CN114988870A - Preparation method of zirconium oxide cellucotton - Google Patents
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6225—Fibres based on zirconium oxide, e.g. zirconates such as PZT
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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Abstract
The invention discloses a preparation method of zirconia fiber. Belongs to the field of new materials. The method comprises the steps of taking basic zirconium carbonate, glacial acetic acid, yttrium nitrate hexahydrate and other additives as main raw materials, dissolving the main raw materials in distilled water according to a certain proportion, and fully stirring the main raw materials at the temperature of 40-80 ℃ until the solution is colorless and uniform; concentrating the solution at 70-80 ℃ under reduced pressure to obtain a proper solution with certain viscosity, and adding solvents such as DMSO, NMP, DMF and DMAc to mix to prepare a precursor solution capable of electrostatic spinning; the precursor spinning solution is subjected to electrostatic spinning to obtain fibril, and then the zirconium oxide cellucotton is prepared through high-temperature heat treatment. The zirconia fiber has the diameter of 100-2000 nm, is continuous and good in flexibility, and the volume density range of cellucotton is 8mg/cm 3 ‑300mg/cm 3 Can be used in the field of heat insulation and preservation.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a preparation method of zirconia ceramic fiber.
Background
The low-temperature performance of the power battery of the new energy automobile seems to determine the limitation of the sales area of the electric automobile, but under the support of national policies and the common efforts of engineers, one of the methods for solving the low-temperature performance of the power battery is as follows: the heat preservation design is suitable for the birth, and common heat preservation functions comprise passive heat preservation, active heat preservation and charging heat preservation. Regardless of the insulation scheme, the battery pack usually requires a thermal insulation buffer medium, and materials such as foamed silica gel, mica, aerogel composite materials and the like are generally used. However, the mica has a high density, so that the thermal conductivity of the foamed silica gel is difficult to meet the increasingly stringent requirements, and the application of the aerogel material is limited due to the fragile characteristic of the aerogel material.
In conclusion, the existing materials are difficult to provide complete thermal protection for the battery, and once the problems of thermal runaway and the like of the battery occur, accidents such as combustion and even explosion are easily caused, so that new materials meeting the requirements are urgently needed for protecting the battery.
Disclosure of Invention
The invention discloses a preparation method of zirconia fiber cotton, and aims to provide a novel method for preparing a zirconia ceramic fiber cotton material with low thermal conductivity, so as to solve the problem that the existing power battery has increasingly strict use requirements on heat-insulating and flame-retardant materials.
In order to achieve the purpose, the preparation method of the zirconium oxide cellucotton is realized by a two-step technical scheme, wherein firstly, a spinning precursor solution is prepared, then, the spinning precursor solution is used for carrying out an electrostatic spinning process to obtain fibrils, and the fibrils are subjected to heat treatment to obtain the zirconium oxide ceramic fibers.
Firstly, preparing a spinning precursor solution in step 1, and preparing the spinning precursor solution according to the following steps:
the following raw materials are used in the invention: zirconium basic carbonate, glacial acetic acid (acetic acid), yttrium nitrate, yttrium chloride, gadolinium nitrate, cerium chloride, aluminum nitrate, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP), distilled water, and the like.
Wherein zirconium basic carbonate is used as a zirconium source; yttrium nitrate, yttrium chloride, gadolinium nitrate, cerium chloride, aluminum chloride and aluminum nitrate are used as stabilizing agents of the zirconia fiber; n, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP), distilled water as a solvent.
Firstly, preparing basic zirconium carbonate: glacial acetic acid: distilled water: 100% stabilizer: (30-120): (100-200): (0-20), respectively weighing basic zirconium carbonate, glacial acetic acid, a stabilizer and distilled water, and fully stirring at the temperature of 30-80 ℃ until the solution is colorless and uniform; and then directly stirring and evaporating the solution at 50-80 ℃ or concentrating under reduced pressure to obtain a solution a with certain viscosity, adding a solvent into the solution a, uniformly mixing to prepare a precursor solution b for electrostatic spinning, and using the precursor solution b for preparing fibers by electrostatic spinning. Wherein the stabilizer can be yttrium nitrate, yttrium chloride, gadolinium nitrate, cerium chloride, aluminum nitrate. N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP) and distilled water can be added into the solvent, and the adding proportion of the solvent is 0-50% of the total mass ratio of the precursor solution b.
Then step 2, using the spinning precursor solution b prepared in step 1 as a raw material, preparing fibers by using an electrostatic spinning method, and then performing heat treatment on the prepared fibrils to finally obtain the zirconia ceramic fibers, wherein the process comprises the following steps:
adding the prepared spinning precursor solution b into an injector with a dispensing needle head, and performing high-voltage electrostatic spinning by adopting a high-voltage electrostatic spinning method, wherein the process conditions are as follows: the single needle liquid supply flow range is 0.01-20mL/h, the voltage range is 5-100kV, and the collection distance is 5-50 cm.
The prepared fiber is fibril, and the zirconia ceramic fiber is obtained after heat treatment, wherein the heat treatment process comprises the steps of raising the temperature at the speed of 1-5 ℃/min to 600-1200 ℃, preserving the temperature for 3h, and then reducing the temperature to obtain the zirconia ceramic fiber. The diameter range of the prepared zirconia ceramic fiber is 10-2000nm, and the volume density of cellucotton is 1mg/cm 3 -300mg/cm 3 A range.
The preparation method of the zirconium oxide cellucotton has the following advantages:
the zirconium oxide fiber cotton material prepared by combining the electrostatic spinning technology with the heat treatment has low heat conductivity, and achieves the heat insulation effect by forming a cotton structure by fiber accumulation.
The fiber prepared by the method has controllable diameter range and adjustable density of the cellucotton.
The preparation method is simple and easy to implement, has excellent stability and is low in cost.
Drawings
FIG. 1 is an SEM image of a zirconia ceramic fiber showing that the fiber is continuous and uniform and has a diameter of about 500 nm.
Figure 2 is a digital photograph of zirconia ceramic fiber cotton, and it can be seen from figure 1 that zirconia ceramic fibers are interlaced and stacked to form zirconia ceramic fiber cotton.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
(1) Preparing yttrium zirconate precursor sol spinning solution:
raw materials: basic zirconium carbonate, glacial acetic acid (acetic acid), yttrium nitrate and distilled water
Weighing 100g of basic zirconium carbonate, 100g of glacial acetic acid, 8g of yttrium nitrate and 150g of distilled water, and stirring at the temperature of 60 ℃; after the solid is completely dissolved, the reaction solution is converted into a transparent solution, and the transparent solution is decompressed and concentrated at 60 ℃ until a colorless transparent yttrium zirconate sol spinning solution is obtained; the spinning aid conventionally required for electrospinning is not added.
(2) Electrostatic spinning
Adding yttrium zirconate sol spinning solution into a syringe with a 23G dispensing needle head, pushing a propulsion pump at the speed of 3mL/h to extrude the solution into the syringe, and covering an aluminum foil on a receiving device to collect fibers; and spraying the spinning solution from a dispensing needle at the temperature of 25 ℃, the humidity of 50%, the voltage of 15kV and the receiving distance of 10cm to obtain the yttrium zirconate precursor fiber.
(3) High temperature heat treatment
Placing the fibril prepared by electrostatic spinning in a program-controlled sintering furnace for medium-high temperature heat treatment, heating to 120 ℃ at a heating rate of 3 ℃/min, preserving heat for 1h, heating to 200 ℃ at a heating rate of 1 ℃/min, preserving heat for 1h, heating to 350 ℃ at a heating rate of 1 ℃/min, preserving heat for 2h, heating to 600 ℃ at a heating rate of 2 ℃/min, preserving heat for 2h, heating to 800 ℃ at a heating rate of 5 ℃/min, and preserving heat for 3 h. Thus obtaining the zirconia cellucotton. The diameter range of the prepared zirconia ceramic fiber is 100-1500nm, and the volume density of the fiber cotton is 10mg/cm 3 -100mg/cm 3 A range.
Example 2
(1) Preparing yttrium zirconate precursor sol spinning solution:
raw materials: basic zirconium carbonate, glacial acetic acid (acetic acid), yttrium nitrate, distilled water, dimethyl sulfoxide (DMSO)
Weighing 100g of basic zirconium carbonate, 75g of glacial acetic acid, 8g of yttrium nitrate and 1700g of distilled water, and stirring at the temperature of 60 ℃; and (3) after the solid is completely dissolved, converting the reaction solution into a transparent solution, concentrating at 70 ℃ under reduced pressure until a colorless transparent solution a is obtained, then adding 10 wt% of DMSO, and uniformly stirring to obtain an electrostatic spinning precursor solution b.
(2) Electrostatic spinning
Adding the zirconium spinning solution b into a syringe with a 23G dispensing needle, pushing a propulsion pump at the speed of 5mL/h to extrude the solution in the syringe, and covering an aluminum foil on a receiving device to collect fibers; and (3) spraying the spinning solution from a dispensing needle head at the voltage of 30kV and the acceptance distance of 10cm to obtain precursor cellucotton.
(3) High temperature heat treatment
Drying fibril prepared by electrospinning in a drying oven at 100 ℃ for 24h, and performing heat treatment in a muffle furnace at 800 ℃ for 4h, wherein the raw temperature is controlled at 2 ℃/min. And obtaining the zirconia cellucotton after heat treatment. The diameter range of the prepared zirconia ceramic fiber is 20-1000nm, and the volume density of the cellucotton is 10mg/cm 3 -100mg/cm 3 And (3) a range.
Example 3
(1) Preparing yttrium zirconate precursor sol spinning solution:
raw materials: zirconium basic carbonate, glacial acetic acid (acetic acid), gadolinium nitrate, distilled water, N-dimethylacetamide (DMAc)
Stirring 100g of basic zirconium carbonate, 75g of glacial acetic acid, 6g of gadolinium nitrate and 1700g of distilled water at the temperature of 60 ℃; and (3) after the solid is completely dissolved, converting the reaction solution into a transparent solution, concentrating at 70 ℃ under reduced pressure until a colorless transparent solution a is obtained, then adding 5 wt% of DMAc, and uniformly stirring to obtain an electrostatic spinning precursor solution b.
(2) Electrostatic spinning
Adding the zirconium spinning solution b into a syringe with a 25G dispensing needle, pushing a propulsion pump at the speed of 5mL/h to extrude the solution in the syringe, and covering an aluminum foil on a receiving device to collect fibers; and (3) spraying the spinning solution from a dispensing needle head at the voltage of 25kV and the acceptance distance of 8cm to obtain precursor cellucotton.
(3) High temperature heat treatment
Placing the fibril prepared by electrostatic spinning in a program-controlled sintering furnace to carry out medium-high temperature heat treatment, raising the temperature to 120 ℃ at the rate of 3 ℃/min, keeping the temperature for 1h, raising the temperature to 200 ℃ at the rate of 1 ℃/min, keeping the temperature for 1h, raising the temperature to 350 ℃ at the rate of 1 ℃/min, keeping the temperature for 2h, raising the temperature to 600 ℃ at the rate of 2 ℃/min, keeping the temperature for 2h, raising the temperature to 800 ℃ at the rate of 5 ℃/min, and keeping the temperature for 3 h. Thus obtaining the zirconia cellucotton. The diameter range of the prepared zirconia ceramic fiber is 40-1200nm, and the volume density of the cellucotton is 1mg/cm 3 -100mg/cm 3
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. A zirconia fiber cotton material is characterized in that:
the raw materials comprise: using zirconium basic carbonate as a zirconium source; glacial acetic acid (acetic acid) as a hydrolysis regulator; yttrium nitrate, yttrium chloride, gadolinium nitrate, cerium chloride, aluminum chloride and aluminum nitrate are used as stabilizers; n, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), Dimethylsulfoxide (DMSO), N-methylpyrrolidone (NMP), distilled water, and the like are used as a solvent.
2. A preparation method of zirconia ceramic fiber is characterized by comprising the following process steps:
step 1: preparing a solution by using basic zirconium carbonate, acetic acid, a stabilizer and distilled water, and preparing a solution a in a vacuum distillation or heating evaporation mode; then adding N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP), distilled water and the like as solvents to prepare a spinning precursor solution b;
step 2: and (3) preparing the fiber by using the spinning precursor solution b prepared in the previous step and an electrostatic spinning method, and performing heat treatment on the obtained fibril at 600-1200 ℃ to obtain the zirconium oxide fiber.
3. The process as claimed in claim 1 or 2, wherein the raw materials are as follows: basic zirconium carbonate: glacial acetic acid: distilled water: 100% stabilizer: (30-120): (100-200): (0-20) preparing a solution a, and then adding a solvent into the solution a to prepare a spinning precursor solution b, wherein the addition amount of the solvent is 0-50 wt%.
4. The spinning precursor solution b prepared according to the claims 1, 2 and 3, the fibers are prepared by using the electrospinning process, and the zirconia ceramic fibers are obtained after the fibrils are subjected to heat treatment at 600-1200 ℃. The electrostatic spinning process conditions comprise that the single-needle injection flow rate is 0.01-20mL/h, the voltage range is 5-100kV, and the collection distance is 5-50 cm.
5. The method of claim 1, 2 or 3, wherein the prepared spinning precursor solution is used for preparing fibers by an electrospinning method, the obtained fibrils are subjected to heat treatment to obtain zirconia fiber cotton, which is a zirconia ceramic fiber, the spinning precursor solution b is used as a raw material for the electrospinning preparation method, the diameter of the prepared fibers by the electrospinning method is in the range of 10-2000nm, and the volume density of the fiber cotton is 1mg/cm 3 -300mg/cm 3 And (3) a range.
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Citations (8)
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|---|---|---|---|---|
| JPS62162624A (en) * | 1985-12-10 | 1987-07-18 | Etsuro Kato | Agglomerated particle of monoclinic zirconia ultrafine crystal oriented in fiber-bundle form and production thereof |
| TW495569B (en) * | 1999-08-24 | 2002-07-21 | Basf Ag | Production of zirconium dioxide fibers |
| JP2006336121A (en) * | 2005-05-31 | 2006-12-14 | Teijin Ltd | Method for producing zirconia fiber |
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| CN105133050A (en) * | 2015-09-24 | 2015-12-09 | 江西美赛材料有限公司 | Method for preparing zirconia nanofiber by utilizing electrospinning technology and product prepared by same |
| CN106012105A (en) * | 2016-07-26 | 2016-10-12 | 苏州大学 | Method for preparing zirconium oxide nanometer fiber through bubble spinning |
| CN112608157A (en) * | 2021-01-05 | 2021-04-06 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of zirconia fiber |
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2022
- 2022-06-20 CN CN202210698599.5A patent/CN114988870A/en active Pending
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| TW495569B (en) * | 1999-08-24 | 2002-07-21 | Basf Ag | Production of zirconium dioxide fibers |
| JP2006336121A (en) * | 2005-05-31 | 2006-12-14 | Teijin Ltd | Method for producing zirconia fiber |
| CN102617870A (en) * | 2012-03-31 | 2012-08-01 | 中国地质大学（武汉） | Method for preparing modified epoxy resin composite material |
| JP2015094055A (en) * | 2013-11-14 | 2015-05-18 | 独立行政法人物質・材料研究機構 | Zirconia continuous fiber and method for producing the same |
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| CN106012105A (en) * | 2016-07-26 | 2016-10-12 | 苏州大学 | Method for preparing zirconium oxide nanometer fiber through bubble spinning |
| CN112608157A (en) * | 2021-01-05 | 2021-04-06 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of zirconia fiber |
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| 中国科学技术协会主编: "《重大科学问题和工程技术难题》", 中国科学技术出版社 * |
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| 李茹等: "静电纺丝法制备超细氧化锆纤维", 《现代技术陶瓷》 * |
| 杨清会等: "静电纺丝制备的ZrO2纳米纤维及其应用的研究进展", 《材料导报》 * |
| 程德红: "《柞蚕丝染色整理及综合利用》", 30 April 2019, 中国纺织出版社 * |
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