CN105948810B - A kind of three-dimensional netted through-hole composite material and its preparation - Google Patents
A kind of three-dimensional netted through-hole composite material and its preparation Download PDFInfo
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- CN105948810B CN105948810B CN201610313313.1A CN201610313313A CN105948810B CN 105948810 B CN105948810 B CN 105948810B CN 201610313313 A CN201610313313 A CN 201610313313A CN 105948810 B CN105948810 B CN 105948810B
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5244—Silicon carbide
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The present invention relates to a kind of three-dimensional netted through-hole composite material and its preparations, belong to through-hole composite Materials Design preparing technical field.Three-dimensional netted through-hole composite material of the present invention includes fibrous layer, silicon carbide layer containing Be, and the silicon carbide layer containing Be is coated on fibrous layer；The mass percentage of Be is more than or equal to 0.1% in the three-dimensional netted through-hole composite material；The porosity of the three-dimensional netted through-hole composite material is more than or equal to 50%.Preparation method is：The braided fiber on the structural member with tridimensional network obtains precast body and is placed in maceration extract, dipping, the precast body after being impregnated；Then the precast body after dipping is heated to 240~360 DEG C, heat preservation obtains semi-finished product；Semi-finished product, which are placed in oxygen-containing atmosphere, carries out pre-oxidation treatment, obtains pre-oxidation base；Finally pre-oxidation base is sintered, obtains three-dimensional netted through-hole composite material；The temperature of the sintering is 1100~1500 DEG C.
Description
Technical field
The present invention relates to a kind of three-dimensional netted through-hole composite material and its preparations, belong to through-hole composite Materials Design and prepare skill
Art field.
Background technology
Three-dimensional netted through-hole structure composite material have porosity height, permeability height, large specific surface area, bulk density it is small,
The comprehensive performances such as the low, good mechanical performance of thermal conductivity, are widely used civilian, and about the three dimensional network of high heat conduction
Shape through-hole structure composite material and its preparation are also paid close attention at civilian aspect.Three-dimensional netted through-hole composite material and its system
Preparation Method there is important influence, existing porous material to have its performance：Foamed plastics, foamed ceramics (predominantly silicon carbide
Porous ceramics), foam glass and foam metal (predominantly foam copper or nickel foam).Its technology of preparing mainly has：Particle is sintered
Method, template, addition pore creating material method, direct foaming etc..
There has been no about three-dimensional netted through-hole fiber reinforcement silicon carbide containing beryllium (silicon carbide fiber reinforced) composite material at present
And preparation method thereof report.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of good heat conductivity, the three-dimensional netted of excellent in mechanical performance to lead to
The preparation method of hole composite material and the material.
A kind of three-dimensional netted through-hole composite material of the present invention, the three-dimensional netted through-hole composite material include fibrous layer, contain
Be silicon carbide layers, the silicon carbide layer containing Be are coated on fibrous layer；The quality of Be in the three-dimensional netted through-hole composite material
Percentage composition is more than or equal to 0.1%；The porosity of the three-dimensional netted through-hole composite material is more than or equal to 50%.
A kind of three-dimensional netted through-hole composite material of the present invention, the quality percentage of Be in the three-dimensional netted through-hole composite material
Content is 0.1-0.8%, preferably 0.5-0.8%.
The porosity of a kind of three-dimensional netted through-hole composite material of the present invention, the three-dimensional netted through-hole composite material is 50-
85%.Preferably 60-80% is more preferably 70%-80%.
A kind of three-dimensional netted through-hole composite material of the present invention, in the three-dimensional netted through-hole composite material, closed pore hole
Rate is less than 0.2%.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, includes the following steps：
Step 1
The braided fiber on the structural member with tridimensional network, obtains precast body；
Step 2
Precast body obtained by step 1 is placed in maceration extract, is impregnated, the precast body after being impregnated；Contain in the maceration extract
There is Polycarbosilane containing beryllium；
Step 3
Precast body after dipping obtained by step 2 is heated to 240~360 DEG C, heat preservation obtains semi-finished product；
Step 4
It by semi-finished product obtained by step 3, is placed in oxygen-containing atmosphere and carries out pre-oxidation treatment, obtain pre-oxidation base；The pre- oxygen
The temperature for changing processing is 180~230 DEG C；
Step 5
Under protective atmosphere, pre-oxidation base obtained by step 4 is sintered, three-dimensional netted through-hole composite material is obtained；Institute
The temperature for stating sintering is 1100~1500 DEG C.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the knot of tridimensional network described in step 1
Component is resin structure part.
Preferably, the porosity of the resin structure part is 40%~50%.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the aperture of hole is in the resin structure part
1~3mm, preferably 2~3mm, further preferably 2~2.5mm.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the resin are polyethylene, polypropylene, gather
Vinyl chloride, polystyrene, polylactide, polyamide, ABS (acrylonitrile-butadiene-styrene copolymer) etc., preferred polyamide,
Polylactide and ABS, further preferably polyamide and ABS.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the resin structure part pass through 3D printing system
It is standby.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the fiber described in step 1 are selected from carbon fiber
At least one of dimension, silicon carbide fibre, glass fibre, alumina fibre.Or other fibers can also be used for the present invention.
Preferably, a kind of three-dimensional netted through-hole composite material and preparation method of the present invention, it is fine described in step 1
Dimension is the fiber after Overheating Treatment；The temperature of the heat treatment is 400~600 DEG C, preferably 400~550 DEG C, further excellent
It is selected as 500~550 DEG C；Time is 0.5~2h, preferably 0.5~1.5h, further preferably 1~1.5h.
Precast body obtained by step 1 is placed in maceration extract by a kind of preparation method of three-dimensional netted through-hole composite material of the present invention
In, it is put into vacuum drying chamber after dipping, is preferably less than in the case where pressure is less than 0.07MPa and is equal to 0.03MPa, in 50~60 DEG C
Dry 12~48h, obtains prefabricated component.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, maceration extract described in step 2 have containing the poly- carbon of beryllium
Silane and solvent in mass ratio, Polycarbosilane containing beryllium：Solvent=1:1~4 composition；The solvent is selected from dimethylbenzene, n-hexane, two
At least one of Ethenylbenzene, tetrahydrofuran.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, is stated in Polycarbosilane containing beryllium, the quality hundred of beryllium
It is 0.1~1% to divide content, preferably 0.5~1%, further preferably 0.8~1%.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the Polycarbosilane containing beryllium is to pass through levulinic
What ketone beryllium was synthesized with Polycarbosilane, the number-average molecular weight of Polycarbosilane containing beryllium 12000 hereinafter, preferably 10000~
There are Si -- H bond in 12000, further preferably 11000~11500 on the branch of the Polycarbosilane.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention,
When the structural member of the tridimensional network described in the step 1 is resin structure part,
Precast body after dipping obtained by step 2 is heated to 240~360 DEG C, keeps the temperature 2~8h, removes resin matrix；
To semi-finished product.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, pre-oxidation treatment be controlled at 180~
230 DEG C, preferably 200~230 DEG C, further preferably 200~220 DEG C；Time is 2~12h, preferably 6~12h, into one
Step is preferably 6~8h.
A kind of preparation method of three-dimensional netted through-hole composite material of the present invention, the temperature being sintered described in step 5 are 1100
The time of~1500 DEG C, preferably 1250~1500 DEG C, further preferably 1250~1400 DEG C, sintering is 1~5h, preferably
2.5~5h, further preferably 2.5~3h obtain the three-dimensional netted through-hole fiber reinforcement composite wood of composite material of silicon carbide containing beryllium
Material.
A kind of three-dimensional netted through-hole composite material and preparation method of the present invention, the protective atmosphere is by nitrogen, argon gas, helium
At least one of gas is constituted.
It, can be according to actual demand, repeated impregnations, pre-oxidation, sintering process in scheme designed by the present invention.
Principle and advantage
Principle
The advantages that present invention incorporates 3D printing, three-dimensional fiber weave and Polymeric sponge methods, is prepared for a kind of tool
There is the three-dimensional netted through-hole structure controllable three-dimensional netted through-hole composite wood of pore size, through-hole rate, porosity and thermal conductivity simultaneously
Material.
The present invention mainly has following advantage：
(1) by 3D printing, three-dimensional fiber weaving method, prepared three-dimensional netted through-hole composite material has three dimensional network
Shape, through-hole structure；
(2) present invention is compiled using continuous fiber as establishment body in the structural member of decomposable tridimensional network
Knit, by impregnating Polycarbosilane containing beryllium, then again decomposition texture part and sintering so that prepared composite material with good
Good mechanical property (stretching, compression and bending property)；
(3) thermal conductivity of material prepared by is preferable；
(4) present invention is prepared by precursor pyrolysis and hot pressing, and processing temperature is low；
(5) this method has the characteristics that low processing cost, efficient.
In short, three-dimensional netted through-hole composite material prepared by the present invention have tridimensional network, through-hole, heat conduction it is good,
The advantages such as excellent in mechanical performance, processing temperature be low.
Description of the drawings
Attached drawing 1 is the photo figure in kind of finished product prepared by the embodiment of the present invention 3.
Specific implementation mode
In conjunction with specific example, the present invention is further explained, and present example is described in detail below.
Example 1
Step 1
In mass ratio, Polycarbosilane containing beryllium：Dimethylbenzene=1:1, it is mixed and uniformly obtains precursor maceration extract.It is described to contain
In beryllium Polycarbosilane, the mass percentage of beryllium is 0.2%, molecular weight 11000.
Step 2
It is 1.5mm, the structural member that porosity is 40% to prepare pore size with resin.
Step 3
Resin structure part in conjunction with prepared by step 2 and (temperature is 500 DEG C after pretreatment；Time is 2h) company
The three-dimensional netted braided part of continuous fibrage, and be impregnated in the precursor solution in step 1, it is put into vacuum drying chamber,
60 DEG C are heated to, vacuum degree is -0.05MPa, and time 12h obtains prefabricated component；
Step 4
Prefabricated component prepared by step 3 is positioned in Muffle furnace and is heated to 260 DEG C, and keeps the temperature 3h, removes resin bone
Frame.
Step 5
The obtained prefabricated component prefabricated component of step 4 is put into air dry oven, is heated to 180 DEG C, heat preservation 4h carries out pre-
Oxidation processes.
Step 6
Under protective atmosphere, the three-dimensional netted through-hole prefabricated component after being pre-oxidized to the step Five Classics is put into tube furnace, lazy
Property atmosphere under, be heated to 1200 DEG C, heat preservation 1h carries out ceramic treatment, finally obtains three-dimensional netted through-hole composite material.Gained
The content of Be is in product：0.1%
1 three-dimensional netted through-hole composite property index of table
| Porosity | 65%~70% |
| Density | 0.3~0.6g/cm3 |
| Thermal conductivity | 3W/(m·K) |
| Compression performance | 2.5MPa |
Example 2
Step 1
In mass ratio, Polycarbosilane containing beryllium：Dimethylbenzene=1:3, it is mixed and uniformly obtains precursor maceration extract.It is described to contain
In beryllium Polycarbosilane, the mass percentage of beryllium is 0.5%, molecular weight 10000.
Step 2
It is 3mm, the structural member that porosity is 50% to prepare pore size with resin.
Step 3
Resin structure part in conjunction with prepared by step 2 and (temperature is 600 DEG C after pretreatment；Time is 2h) company
Continuous carbon fiber weaves three-dimensional netted braided part, and is impregnated in the precursor solution in step 1, is put into vacuum drying chamber
In, 60 DEG C are heated to, vacuum degree is -0.09MPa, and time 48h obtains prefabricated component；
Step 4
Prefabricated component prepared by step 3 is positioned in Muffle furnace and is heated to 330 DEG C, and keeps the temperature 6h, removes resin bone
Frame.
Step 5
The obtained prefabricated component prefabricated component of step 4 is put into air dry oven, is heated to 180 DEG C, heat preservation 10h is carried out
Pre-oxidation treatment.
Step 6
Under protective atmosphere, the three-dimensional netted through-hole prefabricated component after being pre-oxidized to the step Five Classics is put into tube furnace, lazy
Property atmosphere under, be heated to 1400 DEG C, heat preservation 3h carries out ceramic treatment, finally obtains three-dimensional netted through-hole composite material.Gained
The content of Be is in product：0.35%
2 three-dimensional netted through-hole composite property index of table
| Porosity | 50%~60% |
| Density | 0.4~0.7g/cm3 |
| Thermal conductivity | 6W/(m·K) |
| Compression performance | 1.8MPa |
Example 3
Step 1
In mass ratio, Polycarbosilane containing beryllium：Dimethylbenzene=1:2, it is mixed and uniformly obtains precursor maceration extract.It is described to contain
In beryllium Polycarbosilane, the mass percentage of beryllium is 0.8%, molecular weight 12000.
Step 2
It is 2mm, the structural member that porosity is 55% to prepare pore size with resin.
Step 3
Resin structure part in conjunction with prepared by step 2 and (temperature is 500 DEG C after pretreatment；Time is 1h) company
Continuous carbon fiber weaves three-dimensional netted braided part, and is impregnated in the precursor solution in step 1, is put into vacuum drying chamber
In, 60 DEG C are heated to, vacuum degree is -0.07MPa, and the time is for 24 hours, to obtain prefabricated component；
Step 4
Prefabricated component prepared by step 3 is positioned in Muffle furnace and is heated to 300 DEG C, and keeps the temperature 4h, removes resin bone
Frame.
Step 5
The obtained prefabricated component prefabricated component of step 4 is put into air dry oven, is heated to 230 DEG C, heat preservation 8h carries out pre-
Oxidation processes.
Step 6
Under protective atmosphere, the three-dimensional netted through-hole prefabricated component after being pre-oxidized to the step Five Classics is put into tube furnace, lazy
Property atmosphere under, be heated to 1300 DEG C, heat preservation 2h carries out ceramic treatment, finally obtains three-dimensional netted through-hole composite material.Gained
The content of Be is in product：0.6%
3 three-dimensional netted through-hole composite property index of table
| Porosity | 65%~80% |
| Density | 0.25~0.5g/cm3 |
| Thermal conductivity | 5W/(m·K) |
| Compression performance | 3.5MPa |
It please fill into following comparative example
Comparative example 1
The uniform embodiment of other conditions 1 is consistent, the difference is that, step 4 in embodiment 1,5 are omitted；Gained produces
The performance of product is：
4 three-dimensional netted through-hole composite property index of table
| Porosity | 45%~55% |
| Density | 0.5~0.8g/cm3 |
| Thermal conductivity | 2.5W/(m·K) |
| Compression performance | 2.2MPa |
Comparative example 2
The uniform embodiment 1 of other conditions is consistent, the difference is that, directly continuous fiber is used to weave three-dimensional netted braiding
Part；Then impregnation is carried out to it；The performance of products obtained therefrom is：
1 three-dimensional netted through-hole composite property index of table
| Porosity | 60%~70% |
| Density | 0.4~0.6g/cm3 |
| Thermal conductivity | 2.2W/(m·K) |
| Compression performance | 1.7MPa |
Claims (8)
1. a kind of three-dimensional netted through-hole composite material, it is characterised in that：The three-dimensional netted through-hole composite material include fibrous layer,
Silicon carbide layer containing Be, the silicon carbide layer containing Be are coated on fibrous layer；The matter of Be in the three-dimensional netted through-hole composite material
It measures percentage composition and is more than or equal to 0.1%；The porosity of the three-dimensional netted through-hole composite material is more than or equal to 50%；
The three-dimensional netted through-hole composite material is obtained by following preparation methods；The preparation method includes the following steps：
Step 1
The braided fiber on the structural member with tridimensional network, obtains precast body；Tridimensional network described in step 1
Structural member be resin structure part；
Step 2
Precast body obtained by step 1 is placed in maceration extract, is impregnated, the precast body after being impregnated；Contain in the maceration extract
Beryllium Polycarbosilane；
Step 3
Precast body after dipping obtained by step 2 is heated to 240~360 DEG C, heat preservation obtains semi-finished product；
Step 4
It by semi-finished product obtained by step 3, is placed in oxygen-containing atmosphere and carries out pre-oxidation treatment, obtain pre-oxidation base；At the pre-oxidation
The temperature of reason is 180~230 DEG C；
Step 5
Under protective atmosphere, pre-oxidation base obtained by step 4 is sintered, three-dimensional netted through-hole composite material is obtained；The burning
The temperature of knot is 1100~1500 DEG C.
2. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：The three-dimensional netted through-hole
The mass percentage of Be is 0.1-0.8% in composite material.
3. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：The three-dimensional netted through-hole
The porosity of composite material is 50-85%；In the three-dimensional netted through-hole composite material, rate of closed hole is less than 0.2%.
4. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：
The porosity of the resin structure part is 40%~50%；
The aperture of hole is 1~3mm in the resin structure part；
The one kind of the resin in polyethylene, polypropylene, polyvinyl chloride, polystyrene, polylactide, polyamide, ABS.
5. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：The resin structure part is logical
Cross 3D printing preparation.
6. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：
Fiber described in step 1 is selected from least one of carbon fiber, silicon carbide fibre, glass fibre, alumina fibre；
Maceration extract described in step 2 has Polycarbosilane containing beryllium and solvent in mass ratio, Polycarbosilane containing beryllium：Solvent=1:1~4
Composition；The solvent is selected from least one of dimethylbenzene, n-hexane, divinylbenzene, tetrahydrofuran.
7. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：
When the structural member of the tridimensional network described in the step 1 is resin structure part,
Precast body after dipping obtained by step 2 is heated to 240~360 DEG C, keeps the temperature 2~8h, removes resin matrix；Obtain half
Finished product.
8. a kind of three-dimensional netted through-hole composite material according to claim 1, it is characterised in that：
In step 4, it is 2~12h that pre-oxidation treatment, which is controlled at 180~230 DEG C, time,；
The temperature being sintered described in step 5 is 1100~1500 DEG C, the time of sintering is 1~5h.
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| CN110542632B (en) * | 2018-12-15 | 2022-03-22 | 嘉思特华剑医疗器材(天津)有限公司 | Method for measuring sleeve through hole rate of 3D printing titanium alloy bone trabecula structure |
| CN110542633B (en) * | 2018-12-15 | 2022-03-22 | 嘉思特华剑医疗器材(天津)有限公司 | Measuring method for through hole rate of 3D-printed titanium alloy bone trabecula mortar cup |
| CN112624764B (en) * | 2020-12-30 | 2022-07-29 | 巴中意科碳素股份有限公司 | Method for preventing isostatic pressing graphite from sintering and cracking |
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