CN106216705A - A kind of preparation method of 3D printing fine grained simple substance globular metallic powder - Google Patents
A kind of preparation method of 3D printing fine grained simple substance globular metallic powder Download PDFInfo
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- CN106216705A CN106216705A CN201610832136.8A CN201610832136A CN106216705A CN 106216705 A CN106216705 A CN 106216705A CN 201610832136 A CN201610832136 A CN 201610832136A CN 106216705 A CN106216705 A CN 106216705A
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention relates to the preparation method of a kind of 3D printing fine grained simple substance globular metallic powder, belong to metal dust preparing technical field.This preparation method uses high pure metal bulk to be raw material, and in an inert atmosphere by arc evaporation, the conduction of heat and the activity that are filled with hydrogen control metal gas atom are allowed to cool deposition and obtain high purity elemental nano metal powder granule simultaneously;Then high purity elemental nano metal powder is carried out agglomeration granulation, obtain the micron order elemental metals powder of higher density;Finally micron order elemental metals powder after pelletize is carried out heat treatment, by degumming and densification consolidation, it is thus achieved that granularity, sphericity, mobility and oxygen content meet 3D and print the elemental metals powder particle required.This method is compared with other processes, strong to the controllability of the sphericity of metallic particles, particle diameter distribution and oxygen content, and has that technique is simple and the advantage of low cost.
Description
Technical field
The present invention relates to the preparation method of a kind of 3D printing fine grained simple substance globular metallic powder, belong to metal dust system
Standby technical field.
Background technology
It is all with chemistry etc. that 3D printing technique combines digital modeling techniques, Electromechanical Control technology, information technology, material science
Multi-field cutting edge technology, has been applied to product prototype, Making mold, biological engineering and the field such as medical science, jewelry-making, can replace
The efficiency for conventional fine processing technique and promoting making to a great extent and measure of precision.But, 3D prints technical process
Metal powder material is had higher requirement, as required particle size range at 20-50 micron, there is high sphericity and hypoxia contains
Amount etc..At present, the domestic required basic dependence on import of fine grain globular metallic powder, owing to the preparation technology of powder exists raw material
Bottleneck problem that utilization rate is low, expensive, this constrain largely the popularization of China's metal 3D printing technique with should
With.
Existing metal dust technology of preparing mainly has: mechanical attrition method, atomization, plasma rotating electrode process, physics
Chemical method etc..Wherein, gas atomization is one of main method preparing superfine metal and alloy powder, but the one of its maximum
Problem is exactly that productivity is low, and the metal or alloy powder size prepared reaches the yield rate of below 50 μm and only has about 30%;Ball
Mill method is only used for fragile material, and usual oxygen content is higher and uncontrollable powder particle pattern;Plasma rotating electrode process system
Standby powder diameter is relatively big, typically larger than 50 μm;Electrochemistry, reducing process are relatively costly, and the solvent and the reducing agent that use have more
Severe toxicity, and it is readily incorporated the impurity such as halogen, sulfur.CN201010219344.3 discloses a kind of ultra-fine and nano WC-Co composite powder
Agglomerating prilling method, after utilizing this method that ultra-fine and nano WC-Co composite powder are carried out agglomeration granulation, agglomerated particle can be direct
For hot-spraying technique, it is possible to preparation has a hard alloy coating of the ultra-fine of excellent comprehensive performance and nanostructured, but for
The requirement of 3D printing metal or alloy powder also has certain gap, needs to study the most further.Therefore, the most urgent
Demand low cost, high-purity, the 3D of size tunable print by the preparation method of metal or alloy powder.
Summary of the invention
Above-mentioned limitation based on prior art, the present invention provides a kind of 3D printing fine grained simple substance globular metallic powder
Preparation method.For solving, 3D printing metal or alloy powder purity is low, particle diameter is uncontrollable and raw material availability is low, price
The problems such as costliness.
Technical scheme is as follows:
The preparation method of a kind of 3D printing fine grained simple substance globular metallic powder, it is characterised in that this preparation method is adopted
It is raw material with high pure metal bulk, in an inert atmosphere by arc evaporation, is filled with hydrogen control metal gas former simultaneously
Conduction of heat and the activity of son are allowed to cool deposition and obtain high purity elemental nano metal powder granule;Then high purity elemental metal is received
Rice flour end carries out agglomeration granulation, obtains the micron order elemental metals powder of higher density;Finally to micron order elemental gold after pelletize
Belong to powder and carry out heat treatment, by degumming and densification consolidation, it is thus achieved that granularity, sphericity, mobility and oxygen content meet
3D prints the elemental metals powder particle required, it specifically includes following steps:
(1) using high pure metal bulk as anode, tungsten is negative electrode, under noble gas with hydrogen environment, is made by electric discharge
Generate gas atom with forming high intensity electric arc evaporated metal, form the solid-state elemental metals that particle diameter is 20~80nm after condensation and receive
Rice grain, wherein the composition of metal block material is selected from Fe, Co, Ni or Zn, and noble gas with the order that is passed through of hydrogen is: first take out true
Sky, then pass to argon carry out the starting the arc start evaporation, be passed through hydrogen the most again and carry out continuous evaporation;
(2) elemental metals nano-particle polyvinyl alcohol, Polyethylene Glycol and deionized water and step (1) prepared is by necessarily
Ratio, combining to prepare by ball milling and mechanical agitation obtains stable suspension slip, then utilizes closed cycle spray to do
Dry equipment carries out agglomeration granulation, it is thus achieved that the spherical metallic particles of 20~50 μm, and being wherein dried medium is argon;Ball milling and machinery stir
Mix and combine, first carry out ball milling, carry out mechanical agitation the most again;
(3) spherical metallic particles using the tube furnace of argon shield to prepare step (2) carries out heat treatment, first stage
Heat treatment temperature is 250~350 DEG C, temperature retention time 90~150min;Second stage heat treatment temperature is Tm/ 2+80~Tm/2+
180 DEG C, TmFor elemental metals fusing point, temperature retention time is 120~180min;Finally cool to room temperature with the furnace, obtain being applicable to 3D
The fine grained simple substance globular metallic powder of printing demand;
Wherein, the pressure ratio being filled with hydrogen and argon in step (1) is 1:1~3, is passed through argon and reaches to vacuum pressure
0.04~0.06MPa carries out the starting the arc, then passes to hydrogen to vacuum pressure and reaches 0.01~0.03MPa and carry out continuous evaporation;
In step (2), the slurry ball-milling time is 40~80min, and rotating speed is 300~400r/min, and the mechanical agitation time is 20
~40min, stir speed (S.S.) is 100~200r/min, it is ensured that total time is 60~120min.
Technical characteristic and the advantage of the present invention mainly have: (1), during the metal starting the arc is evaporated, is filled with hydrogen, at height
The lower hydrogen of temperature, as heat-conducting medium, can improve productivity and control the activity of metal gas atom, the elemental gold that product is mutually pure
Belong to nanoparticle;(2) aaerosol solution slip is prepared with the nano metal powder that thing is mutually pure for original material.In the present invention, surely
The preparation determining distributed slurry has vital effect to pattern and the particle diameter distribution of prilling powder, uses ball milling to stir with machinery
Mixing the mode combined, the effect of first stage ball milling is to smash nanoparticle agglomerates body, makes organic binder bond and dispersant exist
The absorption of particle surface reaches balance, and second stage uses the mechanical agitation that energy is relatively low, and effect is discharged in slip and is mingled with
Bubble also makes the macromolecular chain of organic additive connect the tridimensional network that formation is uniform and stable;(3) by spray drying
Method carries out pelletize to prepared stable suspersion solution slip, it is possible to obtain have good sphericity, low oxygen content and relatively
The micron particles of high-compactness.In the present invention, drying tower is closed, and dry medium is noble gas, can effectively control
Oxygen content in the metal powder granulates of preparation eventually.(4) Technology for Heating Processing after pelletize, meets 3D printing requirement to final acquisition
Metal dust extremely important.In the present invention, using stage heat treatment mode, the effect of first stage heat treatment is to make pelletize
During add organic binder bond volatilization;The effect of second stage heat treatment is to make to form solid phase between metal powder granulates to glue
Knot, both ensures have enough interparticle bond strength and consistency, does not the most occur granule (or internal microstructure) to be quickly roughened
Or it is integral sintered.The present invention is combined by the parameter regulating and controlling each processing step, can prepare and have excellent sphericity, Gao Liu
Dynamic property, low oxygen content and mean diameter and particle diameter distribution meet 3D and print the pure elemental metals powder required.Meanwhile, this method with
Other processes are compared, strong to the controllability of sphericity, particle diameter distribution and the oxygen content of metallic particles, and have technique letter
Single advantage with low cost.
Accompanying drawing explanation
The thing of nano metal powder prepared by Fig. 1 a-Fig. 1 c present invention detects collection of illustrative plates mutually;Nanometer during wherein a is embodiment 1
The thing of cobalt powder detects collection of illustrative plates mutually, and b is that in embodiment 2, the thing of nanometer iron powder detects collection of illustrative plates mutually, and c is nano-nickel powder in embodiment 3
Thing detects collection of illustrative plates (wherein before test, determinand vaseline being wrapped up anti-oxidation) mutually.
The microstructure of nano metal powder, crystal structure and particle diameter distribution prepared by Fig. 2 a-Fig. 2 c present invention;Wherein a
For the high power transmission electron microscope shape appearance figure of nano-cobalt powder in embodiment 1, b is that the SEAD collection of illustrative plates of nanometer iron powder granule is with vertical
The calibration result of square crystal structure, c is the particle diameter distribution statistics result of nano-nickel powder granule.
The thing of 3D printing micron-size spherical metal dust prepared by Fig. 3 a-Fig. 3 c present invention detects collection of illustrative plates mutually;Wherein a is
In embodiment 1, the thing of cobalt powder detects collection of illustrative plates mutually, and b is that in embodiment 2, the thing of iron powder detects collection of illustrative plates mutually, and c is nikel powder in embodiment 3
Thing detects collection of illustrative plates mutually.
The microstructure of 3D printing metal powder granulates prepared by Fig. 4 a-Fig. 4 c present invention and particle diameter distribution;Wherein a is
The high power shape appearance figure of single metal cobalt granule in embodiment 1, b is the scanning electron microscope shape appearance figure of iron granule in embodiment 2, c
For the particle diameter distribution statistics result of metallic nickel powder granule in embodiment 3.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following example.
Table 1 embodiment of the present invention 1, execute example 2 and metallic cobalt, ferrum and nickel by powder granule that embodiment 3 prepares spherical
Degree, mobility and Density Detection result.
Embodiment 1, using raw material high-purity cobalt bulk (purity 99.99wt%) as anode, tungsten is negative electrode, and first evacuation is passed through
Argon reaches 0.04MPa to vacuum pressure, forms high intensity electric arc by discharge process, and the starting the arc is passed through hydrogen to vacuum after completing
Pressure reaches 0.03MPa, forms solid-state high-purity cobalt nano-particle by the condensation of evaporated metal gas atom, and its thing detects collection of illustrative plates mutually
Such as Fig. 1 a, microstructure such as Fig. 2 a;Utilize existing patented technology (granted patent number 201010219344.3), by cobalt nano-particle
Mix with polyvinyl alcohol, Polyethylene Glycol and deionized water, then ball milling 60min, then mechanical agitation 20min, obtain uniform and stable
Suspension slip, utilize closed cycle spray drying equipment to carry out agglomeration granulation, it is thus achieved that the spherical cobalt granule of 20~50 μm;Adopt
With the tube furnace of argon shield, the cobalt dust after pelletize being carried out heat treatment, first stage heat treatment temperature is 250 DEG C, during insulation
Between 150min;Second stage heat treatment temperature is 915 DEG C, and temperature retention time is 120min;Finally cool to room temperature with the furnace, held concurrently
Tool high compactness and the fine grained micron-size spherical cobalt dust of mobility.The cobalt powder thing prepared detects collection of illustrative plates such as Fig. 3 a mutually,
High power pattern such as Fig. 4 a of single metal cobalt granule, its sphericity, apparent density, mobility and measurement of oxygen content the results are shown in Table 1.
Embodiment 2, using raw material high purity iron bulk (purity 99.99wt%) as anode, be first passed through argon to vacuum pressure
Reaching 0.05MPa, form high intensity electric arc by discharge process, the starting the arc is passed through hydrogen after completing and reaches to vacuum pressure
0.02MPa, forms solid-state high purity iron nano-particle by the condensation of evaporated metal gas atom, and its thing detects collection of illustrative plates such as Fig. 1 b mutually,
SEAD collection of illustrative plates and crystal face calibration result such as Fig. 2 b of cubic crystal structure;Utilize existing patented technology (granted patent
Numbers 201010219344.3), iron nano-particle is mixed with polyvinyl alcohol, Polyethylene Glycol and deionized water, ball milling 70min, then
Mechanical agitation 30min obtains uniform and stable suspension slip, utilizes closed cycle spray drying equipment to carry out agglomeration granulation, obtains
Obtain the spherical iron particles of 20~50 μm;The tube furnace using argon shield carries out heat treatment, the first rank to the iron powder after pelletize
Section heat treatment temperature is 300 DEG C, temperature retention time 120min;Second stage heat treatment temperature is 920 DEG C, and temperature retention time is
150min;Finally cool to room temperature with the furnace, obtain having concurrently the fine grained micron-size spherical iron powder of high compactness and mobility.System
The standby iron powder thing obtained detects collection of illustrative plates such as Fig. 3 b mutually, and scanning electron microscope pattern such as Fig. 4 b of iron granule, its sphericity, pine fill close
Degree, mobility and measurement of oxygen content the results are shown in Table 1.
Embodiment 3, using raw material high purity nickel bulk (purity 99.99wt%) as anode, be first passed through argon to vacuum pressure
Reaching 0.06MPa, form high intensity electric arc by discharge process, the starting the arc is passed through hydrogen after completing and reaches to vacuum pressure
0.01MPa, forms solid-state high purity nickel nano-particle by the condensation of evaporated metal gas atom, and its thing detects collection of illustrative plates such as Fig. 1 c mutually,
Particle diameter distribution statistics result such as Fig. 2 c of nano nickel powder particle;Utilize existing patented technology (granted patent number
201010219344.3), nano nickel particles is mixed with polyvinyl alcohol, Polyethylene Glycol and deionized water, then ball milling 80min,
Mechanical agitation 40min obtains uniform and stable suspension slip again, utilizes closed cycle spray drying equipment to carry out agglomeration granulation,
Obtain the spherical nickel granule of 20~50 μm;The tube furnace using argon shield carries out heat treatment to the nickel by powder after pelletize, and first
Phase heat treatment temperature is 350 DEG C, temperature retention time 90min;Second stage heat treatment temperature is 810 DEG C, and temperature retention time is
180min;Finally cool to room temperature with the furnace, obtain having concurrently the fine grained micron-size spherical nickel by powder of high compactness and mobility.System
The standby nikel powder thing obtained detects collection of illustrative plates such as Fig. 3 c mutually, and particle diameter distribution statistics result such as Fig. 4 c of granule, its sphericity, pine fill close
Degree, mobility and measurement of oxygen content the results are shown in Table 1.
The physical parameter of the metal dust that table 1 embodiment of the present invention 1, embodiment 2 and embodiment 3 prepare
Claims (1)
1. a 3D prints by the preparation method of fine grained simple substance globular metallic powder, it is characterised in that this preparation method uses
High pure metal bulk is raw material, in an inert atmosphere by arc evaporation, is filled with hydrogen simultaneously and controls metal gas atom
Conduction of heat and activity be allowed to cool deposition and obtain high purity elemental nano metal powder granule;Then to high purity elemental metal nano
Powder carries out agglomeration granulation, obtains the micron order elemental metals powder of higher density;Finally to micron order elemental metals after pelletize
Powder carries out heat treatment, by degumming and densification consolidation, it is thus achieved that granularity, sphericity, mobility and oxygen content meet 3D
Printing the elemental metals powder particle required, it specifically includes following steps:
(1) using high pure metal bulk as anode, tungsten is negative electrode, under noble gas with hydrogen environment, by discharge process shape
Become high intensity electric arc evaporated metal to generate gas atom, after condensation, form the solid-state elemental metals nanometer that particle diameter is 20~80nm
Grain, wherein the composition of metal block material is selected from Fe, Co, Ni or Zn, and noble gas with the order that is passed through of hydrogen is: first evacuation, so
After be passed through argon carry out the starting the arc start evaporation, be passed through hydrogen the most again and carry out continuous evaporation;
(2) elemental metals nano-particle polyvinyl alcohol, Polyethylene Glycol and deionized water and step (1) prepared is by a definite proportion
Example, combining to prepare by ball milling and mechanical agitation obtains stable suspension slip, then utilizes closed cycle spray to be dried
Equipment carries out agglomeration granulation, it is thus achieved that the spherical metallic particles of 20~50 μm, and being wherein dried medium is argon;Ball milling and mechanical agitation
Combine, first carry out ball milling, carry out mechanical agitation the most again;
(3) tube furnace of argon shield is used spherical metallic particles prepared by step (2) to be carried out heat treatment, at first stage heat
Reason temperature is 250~350 DEG C, temperature retention time 90~150min;Second stage heat treatment temperature is Tm/ 2+80~Tm/ 2+180 DEG C,
TmFor elemental metals fusing point, temperature retention time is 120~180min;Finally cooling to room temperature with the furnace, obtaining being applicable to 3D printing needs
The fine grained simple substance globular metallic powder asked;
Wherein, the pressure ratio being filled with hydrogen and argon in step (1) is 1:1~3, be passed through argon to vacuum pressure reach 0.04~
0.06MPa carries out the starting the arc, then passes to hydrogen to vacuum pressure and reaches 0.01~0.03MPa and carry out continuous evaporation;
In step (2), the slurry ball-milling time is 40~80min, and rotating speed is 300~400r/min, the mechanical agitation time be 20~
40min, stir speed (S.S.) is 100~200r/min, it is ensured that total time is 60~120min.
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Cited By (11)
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CN106623953A (en) * | 2016-12-28 | 2017-05-10 | 东莞市精研粉体科技有限公司 | Preparing method of low-reflectivity spherical copper powder for 3D printing |
CN108262473A (en) * | 2016-12-30 | 2018-07-10 | 西门子公司 | The method of the component of 3D printing composite powder, printing equipped with embedded component and the component and its printer model |
CN108274011A (en) * | 2018-03-06 | 2018-07-13 | 北京工业大学 | A kind of preparation method with bimodal distribution metal powder suitable for 3D printing |
CN109877343A (en) * | 2019-04-04 | 2019-06-14 | 北京工业大学 | A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing |
CN110614376A (en) * | 2019-09-12 | 2019-12-27 | 北京工业大学 | Preparation method of tungsten-copper composite powder for 3D printing |
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CN112105471A (en) * | 2018-03-05 | 2020-12-18 | 全球先进金属美国股份有限公司 | Anode and capacitor containing spherical powder |
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