CN110105078A - A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material - Google Patents
A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material Download PDFInfo
- Publication number
- CN110105078A CN110105078A CN201910342019.7A CN201910342019A CN110105078A CN 110105078 A CN110105078 A CN 110105078A CN 201910342019 A CN201910342019 A CN 201910342019A CN 110105078 A CN110105078 A CN 110105078A
- Authority
- CN
- China
- Prior art keywords
- carbon
- carbon fibe
- felt
- thermal insulation
- insulation material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of preparation methods of Carbon fibe sewing charcoal felt hardening plate thermal insulation material.This method specific steps are as follows: one, using the soft felt of Carbon fibe as main raw material(s)；Two, Carbon fibe is longitudinally sewn into type；Three, the configuration of resin maceration extract；Four, resin impregnates；Five, curing process；Six, charing process；Seven, high temperature purification treatment；Eight, it is machined；Nine, hardening plate thermal insulation material is made after surface coated treatment.The present invention is using the soft felt of Carbon fibe as main raw material(s), the moulding process that Carbon fibe longitudinally sews, low-density of the resin carbon matrix as reinforcement, the hardening plate thermal insulation material with certain mechanical strength, and after surface covering sealing pores, have the characteristics that density is low, be not easy to be layered, thermal coefficient is low, good high-temperature stability and processability are strong, and process costs are low.
Description
Technical field
The present invention relates to the preparation methods that a kind of Carbon fibe sews hardening plate thermal insulation material, belong to high temperature furnace used thermal field material
Expect accessory technical field.
Background technique
High temperature furnace obtains extensively as one of the fields such as powder metallurgy, new material, new energy, national defense industry commonly used equipment
Application.High temperature furnace used thermal field material has function and structure double effects, and as consumable part, annual consumption is huge.
In recent years, the progress due to carbon/carbon composite technology of preparing and itself excellent mechanical property, thermal insulation property and anticorrosive, anti-
The performances such as airflow scouring make high temperature furnace used thermal field material gradually turn to carbon/carbon composite by graphite material.
Most of hot component internal layers of high temperature furnace use soft charcoal felt, and outer layer piles up ceramic fibre as thermal insulation material, uses one
After the section time, due to damaged or charcoal deposition etc., thermal insulation property decline, it is necessary to replace, disassembling, assembling and replacing is time-consuming and laborious.And
And Conventional insulation soft charcoal felt has small Carbon fibe to fall off in high temperature furnace in, easily causes the pollution to product, separately
It is also easy to cause the short circuit of heater element outside, causes the damage of heating element and furnace chamber or reduce its service life.It is kept the temperature with soft charcoal felt
Material is compared, and hardening insulation quilt can be processed with enough sizes under high-purity, low heat conductivity, certain mechanical strength and high temperature
Stability, it is often more important that product has stronger processability in the case where low-density, becomes the thermal insulating material of a new generation
Material.
According to data searching, in Chinese invention patent CN1994972, a kind of crystalline silicon growth furnace is disclosed with high purity cured
The manufacturing method of charcoal felt, manufactured high purity cured charcoal felt high-strength light and quality are stablized, and using reliable, but technical process is multiple
Miscellaneous, the manufacturing cycle is long.United States Patent (USP) US6602345B1 discloses a kind of heater assembly of crystal growing furnace, and thermal insulation layer is adopted
With cured charcoal felt or solidification Carbon foam production.In U.S. Patent No. US 3121050, Ford etc. is organic by pyrolysis thermosetting property
Polymer obtains Reticulated Vitreous Carbon foam for the first time.It is mostly the low glass of mechanical strength with organic polymer charring preparation Carbon foam
Charcoal uses Carbon foam as thermal insulation material.The Chinese invention patent of Publication No. CN 101173839A discloses a kind of Carbon foam
The manufacturing method of extraordinarily high temperature macrotype hard heat-insulating room makes heat-insulating room prefabricated blank using Carbon foam, by heat-insulating room prefabricated blank and type
Mould bonding, by solidification, demoulding, the impermeable applying film of system, coating anticorrosion and antioxidant and integral sintered and be made.Publication number
A kind of insulation cover for crucible and preparation method thereof is disclosed for the Chinese invention patent of CN 101003914A, which selects fiber
Arranging has the insulation cover for crucible for concentrating the long fibre graphite insulation quilt production excellent thermal insulation performance tended to.Publication No. CN
The Chinese invention patent of 1011948327A discloses a kind of preparation method of work hardening insulation quilt for high temperature furnace, the patent
Each layer charcoal felt bonding forming is caused due to the difference of thermal expansion coefficient between bonding agent and charcoal felt ontology using resin adhesive
Charcoal felt easily generates layering in heating cooling use process repeatedly.
But high purity cured charcoal felt, cured charcoal felt or the solidification Carbon foam heat-barrier material being previously mentioned in above-mentioned patent, all it is
It is formed by means of mold or mould, is easily layered between product machinability is not strong or felt body.
Summary of the invention
Technology of the invention solves the problems, such as: provide it is a kind of using the soft felt of Carbon fibe as main raw material(s), Carbon fibe
The moulding process longitudinally sewed, low-density of the resin carbon matrix as reinforcement, the hardening plate with certain mechanical strength are protected
Adiabator, and after surface covering sealing pores, has that density is low, be not easy to be layered, thermal coefficient is low, good high-temperature stable
The features such as property and processability are strong, and process costs are low.
To achieve the goals above, the technical scheme adopted by the invention is that: a kind of sewing hardening plate heat preservation of Carbon fibe
The preparation method of material, it is characterised in that method includes the following steps:
Step 1: using the soft felt of Carbon fibe as main raw material(s), soft felt density domination is in 0.06g/cm3-0.14g/cm3,
With a thickness of 4mm-15mm.
Step 2: Carbon fibe is longitudinally sewn into type, and cystosepiment tooling equidimension is placed in lowest level, then according to setting
The number of plies spread the soft felt of Carbon fibe, inserted in inside soft felt using dental nerve hook by Carbon fibe is longitudinally perpendicular, by each soft felt of layer Carbon fibe
It is connected to form entirety with Carbon fibe.
Step 3: configuration resin maceration extract resin and solvent is mixed according to a certain percentage, mixed weight ratio
It is stirred evenly for resin: solvent=1:2-15.
Step 4: the Carbon fibe felt sewed is immersed in step 3 in configured resin maceration extract, resin dipping
Until liquid floods Carbon fibe felt completely.
Step 5: Carbon fibe felt after impregnation in step 4 is placed in progress precuring processing, precuring in curing oven
Temperature is 60 DEG C -100 DEG C, and after precuring 1h-4h, carbon felt 180 degree is overturn, and continues curing process, solidification temperature
Degree is 100 DEG C -200 DEG C, so that resin distribution is relatively uniform in felt body.
Step 6: the carbon felt of curing process in step 5 being placed in retort and carries out charing process, charing temperature
Degree is 800 DEG C -1000 DEG C.
Step 7: carbon felt after hardening that step 6 is come out of the stove being placed in high temperature furnace and carries out high-temperature process, processing temperature
Degree is 1600 DEG C -2500 DEG C.
Step 8: carbon felt after hardening that step 7 is come out of the stove is machined according to drawing, Carbon fibe is made
Harden thermal insulation material blank.
Step 9: the hardening charcoal fiber heat preservation material blank after step 8 is processed carries out surface covering sealing pores, first
The preparation of first layer tie coat is first carried out, graphite powder addition is regard as coating in resin solution, uniformly brushes after processing
Carbon fibe hardens thermal insulation material green body upper and lower surface and side, and curing process, solidification temperature 160 are then carried out in curing oven
℃-240℃.Secondly the preparation of second layer dense coating is carried out, carborundum powder addition is regard as coating in resin solution, uniformly applies
Brush hardens thermal insulation material green body upper and lower surface and side in Carbon fibe.Third layer pyrolysis carbon coating preparation is finally carried out, by Carbon fiber
Dimension hardening thermal insulation material green body is placed in chemical vapor deposition stove, and using propylene as carbon source, nitrogen is diluent gas, is pyrolyzed
Carbon coating preparation is made Carbon fibe and hardens thermal insulation material.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 1
The soft felt of the Carbon fibe stated is PAN base charcoal felt or graphite felt, one of viscose glue base charcoal felt or graphite felt.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 2
The Carbon fibe stated is PAN based carbon fiber, and tow number is one of 1K, 3K or 6K.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 3
The resin stated is furane resins or phenolic resin, and solvent is alcohol or acetone.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 4
The impregnation technology stated, dip time 2h-15h.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 5
The precuring heating rate stated is 3 DEG C/h-15 DEG C/h, and solidification heating rate is 5 DEG C/h-15 DEG C/h, curing time 1h-5h.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 6
The carbonization heating rate stated is 3 DEG C/h-25 DEG C/h, carbonization time 2h-8h.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 7
The high-temperature process heating rate stated is 3 DEG C/h-15 DEG C/h, and the processing time is 2h-6h, vacuum degree≤1000Pa in furnace.
A kind of preparation method of above-mentioned Carbon fibe sewing hardening plate thermal insulation material, which is characterized in that institute in step 9
The graphite powder mesh number stated is 400 mesh and hereinafter, resin solution is with the resin maceration extract of step 3, and graphite powder adds in resin solution
Dosage is 5.0wt%-30wt%, and curing process heating rate is 3 DEG C/h-15 DEG C/h, keeps the temperature 2h-4h.Carborundum powder mesh number is
800 mesh and hereinafter, resin solution with step 3 resin maceration extract, carborundum powder in resin solution additive amount be 8.0wt%-
20wt%.It is pyrolyzed in carbon coating preparation, depositing temperature is 960 DEG C -1080 DEG C, and propylene gas flow and nitrogen gas flow are
1.0m3/h-3.0m3/ h, sedimentation time 30min-60min.
The hardening plate thermal insulation material prepared using the technical program, final densities 0.20g/cm3-0.60g/cm3,
Thermal coefficient≤0.4W/m.K, purity≤1000ppm, anti-airflow scouring and oxidation resistance are strong, are not easy to be layered.
Compared with the prior art, the present invention has the following advantages:
1, compared with conventional fabrication techniques, the moulding process of Carbon fibe longitudinal seam charcoal processing felt of the present invention is not needed by it
His mold or mould molding, longitudinal Carbon fibe is strong to be connected each layer charcoal felt integral, is acted in high temperature circulation thermal stress
Under be not likely to produce layering, globality is more preferable.
2, after high temperature purification treatment of the present invention, machining, surface carries out three layers of composite coating processing, and transition zone makes felt
Binding performance between body and outer coating is good, not easily to fall off, and outer two layers of antioxidant coating to harden plate thermal insulation material
With excellent anti-airflow scouring ability and oxidation resistance, service life of the thermal insulation material in high temperature furnace is substantially prolonged.
Detailed description of the invention
Fig. 1 is the process flow diagram that the present invention prepares Carbon fibe sewing hardening plate thermal insulation material.
Fig. 2 is Carbon fibe sewing charcoal felt molding figure；
Fig. 2 (a) is that Carbon fibe is sewn into type profile figure；Fig. 2 (b) is Carbon fibe sewing molding top view；
1- foam tooling；The soft felt of 2- Carbon fibe；3- dental nerve hook；4- Carbon fibe.
Specific embodiment
Embodiment 1
Step 1: using PAN base charcoal felt as main raw material(s), soft felt density domination is in 0.06g/cm3, with a thickness of 4mm.
Step 2: Carbon fibe is longitudinally sewn into type, and Carbon fibe is PAN based carbon fiber, and tow number is 1K, by cystosepiment tooling
1 equidimension is placed in lowest level, is then laid with 12 layers of PAN charcoal felt 2, is inserted in soft felt using dental nerve hook 3 by Carbon fibe 4 is longitudinally perpendicular
Each soft felt of layer Carbon fibe is connected to form entirety by face with Carbon fibe.
Step 3: configuration resin maceration extract, resin is furane resins, and solvent is alcohol, and resin and solvent are pressed to the weight of 1:2
The mixing of amount ratio, stirs evenly.
Step 4: the Carbon fibe felt sewed is immersed in step 3 in configured resin maceration extract, resin dipping
Until liquid floods Carbon fibe felt completely, dip time 2h.
Step 5: Carbon fibe felt after impregnation in step 4 is placed in progress precuring processing, precuring in curing oven
Temperature is 60 DEG C, and heating rate is 3 DEG C/h, after precuring 1h, carbon felt 180 degree is overturn, curing process is continued,
Solidification temperature is 100 DEG C, and heating rate is 5 DEG C/h, curing time 1h, so that resin distribution is relatively uniform in felt body.
Step 6: the carbon felt of curing process in step 5 being placed in retort and carries out charing process, charing temperature
Degree is 800 DEG C, and carbonization heating rate is 3 DEG C/h, carbonization time 2h.
Step 7: carbon felt after hardening that step 6 is come out of the stove being placed in high temperature furnace and carries out high-temperature process, processing temperature
Degree is 1600 DEG C, and heating rate is 3 DEG C/h, handles time 2h, vacuum degree≤1000Pa in furnace.
Step 8: carbon felt after hardening that step 7 is come out of the stove is machined according to drawing, Carbon fibe is made
Harden thermal insulation material blank.
Step 9: the hardening charcoal fiber heat preservation material blank after step 8 is processed carries out surface covering sealing pores, first
The preparation of first layer tie coat is first carried out, graphite powder addition is regard as coating in resin solution, uniformly brushes after processing
Carbon fibe hardens thermal insulation material green body upper and lower surface and side, and graphite powder mesh number is 450 mesh, the same step 3 of resin solution, graphite
Powder additive amount in resin solution is 5.0wt%.Then curing process is carried out in curing oven, solidification temperature is 160 DEG C, heating
Rate is 3 DEG C/h.Secondly the preparation of second layer dense coating is carried out, regard carborundum powder addition as coating in resin solution,
Even brush hardens thermal insulation material green body upper and lower surface and side in Carbon fibe, and carborundum powder mesh number is 800 mesh, and resin solution is synchronous
Rapid three, carborundum powder additive amount in resin solution is 8.0wt%.Third layer pyrolysis carbon coating preparation is finally carried out, by Carbon fiber
Dimension hardening thermal insulation material green body is placed in chemical vapor deposition stove, and using propylene as carbon source, nitrogen is diluent gas, depositing temperature
It is 960 DEG C, propylene gas flow and nitrogen gas flow are 1.0m3/ h, sedimentation time 30min.Carry out pyrolysis carbon coating system
It is standby, Carbon fibe is made and hardens thermal insulation material.
The hardening plate thermal insulation material prepared using the technical program, final densities 0.20g/cm3, thermal coefficient
0.20W/m.K, purity 800ppm.
Embodiment 2
Step 1: using PAN base graphite felt as main raw material(s), soft felt density domination is in 0.08g/cm3, with a thickness of
10mm。
Step 2: Carbon fibe is longitudinally sewn into type, and Carbon fibe is PAN based carbon fiber, and tow number is 3K, by cystosepiment tooling
1 equidimension is placed in lowest level, is then laid with 6 layers of PAN base graphite felt 2, is inserted in using dental nerve hook 3 by Carbon fibe (4) is longitudinally perpendicular
Inside soft felt, each soft felt of layer Carbon fibe is connected to form entirety with Carbon fibe.
Step 3: configuration resin maceration extract, resin is phenolic resin, and solvent is acetone, and resin and solvent are pressed to the weight of 1:6
The mixing of amount ratio, stirs evenly.
Step 4: the Carbon fibe felt sewed is immersed in step 3 in configured resin maceration extract, resin dipping
Until liquid floods Carbon fibe felt completely, dip time 6h.
Step 5: Carbon fibe felt after impregnation in step 4 is placed in progress precuring processing, precuring in curing oven
Temperature is 80 DEG C, and heating rate is 8 DEG C/h, after precuring 2h, carbon felt 180 degree is overturn, curing process is continued,
Solidification temperature is 150 DEG C, and heating rate is 10 DEG C/h, curing time 3h, so that resin distribution is relatively uniform in felt body.
Step 6: the carbon felt of curing process in step 5 being placed in retort and carries out charing process, charing temperature
Degree is 900 DEG C, and carbonization heating rate is 12 DEG C/h, carbonization time 5h.
Step 7: carbon felt after hardening that step 6 is come out of the stove being placed in high temperature furnace and carries out high-temperature process, processing temperature
Degree is 2000 DEG C, and heating rate is 7 DEG C/h, handles time 4h, vacuum degree≤1000Pa in furnace.
Step 8: carbon felt after hardening that step 7 is come out of the stove is machined according to drawing, Carbon fibe is made
Harden thermal insulation material blank.
Step 9: the hardening charcoal fiber heat preservation material blank after step 8 is processed carries out surface covering sealing pores, first
The preparation of first layer tie coat is first carried out, graphite powder addition is regard as coating in resin solution, uniformly brushes after processing
Carbon fibe hardens thermal insulation material green body upper and lower surface and side, and graphite powder mesh number is 500 mesh, the same step 3 of resin solution, graphite
Powder additive amount in resin solution is 15wt%.Then curing process is carried out in curing oven, solidification temperature is 200 DEG C, heating
Rate is 8 DEG C/h.Secondly the preparation of second layer dense coating is carried out, regard carborundum powder addition as coating in resin solution,
Even brush hardens thermal insulation material green body upper and lower surface and side in Carbon fibe, and carborundum powder mesh number is 800 mesh, and resin solution is synchronous
Rapid three, carborundum powder additive amount in resin solution is 15wt%.Third layer pyrolysis carbon coating preparation is finally carried out, by Carbon fibe
Hardening thermal insulation material green body is placed in chemical vapor deposition stove, and using propylene as carbon source, nitrogen is diluent gas, and depositing temperature is
1040 DEG C, propylene gas flow and nitrogen gas flow are 2.0m3/ h, sedimentation time 45min.Carry out pyrolysis carbon coating system
It is standby, Carbon fibe is made and hardens thermal insulation material.
The hardening plate thermal insulation material prepared using the technical program, final densities 0.40g/cm3, thermal coefficient
0.30W/m.K, purity 500ppm.
Embodiment 3
Step 1: using viscose glue base charcoal felt as main raw material(s), soft felt density domination is in 0.14g/cm3, with a thickness of
15mm。
Step 2: Carbon fibe is longitudinally sewn into type, and Carbon fibe is PAN based carbon fiber, and tow number is 6K, by cystosepiment tooling
1 equidimension is placed in lowest level, is then laid with 4 layers of viscose glue base charcoal felt 2, inserts in soft felt for Carbon fibe 4 is longitudinally perpendicular using dental nerve hook 3
Each soft felt of layer Carbon fibe is connected to form entirety by the inside with Carbon fibe.
Step 3: configuration resin maceration extract, resin is phenolic resin, and solvent is alcohol, by resin and solvent by 1:15's
Weight ratio mixing, stirs evenly.
Step 4: the Carbon fibe felt sewed is immersed in step 3 in configured resin maceration extract, resin dipping
Until liquid floods Carbon fibe felt completely, dip time 15h.
Step 5: Carbon fibe felt after impregnation in step 4 is placed in progress precuring processing, precuring in curing oven
Temperature is 100 DEG C, and heating rate is 15 DEG C/h, after precuring 4h, carbon felt 180 degree is overturn, is continued at solidification
Reason, solidification temperature are 200 DEG C, and heating rate is 15 DEG C/h, curing time 5h, so that resin distribution is relatively uniform in felt body.
Step 6: the carbon felt of curing process in step 5 being placed in retort and carries out charing process, charing temperature
Degree is 1000 DEG C, and carbonization heating rate is 25 DEG C/h, carbonization time 8h.
Step 7: carbon felt after hardening that step 6 is come out of the stove being placed in high temperature furnace and carries out high-temperature process, processing temperature
Degree is 2500 DEG C, and heating rate is 15 DEG C/h, handles time 6h, vacuum degree≤1000Pa in furnace.
Step 8: carbon felt after hardening that step 7 is come out of the stove is machined according to drawing, Carbon fibe is made
Harden thermal insulation material blank.
Step 9: the hardening charcoal fiber heat preservation material blank after step 8 is processed carries out surface covering sealing pores, first
The preparation of first layer tie coat is first carried out, graphite powder addition is regard as coating in resin solution, uniformly brushes after processing
Carbon fibe hardens thermal insulation material green body upper and lower surface and side, and graphite powder mesh number is 600 mesh, the same step 3 of resin solution, graphite
Powder additive amount in resin solution is 30wt%.Then curing process is carried out in curing oven, solidification temperature is 240 DEG C, heating
Rate is 15 DEG C/h.Secondly the preparation of second layer dense coating is carried out, regard carborundum powder addition as coating in resin solution,
Even brush hardens thermal insulation material green body upper and lower surface and side in Carbon fibe, and carborundum powder mesh number is 1000 mesh, and resin solution is same
Step 3, carborundum powder additive amount in resin solution is 20wt%.Third layer pyrolysis carbon coating preparation is finally carried out, by Carbon fiber
Dimension hardening thermal insulation material green body is placed in chemical vapor deposition stove, and using propylene as carbon source, nitrogen is diluent gas, depositing temperature
It is 1080 DEG C, propylene gas flow and nitrogen gas flow are 3.0m3/ h, sedimentation time 60min.Carry out pyrolysis carbon coating system
It is standby, Carbon fibe is made and hardens thermal insulation material.
The hardening plate thermal insulation material prepared using the technical program, final densities 0.45g/cm3, thermal coefficient
0.35W/m.K, purity 300ppm.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent structure transformation to the above embodiments, still fall within skill of the present invention
In the protection scope of art scheme.
Claims (9)
1. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material, it is characterised in that method includes the following steps:
Step 1: using the soft felt of Carbon fibe as main raw material(s), soft felt density domination is in 0.06g/cm3-0.14g/cm3, thickness
For 4mm-15mm；
Step 2: Carbon fibe is longitudinally sewn into type, cystosepiment tooling equidimension is placed in lowest level, then according to the layer set
Number spreads the soft felt of Carbon fibe, is inserted in inside soft felt using dental nerve hook by Carbon fibe is longitudinally perpendicular, by the soft felt charcoal of each layer Carbon fibe
Fiber connects to form entirety；
Step 3: resin and solvent are mixed configuration resin maceration extract according to a certain percentage, and mixed weight ratio is tree
Rouge: solvent=1:2-15 stirs evenly；
Step 4: the Carbon fibe felt sewed is immersed in step 3 in configured resin maceration extract, resin maceration extract is complete
Until total flooding Carbon fibe felt；
Step 5: Carbon fibe felt after impregnation in step 4 is placed in progress precuring processing, precuring temperature in curing oven
It is 60 DEG C -100 DEG C, after precuring 1h-4h, carbon felt 180 degree is overturn, curing process is continued, solidification temperature is
100 DEG C -200 DEG C, so that resin distribution is relatively uniform in felt body；
Step 6: the carbon felt of curing process in step 5 being placed in retort and carries out charing process, and carbonization temperature is
800℃-1000℃；
Step 7: carbon felt after hardening that step 6 is come out of the stove is placed in high temperature furnace and carries out high-temperature process, treatment temperature is
1600℃-2500℃；
Step 8: carbon felt after hardening that step 7 is come out of the stove is machined according to drawing, Carbon fibe hardening is made
Thermal insulation material blank；
Step 9: hardening charcoal fiber heat preservation material blank after step 8 is processed carries out surface covering sealing pores, first into
The preparation of row first layer tie coat regard graphite powder addition as coating in resin solution, uniformly brushes Carbon fiber after processing
Dimension hardening thermal insulation material green body upper and lower surface and side, then carries out curing process in curing oven, and solidification temperature is 160 DEG C-
240℃；Secondly the preparation of second layer dense coating is carried out, carborundum powder addition is regard as coating in resin solution, uniformly brushes
Thermal insulation material green body upper and lower surface and side are hardened in Carbon fibe；Third layer pyrolysis carbon coating preparation is finally carried out, by Carbon fibe
Hardening thermal insulation material green body is placed in chemical vapor deposition stove, and using propylene as carbon source, nitrogen is diluent gas, carries out pyrolytic carbon
Coating preparation is made Carbon fibe and hardens thermal insulation material.
2. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
The soft felt of Carbon fibe described in rapid one is PAN base charcoal felt or graphite felt, one of viscose glue base charcoal felt or graphite felt.
3. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Carbon fibe described in rapid two is PAN based carbon fiber, and tow number is one of 1K, 3K or 6K.
4. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Resin described in rapid three is furane resins or phenolic resin, and solvent is alcohol or acetone.
5. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Impregnation technology described in rapid four, dip time 2h-15h.
6. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Precuring heating rate described in rapid five is 3 DEG C/h-15 DEG C/h, and solidification heating rate is 5 DEG C/h-15 DEG C/h, curing time
For 1h-5h.
7. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Carbonization heating rate described in rapid six is 3 DEG C/h-25 DEG C/h, carbonization time 2h-8h.
8. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
High-temperature process heating rate described in rapid seven is 3 DEG C/h-15 DEG C/h, and the processing time is 2h-6h, vacuum degree in furnace≤
1000Pa。
9. a kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material as described in claim 1, which is characterized in that step
Graphite powder mesh number described in rapid nine is for 400 mesh and hereinafter, resin solution is with the resin maceration extract of step 3, and graphite powder is in resin
Additive amount is 5.0wt%-30wt% in solution, and curing process heating rate is 3 DEG C/h-15 DEG C/h, keeps the temperature 2h-4h；Silicon carbide
Powder mesh number is 800 mesh and hereinafter, resin solution is with the resin maceration extract of step 3, and carborundum powder additive amount in resin solution is
8.0wt%-20wt%.It is pyrolyzed in carbon coating preparation, depositing temperature is 960 DEG C -1080 DEG C, propylene gas flow and nitrogen gas
Flow is 1.0m3/h-3.0m3/ h, sedimentation time 30min-60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910342019.7A CN110105078A (en) | 2019-04-26 | 2019-04-26 | A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910342019.7A CN110105078A (en) | 2019-04-26 | 2019-04-26 | A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110105078A true CN110105078A (en) | 2019-08-09 |
Family
ID=67486813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910342019.7A Pending CN110105078A (en) | 2019-04-26 | 2019-04-26 | A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110105078A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111996813A (en) * | 2020-08-27 | 2020-11-27 | 佛山市石金科技有限公司 | Coating of hard felt and preparation method thereof |
| CN112479731A (en) * | 2020-12-23 | 2021-03-12 | 西安美兰德新材料有限责任公司 | Preparation method of carbon fiber sewing hardening heat-insulation material |
| CN113024265A (en) * | 2021-03-10 | 2021-06-25 | 上海骐杰碳素材料有限公司 | Soft felt with surface treatment and manufacturing method thereof |
| CN113235307A (en) * | 2021-04-26 | 2021-08-10 | 因达孚先进材料(苏州)有限公司 | Hard heat-preservation viscose-based graphite felt and preparation method thereof |
| CN114920573A (en) * | 2022-06-06 | 2022-08-19 | 吉林联科特种石墨材料有限公司 | Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material |
| CN114956843A (en) * | 2022-05-25 | 2022-08-30 | 西安鑫垚陶瓷复合材料有限公司 | Preparation method of ceramic matrix composite material light lattice structure |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948327A (en) * | 2010-08-17 | 2011-01-19 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
| CN103183518A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Method for preparing carbon/carbon composite material draft tube |
| CN103496997A (en) * | 2013-09-06 | 2014-01-08 | 航天材料及工艺研究所 | Preparation method for carbon/carbon composite material thermal-insulation hard felt |
-
2019
- 2019-04-26 CN CN201910342019.7A patent/CN110105078A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948327A (en) * | 2010-08-17 | 2011-01-19 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
| CN103183518A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Method for preparing carbon/carbon composite material draft tube |
| CN103496997A (en) * | 2013-09-06 | 2014-01-08 | 航天材料及工艺研究所 | Preparation method for carbon/carbon composite material thermal-insulation hard felt |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111996813A (en) * | 2020-08-27 | 2020-11-27 | 佛山市石金科技有限公司 | Coating of hard felt and preparation method thereof |
| CN112479731A (en) * | 2020-12-23 | 2021-03-12 | 西安美兰德新材料有限责任公司 | Preparation method of carbon fiber sewing hardening heat-insulation material |
| CN113024265A (en) * | 2021-03-10 | 2021-06-25 | 上海骐杰碳素材料有限公司 | Soft felt with surface treatment and manufacturing method thereof |
| CN113235307A (en) * | 2021-04-26 | 2021-08-10 | 因达孚先进材料(苏州)有限公司 | Hard heat-preservation viscose-based graphite felt and preparation method thereof |
| CN114956843A (en) * | 2022-05-25 | 2022-08-30 | 西安鑫垚陶瓷复合材料有限公司 | Preparation method of ceramic matrix composite material light lattice structure |
| CN114920573A (en) * | 2022-06-06 | 2022-08-19 | 吉林联科特种石墨材料有限公司 | Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110105078A (en) | A kind of preparation method of Carbon fibe sewing hardening plate thermal insulation material | |
| CN110105079A (en) | A kind of preparation method of Carbon fibe sewing hardening heat preservation cylinder | |
| CN101948327B (en) | Method for preparing work hardening insulation quilt for high temperature furnace | |
| CN104230368B (en) | Asphalt base carbon fiber non-woven mat warming plate and manufacture method thereof | |
| CN112479731A (en) | Preparation method of carbon fiber sewing hardening heat-insulation material | |
| CN103496997A (en) | Preparation method for carbon/carbon composite material thermal-insulation hard felt | |
| CN102173844A (en) | Carbon fiber reinforced boron nitride composite and preparation method thereof | |
| CN104261853A (en) | Pitch-based carbon fiber non-woven felt heat-insulating cylinder and preparation method thereof | |
| CN115028466B (en) | Carbon fiber composite material and preparation method thereof | |
| CN106116626A (en) | A kind of preparation method of oxidation resistant carbon carbon composite heat-insulated material | |
| CN104529533B (en) | The preparation method of graphite-pipe for a kind of heat exchanger | |
| CN105272256A (en) | High-heat conduction graphite foam/carbon composite material and preparation method thereof | |
| CN112110743A (en) | CVI, PIP and RMI combined process for preparing carbon/carbon ceramic composite material brake disc | |
| CN103342573B (en) | Method for increasing thermal conductivity of carbon/carbon composite material of diamond film | |
| CN105541365A (en) | Preparation method of high-temperature furnace hardening insulation material | |
| CN113121253B (en) | Ultrahigh-temperature C/SiHfBCN ceramic matrix composite material and preparation method thereof | |
| CN105272330B (en) | A kind of quick method for preparing high heat conductance carbon/carbon composite | |
| CN110698794A (en) | Environment-friendly PVC floor base material added with active bamboo charcoal and production process thereof | |
| CN112723898A (en) | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace | |
| CN104177111B (en) | A kind of slip casting prepares the method for carbon/carbon composite profiles | |
| CN115677380B (en) | Preparation method of thermal field thermal insulation piece composite ceramic coating | |
| CN116283332A (en) | Preparation method of pitch-based carbon/carbon composite material with high thermal conductivity in thickness direction | |
| CN115231923A (en) | Structure function integrated ceramic matrix composite and preparation method thereof | |
| CN104191717B (en) | Carbon fiber thermal insulation sheet material precast body and preparation method thereof | |
| CN114956848A (en) | Preparation method of integrated cylindrical heat-insulating material with graphite efficient barrier layer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |