CN114057429A - Ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and preparation method thereof - Google Patents
Ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 81
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 20
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 19
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 229920000193 polymethacrylate Polymers 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 4
- 239000000123 paper Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 125000005234 alkyl aluminium group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- 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
-
- 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
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses an ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and a preparation method thereof, belonging to the field of functional materials. The method for preparing the fiber sheet comprises the following steps: (1) soaking the PVA fiber web in a lithium polysilicate aqueous solution, and drying to obtain the PVA fiber web containing lithium polysilicate; (2) coating the alumina ceramic slurry on the surface of a PVA fiber net containing lithium polysilicate, drying, and sintering at a high temperature to obtain the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet; wherein the alumina ceramic slurry is prepared by mixing alumina powder, methylene bisacrylamide, tetramethylethylenediamine, ammonium persulfate, ammonium polymethacrylate and water according to a mass ratio of 60: 2-4: 1-3: 1-3: 1: 180 by ball milling. The fiber sheet can resist calcination for 10 minutes at 1200 ℃, the mass loss at high temperature is less than 5%, the heat conductivity coefficient is less than 0.5W/(m.K), and the thickness of the sheet is only 0.01mm-0.1 mm.
Description
Technical Field
The invention relates to an ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and a preparation method thereof, belonging to the field of functional materials.
Background
The alumina fiber is one of high-performance ceramic fibers, and the main component is Al2O3The fiber is in the form of short fiber, long fiber, whisker and the like, and has the characteristics of high modulus, high strength, high melting point, high-temperature oxidation resistance, low heat conductivity coefficient and the like. The alumina fiber has higher surface activity and is easy to be compounded with metal and ceramic matrixes, and the advantages enable the alumina fiber to be widely appliedThe method is applied to the field of aviation and aerospace high-temperature thermal protection engineering. At present, according to the high temperature resistant requirement of an aircraft and the specific structure of a hot end part, a single alumina fiber product such as fiber paper, fiber felt, fiber mat, fiber board and the like or a plurality of components are mainly selected to prepare a rigid or flexible heat insulation material for heat insulation protection.
The alumina fiber is mostly made of easily available metal oxides, inorganic salts, and the like. It can be prepared by directly spinning from aqueous solution, sol or other solvents, or by using viscose as carrier. With the development of recent years, the preparation method of the alumina fiber is improved, and the preparation method is mainly divided into the following parts: the slurry method is to take alumina powder as main raw material, add dispersant, rheological agent and sintering aid, make some spinnable slurry under certain conditions, finally obtain fiber by extrusion, drying and sintering. The pre-polymerization method is to polymerize alkyl aluminum and other additives under certain conditions to form an aluminoxane polymer, then dissolve the polymer in an organic solvent added with an organic silicon compound, obtain a spinnable viscous liquid through concentration, prepare precursor fibers through dry spinning, and then calcine the precursor fibers to obtain the polycrystalline continuous alumina fibers. The impregnation method adopts inorganic aluminum salt as impregnation liquid, viscose fiber with good hydrophilic performance as impregnation object substrate fiber, the inorganic aluminum salt is uniformly mixed under certain conditions, the inorganic salt is dispersed in the substrate fiber in a molecular state, and the alumina fiber is obtained through the steps of impregnation, drying, sintering, weaving and the like. The sol-gel method is also called colloid chemical method, and the method uses aluminum alkoxide or inorganic salt as raw material, adds other organic acid catalyst, dissolves in alcohol or water uniformly, obtains sol through alcoholysis (or hydrolysis) and polymerization reaction, and obtains gel fiber after concentrating and reaching certain viscosity and spinning, and finally obtains alumina fiber through heat treatment.
Conventional alumina continuous fiber sheets (fiber papers) are made of alumina fibers (Al)2O3) Deionized water (H)2O) and dispersing agent are used as raw materials, a high-speed stirrer is used for stirring and mixing for 5-10min to obtain slurry, and the alumina fiber paper is prepared by adopting a filtering and forming process. But the cost of the method is high,the process is complicated, the product performance is not easy to control, the preparation of the ultrathin fiber sheet cannot be realized, and the quality of the preparation result is poor.
Disclosure of Invention
[ problem ] to
The traditional alumina continuous fiber sheet is generally thick, and cannot meet the requirements of light weight, ultra-thin property and ultrahigh temperature resistance.
[ solution ]
In order to solve the problems, the PVA fiber web without the slurry is firstly soaked in the lithium polysilicate aqueous solution, is coated with the alumina ceramic slurry after being dried at high temperature, and is dried at high temperature again until the PVA fiber web does not fall off powder, so that the preparation of the alumina continuous fiber sheet is realized.
The first object of the present invention is to provide a method for preparing an ultra-thin high temperature resistant alumina/PVA continuous fiber sheet, comprising the steps of:
(1) soaking the PVA fiber web in a lithium polysilicate aqueous solution, and drying to obtain the PVA fiber web containing lithium polysilicate;
(2) coating alumina ceramic slurry on the surface of the PVA fiber web containing lithium polysilicate in the step (1), drying, and sintering at high temperature to obtain the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet;
the alumina ceramic slurry is prepared by mixing alumina powder, Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water according to a mass ratio of 60: 2-4: 1-3: 1-3: 1: 180 by ball milling.
In one embodiment of the present invention, the alumina powder (particle size of 25 μm), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate, and water are mixed in a mass ratio of 60: 3: 2: 2: 1: 180.
in one embodiment of the present invention, the preparation method of the PVA fiber web in the step (1) comprises:
dissolving PVA in water to form PVA water solution; depositing the nano-fibers prepared from the spinning solution on a net connecting curtain, and drying to obtain a PVA fiber net; wherein the molecular weight of PVA is 20000-95000, and the mass concentration of PVA aqueous solution is 15%; the spinning method adopts electrostatic spinning, and comprises the following specific steps: pouring PVA spinning solution into a semi-cylindrical solution tank, switching on a power supply, and setting the spinning voltage to be 60kV, the rotating speed of a generator to be 10r/min, the spinning distance to be 180mm and the rotating speed of a receiver to be 1m/min through a control panel; the spiral sheet rotates in a solution tank filled with spinning solution at a set speed, so that the spinning solution is attached to the tip of the spiral sheet and brings the liquid to a spinning area, jet flow is formed under the action of an electric field, and the prepared PVA nano fiber is uniformly deposited on the net connecting curtain.
In one embodiment of the present invention, the PVA web in the step (1) has a thickness of 0.005 to 0.08 mm.
In one embodiment of the present invention, the mass concentration of the aqueous lithium polysilicate solution in the step (1) is 8 to 12%, and more preferably 10%.
In one embodiment of the present invention, the impregnation in step (1) is carried out at 20-30 ℃ for 10-20 min.
In one embodiment of the present invention, the drying in step (1) is drying at 100-.
In one embodiment of the present invention, the alumina ceramic slurry of step (2) is coated to a thickness of 0.005mm to 0.02 mm.
In one embodiment of the present invention, the drying in step (2) is drying at 100-.
In one embodiment of the present invention, the high-temperature sintering temperature in step (2) is 800-.
In one embodiment of the present invention, the alumina powder of step (2) has a particle size of 20 to 32 μm.
In one embodiment of the present invention, the specific parameters of the ball milling in the step (2) are as follows: and (3) carrying out ball milling for 2-8h by using a planetary ball mill to reduce the particle size of the alumina to below 6 mu m.
The second purpose of the invention is that the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet prepared by the method is provided.
The third purpose of the invention is to apply the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet material in the field of aerospace.
[ advantageous effects ]
The method of the invention is easy to form aluminum-containing fiber, can be made into fiber products with complex shapes, can realize the functions of light weight, ultra-thin property, ultrahigh temperature resistance, heat insulation and heat preservation, can resist calcination for 10 minutes at 1200 ℃, has the mass loss of less than 5 percent at high temperature, has the heat conductivity coefficient of less than 0.5W/(m.K), and has the sheet thickness of only 0.01mm-0.1mm, so as to meet the use requirements of high temperature resistant parts of aircrafts.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The test method comprises the following steps:
testing of mass loss under high temperature application: calcining at 1200 deg.C for 10 min; mass loss rate msThe mass loss value delta m of the fiber paper after being subjected to high temperature and the mass m of the test piece before high temperature0The ratio of.
Testing of thermal conductivity coefficient: the thermal coefficient was tested according to the national standard GB/T10297-1998.
Testing of tensile strength: the tensile strength was measured according to the national standard GB/T453-1989.
Example 1
A method for preparing an ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet comprises the following steps:
(1) dissolving PVA with molecular weight of 65000 in water to form PVA water solution with mass concentration of 15%; depositing the nano-fibers prepared from the spinning solution on a net connecting curtain, and drying to obtain a PVA fiber net; the spinning method adopts electrostatic spinning, and comprises the following specific steps: pouring PVA spinning solution into a semi-cylindrical solution tank, switching on a power supply, and setting the spinning voltage to be 60kV, the rotating speed of a generator to be 10r/min, the spinning distance to be 180mm and the rotating speed of a receiver to be 1m/min through a control panel; the spiral sheet rotates in a solution tank filled with spinning solution at a set speed, so that the spinning solution is attached to the tip of the spiral sheet and brings the liquid to a spinning area, jet flow is formed under the action of an electric field, and the prepared PVA nanofibers are uniformly deposited on the net connecting curtain; the thickness is 0.05 mm;
(2) soaking the PVA fiber web obtained in the step (1) in a lithium polysilicate aqueous solution with the mass concentration of 10%, taking out, drying at 120 ℃ for 120s, and then calcining at 1000 ℃ for 2min to obtain the PVA fiber web containing lithium polysilicate; wherein the soaking is carried out at 25 ℃ for 15 min;
(3) mixing alumina powder (with a particle size of 25 μm), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water according to a mass ratio of 60: 3: 2: 2: 1: 180, ball-milling for 5 hours by using a planetary ball mill, and reducing the grain diameter of the alumina to 3-6 mu m to obtain alumina ceramic slurry; and (3) coating the alumina ceramic slurry on the surface (with the thickness of 0.03mm) of the PVA fiber web containing lithium polysilicate in the step (2), and drying at 120 ℃ for 120 seconds to obtain the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet (with the thickness of 0.08 mm).
Example 2
Adjusting alumina powder (with the particle size of 25 mu m), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water in the alumina ceramic slurry according to a mass ratio of 60: 2: 1: 1: 1: 180, otherwise, the same as in example 1, to obtain a fiber sheet.
Example 3
Adjusting alumina powder (with the particle size of 25 mu m), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water in the alumina ceramic slurry according to a mass ratio of 60: 4: 3: 3: 1: 180, otherwise, the same as in example 1, to obtain a fiber sheet.
Comparative example 1
The PVA web in example 1 was prepared as a PVA nonwoven fabric (commercially available, 30 g/m)2) The rest was the same as in example 1 to obtain a fiber sheet.
Comparative example 2
The aqueous solution of lithium polysilicate having a mass concentration of 10% was adjusted to an aqueous solution of polyacrylate having a mass concentration of 10%, and the rest was kept the same as in example 1, thereby obtaining a fiber sheet.
Comparative example 3
The mass concentration of the aqueous solution of lithium polysilicate was adjusted to 15%, and the balance was maintained in the same manner as in example 1, thereby obtaining a fiber sheet.
Comparative example 4
The mass concentration of the aqueous solution of lithium polysilicate was adjusted to 5%, and the balance was maintained in the same manner as in example 1, thereby obtaining a fiber sheet.
Comparative example 5
The alumina in the alumina ceramic slurry was adjusted to be silica, and the balance was kept in the same manner as in example 1 to obtain a fiber sheet.
Comparative example 6
Adjusting alumina powder (with the particle size of 25 mu m), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water in the alumina ceramic slurry according to a mass ratio of 60: 1: 4: 2: 1: 180, otherwise, the same as in example 1, to obtain a fiber sheet.
Comparative example 7
Step (2) in example 1 was omitted, and a fiber sheet was obtained in the same manner as in example 1.
Comparative example 8
Step (3) in example 1 was omitted, and a fiber sheet was obtained in the same manner as in example 1.
Comparative example 9
A method of making a fibrous sheet comprising the steps of:
(1) same as example 1, step (1);
(2) mixing alumina powder (with the particle size of 40 mu m), Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water according to the mass ratio of 60: 3: 2: 2: 1: 180, ball milling for 5 hours by using a planetary ball mill to obtain alumina ceramic slurry;
mixing the obtained alumina ceramic slurry and a 10% lithium polysilicate aqueous solution according to a mass ratio of 1: 1, uniformly mixing to obtain a mixed solution;
then, the PVA fiber web obtained in the step (1) was dipped in the mixed solution, taken out, dried at 120 ℃ for 120 seconds, and then calcined at 1000 ℃ for 2 minutes to obtain a fiber sheet (thickness of 0.08 mm).
The fiber sheets obtained in example 1 and comparative examples 1 to 9 were subjected to the performance test, and the test results were as follows:
table 1 test results of fiber sheets obtained in example 1 and comparative examples 1 to 9
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing an ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet is characterized by comprising the following steps:
(1) soaking the PVA fiber web in a lithium polysilicate aqueous solution, and drying to obtain the PVA fiber web containing lithium polysilicate;
(2) coating alumina ceramic slurry on the surface of the PVA fiber web containing lithium polysilicate in the step (1), drying, and sintering at high temperature to obtain the ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet;
the alumina ceramic slurry is prepared by mixing alumina powder, Methylene Bisacrylamide (MBAM), Tetramethylethylenediamine (TEMED), Ammonium Persulfate (APS), ammonium polymethacrylate and water according to a mass ratio of 60: 2-4: 1-3: 1-3: 1: 180 by ball milling.
2. The method of claim 1, wherein the thickness of the PVA web in step (1) is 0.005-0.08 mm.
3. The method according to claim 1, wherein the mass concentration of the aqueous solution of lithium polysilicate of step (1) is 8-12%.
4. The method according to claim 1, wherein the alumina ceramic slurry of step (2) is coated to a thickness of 0.005mm to 0.02 mm.
5. The method as claimed in claim 1, wherein the high temperature sintering temperature in step (2) is 800-1300 ℃, and the sintering time is 1-3 min.
6. The method of claim 1, wherein the specific parameters of the ball milling in the step (2) are as follows: and (3) carrying out ball milling for 2-8h by using a planetary ball mill to reduce the particle size of the alumina to below 6 mu m.
7. The method as claimed in claim 1, wherein the drying in step (1) is performed at 100 ℃ and 120 ℃ for 100 seconds and 150 seconds.
8. The method as claimed in claim 1, wherein the impregnation in step (1) is carried out at 20-30 ℃ for 10-20 min.
9. The ultra-thin high temperature resistant alumina/PVA continuous fiber sheet prepared by the method of any one of claims 1 to 8.
10. The use of the ultra-thin refractory alumina/PVA continuous fiber sheet of claim 9 in the aerospace field.
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| CN102627448A (en) * | 2012-03-31 | 2012-08-08 | 江苏大学 | Method for preparing ceramic fibers |
| CN109891014A (en) * | 2016-10-28 | 2019-06-14 | 电化株式会社 | The manufacturing method and aluminum oxide continuous fiber sheet material of aluminum oxide continuous fiber sheet material |
| CN110357589A (en) * | 2019-07-17 | 2019-10-22 | 辽宁英冠高技术陶瓷股份有限公司 | A kind of Aqueous injection moulding process of structural ceramics |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627448A (en) * | 2012-03-31 | 2012-08-08 | 江苏大学 | Method for preparing ceramic fibers |
| CN109891014A (en) * | 2016-10-28 | 2019-06-14 | 电化株式会社 | The manufacturing method and aluminum oxide continuous fiber sheet material of aluminum oxide continuous fiber sheet material |
| CN110357589A (en) * | 2019-07-17 | 2019-10-22 | 辽宁英冠高技术陶瓷股份有限公司 | A kind of Aqueous injection moulding process of structural ceramics |
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