porous material |
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| JP2005314806A (en) * | 2004-03-29 | 2005-11-10 | Nano Gijutsu Kenkyusho:Kk | Powder of nano crystalline copper metal and nano crystalline copper alloy having high hardness and high electric conductivity, bulk material of nano crystalline copper or copper alloy having high hardness, high strength, high electric conductivity and high toughness, and production method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195559A (en) * | 2017-04-27 | 2017-09-22 | 华中科技大学 | A kind of method for covering tin nano porous copper low-temperature bonding |
| CN110364498A (en) * | 2019-05-28 | 2019-10-22 | 广东省智能制造研究所 | A kind of porous flat plate formula radiator, system and manufacturing method |
| CN111020260A (en) * | 2019-12-13 | 2020-04-17 | 昆明理工大学 | Preparation method of layered copper-based composite material |
| CN111020260B (en) * | 2019-12-13 | 2021-07-23 | 昆明理工大学 | Preparation method of layered copper-based composite material |
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Application publication date: 20161109 |