CN101850420A - Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating - Google Patents
Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating Download PDFInfo
- Publication number
- CN101850420A CN101850420A CN 201010209856 CN201010209856A CN101850420A CN 101850420 A CN101850420 A CN 101850420A CN 201010209856 CN201010209856 CN 201010209856 CN 201010209856 A CN201010209856 A CN 201010209856A CN 101850420 A CN101850420 A CN 101850420A
- Authority
- CN
- China
- Prior art keywords
- tungsten
- powder
- copper
- quality
- cuo
- 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.)
- Granted
Links
Images
Abstract
The invention discloses a preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of a cladding coating. The method comprises the following steps of: uniformly mixing CuO powder with the mass of m1 with WO3 powder with the mass of m2; placing the mixed powder in a furnace for sintering; adding ground CuWO4 powder into CuO powder with the mass of m3, mixing, and placing the mixture into a hydrogen reduction furnace; introducing hydrogen into the furnace with the introduction rate of 33L/min; raising the temperature to 360 DEG C with the temperature raising speed of 5-10 DEG C/min, keeping the temperature for 10min, raising the temperature to 800 DEG C with the temperature raising speed of 3-5 DEG C/min, and keeping the temperature for 30 min; stopping introducing hydrogen, introducing helium with the speed of 20L/min, cooling along with the furnace to room temperature, and stopping introducing helium to obtain the tungsten-cladding-copper nanometer composite powder. By adopting the preparation process, the thickness of the tungsten cladding coating can be precisely controlled in the nanometer order of magnitude, thereby the application requirements of different tungsten and copper proportion contents can be satisfied.
Description
Technical field
The invention belongs to tungsten coating copper composite powder system and be equipped with technical field, be specifically related to the preparation method that the controlled tungsten of a kind of coating thickness coats copper nanometer composite powder.
Background technology
Coated composite powder (coatedpowder) is to be coated on particle surface and the composite powder that forms by one deck xenogenesis composition.In recent years, the research of powder coating technology has obtained certain progress, and the preparation and the application of metallic cover powder have received concern.Two or more powder granule coats or Combined Processing through the surface, can obtain a kind of high-performance composite powder material.Composite granule not only has the performance of single powder, also have compound collaborative multi-functional, overcome two kinds of powders shortcoming, the effects such as contact area that change the single particle surface nature, increase two or more components separately.
The nanometer coated powder of copper blapharoplast and tungsten clad be combined into had both had characteristics such as high temperature resistant, the high strength, high density of tungsten, had the electric-conductivity heat-conductivity high of copper, good plasticity again.This nanometer coats composite granule owing to can promote greatly than table, has the not available good sintering character of micron-class superfine powder.In addition, in field of powder metallurgy, the intensity of the metallic composite that nanoscale coated powder compacting sintering becomes and tensile property are compared the lifting of the sample tenfold of common flour system one-tenth, and have advantages such as quality distributed components zero defect concurrently, its product will be widely used in each industrial departments such as space flight, electronics, machinery, electrical equipment.
The at present domestic mature technology that does not still have preparation coating thickness controllable nano coated powder.Simultaneously, along with the high speed development and the crisis of resource of modernization industry, press for searching more and prepare the requirements at the higher level that advanced nanometer copper tungsten coated powder satisfies the different field application with exercisable means more economically.
Summary of the invention
The purpose of this invention is to provide the preparation method that the controlled tungsten of a kind of coating thickness coats copper nanometer composite powder, having solved existing tungsten coating copper clad powder coating thickness can't accurately control, and coats not exclusively the problem of coating thickness lack of homogeneity.
Technical scheme provided by the present invention is, the controlled tungsten of a kind of coating thickness coats the preparation method of copper nanometer composite powder, and needing preparation quality be that the tungsten of M coats the copper composite powder body, and the thickness of clad is H, and its operating procedure is as follows:
Step 1 calculates required WO according to following formula
3Quality m
1
Wherein, M is the quality that required preparation tungsten coats the copper composite powder body, and x is that tungsten coats shared mass percent in the copper composite powder body, k at tungsten
1=1.2 is correction factor;
Described WO
3Granularity be 1.5um;
Step 2 is calculated the quality m of required CuO
2
The quality of cupric oxide: m
2=0.345m
1
Step 3, CuWO
4Preparation
With quality is m
2CuO powder and quality be m
1WO
3Powder evenly mixes, and places stove to carry out sintering mixed powder again, and programming rate remains on 5 ~ 15 ℃/min, just forms lurid CuWO when temperature in the stove reaches 900 ℃ of insulations after 30 minutes
4Powder cools to room temperature then with the furnace;
Step 4 is ground
The CuWO that step 3 is prepared
4Powder grinds;
Step 5, reduction
CuWO after grinding
4Adding quality in the powder is m
3The CuO powder, the even mixing of two kinds of powders is placed in the hydrogen reducing furnace, feeds hydrogen in stove, Ventilation Rate is 33L/min, again with the programming rate of 5 ~ 10 degrees centigrade of per minutes, be warming up to 360 ℃ of insulations 10 minutes, the speed with 3 ~ 5 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min, stop logical hydrogen, feed helium with the speed of 20L/min and cool off, stop helium injection gas after being cooled to room temperature, promptly obtain tungsten and coat copper nanometer composite powder with stove;
Wherein, m
3=M * (1.77y-0.5221);
M is the quality that required preparation tungsten coats the copper composite powder body, and y is that copper coats shared mass percent in the copper composite powder body at tungsten;
The granularity of the CuO powder that uses is to select according to the coating thickness H that required preparation tungsten coats the copper composite powder body in above-mentioned steps 3 and the step 5: if 6nm≤H＜10nm then selects the CuO granularity of 3um; If 10nm≤H＜15nm then selects the CuO granularity of 6um; If 15nm≤H＜20nm then selects the CuO granularity of 9um; If 20nm≤H＜28nm then selects the CuO granularity of 12um; If 28nm≤H≤32nm then selects the CuO granularity of 15um.
Wherein, in the step 3 with CuO powder and WO
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min.
Wherein, in the step 4 at CuWO
4Powder adds the equidirectional absolute ethyl alcohol that is ground to of absolute ethyl alcohol and volatilizees fully, again with CuWO
4Powder was dried 45 minutes under 50 ℃ condition.
Wherein, in the step 5 with CuWO
4Powder and CuO powder evenly mix by planetary ball mill, and drum's speed of rotation is 400r/min, ball milling time 60min.
The invention has the beneficial effects as follows, the first, the tungsten coating copper nano body granularity of preparing by technology of the present invention reaches 40 ~ 60 nano-powder yardsticks; The second, the present invention can accurately control the thickness of W clad in nanometer scale, thereby can satisfy the application requirements of different tungsten copper ratio content; The 3rd, this nanometer coated powder has good sintering character, and this lays the foundation for powder metallurgy prepares tungsten-copper composite material.
Description of drawings
Fig. 1 is that the embodiment of the invention 1 is prepared coating thickness coats the copper nanometer composite powder particle for 8nm tungsten transmission electron microscope photo figure;
Fig. 2 is that the embodiment of the invention 2 is prepared coating thickness coats the copper nanometer composite powder particle for 12nm tungsten transmission electron microscope photo figure;
Fig. 3 is that the embodiment of the invention 3 is prepared coating thickness coats the copper nanometer composite powder particle for 18nm tungsten transmission electron microscope photo figure;
Fig. 4 is that the embodiment of the invention 4 is prepared coating thickness coats the copper nanometer composite powder particle for 28nm tungsten transmission electron microscope photo figure.
The specific embodiment
The invention discloses the preparation method that the controlled tungsten of a kind of coating thickness coats copper nanometer composite powder, needing preparation quality is the tungsten coating copper composite powder body of M, and the thickness of clad is H, and its operating procedure is as follows:
Step 1 is calculated tungstic acid (WO
3) quality m
1
Selecting granularity is the tungstic acid of 1.5um; Foundation needs the mass M of preparation tungsten coating copper composite powder body, and tungsten shared mass percent x in tungsten coating copper composite powder body, calculates the quality of required tungsten, presses chemical molecular formula WO then
3,, calculate required in theory tungstic acid (WO according to the ratio (79.29%) and the aforementioned calculation quality that obtains tungsten of tungsten atom quality in tungstic acid
3) quality, in the actual mechanical process, tungsten generation loss for this reason, is got correction factor k
1=1.2, the mass value of tungstic acid to be revised, the quality of promptly required tungstic acid is:
Step 2 calculates the quality m of required first cupric oxide (CuO)
2
The quality of the tungstic acid that calculates by step 1, by reaction equation:
WO
3+CuO＝CuWO
4
Calculate the quality of cupric oxide: m
2=0.345m
1
Wherein, the granularity of CuO powder coats according to required preparation tungsten that the coating thickness H of copper composite powder body decides: if 6nm≤H＜10nm then selects the CuO granularity of 3um; If 10nm≤H＜15nm then selects the CuO granularity of 6um; If 15nm≤H＜20nm then selects the CuO granularity of 9um; If 20nm≤H＜28nm then selects the CuO granularity of 12um; If 28nm≤H≤32nm then selects the CuO granularity of 15um; The selection of CuO powder granularity draws through a large amount of experiments repeatedly, if it is thick more to make coating thickness H, then the granularity of the cupric oxide powder of Xuan Zeing is big more;
Step 3, high-purity copper tungstate (CuWO
4) preparation
With CuO powder and WO
3Powder evenly mixes drum's speed of rotation 400r ∕ min, ball milling time 180min by calculating good quality by planetary ball mill; Place Muffle furnace to carry out sintering the powder that mixes, CuWO
4Beginning to generate temperature is 550～575 ℃, and programming rate remains on 5 ~ 15 ℃/min, accelerates CuWO with temperature rising reaction speed
4Content constantly increases, and temperature reaches 900 ℃ and will be converted into copper tungstate fully in stove, and temperature reaches 900 ℃ and continues insulation and just form lurid CuWO after 30 minutes in stove
4Powder (purity is 99.8%) cools to room temperature then with the furnace;
Step 4 is ground
Because there be a small amount of the reunion in the copper tungstate that step 3 chemical reaction generates, the copper tungstate that at every turn prepares all needs to grind.During grinding, copper tungstate is put into glass mortar, the amount of putting into is no more than 1/3rd of mortar volume at every turn, the standard adding absolute ethyl alcohol that adds the 10ml absolute ethyl alcohol again by every 50g copper tungstate, the equidirectional absolute ethyl alcohol that is ground to volatilizees fully, connect mortar again and put into baking oven together, under 50 ℃, dried 45 minutes;
Step 5, reduction
In order to satisfy certain ratio requirement of tungsten copper group member, the CuWO after grinding
4Adding quality in the powder in advance is m
3Cupric oxide (just second portion cupric oxide, the selection of its granularity is identical with step 2), two kinds of powders are mixed by planetary ball mill, rotational speed of ball-mill is 400r/min, the ball milling time is 60min; Pave after the mixing and put into the rectangular ceramic crucible tongs, place hydrogen reducing furnace, feed hydrogen in stove, Ventilation Rate is 33L/min, programming rate with 5 ~ 10 degrees centigrade of per minutes, be warming up to 360 ℃ of insulations 10 minutes, the speed with 3 ~ 5 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min, stop logical hydrogen, feed helium with the speed of 20L/min and cool off, stop helium injection gas after being cooled to room temperature, promptly obtain tungsten and coat copper nanometer composite powder with stove;
Wherein, m
3Computing formula be:
M is the quality that required preparation tungsten coats the copper composite powder body, and y is that copper coats shared mass percent in the copper composite powder body at tungsten, the 80%th, and according to chemical formula CuO, the ratio of copper atom quality in cupric oxide.
Characteristics of the present invention are that the coating thickness that prepared tungsten coating copper powder body particle reaches nano-scale, powder is controlled, covers fully, and thickness is even, and simultaneously, the tungsten that can prepare different ratio requirement coats the copper nano body, and operation is simple, economical and efficient.
Embodiment 1
Need produce the 100g coating thickness is the tungsten coating copper composite powder body of 8nm, and wherein, tungsten coats shared mass percent x=50% in the copper composite powder body at tungsten, and copper coats shared mass percent y=50% in the copper composite powder body at tungsten;
Step 1 is calculated required tungstic acid (WO
3) quality m
1
Selecting granularity is the 1.5um tungstic acid.According to needing preparation tungsten to coat the mass M=100g of copper composite powder body, and the mass percent W50Cu50 of tungsten and copper in this coated powder, calculate the quality 50g of required tungsten, then by following chemical molecular formula WO
3,, calculate required in theory tungstic acid (WO according to the ratio (79.29%) of tungsten atom quality in tungstic acid and the quality 50g of the tungsten that obtains of aforementioned calculation
3) quality 63.06g, in the actual mechanical process, tungsten generation loss for this reason, is got correction factor k
1=1.2, the mass value of tungstic acid to be revised, the quality of promptly required tungstic acid is m
1=75.672g;
Step 2 is calculated the quality m of required cupric oxide
2
The quality 75.672g of the tungstic acid that calculates by step 1, by reaction equation:
WO
3+CuO＝CuWO
4
Calculate the quality of cupric oxide: m
2=0.345m
1=26.11g;
Step 3, high-purity copper tungstate (CuWO
4) preparation
With quality is that 26.11g, granularity are that CuO powder and 75.672g, the granularity of 3um is the WO of 1.5um
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min; Place Muffle furnace to carry out sintering the powder that mixes, programming rate is 5 ℃/min, can form lurid pure CuWO when temperature in the stove reaches 900 ℃ of continuation insulations after 30 minutes
4Powder (purity is 99.8%) cools to room temperature then with the furnace.
Step 4 is ground
To make the 101.78g copper tungstate and put into glass mortar, and add the 20ml absolute ethyl alcohol, the equidirectional absolute ethyl alcohol that is ground to volatilizees fully, connects mortar again and puts into baking oven together, under 50 ℃, dries 45 minutes;
Step 5, reduction preparation nanometer coated powder
With the CuWO after grinding
4Add 36.3g in the powder, granularity is the cupric oxide powder of 3um, two kinds of powders are mixed by planetary ball mill, rotational speed of ball-mill is 400r/min, the ball milling time is 60min, pave after the mixing and put into the rectangular ceramic crucible tongs, place hydrogen reducing furnace, feed hydrogen in stove, Ventilation Rate is 33L/min, programming rate with 5 degrees centigrade of per minutes, be warming up to 360 ℃ of insulations 10 minutes, the speed with 3 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min, stop logical hydrogen, feed helium with the speed of 20L/min and cool off, stop helium injection gas after being cooled to room temperature, promptly make 100g tungsten and coat copper nanometer composite powder with stove.
The tungsten for preparing coats copper nanometer composite powder, and as shown in Figure 1, the black copper matrix is in the tungsten clad of the about 8nm of a bed thickness, and covering fully, and thickness is even, and the granularity that tungsten coats the copper composite powder body is 40 ~ 60 nanometers.
Embodiment 2
Need produce the 200g coating thickness is the tungsten coating copper composite powder body of 12nm, and wherein, tungsten coats shared mass percent x=40% in the copper composite powder body at tungsten, and copper coats shared mass percent y=60% in the copper composite powder body at tungsten;
Step 1 is calculated required tungstic acid (WO
3) quality m
1
Selecting granularity is the tungstic acid of 1.5um.According to needing preparation tungsten to coat the mass M=200g of copper composite powder body, and the mass percent W40Cu60 of tungsten and copper in this coated powder, calculate the quality 80g of required tungsten, then by following chemical molecular formula WO
3,, calculate required in theory tungstic acid (WO according to the ratio (79.29%) of tungsten atom quality in tungstic acid and the quality 80g of the tungsten that obtains of aforementioned calculation
3) quality 100.9g, in the actual mechanical process, tungsten generation loss for this reason, is got correction factor k
1=1.2, the mass value of tungstic acid to be revised, the quality of promptly required tungstic acid is m
1=121g.
Step 2 is calculated the quality m of required cupric oxide (CuO)
2
The quality 121g of the tungstic acid that calculates by step 1, by reaction equation:
WO
3+CuO＝CuWO
4
Calculate the quality of cupric oxide: m
2=0.345m
1=41.74g;
Step 3, high-purity copper tungstate (CuWO
4) preparation
With quality is that 41.74g, granularity are that CuO powder and the quality of 6um is that 121g, granularity are the WO of 1.5um
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min; Place Muffle furnace to carry out sintering the powder that mixes, programming rate is 8 ℃/min, can form lurid pure CuWO when temperature in the stove reaches 900 ℃ of continuation insulations after 30 minutes
4Powder (purity is 99.8%) cools to room temperature then with the furnace;
Step 4 is ground
To make the 162.74g copper tungstate and put into glass mortar, and add the 32.5ml absolute ethyl alcohol, the equidirectional absolute ethyl alcohol that is ground to volatilizees fully, connects mortar again and puts into baking oven together, under 50 ℃, dries 45 minutes;
Step 5, reduction preparation nanometer coated powder
With the CuWO after grinding
4Add 107.98g in the powder, granularity is the cupric oxide powder of 6um, two kinds of powders are mixed by planetary ball mill, rotational speed of ball-mill is 400r/min, the ball milling time is 60min, paves after the mixing and puts into the rectangular ceramic crucible tongs, places hydrogen reducing furnace, in stove, feed hydrogen, Ventilation Rate is 33L/min, with the programming rate of 8 degrees centigrade of per minutes, is warming up to 360 ℃ of insulations 10 minutes, speed with 4 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min stops logical hydrogen, feeds helium with the speed of 20L/min and cools off with stove, stop helium injection gas after being cooled to room temperature, promptly make 200g tungsten and coat copper nanometer composite powder.
The tungsten for preparing coats copper nanometer composite powder, and as shown in Figure 2, the black copper matrix is in the tungsten clad of the about 12nm of a bed thickness, and covering fully, and thickness is even, and the granularity that tungsten coats the copper composite powder body is 40 ~ 60 nanometers.
Embodiment 3
Need produce the 500g coating thickness is the tungsten coating copper composite powder body of 18nm, and wherein, tungsten coats shared mass percent x=30% in the copper composite powder body at tungsten, and copper coats shared mass percent y=70% in the copper composite powder body at tungsten;
Step 1 is calculated tungstic acid (WO
3) quality m
1
Selecting granularity is the tungstic acid of 1.5um.According to needing preparation tungsten to coat the mass M=500g of copper composite powder body, and the mass percent W30Cu70 of tungsten and copper in this coated powder, calculate the quality 150g of required tungsten, then by following chemical molecular formula WO
3,, calculate required in theory tungstic acid (WO according to the ratio (79.29%) of tungsten atom quality in tungstic acid and the quality 150g of the tungsten that obtains of aforementioned calculation
3) quality 189.18g, in the actual mechanical process, tungsten generation loss for this reason, is got correction factor k
1=1.2, the mass value of tungstic acid to be revised, the quality of promptly required tungstic acid is m
1=227g;
Step 2 is calculated the quality m of required cupric oxide
2
The quality 227g of the tungstic acid that calculates by step 1, by reaction equation:
WO
3+CuO＝CuWO
4
Calculate the quality of cupric oxide: m
2=0.345m
1=78.315g;
Step 3, high-purity copper tungstate (CuWO
4) preparation
With quality is that 78.315g, granularity are that CuO powder and the quality of 9um is that 227g, granularity are the WO of 1.5um
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min; Place Muffle furnace to carry out sintering the powder that mixes, programming rate is 12 ℃/min, and temperature reaches and can form lurid pure CuWO after 900 ℃ of continuation are incubated 30 minutes in stove
4Powder (purity is 99.8%) cools to room temperature then with the furnace;
Step 4 is ground
To make the 305.32g copper tungstate and put into glass mortar, and add the 61ml absolute ethyl alcohol, the equidirectional absolute ethyl alcohol that is ground to volatilizees fully, connects mortar again and puts into baking oven together, under 50 ℃, dries 45 minutes;
Step 5, reduction preparation nanometer coated powder
With the CuWO after grinding
4Add 358.45g in the powder, the cupric oxide powder of granularity 9um, two kinds of powders are mixed by planetary ball mill, rotational speed of ball-mill is 400r/min, the ball milling time is 60min, paves after the mixing and puts into the rectangular ceramic crucible tongs, places hydrogen reducing furnace, in stove, feed hydrogen, Ventilation Rate is 33L/min, with the programming rate of 8 degrees centigrade of per minutes, is warming up to 360 ℃ of insulations 10 minutes, speed with 4 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min stops logical hydrogen, feeds helium with the speed of 20L/min and cools off with stove, stop helium injection gas after being cooled to room temperature, promptly make 500g tungsten and coat copper nanometer composite powder.
The tungsten for preparing coats copper nanometer composite powder, and as shown in Figure 3, the black copper matrix is in the tungsten clad of the about 18nm of a bed thickness, and covering fully, and thickness is even, and the granularity that tungsten coats the copper composite powder body is 40 ~ 60 nanometers.
Embodiment 4
Need produce the 1000g coating thickness is the tungsten coating copper composite powder body of 28nm, and wherein, tungsten coats shared mass percent x=20% in the copper composite powder body at tungsten, and copper coats shared mass percent y=80% in the copper composite powder body at tungsten;
Step 1 is calculated tungstic acid (WO
3) quality m
1
Selecting granularity is the tungstic acid of 1.5um.According to needing preparation tungsten to coat the mass M=1000g of copper composite powder body, and the mass percent W20Cu80 of tungsten and copper in this coated powder, calculate the quality 200g of required tungsten, then by following chemical molecular formula WO
3,, calculate required in theory tungstic acid (WO according to the ratio (79.29%) of tungsten atom quality in tungstic acid and the quality 200g of the tungsten that obtains of aforementioned calculation
3) quality 252.24g, in the actual mechanical process, tungsten generation loss for this reason, is got correction factor k
1=1.2, the mass value of tungstic acid to be revised, the quality of promptly required tungstic acid is m
1=302.69g;
Step 2 is calculated required oxidation copper mass m
2
The quality 302.69g of the tungstic acid that calculates by step 1, by reaction equation:
WO
3+CuO＝CuWO
4
Calculate the quality of cupric oxide: m
2=0.345m
1=104.43g;
Step 3, high-purity copper tungstate (CuWO
4) preparation
With quality is that 104.43g, granularity are that CuO powder and 302.69g, the granularity of 15um is the WO of 1.5um
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min; Place Muffle furnace to carry out sintering the powder that mixes, programming rate is 15 ℃/min, and temperature reaches and can form lurid pure CuWO after 900 ℃ of continuation are incubated 30 minutes in stove
4Powder (purity is 99.8%) cools to room temperature then with the furnace;
Step 4 is ground
To make the 407.12g copper tungstate and put into glass mortar, and add the 81.4ml absolute ethyl alcohol, the equidirectional absolute ethyl alcohol that is ground to volatilizees fully, connects mortar again and puts into baking oven together, under 50 ℃, dries 45 minutes;
Step 5, reduction preparation nanometer coated powder
With the CuWO after grinding
4Add 894g in the powder, granularity is the cupric oxide powder of 15um, two kinds of powders are mixed by planetary ball mill, rotating speed is 400r/min, the ball milling time is 60min, pave after the mixing and put into the rectangular ceramic crucible tongs, place hydrogen reducing furnace, feed hydrogen in stove, Ventilation Rate is 33L/min, programming rate with 10 degrees centigrade of per minutes, be warming up to 360 ℃ of insulations 10 minutes, the speed with 5 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min, stop logical hydrogen, feed helium with the speed of 20L/min and cool off, stop helium injection gas after being cooled to room temperature, promptly make 1000g tungsten and coat copper nanometer composite powder with stove.
The tungsten for preparing coats copper nanometer composite powder, and as shown in Figure 4, the black copper matrix is in the tungsten clad of the about 28nm of a bed thickness, and covering fully, and thickness is even, and the granularity that tungsten coats the copper composite powder body is 40 ~ 60 nanometers.
Claims (4)
1. the preparation method of the controlled tungsten coating of a coating thickness copper nanometer composite powder is characterized in that, needing preparation quality be the tungsten coating copper composite powder body of M, and the thickness of clad is H, and its operating procedure is as follows:
Step 1 calculates required WO according to following formula
3Quality m
1
Wherein, M is the quality that required preparation tungsten coats the copper composite powder body, and x is that tungsten coats shared mass percent in the copper composite powder body, k at tungsten
1=1.2 is correction factor;
Described WO
3Granularity be 1.5um;
Step 2 is calculated the quality m of required CuO
2
The quality of cupric oxide: m
2=0.345m
1
Step 3, CuWO
4Preparation
With quality is m
2CuO powder and quality be m
1WO
3Powder evenly mixes, and places stove to carry out sintering mixed powder again, and programming rate remains on 5 ~ 15 ℃/min, just forms lurid CuWO when temperature in the stove reaches 900 ℃ of insulations after 30 minutes
4Powder cools to room temperature then with the furnace;
Step 4 is ground
The CuWO that step 3 is prepared
4Powder grinds;
Step 5, reduction
CuWO after grinding
4Adding quality in the powder is m
3The CuO powder, the even mixing of two kinds of powders is placed in the hydrogen reducing furnace, feeds hydrogen in stove, Ventilation Rate is 33L/min, again with the programming rate of 5 ~ 10 degrees centigrade of per minutes, be warming up to 360 ℃ of insulations 10 minutes, the speed with 3 ~ 5 degrees centigrade of per minutes is warming up to 800 ℃ again, insulation 30min, stop logical hydrogen, feed helium with the speed of 20L/min and cool off, stop helium injection gas after being cooled to room temperature, promptly obtain tungsten and coat copper nanometer composite powder with stove;
Wherein, m
3=M * (1.77y-0.5221);
M is the quality that required preparation tungsten coats the copper composite powder body, and y is that copper coats shared mass percent in the copper composite powder body at tungsten;
The granularity of the CuO powder that uses is to select according to the coating thickness H that required preparation tungsten coats the copper composite powder body in above-mentioned steps 3 and the step 5: if 6nm≤H＜10nm then selects the CuO granularity of 3um; If 10nm≤H＜15nm then selects the CuO granularity of 6um; If 15nm≤H＜20nm then selects the CuO granularity of 9um; If 20nm≤H＜28nm then selects the CuO granularity of 12um; If 28nm≤H≤32nm then selects the CuO granularity of 15um.
2. coat the preparation method of copper nanometer composite powder according to the described tungsten of claim 1, it is characterized in that: in the described step 3 with CuO powder and WO
3Powder evenly mixes by planetary ball mill, drum's speed of rotation 400r ∕ min, ball milling time 180min.
3. coat the preparation method of copper nanometer composite powder according to the described tungsten of claim 1, it is characterized in that: in the described step 4 at CuWO
4Powder adds the equidirectional absolute ethyl alcohol that is ground to of absolute ethyl alcohol and volatilizees fully, again with CuWO
4Powder was dried 45 minutes under 50 ℃ condition.
4. coat the preparation method of copper nanometer composite powder according to the described tungsten of claim 1, it is characterized in that: in the described step 5 with CuWO
4Powder and CuO powder evenly mix by planetary ball mill, and drum's speed of rotation is 400r/min, ball milling time 60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102098561A CN101850420B (en) | 2010-06-25 | 2010-06-25 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102098561A CN101850420B (en) | 2010-06-25 | 2010-06-25 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101850420A true CN101850420A (en) | 2010-10-06 |
| CN101850420B CN101850420B (en) | 2012-02-08 |
Family
ID=42802191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102098561A Expired - Fee Related CN101850420B (en) | 2010-06-25 | 2010-06-25 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101850420B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252101A (en) * | 2016-09-27 | 2016-12-21 | 西北工业大学 | The preparation method of ultracapacitor nanometer Cupric wolframate. polyhedron electrode material |
| CN110172607A (en) * | 2019-04-11 | 2019-08-27 | 全球能源互联网欧洲研究院 | A kind of preparation method of graphene enhancing Cu tailings |
| CN108927527B (en) * | 2017-05-24 | 2021-10-08 | 河南科技大学 | Preparation method of nano W-xCu alloy and nano W-xCu alloy |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1363708A (en) * | 2001-12-13 | 2002-08-14 | 北京科技大学 | Process for preparing W-Cu alloy with superfine crystal grains |
| CN1539579A (en) * | 2003-04-22 | 2004-10-27 | 中南大学 | Method for preparing high diffusive composite powder of wolfram steel |
| CN1730207A (en) * | 2005-08-04 | 2006-02-08 | 自贡硬质合金有限责任公司 | Production method of tungsten copper composite powder |
| CN101288905A (en) * | 2008-06-03 | 2008-10-22 | 西安理工大学 | Preparation method of copper cladding tungsten composite powder |
| CN101428345A (en) * | 2007-11-09 | 2009-05-13 | 北京有色金属研究总院 | Method of manufacturing ultrafine molybdenum powder or ultrafine tungsten powder surface clad metal copper |
-
2010
- 2010-06-25 CN CN2010102098561A patent/CN101850420B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1363708A (en) * | 2001-12-13 | 2002-08-14 | 北京科技大学 | Process for preparing W-Cu alloy with superfine crystal grains |
| CN1539579A (en) * | 2003-04-22 | 2004-10-27 | 中南大学 | Method for preparing high diffusive composite powder of wolfram steel |
| CN1730207A (en) * | 2005-08-04 | 2006-02-08 | 自贡硬质合金有限责任公司 | Production method of tungsten copper composite powder |
| CN101428345A (en) * | 2007-11-09 | 2009-05-13 | 北京有色金属研究总院 | Method of manufacturing ultrafine molybdenum powder or ultrafine tungsten powder surface clad metal copper |
| CN101288905A (en) * | 2008-06-03 | 2008-10-22 | 西安理工大学 | Preparation method of copper cladding tungsten composite powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252101A (en) * | 2016-09-27 | 2016-12-21 | 西北工业大学 | The preparation method of ultracapacitor nanometer Cupric wolframate. polyhedron electrode material |
| CN106252101B (en) * | 2016-09-27 | 2018-06-08 | 西北工业大学 | The preparation method of ultracapacitor nanometer copper tungstate polyhedron electrode material |
| CN108927527B (en) * | 2017-05-24 | 2021-10-08 | 河南科技大学 | Preparation method of nano W-xCu alloy and nano W-xCu alloy |
| CN110172607A (en) * | 2019-04-11 | 2019-08-27 | 全球能源互联网欧洲研究院 | A kind of preparation method of graphene enhancing Cu tailings |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101850420B (en) | 2012-02-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104700961B (en) | A kind of graphene/silver composite material and preparation method thereof | |
| CN106435323B (en) | A kind of oxide dispersion intensifying ODS high-entropy alloys and preparation method thereof | |
| CN104711443B (en) | A kind of graphene/copper composite material and preparation method thereof | |
| CN105695788B (en) | A kind of graphene enhancing nickel-base composite material and preparation method thereof | |
| CN102277525B (en) | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel | |
| CN105624445A (en) | Preparation method of graphene-reinforced copper-based composite | |
| CN107604186B (en) | A kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method | |
| CN105063403A (en) | Preparation method of copper matrix graphene alloy | |
| CN104651703B (en) | A kind of method preparing oxide dispersion intensifying ferrous alloy | |
| CN102676858B (en) | Preparation method of high density boral metal matrix composite material | |
| CN103924111B (en) | The preparation method of a kind of Wimet nanometer particle size powder and high performance sintered block materials | |
| CN105063402A (en) | Preparation method of aluminum base graphene alloy | |
| Liu et al. | Quantitative characterization of the microstructure and properties of nanocrystalline WC–Co bulk | |
| CN104630639B (en) | A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method | |
| CN102747254A (en) | Reinforced intragranular aluminum matrix composites with nano ceramic particles added externally and preparation process thereof | |
| CN101709436A (en) | Preparation method of high thermal conductivity aluminum matrix composite | |
| CN107598175A (en) | A kind of graphene and titanium alloy composite powder ball-milling preparation method | |
| CN101850420B (en) | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating | |
| CN102554215B (en) | Thermal treatment method for nanometer tantalum powder | |
| Gai et al. | Particle shape modification and related property improvements | |
| He et al. | State and effect of oxygen on high entropy alloys prepared by powder metallurgy | |
| Tyrpekl et al. | Synthesis of dense yttrium-stabilised hafnia pellets for nuclear applications by spark plasma sintering | |
| CN103934451A (en) | Method for preparing aluminum oxide dispersion strengthening copper alloy powder | |
| CN102924083B (en) | Method for preparing zirconium carbide ceramic powder | |
| CN105478745B (en) | A kind of method that low-temperature sintering prepares tungsten slab |
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: 20120208 Termination date: 20140625 |
|
| EXPY | Termination of patent right or utility model |