CN109422920A - It is composite porous and preparation method thereof - Google Patents
It is composite porous and preparation method thereof Download PDFInfo
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- CN109422920A CN109422920A CN201710756248.4A CN201710756248A CN109422920A CN 109422920 A CN109422920 A CN 109422920A CN 201710756248 A CN201710756248 A CN 201710756248A CN 109422920 A CN109422920 A CN 109422920A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2465/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
It is composite porous and preparation method thereof the present invention relates to one kind.This is composite porous using porous material as skeleton, one or more layers membrane structure is coated on skeleton;The hole of the porous material is through-hole;Or the material for the three-dimensional structure for forming above-mentioned material hollow out.The composite porous preparation method, be in the method for vacuum vapor deposition on porous material skeleton plated film.The advantages of of the invention is composite porous low with density, and specific strength is high, good heat insulating.Composite porous preparation method of the invention has simple process, and industrialized requirement may be implemented in the unrestricted advantage of the size of product.
Description
Technical field
It is specifically a kind of composite porous and preparation method thereof the present invention relates to structure function material field.
Background technique
For opposite continuous media material, porous material is since its is light-weight, specific strength is high, sound insulation, heat-insulated, good penetrability
The features such as and be widely used in the neck such as packaging, building masonry wall and interior trim, furniture, medical instrument, shipbuilding industry and aerospace
Domain.Porous material can be divided into organic and inorganic two major classes, and organic porous material mainly has polystyrene foam (EPS) and poly- ammonia
Ester foam (PU), and most widely used and representative inorganic porous material is porous metal material.
The preparation method of traditional organic porous material uses foam process.By taking prepared by polyurethane foam as an example, it is to send out
It under the action of a variety of auxiliary agents such as infusion, catalyst, fire retardant, is mixed by special equipment, is formed through high pressure painting foam-in-place
High molecular polymer.The polyurethane so prepared is mainly characterized by porosity, with density is low, specific strength is high, heat insulating ability
Characteristics can be waited well.But a disadvantage is that: 1) mechanical strength of material have anisotropy, and foam direction intensity highest;2) intolerant to height
Temperature, meeting spontaneous combustion, and also once burning will generate the hydrogen cyanide gas containing severe toxicity.
Prepare porous metal material common method be by liquid metal penetrate into porous sodium chloride in, by sodium chloride is molten remove after
It can be obtained porous metals.Porous metal material specific strength is high, high temperature resistant, but complex process, at high cost, also not corrosion-resistant.
Summary of the invention
An object of the present invention is to provide a kind of composite porous.
It is a further object of the present invention to provide the composite porous preparation methods.
To realize that above-mentioned goal of the invention, the present invention provide technical solution below:
It is a kind of composite porous, using porous material as skeleton, one or more layers membrane structure is coated on skeleton;Institute
The hole for the porous material stated is through-hole;
Or
The material for the three-dimensional structure that above-mentioned material hollow out is formed.
Preferably, the diameter in the hole of the porous material is 100 nanometers to 1 millimeter.
Porous material just refers to the framework material as substrate, is also expressed as " porous material skeleton ", " perforated substrate bone
Frame ".In the present invention, they are meant that equivalent.
The film, material is by Parylene and/or following material: in inorganic oxide, nitride or carbide
It is one or more of.
Parylene (Parylene), i.e. Parylene are a kind of high molecular material, including c-type (Parylene C), N
Type (Parylene N), F type (Parylene F), D type (Parylene D) and various other Parylenes.It is also possible to
State one of material or a variety of.
Preferably, the film is the Parylene that film thickness is 0.1-50 microns.
Preferably, the film is the inorganic oxide that film thickness is 0.01-1 microns, one in nitride or carbide
Kind is several.
It is furthermore preferred that the film is the two or more layers of following material:
The Parylene that film thickness is 0.1-50 microns;
With
One or more of inorganic oxide, nitride or the carbide that film thickness is 0.01-1 microns.
It is furthermore preferred that the film is the hybrid films for the materials described below that film thickness is 0.1-200 microns:
Parylene
With
One or more of inorganic oxide, nitride or carbide.
Above-mentioned inorganic oxide, nitride or carbide be aluminium oxide, titanium oxide, zinc oxide, zirconium oxide, tantalum oxide,
One or more of silica, silicon carbide, silicon nitride.
Another technical solution of the invention is as follows:
Composite porous preparation method, in the method for vacuum vapor deposition on porous material skeleton plated film, it is described
Film be Parylene film and/or following inorganic material film:
One or more of inorganic oxide, nitride or carbide.
Vacuum vapor deposition refers to carry out under vacuum conditions, there is a deposition of chemical reaction.Including but not limited to: vacuum
Chemical vapor deposition (chemical vapor deposition CVD) and atomic layer deposition (Atomic Layer under environment
Deposition, abbreviation ALD).
In the present invention, when plating Parylene film, using chemical vapor deposition;
In the present invention, when plating inorganic material film, using atomic layer deposition.
In the preparation method, the inorganic oxide, nitride or carbide are aluminium oxide, titanium oxide, zinc oxide, oxygen
Change one or more of zirconium, tantalum oxide, silica, silicon carbide, silicon nitride.
The preparation method further includes subsequent processing steps: removing Parylene film and porous material bone using the method for ablation
Frame, or inorganic material film is removed using the method for chemical attack.
Ablation processes can be carried out under vacuum, can not also be carried out under vacuum conditions.Ablation can be by oxidation
Agent such as oxygen is realized.
The chemical attack is to import corrosive gas place the material under vacuum environment or in antivacuum gas phase.
The chemical component of above-mentioned corrosive gas is HCl, HF, H2SO4One of or it is a variety of.
The chemical attack is also possible to place the material in corrosive liquids, the chemistry of the corrosive liquids
Ingredient is one of hydrochloric acid, hydrofluoric acid, sulfuric acid, sodium hydroxide.
It is of the invention composite porous to have the advantage that
1. compared with existing organic porous material, of the invention composite porous have highest specific strength, such as Fig. 8
It is shown.
2. good heat insulating.Fig. 9 thermal conductivity comparison diagram shows composite porous thermal conductivity and titanium dioxide of the invention
Silica aerogel it is suitable, it is lower than polyurethane foam plastics.
3. density is low, light-weight.Figure 10 compares the density of several frequently seen porous material, it can be seen that novel porous multiple
The density of condensation material is suitable with polyurethane foam.
4. there are the characteristics such as high temperature resistant, corrosion-resistant by high temperature ablation or the composite material of chemical attack subsequent processing.
Composite porous preparation method of the invention has the advantage that simple process and low cost, and the size of product is not
It is restricted, industrialized requirement may be implemented.
Detailed description of the invention
For convenience of description, framework material is referred to as " A " or " materials A ", and Parylene is " B " or " material B ";Inorganic material
Material, i.e. one or more of inorganic oxide, nitride or carbide are " C " or " material C ".
Fig. 1 is the structural schematic diagram of composite material of the invention.Material B is plated on framework material A.
Fig. 2 is the structural schematic diagram of composite material of the invention.Material C is plated on framework material A.
Fig. 3 is the structural schematic diagram of composite material of the invention.Material B and C are alternately plated on A, form stepped construction.
Fig. 4 is the structural schematic diagram of composite material of the invention.Material B and C is plated on A simultaneously.
Fig. 5 is the schematic diagram of the vacuum gas-phase chemical deposition of Parylene film.
Fig. 6 is the schematic diagram of Atomic layer deposition method.
Fig. 7 is process flow chart of the invention.
Fig. 8 is the figure compared with several porous material specific strengths of the embodiment of the present invention 3.
Fig. 9 is the figure compared with several porous material thermal conductivities of the embodiment of the present invention 2.
Figure 10 is the density comparison diagram of the embodiment of the present invention 2 Yu different materials.
Figure 11 is the compression strength of composite material and the relational graph of density.
Specific embodiment
Embodiment 1-3
In embodiment 1-3, materials A is a kind of polystyrene foam (EPS) material, pore size to be distributed as 20 micro-
For rice to 500 microns, density is 0.02 gram/cm3.Material B is Parylene C (Parylene-C).Material B is by Parylene plated film work
Skill is coated on the aperture surface inside materials A.Material B's with a thickness of 5 microns in embodiment 1.The thickness of material B in embodiment 2
It is 12 microns.Material B's with a thickness of 25 microns in embodiment 3.Table 1 compared the thus physics of manufactured composite material and substrate
And mechanical performance.
The comparison of the physics and mechanical performance of 1 composite material of table and substrate
Sample | Substrate | Embodiment 1 | Embodiment 2 | Embodiment 3 |
Density (gram/cm3) | 0.02 | 0.04 | 0.10 | 0.21 |
Compression strength (megapascal) | <0.01 | 0.05 | 0.63 | 2.01 |
Accepted standard is ASTM D1621.
Figure 11 shows the compression strength of composite material and the relationship of density.Wherein triangle represents substrate, and dot represents
Composite material.
As shown in figure 11, it is greater than 0.05 gram/cm in density3When, the compression strength of the material is with its density at approximate
Linear relationship.In density less than 0.05 gram/cm3When, the compression strength of material is mainly determined by substrate characteristics.This is rigid permeable
A theoretical typical example.
Fig. 7 is process flow chart of the invention.The material for preparing embodiment 2, adopts following step:
The first step, materials A, i.e. polystyrene foamed material are placed in plating membrane cavity 4, and Parylene powder material is placed in vaporizer
In 1.
Pipeline is heated to 600-700 DEG C by second step, starting heating furnace 3.
Third step starts vacuum pump 5, until the air pressure in 1,2,4 and 6 is lower than 0.02 support (about 2.67Pa).
4th step starts 7 to 150 DEG C of heater, all Parylene powder materials distillation in 1.
The temperature of heater 7 is set as 25 DEG C by the 5th step.
6th step turns off vacuum pump 5 when the temperature of heater 7 drops to 25 DEG C.
7th step takes out the material plated after the air pressure in plating membrane cavity 4 reaches an atmospheric pressure out of 4.
Embodiment 4
Materials A is polyurethane (PU) foamed material, and pore size is distributed as 100 nanometers to 20 microns, and density is
0.06 gram/cm3。
Material C is inorganic compound thin film, including oxide, nitride and carbide.Material C can be but not limited to
Aluminium oxide, titanium oxide, zinc oxide, zirconium oxide, tantalum oxide, silica, silicon carbide, silicon nitride are also possible to by above-mentioned material row
At alloy material.In example 4, material C is aluminium oxide.The film thickness of material C is 100 nanometers.
The specific vacuum gas-phase chemical deposition of thin-film material C is atomic layer deposition (Atomic Layer
Deposition or ALD).Fig. 6 is the schematic diagram of Atomic layer deposition method.1 is Vacuum Deposition membrane cavity, and 3 be inert gas source, 1 and 3
It is connected by pipeline 2 and valve 12.5 be vacuum pump, and 1 and 5 are connected by pipeline 4.6 and 7 be two different reacting gas sources.6 and 7
It is connect respectively by pipeline 8,9 and valve 10,11 with pipeline 2.
Specific steps are as follows
The first step, porous material A are placed in plating membrane cavity 1.
Second step selects reaction gas 6 and 7 according to the requirement of the film, and 6 and 7 is connected on pipeline 8.In reality
It applies in example 4, reaction gas 6 is vapor, and reaction gas 7 is trimethyl aluminium (trimethylaluminum).
Third step starts vacuum pump 5, until the air pressure in 1,2,4 is lower than 0.02 support (about 2.67Pa).
4th step opens valve 12, and inert gas flows into 1, and is then extracted out by vacuum pump 5.
5th step opens valve 10, after one preset time (about 20 seconds), closes valve 10.
6th step, the one preset time of waiting, about 20 seconds.
7th step opens valve 11, after one preset time (about 20 seconds), closes valve 11.
8th step, the one preset time of waiting, about 20 seconds.
9th step repeats above-mentioned five to eight step, until film thickness reaches scheduled thickness.
Embodiment 5
In embodiment 5, materials A is a kind of porous fibrous material compatible with human immune system.Material B is Parylene
C (Parylene C), material C is aluminium oxide.
Material B is plated on the stephanoporate framework of the inside of materials A by Parylene film plating process as described in example 2 by the first step
Surface, the film thickness of material B are 50 microns.
Second step, using atomic layer deposition as described in example 4 (ALD) method by material C be plated in material B surface its
Middle reaction gas 6 is vapor, and reaction gas 7 is trimethyl aluminium (trimethylaluminum).The film thickness of material C is received for 50
Rice.
Third step is plated on material C (aluminium oxide) film plated again by Parylene film plating process as described in example 2
25 microns of material B.
Since Parylene C and human immune system have good compatibility, thus manufactured porous material can be used for human body
Bioengineering.
Embodiment 6
In embodiment 6, materials A is polyurethane (PU) foamed material, and pore size is distributed as 500 microns to 1 milli
Rice, density are 0.05 gram/cm3.Material B is Parylene C (Parylene-C), the first material C is silica, second of material
Material C is aluminium oxide.
Material B is plated on the stephanoporate framework of the inside of materials A by Parylene film plating process as described in example 2 by the first step
Surface, the film thickness of material B are 20 microns.
The first material C (silica) is plated in by second step by the method for atomic layer deposition as described in example 4 (ALD)
The surface of material B, wherein reaction gas 6 is three (tertiary amoxy) silanols (tris (tert-pentoxy) silanol), reaction
Gas 7 is trimethyl aluminium (trimethylaluminum).The film thickness of silica is 50 nanometers.
It is thin to be plated in silica above-mentioned by the method for atomic layer deposition (ALD) by third step for second of material C (aluminium oxide)
The surface of film, wherein 6 vapor of reaction gas, reaction gas 7 are trimethyl aluminium.The film thickness of aluminium oxide is 50 nanometers.
4th step, it is warm in heating furnace place the material in vacuum furnace after having plated second of material C (aluminium oxide)
Degree is 1200 DEG C, and heating furnace gas is pure oxygen, and pressure is 1 support (about 133.32Pa).With this condition, in materials A material B
Hydrocarbon starts to aoxidize, and is finally detached from the form of gaseous carbon dioxide and vapor, in whole hydrocarbons
After being all oxidized ablation, heating in-furnace temperature is reduced to room temperature.
In embodiment 6, made material structure is three be made of hollow silica and alumina composite film skeleton
Tie up porous three dimensional structure.Such material is in addition to usual characteristic above-mentioned, with more the characteristic of high temperature resistant and corrosion.
Embodiment 7
The resulting material of 5 third step of Example, is placed in hydrochloric acid solution and is post-processed.Hydrochloric acid (aoxidizes material C
Aluminium) it erodes completely.Material is cleaned with clear water again.The material obtained through this method is all had by human body compatibility is good
Machine material is constituted, and thus manufactured porous material spaced between layers can be used for human-body biological engineering.
Embodiment 8
The resulting material of 5 third step of Example, is placed in closed cavity, imports hydrochloric and sulfuric acid water vapour,
Pressure is 0.1 support (about 13.3Pa).Hydrochloric acid and sulfuric acid erode material C (aluminium oxide) completely.Material is taken out from cavity,
It is cleaned again with clear water.
Claims (16)
1. a kind of composite porous, characterized in that using porous material as skeleton, one or more layers film is coated on skeleton
Structure;The hole of the porous material is through-hole;
Or
The material for the three-dimensional structure that above-mentioned material hollow out is formed.
2. as described in claim 1 composite porous, characterized in that the diameter in the hole of the porous material is received for 100
Rice is to 1 millimeter.
3. as described in claim 1 composite porous, characterized in that the film, material by Parylene and/or with
Lower material: one or more of inorganic oxide, nitride or carbide.
4. as claimed in claim 3 composite porous, characterized in that the film is the group that film thickness is 0.1-50 microns
Rayleigh.
5. as claimed in claim 3 composite porous, characterized in that the film is the nothing that film thickness is 0.01-1 microns
One or more of machine oxide, nitride or carbide.
6. as claimed in claim 3 composite porous, characterized in that the film is two layers or more of following material
Layer:
The Parylene that film thickness is 0.1-50 microns;
With
One or more of inorganic oxide, nitride or the carbide that film thickness is 0.01-1 microns.
7. as claimed in claim 3 composite porous, characterized in that the film is that film thickness is 0.1-200 microns
The hybrid films of materials described below:
Parylene
With
One or more of inorganic oxide, nitride or carbide.
8. composite porous as described in claim 3,5,6 or 7, characterized in that the inorganic oxide, nitride or
Carbide is one of aluminium oxide, titanium oxide, zinc oxide, zirconium oxide, tantalum oxide, silica, silicon carbide, silicon nitride or several
Kind.
9. composite porous preparation method described in claim 1, characterized in that in the method for vacuum vapor deposition more
Plated film on Porous materials skeleton, the film are Parylene film and/or following inorganic material film: inorganic oxide, nitride or carbon
One or more of compound.
10. composite porous preparation method as claimed in claim 9, characterized in that the vacuum vapor deposition is adopted
With one of following method:
When plating Parylene film, using chemical vapor deposition;
When plating inorganic material film, using atomic layer deposition.
11. composite porous preparation method as claimed in claim 9, characterized in that the inorganic oxide, nitridation
Object or carbide be one of aluminium oxide, titanium oxide, zinc oxide, zirconium oxide, tantalum oxide, silica, silicon carbide, silicon nitride or
It is several.
12. composite porous preparation method as claimed in claim 9, characterized in that further include subsequent processing steps: adopting
Remove Parylene film and porous material skeleton with the method for ablation, or inorganic material film is removed using the method for chemical attack.
13. composite porous preparation method as claimed in claim 12, characterized in that the chemical attack, be by
Material be placed under vacuum environment or antivacuum gas phase in, import corrosive gas.
14. composite porous preparation method as claimed in claim 13, characterized in that the change of the corrosive gas
Study point is HCl, HF, H2SO4One of or it is a variety of.
15. composite porous preparation method as claimed in claim 12, characterized in that the chemical attack, be by
Material is placed in corrosive liquids.
16. composite porous preparation method as claimed in claim 15, the chemical component of the corrosive liquids are
One of hydrochloric acid, hydrofluoric acid, sulfuric acid, sodium hydroxide.
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CN111354575A (en) * | 2020-04-30 | 2020-06-30 | 苏州北科纳米科技有限公司 | Preparation method of porous mxene foam composite material |
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CN111354575A (en) * | 2020-04-30 | 2020-06-30 | 苏州北科纳米科技有限公司 | Preparation method of porous mxene foam composite material |
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