CN109182813A - In the method for silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites - Google Patents
In the method for silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites Download PDFInfo
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- CN109182813A CN109182813A CN201810962939.4A CN201810962939A CN109182813A CN 109182813 A CN109182813 A CN 109182813A CN 201810962939 A CN201810962939 A CN 201810962939A CN 109182813 A CN109182813 A CN 109182813A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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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 a kind of methods in silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites, including following procedure: using polyvinyl alcohol water solution surface modification treatment silicon powder;In modified silicon micropowder surface supported catalyst presoma;Carbon nanotube is grown in silicon micropowder surface using in-situ chemical vapor deposition technique;The preparation of silico-carbo nanotube/aluminium composite powder;Silico-carbo nanotube/aluminium composite material block compacting-sinter molding;Silico-carbo nanotube/aluminium composite material block extrusion deformation processing.Silico-carbo nanotube/the aluminium composite material prepared using this method, using silicon powder as intermediate vector, inert surface is provided for the growth of carbon nanotube, improves the growth quality and structural intergrity of carbon nanotube, plasticity and toughness are kept well while being obviously improved Tensile strength.
Description
Technical field
The present invention is a kind of method in silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites, is related to multiple
Powder compacting technology and composite materials property are closed, powder metallurgical technology is belonged to.
Background technique
In fields such as aerospace, electronics and automobiles, metal-base composites is because of its high specific strength, specific modulus, good
The excellent properties such as thermally conductive, electric conductivity, wearability, thermal stability and low thermal expansion coefficient, show wide application prospect.
Wherein, aluminum matrix composite is since density is small, corrosion-resistant, processing performance is good, matrix alloy range of choice is wide, heat-treatable strengthened
The advantages such as effect is obvious and preparation process type is abundant, are studied the most extensive and with fastest developing speed.
One of the carbon nanomaterial that carbon nanotube attracts attention as 21 century has critically important researching value and application
Prospect.The Young's modulus theory estimation of single-walled carbon nanotube is up to 5TPa, and it is flat to test the multi-walled carbon nanotube Young's modulus measured
1.8TPa is reached, tensile strength is about 100 times of steel, and density only has the 1/6 of steel.Therefore, it is managed as a kind of mechanical property
The one-dimensional carbon nano material thought, carbon nanotube emerge one after another as the research of composite material reinforcement body, correlative study also great spy
Color.
It is different from the composite pathway of aluminum substrate according to carbon nanotube, outer addition and in-situ method can be divided into.Traditional preparation side
Method is to be dispersed in carbon nanotube in aluminum substrate by additional mode to obtain composite material, ball-milling technology is usually used
Dispersed, and good dispersion effect is often to be obtained by prolonged ball milling, therefore Process During High Energy Ball Milling can destroy it
Structural intergrity, therefore Recent study personnel begin one's study in metal powder surface in-situ growing carbon nano tube, well solve
The problem of carbon nanotube dispersibility.From the point of view of the application market of current aluminum matrix composite, alloy member is added in aluminum substrate
Element make its compared to fine aluminium have can working hardening, heat-treatable strengthened space, expand its application range, become current aluminium base
The trend of composite material research.
Summary of the invention
The purpose of the present invention is to provide one kind in silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites
Method.This method can effectively overcome the problems, such as brought by single carriers affect carbon nano tube growth quality, this method process
Simple and easy, obtained composite materials property is excellent.To achieve the above object, the present invention is to add by the following technical programs
With realization,
A method of in silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites, including following procedure:
(1) polyvinyl alcohol water solution surface modification treatment silicon powder is used:
~5 μm of silicon powder is added to the polyvinyl alcohol water solution of suitable 0.5wt.%, ultrasound, magnetic agitation 2h,
Then it filters, wash, be dried for standby.
(2) in modified silicon micropowder surface supported catalyst presoma:
By the silicon microballoon and cabaltous nitrate hexahydrate [Co (NO3) 6H2O] of the modification of partial size~5 μm according to mass ratio 5:
(0.25~1) is dissolved in dehydrated alcohol, in the stirring of 65 DEG C of constant temperature continuing magnetic forces until being evaporated dehydrated alcohol, then will be evaporated
The silicon powder of supported catalyst presoma is placed in 80 DEG C of baking oven, dries 2h;
(3) carbon nanotube is grown in silicon micropowder surface using in-situ chemical vapor deposition technique:
The silicon powder of supported catalyst presoma made from step (2) is restored under hydrogen atmosphere in tube furnace and is obtained
Cobalt/Si powder, reduction temperature are 450 DEG C;900 DEG C then are warming up to, is passed through the mixed gas reaction of hydrogen, argon gas, methane,
Silicon micropowder surface grows carbon nanotube, is finally cooled to room temperature under the protection of argon atmosphere;
(4) silico-carbo nanotube/aluminium composite powder preparation:
It is according to mass ratio by the silicon powder of in-situ growing carbon nano tube and the ball aluminum powder of partial size~40 μm in step (3)
1:19 carries out ball-milling, obtains silico-carbo nanotube/aluminium composite powder;
(5) silico-carbo nanotube/aluminium composite material block compacting-sinter molding:
Silico-carbo nanotube/aluminium composite powder made from step (4) is pressed with hydraulic press, then in tubular type
It uses argon gas to be sintered as protective atmosphere in furnace, obtains silico-carbo nanotube/aluminium composite material block;
(6) extrusion deformation of silico-carbo nanotube/aluminium composite material block is handled:
Silico-carbo nanotube/aluminium composite material block made from step (5) is put into box type heater and is heated, then into
The processing of row hot extrusion deformation, obtains As-extruded composite material block.
Preferably, in step (3), be passed through the mixed gas reaction of hydrogen, argon gas, methane, gas flow be set as methane/
Hydrogen/argon gas=50/100/400mL/min, reaction time 60min.In step (4), the pressure of compression moulding is 500MPa,
Sintering temperature is set in 600 DEG C, sintering time 1h.
The invention has the following advantages that growing carbon nanometer in silicon micropowder surface using in-situ chemical vapor deposition technique first
Pipe, it is then by low energy ball milling that it is compound with aluminium powder matrix, composite wood is prepared by compression moulding-sintering-hot extrusion technique
Expect block.Silico-carbo nanotube/the aluminium composite material prepared using this method, tensile property realize apparent tensile strength
Promotion, plasticity and toughness still have preferable holding.The present invention is received using chemical vapor deposition process in silicon micropowder surface growth in situ carbon
Mitron, and the design to microstructure of composite structure is realized by ball milling-compression moulding-sintering-hot extrusion technique, it optimizes multiple
The performance of condensation material shows preferable application prospect.
Detailed description of the invention
Fig. 1 is the scanned photograph that silicon powder is coated on aluminium powder surface by ball milling dispersion.
Silicon powder scanned photograph of the Fig. 2 after adhesive treatment.
Fig. 3 is the silicon micropowder surface functional group characterized after adhesive treatment using infrared absorption spectrum.
Fig. 4 is the scanned photograph in embodiment 1 after silicon micropowder surface in-situ growing carbon nano tube.
Fig. 5 is the scanned photograph in embodiment 2 after silicon micropowder surface in-situ growing carbon nano tube.
Fig. 6 is the scanned photograph in embodiment 3 after silicon micropowder surface in-situ growing carbon nano tube.
Fig. 7 is compound by ball milling dispersion with aluminium powder matrix after silicon micropowder surface in-situ growing carbon nano tube in embodiment 3
Scanned photograph.
Fig. 8 is the metallographic structure photo in composite material block parallel extrusion direction section in embodiment 3.
Fig. 9 is composite material and fine aluminium tensile stress strain curve in embodiment 2,3.
Specific embodiment
The present invention grows carbon nanotube in silicon micropowder surface using in-situ chemical vapor deposition technique, and by composite powder system
Standby block composite material.Technology path is as follows:
(1) polyvinyl alcohol water solution surface modification treatment silicon powder is used:
~5 μm of silicon powder is added to the polyvinyl alcohol water solution of suitable 0.5wt.%, ultrasound, magnetic agitation 2h,
Then it filters, wash, be dried for standby under conditions of 60 DEG C in a vacuum drying oven.The poly- second of binder for being 0.5wt.% with concentration
After enol carries out surface adhesion processing to original silicon powder, the powder morphology of acquisition is by scanning electron microscope observation as schemed
Shown in 2, the silicon micropowder surface functional group after adhesive treatment is characterized using infrared absorption spectrum, as shown in Figure 3.
(2) in modified silicon micropowder surface supported catalyst presoma:
By the silicon microballoon and cabaltous nitrate hexahydrate [Co (NO3) 6H2O] of the modification of partial size~5 μm according to mass ratio 5:
(0.25~1) is dissolved in dehydrated alcohol, in the stirring of 65 DEG C of constant temperature continuing magnetic forces until being evaporated dehydrated alcohol, then will be evaporated
The silicon powder of supported catalyst presoma is placed in 80 DEG C of baking oven, dries 2h.
(3) carbon nanotube is grown in silicon micropowder surface using in-situ chemical vapor deposition technique:
The silicon powder of supported catalyst presoma made from step (2) is restored under hydrogen atmosphere in tube furnace and is obtained
Cobalt/Si powder, reduction temperature are 450 DEG C, and gas flow is set as hydrogen 100mL/min.900 DEG C then are warming up to, is passed through hydrogen
Gas, argon gas, methane mixed gas reaction 60min, be finally cooled to room temperature under the protection of argon atmosphere, this carbon nanotube is raw
The gas flow in long stage is set as methane/hydrogen/argon gas=50/100/400mL/min.
(4) silico-carbo nanotube/aluminium composite powder preparation:
It is according to mass ratio by the silicon powder of in-situ growing carbon nano tube and the ball aluminum powder of partial size~40 μm in step (3)
1:19 is placed in 250mL hard stainless steel ball grinder, carries out ball-milling in a planetary ball mill according to ratio of grinding media to material 10:1;Ball
Grinding parameter is 180 revs/min of revolving speed, time 90min.Composite powder after ball milling observes pattern as schemed by scanning electron microscope
Shown in 1.
(5) silico-carbo nanotube/aluminium composite material block compacting-sinter molding:
Silico-carbo nanotube/aluminium composite powder made from step (4) is pressed with hydraulic press, then in tubular type
It uses argon gas to be sintered as protective atmosphere in furnace, obtains silico-carbo nanotube/aluminium composite material block, the pressure of compression moulding
For 500MPa, sintering temperature is set in 600 DEG C, sintering time 1h.
(6) extrusion deformation of silico-carbo nanotube/aluminium composite material block is handled:
Silico-carbo nanotube/aluminium composite material block made from step (5) is put into box type heater and is heated, then into
The processing of row hot extrusion deformation, obtains As-extruded composite material block.When hot extrusion, box type heater set temperature is 530 DEG C, is squeezed
Pressure ratio is 16:1.
Below with reference to examples illustrate the present invention.
Embodiment 1
With polyvinyl alcohol water solution surface modification treatment silicon powder: weigh quality be 5g~5 μm of silicon powder is added to
Then the polyvinyl alcohol water solution of 0.5wt.%, ultrasound, magnetic agitation 2h are filtered, are washed, in a vacuum drying oven 60 DEG C of item
It is dried for standby under part;
By silicon microballoon and the cabaltous nitrate hexahydrate [Co (NO modified of partial size~5 μm3)·6H2O] according to mass ratio 5:
0.25 is added in dehydrated alcohol, in 65 DEG C of constant temperature continuing magnetic force stirrings until being evaporated dehydrated alcohol, the load that then will be evaporated
The silicon powder of catalyst precursor is placed in 80 DEG C of baking oven, dries 2h;It is subsequently placed at lower 450 DEG C of hydrogen atmosphere in tube furnace also
Original obtains cobalt/Si powder, is then warming up to 900 DEG C, is passed through the mixed gas of hydrogen, argon gas, methane, gas flow is set as first
Alkane/hydrogen/argon gas=50/100/400mL/min reacts 60min, is finally cooled to room temperature under the protection of argon atmosphere;It is logical
It is as shown in Figure 4 to over-scan electron microscope observation pattern.
Embodiment 2
With polyvinyl alcohol water solution surface modification treatment silicon powder: weigh quality be 5g~5 μm of silicon powder is added to
Then the polyvinyl alcohol water solution of 0.5wt.%, ultrasound, magnetic agitation 2h are filtered, are washed, in a vacuum drying oven 60 DEG C of item
It is dried for standby under part;
By silicon microballoon and the cabaltous nitrate hexahydrate [Co (NO modified of partial size~5 μm3)·6H2O] according to mass ratio 5:
0.5 is added in dehydrated alcohol, in 65 DEG C of constant temperature continuing magnetic force stirrings until being evaporated dehydrated alcohol, then urges the load being evaporated
The silicon powder of agent presoma is placed in 80 DEG C of baking oven, dries 2h;It is subsequently placed at the lower 450 DEG C of reduction of hydrogen atmosphere in tube furnace
Cobalt/Si powder is obtained, 900 DEG C is then warming up to, is passed through the mixed gas of hydrogen, argon gas, methane, gas flow is set as first
Alkane/hydrogen/argon gas=50/100/400mL/min reacts 60min, is finally cooled to room temperature under the protection of argon atmosphere;It is logical
It is as shown in Figure 5 to over-scan electron microscope observation pattern.
By the ball aluminum powder of silico-carbo nanotube powder and partial size~40 μm after growth according to mass ratio be 1:19, be placed in
In 250mL hard stainless steel ball grinder, ratio of grinding media to material 10:1 carries out ball-milling in a planetary ball mill;Composite powder liquid
Press is pressed, and then uses argon gas to be sintered as protective atmosphere in tube furnace, obtains silico-carbo nanotube/aluminium
Composite material block;Finally composite material block is put into box type heater and is heated to 530 DEG C, then carries out hot extrusion deformation
Processing, extrusion ratio 16:1 obtain As-extruded composite material block;(1) curve institute of its tensile stress strain curve such as Fig. 9
Show.
Embodiment 3
With polyvinyl alcohol water solution surface modification treatment silicon powder: weigh quality be 5g~5 μm of silicon powder is added to
Then the polyvinyl alcohol water solution of 0.5wt.%, ultrasound, magnetic agitation 2h are filtered, are washed, in a vacuum drying oven 60 DEG C of item
It is dried for standby under part;
By silicon microballoon and the cabaltous nitrate hexahydrate [Co (NO modified of partial size~5 μm3)·6H2O] according to mass ratio 5:
1 is added in dehydrated alcohol, in 65 DEG C of constant temperature continuing magnetic force stirrings until being evaporated dehydrated alcohol, the supported catalyst that then will be evaporated
The silicon powder of agent presoma is placed in 80 DEG C of baking oven, dries 2h;The lower 450 DEG C of reduction of hydrogen atmosphere in tube furnace are subsequently placed to obtain
Cobalt/Si powder, be then warming up to 900 DEG C, be passed through the mixed gas of hydrogen, argon gas, methane, gas flow be set as methane/
Hydrogen/argon gas=50/100/400mL/min reacts 60min, is finally cooled to room temperature under the protection of argon atmosphere;By sweeping
It is as shown in Figure 6 to retouch electron microscope observation pattern;
By the ball aluminum powder of silico-carbo nanotube powder and partial size~40 μm after growth according to mass ratio be 1:19, be placed in
In 250mL hard stainless steel ball grinder, ratio of grinding media to material 10:1 carries out ball-milling in a planetary ball mill;Disperse by ball milling
Compound scanned photograph is as shown in Figure 7;Composite powder is pressed with hydraulic press, then used in tube furnace argon gas as
Protective atmosphere is sintered, and obtains silico-carbo nanotube/aluminium composite material block;Composite material block is finally put into box add
It is heated to 530 DEG C in hot stove, then carries out hot extrusion deformation processing, extrusion ratio 16:1 obtains As-extruded composite material block;
Tissue topography by optical microphotograph sem observation composite block body parallel extrusion direction section is as shown in Figure 8;Its tensile stress
Strain curve is as shown in (2) curve of Fig. 9.
Blank control test
The ball aluminum powder of partial size~40 μm 10g is placed in 250mL hard stainless steel ball grinder, is existed according to ratio of grinding media to material 10:1
Ball milling is carried out in planetary ball mill;Powder is pressed with hydraulic press, then uses argon gas as protection in tube furnace
Atmosphere is sintered, and obtains fine aluminium block;Finally material block is put into box type heater and is heated to 530 DEG C, is then carried out
Hot extrusion deformation processing, extrusion ratio 16:1 obtain As-extruded material.Tensile stress strain curve is as shown in Figure 9.
This invention, as intermediate vector and alloy addition element, utilizes in-situ chemical vapor deposition technique by silicon powder
Carbon nanotube is grown on silicon powder, and in conjunction with the mixed powder of low energy mechanical milling process, peptizaiton, it is compound to prepare silico-carbo nanotube/aluminium
Powder, and it is related to composite powder forming technique and composite materials property test, after composite block material warp after molding
Continuous hot extrusion deformation processing, can be further improved compactness, obtain more apparent tensile mechanical properties reinforcing effect
While, composite material plasticity and toughness have good holding.
Claims (3)
1. a kind of method in silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites, including following procedure:
(1) polyvinyl alcohol water solution surface modification treatment silicon powder is used:
~5 μm of silicon powder is added to the polyvinyl alcohol water solution of suitable 0.5wt.%, ultrasound, magnetic agitation 2h, then
It filters, washing, is dried for standby.
(2) in modified silicon micropowder surface supported catalyst presoma:
By the silicon microballoon and cabaltous nitrate hexahydrate [Co (NO3) 6H2O] of the modification of partial size~5 μm according to mass ratio 5:(0.25~
1) it is dissolved in dehydrated alcohol, in 65 DEG C of constant temperature continuing magnetic force stirrings until being evaporated dehydrated alcohol, then urges the load being evaporated
The silicon powder of agent presoma is placed in 80 DEG C of baking oven, dries 2h;
(3) carbon nanotube is grown in silicon micropowder surface using in-situ chemical vapor deposition technique:
By the silicon powder of supported catalyst presoma made from step (2), reduction obtains cobalt/silicon under hydrogen atmosphere in tube furnace
Powder, reduction temperature are 450 DEG C;900 DEG C then are warming up to, is passed through the mixed gas reaction of hydrogen, argon gas, methane, it is micro- in silicon
Powder surface grows carbon nanotube, is finally cooled to room temperature under the protection of argon atmosphere;
(4) silico-carbo nanotube/aluminium composite powder preparation:
By the ball aluminum powder of the silicon powder of in-situ growing carbon nano tube and partial size~40 μm in step (3) according to mass ratio be 1:19
Ball-milling is carried out, silico-carbo nanotube/aluminium composite powder is obtained;
(5) silico-carbo nanotube/aluminium composite material block compacting-sinter molding:
Silico-carbo nanotube/aluminium composite powder made from step (4) is pressed with hydraulic press, then in tube furnace
It uses argon gas to be sintered as protective atmosphere, obtains silico-carbo nanotube/aluminium composite material block;
(6) extrusion deformation of silico-carbo nanotube/aluminium composite material block is handled:
Silico-carbo nanotube/aluminium composite material block made from step (5) is put into box type heater and is heated, heat is then carried out
Extrusion deformation processing, obtains As-extruded composite material block.
2. the method according to claim 1, wherein being passed through the gaseous mixture of hydrogen, argon gas, methane in step (3)
Precursor reactant, gas flow are set as methane/hydrogen/argon gas=50/100/400mL/min, reaction time 60min.
3. being burnt the method according to claim 1, wherein the pressure of compression moulding is 500MPa in step (4)
Junction temperature is set in 600 DEG C, sintering time 1h.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110357592A (en) * | 2019-08-05 | 2019-10-22 | 吴振行 | A kind of ceramic resin of 3D printing and its preparation method and application |
CN110526230A (en) * | 2019-08-29 | 2019-12-03 | 南京行创新材料有限公司 | Photovoltaic scrap silicon is preparing the application in array carbon nano tube |
CN115595479A (en) * | 2022-08-31 | 2023-01-13 | 山东创新精密科技有限公司(Cn) | High-strength hydrophobic aluminum alloy material and preparation method thereof |
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CN107946549A (en) * | 2016-10-13 | 2018-04-20 | 佛山市欣源电子股份有限公司 | A kind of Si/CNTs anode materials and preparation method |
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CN105734459A (en) * | 2014-12-12 | 2016-07-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of carbon nanotube reinforced aluminum base composite material |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110357592A (en) * | 2019-08-05 | 2019-10-22 | 吴振行 | A kind of ceramic resin of 3D printing and its preparation method and application |
CN110526230A (en) * | 2019-08-29 | 2019-12-03 | 南京行创新材料有限公司 | Photovoltaic scrap silicon is preparing the application in array carbon nano tube |
CN115595479A (en) * | 2022-08-31 | 2023-01-13 | 山东创新精密科技有限公司(Cn) | High-strength hydrophobic aluminum alloy material and preparation method thereof |
CN115595479B (en) * | 2022-08-31 | 2023-12-19 | 山东创新精密科技有限公司 | High-strength hydrophobic aluminum alloy material and preparation method thereof |
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Application publication date: 20190111 |
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RJ01 | Rejection of invention patent application after publication |