CN101928867A - Method for preparing tungsten-copper alloy based on loose-loading infiltration method - Google Patents
Method for preparing tungsten-copper alloy based on loose-loading infiltration method Download PDFInfo
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Abstract
The invention discloses a method for preparing a tungsten-copper alloy based on a loose-loading infiltration method. The method comprises the following specific steps of: one, grain size selection of tungsten powder, copper powder and nickel powder; two, material mixing, namely calculating the masses of the tungsten and the copper according to the mass percentage of the tungsten-copper alloy to be prepared, weighing the tungsten powder, weighing the nickel powder which accounts for 0.05 to 0.15 percent of the total mass of the tungsten and the copper and weighing ethanol which accounts for 5 to 15 percent of the total mass of the tungsten and the copper according to the grain size selected in the step one, weighing pre-adding copper powder which is 5 percent of the total mass of the tungsten and the copper, and mechanically mixing the tungsten powder, the nickel powder, the ethanol and the pre-adding copper powder weighed in the step together; three, die-filling, namely filling the mixed powder into a graphite die, dropping gasoline into the die, and tamping the mixture to obtain a blank material; four, infiltration sintering, namely performing the infiltration sintering in a sintering furnace; and five, demoulding. The tungsten-copper alloy prepared by the method has sizes, shapes and components of any requirements, and is prepared without a steel die and a special pressing or forming device.
Description
Technical field
The invention belongs to the Composite Preparation technical field, relate to a kind of method for preparing tungsten-copper alloy based on pine dress infiltration method.
Background technology
Tungsten-copper composite material is by neither dissolving each other of forming of tungsten and copper and do not form the mixed uniformly tissue of two-phase monomer of intermetallic compound, is commonly referred to as tungsten copper pseudoalloy (pseudo-alloy).This just combination makes tungsten-copper composite material become both to have high temperature resistant, high strength, the high-density of tungsten, has the characteristics such as high strength, high-density, high thermal conductivity of copper again, makes it be widely used in every field such as space flight, electronics, machinery, electrical equipment.Yet, high speed development along with modernization industry, some occasion has demand to large-size tungsten-copper alloy, slender rod piece tungsten-copper alloy or special-shaped tungsten-copper alloy, and these tungsten-copper alloys of prior art for preparing need steel die and special-purpose compacting or molding device, cost height and complex process.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the method for tungsten-copper alloy, solved in the prior art higherly, need steel die and special-purpose compacting or the problem of molding device for size, the shape need of preparation tungsten-copper alloy based on pine dress infiltration method.
The technical solution adopted in the present invention is, a kind ofly prepares the method for tungsten-copper alloy based on pine dress infiltration method, and this method is specifically implemented according to the following steps:
Step 1, get tungsten powder, copper powder, nickel powder particulate material respectively, tungsten powder particle diameter is wherein selected in the ratio that will prepare tungsten-copper alloy;
Step 2, batch mixing:
Calculate the quality of tungsten and copper by the mass percent of made tungsten-copper alloy, total mass number is unit with the gram, and the particle diameter of selecting according to step 1 takes by weighing tungsten powder,
0.05%-0.15% by tungsten and copper total mass takes by weighing nickel powder,
Take by weighing the copper powder conduct by 5% of tungsten and copper total mass and add copper powder in advance,
Other calculates the numerical value of tungsten and copper total mass 5%-15%, is that unit takes by weighing ethanol with this identical numerical value, with the milliliter,
The tungsten powder that this step is alleged, nickel powder, add copper powder and ethanol in advance, common mechanically mixing 6-20 hour, obtain mixed powder;
Step 3, dress mould:
The mixed powder that step 2 is obtained is packed in the graphite jig, with the cubic centimetre is the volume that unit calculates graphite jig, calculates the numerical value of this volume 1%, is that unit takes by weighing gasoline with this identical numerical value, with the milliliter, the gasoline that takes by weighing is added in the graphite jig, obtain blank after the tamping;
Step 4, melting infiltration sintering:
The graphite jig that step 3 is installed blank is put into hydrogen or helium high temperature protection atmosphere or vacuum sintering furnace, in the graphite jig upper end copper material is set simultaneously, this copper material quality is 120% of the copper content that calculates of step 2, and 1300 ℃-1400 ℃ of controlled temperature are incubated 2-2.5 hour and carry out melting infiltration sintering;
Step 5, the demoulding: the blank that step 4 is sintered takes out from graphite jig.
The invention has the beneficial effects as follows, efficiently solve the difficult problem of preparation large-size tungsten-copper alloy, slender rod piece tungsten-copper alloy or special-shaped tungsten-copper alloy, the size of prepared tungsten-copper alloy, shape requirement arbitrarily, do not need steel die and special-purpose compacting or molding device, have rapidly and efficiently, make things convenient for the characteristics of economy, chipless or few smear metal.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Pine dress infiltration method of the present invention prepares the method for tungsten-copper composite material, implements according to the following steps:
Step 1. is got tungsten powder, copper powder, nickel powder particulate material respectively:
The tungsten powder particle diameter is selected in the ratio that table 1 will prepare tungsten-copper alloy, select the little tungsten powder of particle diameter when the W content in the tungsten-copper alloy is higher, select the big tungsten powder of particle diameter when W content is on the low side, the tungsten powder of particle diameter of needing when tungsten-copper alloy is selected specific proportions for use to vary in size carries out mix and match, copper powder size is the 48-58 micron, and the nickel powder particle diameter is the 58-75 micron.
Table 1 is a synopsis of selecting suitable tungsten powder particle diameter
The tungsten-copper alloy composition | Density (gram/cubic centimetre) | Tungsten powder particle diameter (micron) | The tungsten powder shape |
W50Cu50 | 12.0 | 60-75 | Subsphaeroidal |
W60Cu40 | 12.8 | 15-55 | Subsphaeroidal |
W70Cu30 | 14.0 | 6-12 | Subsphaeroidal |
W80Cu20 | 15.2 | 0.05-1 | Irregular |
Step 2. batch mixing:
Calculate the quality of tungsten and copper by the mass percent of made tungsten-copper alloy, total mass number is unit with the gram, and the particle diameter of selecting according to step 1 takes by weighing tungsten powder,
0.05%-0.15% by tungsten and copper total mass takes by weighing nickel powder,
Take by weighing the copper powder conduct by 5% of tungsten and copper total mass again and add copper powder in advance,
Pressing the numerical value of tungsten and copper total mass 5%-15% in addition, is that unit takes by weighing ethanol with this identical numerical value, with the milliliter,
The tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance common mechanically mixing 6-20 hour, obtain mixed powder;
Step 3. dress mould:
The mixed powder that step 2 obtains is packed in the graphite jig of " high strength, high-density, high thermal conductivity ", then, with the cubic centimetre is the volume that unit calculates graphite jig, calculate the numerical value of this volume 1% again, with this identical numerical value, with the milliliter is that unit takes by weighing industrial naptha, the industrial naptha that takes by weighing is added in the graphite jig, with its tamping, obtain blank with the pressure of 0.5-240MPa.
Step 4. melting infiltration sintering:
The graphite jig that step 3 is installed blank is put into (hydrogen or helium) high temperature protection atmosphere or vacuum sintering furnace; in the graphite jig upper end copper material that infiltration is used is set simultaneously; the copper material quality that this infiltration is used is 120% of the copper content that calculates of step 2; 1300 ℃-1400 ℃ of controlled temperature are incubated 2-2.5 hour and carry out melting infiltration sintering.
Step 5. demoulding:
The blank that step 4 is sintered takes out from graphite jig, and the pressure during taking-up is 1.5-750MPa.
In step 3, when tungsten-copper alloy parts to be processed were shaped piece, graphite jig was made segmental mandrel, was convenient to the taking-up of part; When tungsten-copper alloy parts to be processed were regular shape, as bar-shaped, tubular or square, graphite jig was made die cavity by the appearance profile line.
Embodiment 1
Preparation size is W70Cu30(tungsten 70 bronze medals 30 of Φ 8 * 150mm) alloy, what present embodiment was made is the pole shape of rule.
Step 1. is selected powder granularity:
Because the W content of made tungsten-copper alloy is 70%, be the subsphaeroidal powder of 6-8 micron so select the median size of tungsten powder, copper powder size is the 48-55 micron, the nickel powder particle diameter is the 58-65 micron.
Step 2. batch mixing: calculating tungsten by the mass percent of made W70Cu30 tungsten-copper alloy is that 74.9 grams and copper are 32.1 to restrain, take by weighing tungsten powder 74.9 grams of the selected particle diameter of step 1, take by weighing nickel powder 0.1 gram that accounts for tungsten and copper total mass per-cent 0.1% again, take by weighing by 5% of tungsten and copper total mass and to add copper powder 5.35 gram in advance, the numerical value that other calculates tungsten and copper total mass 10% is 10 grams, 10 to be numerical value, to be that unit takes by weighing 10 milliliters of ethanol with the milliliter, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance, common mechanically mixing 6 hours.
Step 3. dress mould: the mixed powder 80.26 of step 2 is restrained in the cylindric graphite jig of aperture Φ 8 * 200mm " high strength, high-density, the high thermal conductivity " of packing into, is unit with the cubic centimetre, and the volume that calculates graphite jig is 10cm
3, the numerical value that calculates this volume 1% is 0.1, is that unit takes by weighing 0.1 milliliter in gasoline with numerical value 0.1, with the milliliter, again with the pressure of 0.5MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into high-temperature hydrogen protective atmosphere sintering oven; preset copper content 38.52 grams (120% of 2 copper masses that draw, 32.1 grams calculating gained set by step) simultaneously in the mould upper end; 1400 ℃ of controlled temperature are incubated 2.0 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, the rod iron that blank is used 8 millimeters of diameters from graphite jig takes out with the pressure of about 1.5MPa, promptly gets 8 millimeters of desired diameters, length is greater than 150 millimeters tungsten-copper alloy.
Embodiment 2
Preparation size is W70Cu30(tungsten 70 bronze medals 30 of 100 * 100 * 5mm) alloy, what present embodiment was made is the rectangle of rule.
Step 1. is selected powder granularity
Because the W content of made tungsten-copper alloy is 70%, be the subsphaeroidal powder of 10-12 micron so select the median size of tungsten powder, it is the 50-58 micron that the particle diameter of copper powder is selected, nickel powder particle diameter 60-75 micron.
Step 2. batch mixing: calculating tungsten by the mass percent of made W70Cu30 tungsten-copper alloy is that 497 grams and copper are 216 to restrain, take by weighing tungsten powder 497 grams of the selected particle diameter of step 1, take by weighing nickel powder 0.71 gram that accounts for tungsten and copper total mass per-cent 0.1% again, take by weighing by 5% of tungsten and copper total mass and to add copper powder 35.5 gram in advance, the numerical value that other calculates tungsten and copper total mass 10% is 71 grams, 71 to be numerical value, to be that unit takes by weighing 71 milliliters of ethanol with the milliliter, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance, common mechanically mixing 20 hours.
Step 3. dress mould: mixed powder 533.21 grams of step 2 are packed in the graphite jig of rectangle " high strength, high-density, high thermal conductivity " of 100 * 100 * 20mm, are unit with the cubic centimetre, calculate the volume 200cm of graphite jig
3, the numerical value that calculates this volume 1% is 2, is that unit takes by weighing 2 milliliters in gasoline with numerical value 2, with the milliliter, again with the pressure of 100MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into high temperature helium protective atmosphere sintering oven; preset copper content 255.6 grams (120% of 2 copper masses that draw, 216 grams calculating gained set by step) simultaneously in the mould upper end; 1350 ℃ of controlled temperature are incubated 2.2 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, briquet used 100 * 100 millimeters bloom take out from graphite jig with the pressure of about 300MPa, promptly obtaining the desired end is 100 * 100 millimeters, tall and big in the rectangle tungsten-copper alloy of 5mm.
Embodiment 3
Preparation size is external diameter Φ 200mm, internal diameter Φ 100mm, W60Cu40(tungsten 60 bronze medals 40 of thick 12 mm) alloy, what present embodiment was made is the cylindric of rule.
Step 1. is selected powder granularity:
Because the W content of made tungsten-copper alloy is 60%, be the subsphaeroidal powder of 15-55 micron so select the median size of tungsten powder, it is the 50-58 micron that the particle diameter of copper powder is selected, nickel powder particle diameter 60-75 micron.
Step 2. batch mixing: calculating tungsten by the mass percent of made W60Cu40 tungsten-copper alloy is that 2051.68 grams and copper are 1367.78 to restrain, take by weighing tungsten powder 2051.68 grams of the selected particle diameter of step 1, take by weighing nickel powder 3.42 grams that account for tungsten and copper total mass per-cent 0.1% again, take by weighing by 5% of tungsten and copper total mass and to add copper powder 170.97 gram in advance, the numerical value that other calculates tungsten and copper total mass 10% is 340 grams, 340 to be numerical value, to be that unit takes by weighing 340 milliliters of ethanol with the milliliter, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance, common mechanically mixing 10 hours.
Step 3. dress mould: the mixed powder 2256.85 of step 2 is restrained the internal diameter Φ 200mm that packs into, center bar Φ 100mm, in the graphite jig of thick 30 mm " high strength, high-density, high thermal conductivity ", be that the volume that unit calculates graphite jig is 3400cm with the cubic centimetre
3, the numerical value that calculates this volume 1% is 34, be 34, be that unit takes by weighing 34 milliliters in gasoline with the milliliter with numerical value, again with the pressure of 235.5MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into vacuum sintering furnace, preset copper 1641.34 grams (120% of 2 copper masses that draw, 1367.78 grams calculating gained set by step) simultaneously in the mould upper end, 1300 ℃ of controlled temperature are incubated 2.5 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, briquet is used external diameter Φ 200mm from graphite jig, the rod iron of internal diameter Φ 100mm takes out with the pressure of about 706.5MPa, promptly obtains desired outer diameter Φ 200mm, internal diameter Φ 100mm, thickness is greater than the cylindric tungsten-copper alloy of 12 mm.
Embodiment 4
Preparation size is W50Cu50 (tungsten copper 50) alloy of 150 * 150 * 10mm, and what present embodiment was made is the rectangle of rule.
Step 1. is selected powder granularity
Because the W content of made tungsten-copper alloy is 50%, be the subsphaeroidal powder of 60-65 micron so select the median size of tungsten powder, it is the 50-55 micron that the particle diameter of copper powder is selected, nickel powder particle diameter 70-75 micron.
Step 2. batch mixing: calculating tungsten by the mass percent of made W50Cu50 tungsten-copper alloy is that 1371.6 grams and copper are 1371.6 to restrain, take by weighing tungsten powder 1371.6 grams of the selected particle diameter of step 1, take by weighing nickel powder 1.37 grams that account for tungsten and copper total mass per-cent 0.05% again, take by weighing by 5% of tungsten and copper total mass and to add copper powder 137.2 gram in advance, the numerical value that other calculates tungsten and copper total mass 5% is 137 grams, be 137, be that unit takes by weighing 137 milliliters of ethanol with the milliliter with numerical value, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance, common mechanically mixing 15 hours.
Step 3. dress mould: mixed powder 1510.37 grams that step 2 is obtained are packed in rectangle " high strength, high-density, the high thermal conductivity " graphite jig of 150 * 150 * 10mm, are that the volume that unit calculates graphite jig is 225 cm with the cubic centimetre
3, the numerical value that calculates this volume 1% is 2.25,2.25 being numerical value, being that unit takes by weighing 2.25 milliliters in gasoline with the milliliter, again with the pressure of 100MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into high temperature helium protective atmosphere sintering oven; preset copper content 1645.9 grams (120% of 2 copper masses that draw, 1371.6 grams calculating gained set by step) simultaneously in the mould upper end; 1350 ℃ of controlled temperature are incubated 2.2 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, briquet used 150 * 150 millimeters bloom take out from graphite jig with the pressure of about 300MPa, promptly obtaining the desired end is 150 * 150 millimeters, tall and big in 10 millimeters rectangle tungsten-copper alloy.
Embodiment 5
Preparation size is W80Cu20(tungsten 80 bronze medals 20 of Φ 4 * 300mm) alloy, what present embodiment was made is the carefully bar-shaped of rule.
Step 1. is selected powder granularity:
Because the W content of made tungsten-copper alloy is 80%, be the subsphaeroidal powder of 0.05-1 micron so select the median size of tungsten powder, copper powder size is the 48-55 micron, the nickel powder particle diameter is the 60-65 micron.
Step 2. batch mixing: the mass percent by made W80Cu20 tungsten-copper alloy calculates tungsten powder 47.24 grams and copper 11.81 grams, take by weighing tungsten powder 47.24 grams of the selected particle diameter of step 1, take by weighing nickel powder 0.09 gram that accounts for tungsten and copper total mass per-cent 0.15% again, the numerical value that other calculates tungsten and copper total mass 15% is 9 grams, 9 to be numerical value, to be that unit takes by weighing 9 milliliters of ethanol with the milliliter, take by weighing by 5% of tungsten and copper total mass and to add copper powder 2.95 gram in advance, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance mixed the common mechanically mixing in back 8 hours.
Step 3. dress mould: mixed powder 50.28 grams of step 2 are packed in " high strength, high-density, high thermal conductivity " graphite jig of aperture Φ 4 * 300mm, are that the volume that unit calculates graphite jig is 4cm with the cubic centimetre
3, the numerical value that calculates this volume 1% is 0.04,0.04 being numerical value, being that unit takes by weighing 0.04 milliliter in gasoline with the milliliter, again with the pressure of 0.5MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into high-temperature hydrogen protective atmosphere sintering oven; preset copper content 14.12 grams (120% of 2 copper masses that draw, 11.81 grams calculating gained set by step) simultaneously in the mould upper end; 1400 ℃ of controlled temperature are incubated 2.3 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, the rod iron that briquet is used 4 millimeters of diameters from graphite jig takes out with the pressure of about 2.5MPa, promptly gets 4 millimeters of desired diameters, length is greater than 300 millimeters thin bar-shaped tungsten-copper alloy.
Embodiment 6
Preparation size is L shaped shape, and volume is 1700cm
3W60Cu40(tungsten 60 bronze medals 40) alloy, what present embodiment was made is irregular shape, adopts segmental mandrel to make.
Step 1. is selected powder granularity:
Because the W content of made tungsten-copper alloy is 60%, be the subsphaeroidal powder of 35-55 micron so select the median size of tungsten powder, it is the 50-55 micron that the particle diameter of copper powder is selected, nickel powder particle diameter 60-70 micron.
Step 2. batch mixing: calculating tungsten by the mass percent of made W60Cu40 tungsten-copper alloy is that 1025.84 grams and copper are 683.89 to restrain, take by weighing tungsten powder 1025.84 grams of the selected particle diameter of step 1, take by weighing nickel powder 1.7 grams that account for tungsten and copper total mass per-cent 0.1% again, take by weighing by 5% of tungsten and copper total mass and to add copper powder 85.49 gram in advance, the numerical value that other calculates tungsten and copper total mass 10% is 170 grams, 170 to be numerical value, to be that unit takes by weighing 170 milliliters of ethanol with the milliliter, the tungsten powder that this step is alleged, nickel powder, ethanol and add copper powder in advance, common mechanically mixing 15 hours.
Step 3. dress mould: mixed powder 1128.42 grams of step 2 are packed in the irregular distinguish graphite jig of made, are that the volume that unit calculates graphite jig is 1700cm with the cubic centimetre
3, the numerical value that calculates this volume 1% is 17, be 17, be that unit takes by weighing 17 milliliters in gasoline with the milliliter with numerical value, again with the pressure of 200MPa with its tamping.
Step 4. melting infiltration sintering: the graphite jig that step 3 is installed blank is put into vacuum sintering furnace, preset copper 820.67 grams (120% of 2 copper masses that draw, 683.89 grams calculating gained set by step) simultaneously in the mould upper end, 1350 ℃ of controlled temperature are incubated 2.3 hours and carry out melting infiltration sintering.
Step 5. demoulding: etc. after step 4 sintering finishes, from graphite jig, use rod iron to take out briquet with the pressure of about 650MPa, promptly obtain desired irregular L shaped shape tungsten-copper alloy.
Pine dress infiltration method of the present invention prepares the method for tungsten-copper composite material; the tungsten powder that certain particle size is formed, in advance add copper powder and additive mechanically mixing evenly after; be contained in tamping in the graphite jig of " high strength, high-density, the high thermal conductivity " that will prepare shape; in high temperature protection atmosphere sintering furnace or vacuum oven, adopt infiltration technique to prepare the tungsten-copper composite material that meets the demands at last.The size of the prepared tungsten-copper alloy of the inventive method, shape, composition requirement arbitrarily do not need steel die and special-purpose compacting or molding device, realize rapidly and efficiently, make things convenient for economy, chipless or few smear metal, aim of saving.
Claims (7)
1. one kind prepares the method for tungsten-copper alloy based on pine dress infiltration method, and it is characterized in that: this method is specifically implemented according to the following steps:
Step 1, get tungsten powder, copper powder, nickel powder particulate material respectively, tungsten powder particle diameter is wherein selected in the ratio that will prepare tungsten-copper alloy;
Step 2, batch mixing:
Calculate the quality of tungsten and copper by the mass percent of made tungsten-copper alloy, total mass number is unit with the gram, and the particle diameter of selecting according to step 1 takes by weighing tungsten powder,
0.05%-0.15% by tungsten and copper total mass takes by weighing nickel powder,
Take by weighing the copper powder conduct by 5% of tungsten and copper total mass and add copper powder in advance,
Other calculates the numerical value of tungsten and copper total mass 5%-15%, is that unit takes by weighing ethanol with this identical numerical value, with the milliliter,
The tungsten powder that this step is alleged, nickel powder, add copper powder and ethanol in advance, common mechanically mixing 6-20 hour, obtain mixed powder;
Step 3, dress mould:
The mixed powder that step 2 is obtained is packed in the graphite jig, with the cubic centimetre is the volume that unit calculates graphite jig, calculates the numerical value of this volume 1%, is that unit takes by weighing gasoline with this identical numerical value, with the milliliter, the gasoline that takes by weighing is added in the graphite jig, obtain blank after the tamping;
Step 4, melting infiltration sintering:
The graphite jig that step 3 is installed blank is put into hydrogen or helium high temperature protection atmosphere or vacuum sintering furnace, in the graphite jig upper end copper material is set simultaneously, this copper material quality is 120% of the copper content that calculates of step 2, and 1300 ℃-1400 ℃ of controlled temperature are incubated 2-2.5 hour and carry out melting infiltration sintering;
Step 5, the demoulding: the blank that step 4 is sintered takes out from graphite jig.
2. method according to claim 1 is characterized in that: the choice criteria of tungsten powder particles is in the step 1:
When the tungsten-copper alloy composition was W50Cu50, choosing the tungsten powder particles particle diameter was the 60-75 micron;
When the tungsten-copper alloy composition was W60Cu40, choosing the tungsten powder particles particle diameter was the 15-55 micron;
When the tungsten-copper alloy composition was W70Cu30, choosing the tungsten powder particles particle diameter was the 6-12 micron;
When the tungsten-copper alloy composition was W80Cu20, choosing the tungsten powder particles particle diameter was the 0.05-1 micron.
3. method according to claim 1 is characterized in that: copper powder size is the 48-58 micron in the step 1.
4. method according to claim 1 is characterized in that: the nickel powder particle diameter is the 58-75 micron in the step 1.
5. method according to claim 1 is characterized in that: the pressure of tamping is 0.5-240Mpa in the step 3.
6. method according to claim 1 is characterized in that: the pressure that takes out from graphite jig in the step 5 is 1.5-750Mpa.
7. method according to claim 1 is characterized in that: the graphite jig in the step 3 is the mould of high strength, high-density, high thermal conductivity.
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