CN118326563A - Continuous YAG nanofiber and preparation method thereof - Google Patents
Continuous YAG nanofiber and preparation method thereof Download PDFInfo
- Publication number
- CN118326563A CN118326563A CN202410646501.0A CN202410646501A CN118326563A CN 118326563 A CN118326563 A CN 118326563A CN 202410646501 A CN202410646501 A CN 202410646501A CN 118326563 A CN118326563 A CN 118326563A
- Authority
- CN
- China
- Prior art keywords
- yttrium
- yag
- aluminum
- sol
- stirring
- 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
- 239000002121 nanofiber Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 49
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 29
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000009987 spinning Methods 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 16
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 10
- 150000003746 yttrium Chemical class 0.000 claims abstract description 10
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960002303 citric acid monohydrate Drugs 0.000 claims abstract description 9
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 28
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 3
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 2
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 2
- 238000001523 electrospinning Methods 0.000 claims 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 4
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 4
- 229960004106 citric acid Drugs 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 229920001410 Microfiber Polymers 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- -1 aluminum alkoxide Chemical class 0.000 description 2
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 238000000578 dry spinning Methods 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000003658 microfiber Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Abstract
The invention relates to a preparation method of continuous YAG nanofiber, which comprises the steps of mixing inorganic yttrium salt, citric acid monohydrate and an ethanol water mixture, and then heating and stirring at 30-100 ℃ for 1-10h to obtain yttrium-containing complex liquid; mixing inorganic aluminum salt, organic aluminum salt, oxalic acid and water, and then heating and stirring for 2-8 hours at 30-100 ℃ to obtain aluminum sol; mixing the yttrium-containing complex solution and the aluminum sol in proportion, and then heating and stirring for 0.5-3h at 50-90 ℃ to obtain Y-Al sol; adding polyethylene oxide into the obtained Y-Al sol, and stirring for 1-3h to obtain a precursor spinning solution; and then is obtained through electrostatic spinning and high-temperature heat treatment. The fiber solves the problems of poor flexibility, more broken ends, low purity, long time consumption of the preparation process, high cost, low length-diameter ratio of the fiber and the like of the traditional YAG fiber.
Description
Technical Field
The invention belongs to the technical field of fiber preparation, and particularly relates to a continuous YAG nanofiber and a preparation method thereof.
Background
YAG ceramic, yttrium aluminum garnet, has a molecular formula of Y 3Al5O12 and a melting point of 1942 ℃. YAG ceramics have the advantages of high temperature resistance, thermal shock resistance, high temperature creep resistance, good physical/chemical stability, high temperature strength, excellent structural stability and the like, and have wide application prospects in high temperature structural materials. The YAG ceramic has a plurality of good performances and has been widely applied, but the YAG ceramic is limited to be widely applied in the high-temperature field due to the unavoidable ceramic characteristics of brittleness, poor strength and the like.
The preparation of high aspect ratio ceramic fibers is one of the important methods for improving the strength of ceramic materials. From the perspective of ceramic fiber microstructure, reducing the diameter of the ceramic fiber to the nanometer order of magnitude is expected to obviously improve the performance of the ceramic fiber, and further expansion of the functionality of the ceramic fiber is realized. The current method for preparing ceramic fiber mainly comprises melt spinning, centrifugal spinning, dry spinning, electrostatic spinning and the like. The preparation cost of the fiber prepared by melt spinning is high, and the requirement on equipment is high. The fibers obtained by the centrifugal spinning method are shorter. Continuous fibers can be obtained by a dry spinning method, but the preparation method is difficult and has extremely high cost. In addition, the fiber diameter prepared by the method is in the micron level, and is difficult to refine further. The electrostatic spinning equipment is simple, the operability is strong, the cost is low, the application range is wide, and the method is a method capable of directly and continuously preparing the nanofiber.
CN201510436025.0 (CN 105002601 a) discloses a preparation method of polycrystalline Al 2O3-Y3Al5O12 complex-phase microfiber or pure YAG microfiber, which is to heat and reflux anhydrous aluminum chloride solution and aluminum micropowder to obtain polyaluminum chloride mother liquor a; then adding yttrium nitrate, yttrium acetate and a spinning auxiliary glacial acetic acid to obtain a precursor solution B, concentrating under reduced pressure to obtain a precursor sol, and performing centrifugal spinning, drying and heat treatment to obtain the fiber with the average diameter of 6-7 microns, wherein the fiber has the advantages of high temperature resistance, good creep resistance and the like, but has the defects of low length-diameter ratio of the fiber, short length of the fiber, complex process, high cost and the like.
The existing YAG nanofiber has the defects of poor flexibility, more fiber broken ends, low purity, complex preparation process, long preparation period and the like. The YAG-Al 2O3 nanofiber prepared by Journal of European ceramic society (2020) 2463-2469 has a certain flexibility, the continuous YAG-Al 2O3 nanofiber is obtained by increasing the content of Al 2O3, and the prepared YAG-Al 2O3 nanofiber has good flexibility and tensile strength; however, in this production method, the content of the second phase substance Al 2O3 is too high (30% of the introduced Al 2O3) to result in a product of low YAG purity.
Journal of alloys and compounds 879 (2021) 159978 is used for preparing the YAG nanofiber membrane with good flexibility, and the fiber membrane has the characteristics of light weight and high temperature resistance. However, the method needs to synthesize the acetylacetone polymer powder with spinnability, has higher requirements on the preparation process, longer preparation period and higher preparation cost.
Based on this, the present application has been developed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a continuous YAG nanofiber which is prepared by adopting a citric acid complexation and sol-gel method, and the fiber solves the problems of poor flexibility, more broken ends, low purity, long preparation process time consumption, high cost, low fiber length-diameter ratio and the like of the traditional YAG fiber.
The invention also provides a preparation method of the continuous YAG nanofiber.
In order to achieve the above purpose, the invention adopts the following technical scheme:
A method for preparing continuous YAG nanofibers, comprising the steps of:
1) Mixing inorganic yttrium salt, citric acid monohydrate and ethanol water mixture, and then heating and stirring at 30-100 ℃ for 1-10h to obtain yttrium-containing complex liquid;
2) Mixing inorganic aluminum salt, organic aluminum salt, oxalic acid and water, and then heating and stirring for 2-8 hours at 30-100 ℃ to obtain aluminum sol;
3) The yttrium-containing complex liquid obtained in the step 1) and the aluminum sol obtained in the step 2) are mixed according to the proportion (according to the following nY: nal=3:5, molar ratio), and then heating and stirring at 50-90 ℃ for 0.5-3h to obtain Y-Al sol;
4) Adding polyethylene oxide (PEO) into the Y-Al sol obtained in the step 3), and stirring for 1-3h to obtain a precursor spinning solution;
5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step 4) to obtain continuous YAG precursor fibers;
6) And 5) carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step 5) in an air environment to obtain the continuous YAG nanofiber. The diameter of the fiber is 200-900 nm, the fiber is continuous in microstructure, broken ends are rare, the structure is compact, the surface is smooth, and the purity is high.
Specifically, in step 1), the molar ratio of the inorganic yttrium salt to citric acid monohydrate may be 1:1.5-2. The inorganic yttrium salts include, but are not limited to, one or more of yttrium nitrate, yttrium chloride, yttrium acetate, and the like. Further, in the step 1), the mass fraction of the inorganic yttrium salt in the yttrium-containing complex liquid is 15-30wt%. The ethanol water mixture can be a mixture of ethanol and water in any proportion, wherein the mass ratio of ethanol to water is preferably 1:1-3.
Specifically, in step 2), the molar ratio of the inorganic aluminum salt, the organic aluminum salt, oxalic acid and water is 1:2-2.5:0.03-0.04:1.5-60. The inorganic aluminum salt includes, but is not limited to, one or two of aluminum chloride, aluminum nitrate, etc.; the organoaluminum salt may be an aluminum alkoxide, including, but not limited to, one or both of aluminum isopropoxide, aluminum sec-butoxide, and the like.
Specifically, in the step 4), the molecular weight of the polyethylene oxide is 30-100W, and the addition amount is 0.01-10wt% of the weight of the Y-Al sol.
Specifically, in the step 5), the electrostatic spinning voltage is 18-25kV, the curing distance is 15-25cm, and the propelling speed is 0.5-3mL/h. Further, in the step 6), the high-temperature heat treatment temperature is 800-1300 ℃ and the time is 1-6h. It is further preferable that the temperature is raised to the high-temperature heat treatment temperature at a temperature raising rate of 1 to 10 ℃/min.
The invention also provides the continuous YAG nanofiber prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1) The continuous YAG nanofiber prepared by the invention has good flexibility and the diameter is 200-900 nm; the fiber is continuous in microstructure, rarely broken, compact in structure, smooth in surface and high in purity.
2) The invention adopts citric acid complexation and sol-gel method to prepare precursor spinning solution, and prepares continuous YAG nanofiber by electrostatic spinning technology. The citric acid has multiple functions, and is used as a ligand to be complexed with inorganic yttrium salt so as to be crosslinked with colloid particles in aluminum sol, so that a stable crosslinked network structure is formed, and the spinnability of the precursor spinning solution is improved; but also plays a role of inhibitor, delays the hydrolysis of aluminum salt and obtains Y-Al sol with good stability. The fiber prepared by the method overcomes the defect that other impurity components are easy to introduce in the existing preparation process, improves the purity of the product and ensures the quality of the product; meanwhile, the method is simple to operate and has low requirements on manpower and equipment.
3) The continuous YAG nanofiber prepared by the method is continuous, few in broken ends, high in purity, compact in structure, good in flexibility and wide in application prospect in the fields of high-temperature heat insulation, structural toughening and the like.
4) The preparation method of the continuous YAG nanofiber has the characteristics of simple process, low cost, high purity, good operability and the like.
Drawings
FIG. 1 is an SEM image of continuous YAG nanofiber prepared in example 1;
FIG. 2 is an XRD diffraction pattern of the continuous YAG nanofiber prepared in example 1;
FIG. 3 is a bending drawing of the continuous YAG nanofiber prepared in example 1.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the examples below, the starting materials used are either commercially available products which are commercially available as such or can be prepared by methods conventional in the art. Room temperature refers to 25±5 ℃.
Example 1
A method for preparing continuous YAG nanofiber, comprising the steps of:
(1) Mixing 5g (0.013 mol) of yttrium nitrate hexahydrate, 5.48g (0.026 mol) of citric acid monohydrate, 10g of water and 10g of ethanol, heating and stirring at 70 ℃ for dissolution for 2 hours to obtain clear and transparent yttrium-containing complex liquid;
(2) 7.24g (0.03 mol) of aluminum chloride hexahydrate, 15.3g (0.075 mol) of aluminum isopropoxide, 0.1g (0.001 mol) of oxalic acid and 32.4g (1.8 mol) of water are mixed, heated and stirred at 90 ℃ for 6 hours, and then uniform and transparent aluminum sol is obtained;
(3) Mixing 30.48g of yttrium-containing complex liquid obtained in the step (1) with 11.46g of aluminum sol obtained in the step (2) (nY: nAL=3:5, molar ratio), and heating and stirring at 70 ℃ for 0.5h to obtain transparent Y-Al sol;
(4) Adding 0.4g of PEO with the molecular weight of 60W into the Y-Al sol obtained in the step (3), and stirring for 3 hours to obtain a precursor spinning solution;
(5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step (4) at the temperature of 25 ℃ and the humidity of 10% to prepare continuous YAG precursor fibers, wherein the electrostatic spinning voltage is 25kV, the curing distance is 18cm, and the propelling speed is 1.5 mL/h;
(6) Carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step (5) in an air environment, wherein the heat treatment system is as follows: heating to 1000 ℃ from room temperature at a heating rate of 1 ℃/min, preserving heat for 1h, and cooling to room temperature along with a furnace.
SEM tests were performed on the continuous YAG nanofibers obtained in example 1, and the results are shown in fig. 1. As can be seen from FIG. 1, the fibers are continuous and have few breaks, with diameters between 400 and 700nm.
XRD measurements were performed on the continuous YAG nanofibers obtained in example 1, and the results are shown in FIG. 2. As can be seen from FIG. 2, the XRD diffraction peaks of the fibers all belong to Y 3Al5O12 (PDF#33-0040), which indicates that the fibers contain almost no impurities and have extremely high purity.
The continuous YAG nanofiber obtained in example 1 was subjected to a flexibility test, and the results are shown in fig. 3. As can be seen from fig. 3, the fiber has good flexibility and can be bent 180 degrees without breakage.
Example 2
A method for preparing continuous YAG nanofiber, comprising the steps of:
(1) Mixing 5g (0.013 mol) of yttrium nitrate hexahydrate, 5.48g (0.026 mol) of citric acid monohydrate, 10g of water and 10g of ethanol, heating and stirring at 50 ℃ for dissolution for 5 hours to obtain clear and transparent yttrium-containing complex liquid;
(2) 7.24g (0.03 mol) of aluminum chloride hexahydrate, 15.3g (0.075 mol) of aluminum isopropoxide, 0.1g (0.001 mol) of oxalic acid and 32.4g (1.8 mol) of water are mixed, heated and stirred at 90 ℃ for 6 hours, and then uniform and transparent aluminum sol is obtained;
(3) Mixing 30.48g of yttrium-containing complex liquid obtained in the step (1) with 11.46g of aluminum sol obtained in the step (2) (nY: nAL=3:5, molar ratio), and heating and stirring at 70 ℃ for 0.5h to obtain transparent Y-Al sol;
(4) Adding 0.2g of PEO with the molecular weight of 60W into the Y-Al sol obtained in the step (3), and stirring for 3 hours to obtain a precursor spinning solution;
(5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step (4) at the temperature of 25 ℃ and the humidity of 10% to prepare continuous YAG precursor fibers, wherein the electrostatic spinning voltage is 25kV, the curing distance is 18cm, and the propelling speed is 1.5 mL/h;
(6) Carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step (5) in an air environment, wherein the heat treatment system is as follows: heating to 1000 ℃ from room temperature at a heating rate of 1 ℃/min, preserving heat for 1h, and cooling to room temperature along with a furnace.
Example 3
A method for preparing continuous YAG nanofiber, comprising the steps of:
(1) Mixing 5g (0.013 mol) of yttrium nitrate hexahydrate, 5.48g (0.026 mol) of citric acid monohydrate, 10g of water and 10g of ethanol, heating and stirring at 70 ℃ for dissolution for 2 hours to obtain clear and transparent yttrium-containing complex liquid;
(2) 7.24g (0.03 mol) of aluminum chloride hexahydrate, 15.3g (0.075 mol) of aluminum isopropoxide, 0.1g (0.001 mol) of oxalic acid and 32.4g (1.8 mol) of water are mixed, heated and stirred at 90 ℃ for 8 hours, and then uniform and transparent aluminum sol is obtained;
(3) Mixing 30.48g of yttrium-containing complex liquid obtained in the step (1) with 11.46g of aluminum sol obtained in the step (2) (nY: nAL=3:5, molar ratio), and heating and stirring at 70 ℃ for 0.5h to obtain transparent Y-Al sol;
(4) Adding 0.8g of PEO with the molecular weight of 60W into the Y-Al sol obtained in the step (3), and stirring for 3 hours to obtain a precursor spinning solution;
(5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step (4) at the temperature of 25 ℃ and the humidity of 10% to prepare continuous YAG precursor fibers, wherein the electrostatic spinning voltage is 25kV, the curing distance is 18cm, and the propelling speed is 1.5 mL/h;
(6) Carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step (5) in an air environment, wherein the heat treatment system is as follows: heating to 1000 ℃ from room temperature at a heating rate of 1 ℃/min, preserving heat for 1h, and cooling to room temperature along with a furnace.
Example 4
A method for preparing continuous YAG nanofiber, comprising the steps of:
(1) Mixing 5g (0.013 mol) of yttrium nitrate hexahydrate, 5.48g (0.026 mol) of citric acid monohydrate, 5g of water and 15g of ethanol, heating and stirring at 70 ℃ for dissolution for 2 hours to obtain clear and transparent yttrium-containing complex liquid;
(2) 7.24g (0.03 mol) of aluminum chloride hexahydrate, 15.3g (0.075 mol) of aluminum isopropoxide, 0.1g (0.001 mol) of oxalic acid and 32.4g (1.8 mol) of water are mixed, heated and stirred at 90 ℃ for 6 hours, and then uniform and transparent aluminum sol is obtained;
(3) Mixing 30.48g of yttrium-containing complex liquid obtained in the step (1) with 11.46g of aluminum sol obtained in the step (2) (nY: nAL=3:5, molar ratio), and heating and stirring at 70 ℃ for 0.5h to obtain transparent Y-Al sol;
(4) Adding 0.4g of PEO with the molecular weight of 60W into the Y-Al sol obtained in the step (3), and stirring for 3 hours to obtain a precursor spinning solution;
(5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step (4) at the temperature of 25 ℃ and the humidity of 10% to prepare continuous YAG precursor fibers, wherein the electrostatic spinning voltage is 25kV, the curing distance is 18cm, and the propelling speed is 1.5 mL/h;
(6) Carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step (5) in an air environment, wherein the heat treatment system is as follows: heating to 1000 ℃ from room temperature at a heating rate of 5 ℃/min, preserving heat for 3 hours, and cooling to room temperature along with a furnace.
SEM and XRD tests on the continuous YAG nanofibers obtained in examples 2-4 show that the fibers are continuous and have few broken ends, the diameter is 300-750nm, no impurities are contained in the fibers, and the purity is high. The flexibility test results show that the fiber has good flexibility and is bent 180 degrees without breakage.
Comparative example 1
This comparative example differs from example 1 in that no citric acid was added.
The fiber diameter difference obtained by the preparation of the comparative example is large, and the fiber breakage is large. The fiber is easy to break after being bent, and has no flexibility.
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the scope of the invention.
Claims (10)
1. A method for preparing continuous YAG nanofibers, comprising the steps of:
1) Mixing inorganic yttrium salt, citric acid monohydrate and ethanol water mixture, and then heating and stirring at 30-100 ℃ for 1-10h to obtain yttrium-containing complex liquid;
2) Mixing inorganic aluminum salt, organic aluminum salt, oxalic acid and water, and then heating and stirring for 2-8 hours at 30-100 ℃ to obtain aluminum sol;
3) Mixing the yttrium-containing complex liquid obtained in the step 1) and the aluminum sol obtained in the step 2) according to a proportion, and then heating and stirring for 0.5-3h at 50-90 ℃ to obtain Y-Al sol;
4) Adding polyethylene oxide into the Y-Al sol obtained in the step 3), and stirring for 1-3h to obtain a precursor spinning solution;
5) Carrying out electrostatic spinning on the precursor spinning solution obtained in the step 4) to obtain continuous YAG precursor fibers;
6) And 5) carrying out high-temperature heat treatment on the continuous YAG precursor fiber obtained in the step 5) in an air environment to obtain the continuous YAG nanofiber.
2. The method of preparing continuous YAG nanofibers according to claim 1, wherein in step 1), the molar ratio of said inorganic yttrium salt to citric acid monohydrate is 1:1.5-2; the inorganic yttrium salt comprises one or more of yttrium nitrate, yttrium chloride and yttrium acetate.
3. The method of producing continuous YAG nanofibers according to claim 1, wherein in step 1), the mass fraction of the inorganic yttrium salt in the yttrium-containing complex liquid is 15 to 30 wt%.
4. The method of preparing continuous YAG nanofibers according to claim 1, wherein in step 2), the molar ratio of inorganic aluminum salt, organic aluminum salt, oxalic acid to water is 1:2-2.5:0.03-0.04:1.5-60.
5. The method of producing continuous YAG nanofibers according to claim 4, wherein said inorganic aluminum salt comprises one or both of aluminum chloride and aluminum nitrate; the organic aluminum salt comprises one or two of aluminum isopropoxide and aluminum sec-butoxide.
6. The method of producing continuous YAG nanofibers according to claim 1, wherein in step 4), the polyethylene oxide has a molecular weight of 30 to 100W and is added in an amount of 0.01 to 10wt% based on the weight of Y-Al sol.
7. The method of producing continuous YAG nanofibers according to claim 1, wherein in step 5), the electrospinning voltage is 18-25kV, the solidifying distance is 15-25cm, and the advancing speed is 0.5-3mL/h.
8. The method of producing continuous YAG nanofibers according to claim 1, wherein in step 6), the high temperature heat treatment temperature is 800 to 1300 ℃ for 1 to 6 hours.
9. The method of preparing continuous YAG nanofibers of claim 8, wherein the rate of temperature rise is 1-10 ℃/min.
10. Continuous YAG nanofiber prepared by the preparation method of any one of claims 1 to 9.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118326563A true CN118326563A (en) | 2024-07-12 |
Family
ID=
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11572314B2 (en) | Preparation method for yttrium aluminum garnet continuous fiber | |
| CN104086200B (en) | Preparation method of mullite fiber | |
| CN101381225B (en) | Continuous aluminium oxide base ceramic fibre preparation method | |
| CN101982581B (en) | Method for preparing aluminum oxide nanofiber by electrostatic spinning | |
| CN102965764B (en) | Preparation method of aluminum oxide ceramic continuous fiber | |
| WO2019019365A1 (en) | Method for preparing alumina-zirconia composite continuous ceramic fiber | |
| CN104141181B (en) | A kind of containing SiO2the ZrO of doping2the preparation method of fiber | |
| CN101717257A (en) | Technology of preparing aluminium oxide based continuous fibers by sol-gel process | |
| CN102070326B (en) | Preparation process of multi-element composite alumina-based continuous fibers | |
| CN104086201A (en) | High-purity alumina fiber and preparation method thereof | |
| CN104005115A (en) | Method for preparing aluminum oxide ceramic fibers | |
| CN109437862A (en) | One kind containing 1 ~ 5wt%B2O3Alumina-based ceramic continuous fiber preparation method | |
| CN111995393B (en) | Method for preparing aluminum titanate ceramic fiber from titanium-aluminum polymer precursor | |
| CN102978745A (en) | Preparation method of alumina-based continuous long fiber containing mullite whisker second phase | |
| CN110592724A (en) | Hf-Al-Si complex phase oxide ceramic fiber and preparation method thereof | |
| CN106048780A (en) | Method for preparing alumina-based continuous fiber | |
| CN101590434A (en) | A kind of rare-earth cerium doped alumina nano fiber catalyst carrier material and preparation method thereof | |
| CN106637510A (en) | Preparation method of zirconium oxide fibers | |
| CN114703564B (en) | Preparation method of rare earth lanthanum oxide doped high-temperature-resistant alumina fiber | |
| CN102108567A (en) | Method for preparing superfine magnesia ceramic fibers | |
| CN101516803B (en) | Polycrystalline corundum fibers and method for the production thereof | |
| CN102180656B (en) | Technology for preparing alumina-based continuous fibers by using inorganic aluminum salts | |
| CN118326563A (en) | Continuous YAG nanofiber and preparation method thereof | |
| CN111074426B (en) | Alumina-zirconia composite fiber blanket and preparation method thereof | |
| CN109750388A (en) | A kind of preparation method of deficiency fluorite phase gadolinium zirconate fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication |