CN106542516B - A kind of mesh structural porous carbon of personalized customization type and preparation method thereof - Google Patents
A kind of mesh structural porous carbon of personalized customization type and preparation method thereof Download PDFInfo
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- CN106542516B CN106542516B CN201610920513.3A CN201610920513A CN106542516B CN 106542516 B CN106542516 B CN 106542516B CN 201610920513 A CN201610920513 A CN 201610920513A CN 106542516 B CN106542516 B CN 106542516B
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of mesh structural porous carbon of personalized customization type and preparation method thereof, which has accurate personalized customization type shape and interior microscopic hole.The porosity of the mesh structural porous carbon is 70%~99.5%, and the inscribed circle diameter for forming each face of microcosmic polyhedron of mesh structural porous carbon is 0.2~3mm, and the cross section inscribed circle diameter of polyhedron connecting rod is 0.02~1.5mm.Its manufacturing method is as follows: designing the appearance profile and internal pore structure of porous mathematical model；Mesh structural porous carbon matrix precursor is manufactured using increasing material manufacturing method；Burning material is buried in filling inside porous carbon matrix precursor；The porous carbon matrix precursor that burning material is buried in filling is placed under 500~1000 DEG C of vacuum or protective gas atmosphere and is pyrolyzed；Finally burning material is buried in removal, obtains being graphitized mesh structural porous carbon using 1100~3000 DEG C of graphitization processings.The method overcome the defects of porous polymer pyrolytic process distortion and contraction distortion, compensate for conventional mesh porous carbon preparation method and are difficult to the shortcomings that realizing accurate control to its macroshape and micropore structure.
Description
Technical field:
The invention belongs to manufacture the technical field of mesh structural porous carbon, and in particular to a kind of mesh structural porous carbon of personalized customization type
And preparation method thereof.
Background technique:
Mesh structural porous carbon material is a kind of porous carbon materials with excellent properties, has the advantage that lightweight, high connection
Porosity, high conductivity, high heat conductance, excellent high-temperature stability, strong adsorptivity etc..Mesh structural porous carbon material is deposited in thermal energy
The fields such as storage, adsorbing separation, chemical catalysis, electrode material are widely used, and are supported especially as the carbon skeleton for preparing porous metals
Material shows extremely important function and significance.
The preparation method of mesh structural porous carbon is although many kinds of, but all various degrees the shortcomings that and deficiency.Mesh
The preceding method for preparing mesh structural porous carbon mainly has following a few classes: the methods of foaming, template, direct thermal decomposition method.Foaming
It is to generate a large amount of bubbles by certain physicochemical change using carbon matrix precursor under the action of foaming agent, then solidification rapidly
The mesh structural porous carbon of one kind that pyrolysis is formed, carbon matrix precursor is mainly the organic matter of pitch one kind, and the major defect of this method is
Preparation process is complicated, pore morphology is difficult to control, pore connectivity is lower, is difficult to prepare complicated shape porous carbon.Template packet
A variety of preparation methods are included, most widely used is the organic matter conduct that high carbon residue is then impregnated using polyurethane foam as template
Carbon matrix precursor, final curing pyrolysis prepare mesh structural porous carbon, and this method almost replicates the shape of polyurethane foam, shape
At very high interconnected pore rate, the shape of hole is almost all dodecahedron and the tetrakaidecahedron, but the net of complicated shape
Shape porous carbon is still difficult to directly prepare, and microscopic void shape is also difficult to realize orderly controllable manufacture；Another template is
Using removable sphere as perforating agent template, carbon matrix precursor is then filled in sphere gap, resolidification is pyrolyzed to be formed
Mesh structural porous carbon, this method in addition to disadvantage mentioned above, there is also complex process, interconnected pore rate is low the problems such as.Direct pyrolysis method
Gradually paid attention to as a kind of better simply method of technique, for example, by macromolecule organic, Animal Bone, plant etc. directly as
Carbon matrix precursor prepares mesh structural porous carbon, and the height of complicated shape and microscopic void is prepared in particular with increasing material manufacturing or die methods
Molecular organic presoma, then directly pyrolysis form porous carbon, presently, there are the problem of be this kind of macromolecule organic in heat
Viscous state is undergone in solution preocess, and serious distortion deformation and very big contraction distortion occur under the effect of gravity.
Summary of the invention:
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of personalized customization type is netted more
Hole carbon and preparation method thereof, the mesh structural porous carbon have personalized customization type shape, its microscopic pore structure parameter may be implemented
Accurate control.
In order to achieve the above objectives, the present invention adopts the following technical scheme that realize:
A kind of preparation method of the mesh structural porous carbon of personalized customization type, comprising the following steps:
1) appearance profile and internal holes of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model are utilized
Gap structure, internal stent microscopic void are made of polyhedral elements；
2) using the mathematical model in step 1), the mesh structural porous carbon matrix precursor of personalized customization type is manufactured；
3) burning material is buried in the porous carbon matrix precursor pore interior filling that step 2) obtains；
4) filling for obtaining step 3), which is buried, burns in the porous presoma merging vacuum drying oven of material, at 500~1000 DEG C
At a temperature of, under vacuum or protective gas atmosphere, carry out high temperature pyrolysis processing；
5) the porous carbon template that step 4) pyrolysis obtains is cleaned with cleaning solution with burning material blends are buried, washes away it
In bury burning material, will bracket it is dry after obtain the mesh structural porous carbon template of personalized customization type；
6) in the porous carbon template merging vacuum drying oven obtained step 5), 1100~3000 DEG C at a temperature of, vacuum or
Under protective gas atmosphere, graphitization processing is carried out, personalized customization type is obtained and is graphitized mesh structural porous carbon template.
A further improvement of the present invention lies in that: in step 1), form the interior of each face of polyhedron of mesh structural porous mathematical model
Connecing circular diameter is 0.2~4mm, and the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm.
A further improvement of the present invention lies in that: in step 2), the manufacturing method of porous carbon matrix precursor includes die methods and increasing
Material autofrettage, the type of mesh structural porous carbon matrix precursor include can injection molding and can increasing material manufacturing polymer, polymer specifically includes
Phenolic resin, furane resins, photosensitive resin.
A further improvement of the present invention lies in that: in step 3), buries and burn the mixing that material specifically includes following one or more
Object analog: aluminium powder, titanium valve, iron powder, copper powder, zinc powder, oxide, chloride, carbonate, sulfate, graphite and clay,
In, oxide include silica, zirconium oxide, magnesia, titanium oxide, tantalum oxide, aluminium oxide, iron oxide, zinc oxide, manganese oxide,
Copper oxide, niobium oxide and tungsten oxide, chloride include sodium chloride, magnesium chloride, potassium chloride, calcium chloride, iron chloride, titanium chloride, chlorine
Change tantalum and copper chloride, carbonate includes potassium carbonate, sodium carbonate, calcium carbonate, magnesium carbonate.
A further improvement of the present invention lies in that: in step 4), protection gas is argon gas, hydrogen or nitrogen, heating rate 0.5
~10 DEG C/min, soaking time is 1~10h under maximum temperature.
A further improvement of the present invention lies in that: in step 5), cleaning solution is water, alcohol, acid or alkali, forms mesh structural porous carbon
The inscribed circle diameter in each face of polyhedron be 0.2~3mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.02~
1.5mm, the porosity of the mesh structural porous carbon are 70%~99.5%.
A further improvement of the present invention lies in that: in step 6), protection gas is one of argon gas, hydrogen or nitrogen, heating
Rate is 0.5~10 DEG C/min, and soaking time is 1~3h under maximum temperature, forms the interior of each face of polyhedron of mesh structural porous carbon
Connecing circular diameter is 0.2~3mm, and the cross section inscribed circle diameter of composition polyhedron connecting rod is 0.02~1.5mm, this is mesh structural porous
The porosity of carbon is 70%~99.5%.
The mesh structural porous carbon of personalized customization type of above-mentioned preparation method preparation, the hole of the mesh structural porous carbon of personalized customization type
Gap rate is 70%-99.5%, and interior microscopic pore structure is made of polyhedron truss structure, and polyhedron truss structure is evenly distributed
Or gradient pore structured arrangement.
Compared with existing porous carbon technology of preparing, a kind of preparation method of the mesh structural porous carbon of personalized customization type of the present invention,
Material is burnt as backing material inside the porous presoma of pyrolytic process using burying, and is reduced the distortion of porous carbon template and is shunk change
Shape guarantees that the size of porous carbon template is precisely controlled, realizes the complex appearance of the mesh structural porous carbon of personalized customization type and interior
The accurate control of portion's microscopic void.Porous carbon prepared by the present invention can be applied to chemical vapour deposition technique and prepare porous metals material
Material can also be applied to catalysis, separation, absorption, sensory field such as POROUS TITANIUM, porous tantalum.It will be illustrated respectively below.
The preparation method of porous carbon of the invention specifically has the following advantages:
1, the porous organic matter prepared using increasing material manufacturing and die methods is as presoma, can directly be pyrolyzed prepare it is netted
Porous carbon, preparation process are simple.
2, the direct design and manufacture of complicated netted porous carbon materials, such as orderly and disorderly arranged pore structure, difference are realized
The polyhedral structure of face number, gradient porous pore structure etc..
3, the method for burning material is buried using filling, prevents torsional deformation and reduction of the macromolecule organic in pyrolytic process
Its contraction distortion in pyrolytic process realizes that the complexity of mesh structural porous carbon is personalized while guaranteeing high interconnected pore rate
The accurate control of the direct accurate manufacture and interior microscopic pore shape of Custom Prosthesis shape.
Porous carbon prepared by the present invention specifically has the following advantages:
1, the micropore structure of the porous carbon is controllable, such as porous carbon microscopic units type, element characteristic size.
2, the macro geometry of the porous carbon can design the accurate control that personalized customization type shape controllably may be implemented.
Detailed description of the invention:
Fig. 1 is the electron microscope of the mesh structural porous carbon of personalized customization type prepared.
Fig. 2 is the schematic diagram of the mesh structural porous mathematical model localized micro unit of personalized customization type.
Fig. 3 is the schematic diagram of the mesh structural porous carbon matrix precursor localized micro unit of personalized customization type.
Fig. 4 be in the mesh structural porous carbon matrix precursor of personalized customization type filling bury burn material after, localized micro unit signal
Figure.
Fig. 5 is the localized micro of the mesh structural porous carbon of personalized customization type and the mixture for burying burning material after high temperature pyrolysis
Cell schematics.
Fig. 6 is after over cleaning removal buries and burns material, and the localized micro unit of the mesh structural porous carbon of personalized customization type is illustrated
Figure.
Wherein: 1, mesh structural porous carbon matrix precursor；2, burning material is buried；3, mesh structural porous carbon.
Specific embodiment:
Description is described in further detail to the present invention with reference to the accompanying drawings and examples, it is described be explanation of the invention rather than
It limits.
A kind of preparation method of the mesh structural porous carbon of personalized customization type of the present invention, comprising the following steps:
1) appearance profile and internal holes of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model are utilized
Gap structure, internal stent microscopic void are made of polyhedral elements；Wherein, in order to be different from conventional porous carbon, in design link
It realizes to the arbitrarily complicated shape of the mesh structural porous carbon of personalized customization type, microscopic void parameter, ordered pore structure and gradient pore
Gap structure realizes control, and mathematical model Micro Instructional Design size is as follows: forming the interior of each face of polyhedron of mesh structural porous mathematical model
Connecing circular diameter is 0.2~4mm, and the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm.
2) using the mathematical model in step 1), the mesh structural porous carbon matrix precursor of personalized customization type is manufactured；Porous carbon forerunner
The manufacturing method of body includes die methods and increasing material manufacturing method, and the type of mesh structural porous carbon matrix precursor includes that injection molding and can increase material system
The polymer made, polymer specifically include phenolic resin, furane resins, photosensitive resin.
3) burning material is buried in the porous carbon matrix precursor pore interior filling that step 2) obtains；Bury burn material specifically include it is following
One or more of mixture analog: aluminium powder, titanium valve, iron powder, copper powder, zinc powder, oxide, chloride, carbonate, sulfuric acid
Salt, graphite and clay, wherein oxide includes silica, zirconium oxide, magnesia, titanium oxide, tantalum oxide, aluminium oxide, oxidation
Iron, zinc oxide, manganese oxide, copper oxide, niobium oxide and tungsten oxide, chloride include sodium chloride, magnesium chloride, potassium chloride, calcium chloride,
Iron chloride, titanium chloride, tantalic chloride and copper chloride, carbonate include potassium carbonate, sodium carbonate, calcium carbonate, magnesium carbonate.
4) filling for obtaining step 3), which is buried, burns in the porous presoma merging vacuum drying oven of material, at 500~1000 DEG C
At a temperature of, under vacuum or protective gas atmosphere, carry out high temperature pyrolysis processing；Protection gas is argon gas, hydrogen or nitrogen, and heating rate is
0.5~10 DEG C/min, soaking time is 1~10h under maximum temperature.
5) the porous carbon template that step 4) pyrolysis obtains is cleaned with cleaning solution with burning material blends are buried, washes away it
In bury burning material, will bracket it is dry after obtain the mesh structural porous carbon template of personalized customization type；Cleaning solution be water, alcohol, acid or
Alkali, the porosity of the mesh structural porous carbon are 70%~99.5%, form the inscribed circle diameter in each face of polyhedron of mesh structural porous carbon
For 0.2~3mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.02~1.5mm.
6) in the porous carbon template merging vacuum drying oven obtained step 5), 1100~3000 DEG C at a temperature of, vacuum or
Under protective gas atmosphere, graphitization processing is carried out, personalized customization type is obtained and is graphitized mesh structural porous carbon template, protection gas is argon
One of gas, hydrogen or nitrogen, heating rate are 0.5~10 DEG C/min, and soaking time is 1~3h, composition under maximum temperature
The inscribed circle diameter in each face of the polyhedron of mesh structural porous carbon is 0.2~3mm, and the cross section inscribed circle for forming polyhedron connecting rod is straight
Diameter is 0.02~1.5mm, and the porosity of the mesh structural porous carbon is 70%~99.5%.
The mesh structural porous carbon of personalized customization type of above-mentioned preparation method preparation, using burying, burning material is porous as pyrolytic process
Backing material inside presoma, reduces the distortion and contraction distortion of porous carbon template, guarantees that the size of porous carbon template obtains essence
The accurate control of the complicated shape and internal void of the mesh structural porous carbon of personalized customization type is realized in really control.The mesh structural porous carbon
Porous metal material is prepared applied to chemical vapour deposition technique, such as medical porous titanium, porous tantalum implantation material, medical artificial heart valve
Film, intravascular stent can also be applied to catalysis, separation, absorption, sensory field.
Embodiment 1:
Referring to Fig. 1 to Fig. 6, a kind of mesh structural porous carbon of personalized customization type of the present invention and preparation method thereof, including following step
It is rapid:
Step 1) utilizes the appearance profile of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model and interior
Portion's pore structure, internal stent microscopic void are made of polyhedral elements, form each face of polyhedron of mesh structural porous mathematical model
Inscribed circle diameter be 0.2~4mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm, shown in Figure 2；
The mathematical model that step 2) is based in step 1) produces correspondence with the method for increasing material manufacturing using photosensitive resin
Polymer mold, it is shown in Figure 3 as the mesh structural porous carbon matrix precursor 1 of personalized customization type；
Step 3) is chosen calcium oxide (oxide can also be replaced by or mixtures thereof other above-mentioned oxides) powder and is made
For bury burn material 2, will bury burn material 2 be filled into inside the porous carbon matrix precursor that step 2) obtains, obtain porous carbon matrix precursor with
It buries and burns material mixture, it is shown in Figure 4；
The porous carbon matrix precursor that step 3) obtains is placed among crucible by step 4) with burning material mixture is buried, and then will
Crucible is placed in vacuum drying oven, covers bell, extracted out furnace air with vacuum pump, keeps vacuum state, then 5 DEG C/min
Rate is warming up to 600 DEG C, keeps the temperature 5h, then cools to room temperature with the furnace, crucible is taken out, and obtains porous carbon and bury to burn the mixed of material
Zoarium, it is shown in Figure 5；
The porous carbon that step 4) obtains is placed into beaker by step 5) with the mixture for burning material is buried, by cleaning solution hydrochloric acid
It pours into beaker, until porous carbon, which cleans up not bury, burns material residual, porous carbon is taken out and is spontaneously dried；
The porous carbon template that step 6) obtains step 5) is placed into crucible, and then crucible is placed in vacuum drying oven,
Bell is covered, is extracted out furnace air with vacuum pump, keeps vacuum state, then the rate of 5 DEG C/min is warming up to 1500 DEG C, protects
Warm 2h, then cools to room temperature with the furnace, and crucible is taken out, and obtains personalized customization type and is graphitized mesh structural porous carbon 3, referring to Fig. 6
It is shown.
Embodiment 2:
Referring to Fig. 1 to Fig. 6, a kind of mesh structural porous carbon of personalized customization type of the present invention and preparation method thereof, including following step
It is rapid:
Step 1) utilizes the appearance profile of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model and interior
Portion's pore structure, internal stent microscopic void are made of polyhedral elements, form each face of polyhedron of mesh structural porous mathematical model
Inscribed circle diameter be 0.2~4mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm, shown in Figure 2；
The mathematical model that step 2) is based in step 1) produces correspondence with the method for increasing material manufacturing using photosensitive resin
Polymer mold, it is shown in Figure 3 as the mesh structural porous carbon matrix precursor 1 of personalized customization type；
Step 3) chooses iron powder (elemental powders can also be replaced by or mixtures thereof other above-mentioned elemental powders) conduct
It buries and burns material 2, burning material 2 will be buried and be filled into inside the porous carbon matrix precursor that step 2) obtains, porous carbon matrix precursor is obtained and bury
Material mixture is burnt, it is shown in Figure 4；
The porous carbon matrix precursor that step 3) obtains is placed among crucible by step 4) with burning material mixture is buried, and then will
Crucible is placed in vacuum drying oven, covers bell, is extracted out furnace air with vacuum pump, keeps vacuum state, then 10 DEG C/min
Rate be warming up to 1000 DEG C, keep the temperature 10h, then cool to room temperature with the furnace, crucible is taken out, obtain porous carbon and bury burning material
Mixture, it is shown in Figure 5；
The porous carbon that step 4) obtains is placed into beaker by step 5) with the mixture for burning material is buried, by cleaning solution hydrochloric acid
It pours into beaker, until porous carbon, which cleans up not bury, burns material residual, porous carbon is taken out and is spontaneously dried；
The porous carbon template that step 6) obtains step 5) is placed into crucible, and then crucible is placed in vacuum drying oven,
Bell is covered, is extracted out furnace air with vacuum pump, keeps vacuum state, then the rate of 10 DEG C/min is warming up to 3000 DEG C,
3h is kept the temperature, room temperature is then cooled to the furnace, crucible is taken out, personalized customization type is obtained and is graphitized mesh structural porous carbon 3, referring to figure
Shown in 6.
Embodiment 3:
Referring to Fig. 1 to Fig. 6, a kind of mesh structural porous carbon of personalized customization type of the present invention and preparation method thereof, including following step
It is rapid:
Step 1) utilizes the appearance profile of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model and interior
Portion's pore structure, internal stent microscopic void are made of polyhedral elements, form each face of polyhedron of mesh structural porous mathematical model
Inscribed circle diameter be 0.2~4mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm, shown in Figure 2；
The mathematical model that step 2) is based in step 1) produces corresponding polymer with die methods using phenolic resin
Model, it is shown in Figure 3 as the mesh structural porous carbon matrix precursor 1 of personalized customization type；
Step 3) chooses magnesium chloride powder, and (the chloride powder can also be replaced by or mixtures thereof other above-mentioned chloride powder
Change) as burning material 2 is buried, burning material 2 will be buried and be filled into inside the porous carbon matrix precursor that step 2) obtains, porous carbon forerunner is obtained
Body and bury burn material mixture, it is shown in Figure 4；
The porous carbon matrix precursor that step 3) obtains is placed among crucible by step 4) with burning material mixture is buried, and then will
Crucible is placed in vacuum drying oven, covers bell, extracted out furnace air with vacuum pump, keeps vacuum state, then 1 DEG C/min
Rate is warming up to 800 DEG C, keeps the temperature 1h, then cools to room temperature with the furnace, crucible is taken out, and obtains porous carbon and bury to burn the mixed of material
Zoarium, it is shown in Figure 5；
The porous carbon that step 4) obtains is placed into beaker by step 5) with the mixture for burning material is buried, by cleaning solution hydrochloric acid
It pours into beaker, until porous carbon, which cleans up not bury, burns material residual, porous carbon is taken out and is spontaneously dried；
The porous carbon template that step 6) obtains step 5) is placed into crucible, and then crucible is placed in vacuum drying oven,
Bell is covered, is extracted out furnace air with vacuum pump, keeps vacuum state, then the rate of 1 DEG C/min is warming up to 1100 DEG C, protects
Warm 1h, then cools to room temperature with the furnace, and crucible is taken out, and obtains personalized customization type and is graphitized mesh structural porous carbon 3, referring to Fig. 6
It is shown.
Embodiment 4:
Referring to Fig. 1 to Fig. 6, a kind of mesh structural porous carbon of personalized customization type of the present invention and preparation method thereof, including following step
It is rapid:
Step 1) utilizes the appearance profile of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model and interior
Portion's pore structure, internal stent microscopic void are made of polyhedral elements, form each face of polyhedron of mesh structural porous mathematical model
Inscribed circle diameter be 0.2~4mm, the cross section inscribed circle diameter of polyhedron connecting rod is 0.2~3mm, shown in Figure 2；
The mathematical model that step 2) is based in step 1) produces corresponding polymer with die methods using furane resins
Model, it is shown in Figure 3 as the mesh structural porous carbon matrix precursor 1 of personalized customization type；
Step 3) chooses carbonic acid sodium powder, and (carbonate powder can also be replaced by or mixtures thereof other above-mentioned carbonate powders
Change) as burning material 2 is buried, burning material 2 will be buried and be filled into inside the porous carbon matrix precursor that step 2) obtains, porous carbon forerunner is obtained
Body and bury burn material mixture, it is shown in Figure 4；
The porous carbon matrix precursor that step 3) obtains is placed among crucible by step 4) with burning material mixture is buried, and then will
Crucible is placed in vacuum drying oven, covers bell, extracted out furnace air with vacuum pump, keeps vacuum state, then 1 DEG C/min
Rate is warming up to 800 DEG C, keeps the temperature 1h, then cools to room temperature with the furnace, crucible is taken out, and obtains porous carbon and bury to burn the mixed of material
Zoarium, it is shown in Figure 5；
The porous carbon that step 4) obtains is placed into beaker by step 5) with the mixture for burning material is buried, by cleaning solution hydrochloric acid
It pours into beaker, until porous carbon, which cleans up not bury, burns material residual, porous carbon is taken out and is spontaneously dried；
The porous carbon template that step 6) obtains step 5) is placed into crucible, and then crucible is placed in vacuum drying oven,
Bell is covered, is extracted out furnace air with vacuum pump, keeps vacuum state, then the rate of 1 DEG C/min is warming up to 1100 DEG C, protects
Warm 1h, then cools to room temperature with the furnace, and crucible is taken out, and obtains personalized customization type and is graphitized mesh structural porous carbon 3, referring to Fig. 6
It is shown.
The mesh structural porous carbon of personalized customization type prepared by preparation method of the present invention, the mesh structural porous carbon 3 of the personalized customization type
Porosity be 70%-99.5%, interior microscopic pore structure is made of polyhedron truss structure, and polyhedron truss structure is uniform
Arrangement or gradient pore structured arrangement, and the outer dimension controllable precise of complicated personalized customization type.
Claims (8)
1. a kind of preparation method of the mesh structural porous carbon of personalized customization type, which comprises the following steps:
1) appearance profile and internal void knot of Three-dimensional Design Software design personalized Custom Prosthesis porous support mathematical model are utilized
Structure, internal stent pore structure are made of polyhedral elements；
2) using the mathematical model in step 1), the mesh structural porous carbon matrix precursor of personalized customization type is manufactured；
3) burning material is buried in the porous carbon matrix precursor pore interior filling that step 2) obtains；
4) filling for obtaining step 3), which is buried, burns in the porous presoma merging vacuum drying oven of material, in 500~1000 DEG C of temperature
Under, under vacuum or protective gas atmosphere, carry out high temperature pyrolysis processing；
5) the porous carbon template that step 4) pyrolysis obtains is cleaned with cleaning solution with burning material blends are buried, is washed away therein
Burning material is buried, the mesh structural porous carbon template of personalized customization type will be obtained after bracket drying；
6) in the porous carbon template merging vacuum drying oven obtained step 5), 1100~3000 DEG C at a temperature of, vacuum or protection
Under atmosphere is enclosed, graphitization processing is carried out, personalized customization type is obtained and is graphitized mesh structural porous carbon template.
2. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 1)
In, form porous support mathematical model each face of polyhedron inscribed circle diameter be 0.2~4mm, polyhedron connecting rod it is transversal
Face inscribed circle diameter is 0.2~3mm.
3. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 2)
In, the manufacturing method of porous carbon matrix precursor includes die methods and increasing material manufacturing method, and the type of mesh structural porous carbon matrix precursor includes can
Injection molding and can increasing material manufacturing polymer, polymer specifically includes phenolic resin, furane resins, photosensitive resin.
4. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 3)
In, it buries and burns the mixture analog that material specifically includes following one or more: aluminium powder, titanium valve, iron powder, copper powder, zinc powder, oxidation
Object, chloride, carbonate, sulfate, graphite and clay, wherein oxide includes silica, zirconium oxide, magnesia, oxidation
Titanium, tantalum oxide, aluminium oxide, iron oxide, zinc oxide, manganese oxide, copper oxide, niobium oxide and tungsten oxide, chloride include sodium chloride,
Magnesium chloride, potassium chloride, calcium chloride, iron chloride, titanium chloride, tantalic chloride and copper chloride, carbonate include potassium carbonate, sodium carbonate, carbon
Sour calcium, magnesium carbonate.
5. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 4)
In, protection gas is argon gas, hydrogen or nitrogen, and heating rate is 0.5~10 DEG C/min, under maximum temperature soaking time be 1~
10h。
6. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 5)
In, cleaning solution is water, alcohol, acid or alkali, and the inscribed circle diameter for forming each face of polyhedron of mesh structural porous carbon is 0.2~3mm, more
The cross section inscribed circle diameter of face body connecting rod is 0.02~1.5mm, and the porosity of the mesh structural porous carbon is 70%~99.5%.
7. the preparation method of the mesh structural porous carbon of personalized customization type according to claim 1, it is characterised in that: step 6)
In, protection gas is one of argon gas, hydrogen or nitrogen, and heating rate is 0.5~10 DEG C/min, soaking time under maximum temperature
For 1~3h, the inscribed circle diameter for forming each face of polyhedron of mesh structural porous carbon is 0.2~3mm, forms the cross of polyhedron connecting rod
Section inscribed circle diameter is 0.02~1.5mm, and the porosity of the mesh structural porous carbon is 70%~99.5%.
8. the mesh structural porous carbon of personalized customization type prepared by the preparation method of any one of claim 1-7, it is characterised in that: should
The porosity of the mesh structural porous carbon of personalized customization type is 70%-99.5%, and internal pore structure is made of polyhedron truss structure,
Polyhedron truss structure is evenly distributed or gradient pore structured arrangement.
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| US11192795B2 (en) | 2019-05-01 | 2021-12-07 | Imam Abdulrahman Bin Faisal University | ZnO-porous graphite composites, their use and manufacture |
| CN110479331A (en) * | 2019-08-05 | 2019-11-22 | 江苏大学 | A kind of preparation method and its usage of 3D printing monolithic catalyst |
| CN110761078B (en) * | 2019-11-11 | 2021-04-23 | 中国科学技术大学 | Preparation method and application of black body material |
| CN115050929A (en) * | 2022-08-01 | 2022-09-13 | 深圳市寒暑科技新能源有限公司 | Preparation method of sodium storage hard carbon cathode and sodium storage hard carbon cathode |
| CN115417399B (en) * | 2022-09-30 | 2024-03-26 | 深圳市金牌新能源科技有限责任公司 | Copper-tantalum co-doped hard carbon composite material, and preparation method and application thereof |
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