CN106637510A - Preparation method of zirconium oxide fibers - Google Patents

Preparation method of zirconium oxide fibers Download PDF

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Publication number
CN106637510A
CN106637510A CN201710016727.2A CN201710016727A CN106637510A CN 106637510 A CN106637510 A CN 106637510A CN 201710016727 A CN201710016727 A CN 201710016727A CN 106637510 A CN106637510 A CN 106637510A
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zirconium
zirconium oxide
preparation
acrylic acid
poly
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CN106637510B (en
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任克诚
许元虎
杨家祥
田玉鹏
赵显�
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ANHUI TONGHE CRYSTAL NEW MATERIALS CO LTD
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ANHUI TONGHE CRYSTAL NEW MATERIALS CO LTD
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/04Dry spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

The invention discloses a preparation method of zirconium oxide fibers. The preparation method comprises the following steps of mixing zirconium carbonate, water, acrylic acid, an zirconium oxide crystal phase stabilizing agent and an organic additive to prepare an acrylic polyzirconium sol spinning liquid; performing high-speed centrifugal wire throwing on the acrylic polyzirconium sol spinning liquid, so as to obtain zirconium-containing gel fibers; further sintering at high temperature, so as to obtain the zirconium oxide ceramic fibers. The preparation method of zirconium oxide fibers have the characteristics that the obtaining of raw materials is easy, the preparation method is simple, the environment-friendly effect is good, the preparation method is suitable for scaled production, and the like; the disadvantage of acetic zirconium sol sensitive to humidity is overcame by the prepared acrylic polyzirconium sol spinning liquid; the permeation and absorption of appearance of gel fibers to water can be inhibited; the fibers forming property and production controllability are better; the diameter of the prepared zirconium oxide fibers is 3 to 6mu m, the appearance is smooth, and the diameter is uniform.

Description

A kind of preparation method of Zirconium oxide fibre
Technical field
The present invention relates to a kind of preparation method of Zirconium oxide fibre, belongs to field of inorganic nonmetallic material.
Background technology
Zirconia ceramics fibrous material have that high temperature resistant, thermal conductivity factor be little, acid-alkali-corrosive-resisting strong and normal temperature under for insulation There is the advantageous property such as electric conductivity under body, high temperature, in national defence hard-core technology and civilian high-end heat-insulated wait field to have huge answering Use demand.However, the technology of preparing of zirconia ceramics fibrous material is mainly rested in minority developed country hand, domestic zirconium oxide The correlative study of ceramic fibre material is started late, and technology falls behind relatively.Development technology is simple, be suitable to the preparation of industrialized production Method, produces high-temperature stability high significant with the strong zirconia ceramics fibrous material of mechanical performance.
At present, the preparation method of zirconia ceramics fiber mainly has infusion process, co-blended spinning method and colloidal sol spin processes etc..Leaching Stain method soaks viscose fiber using zirconyl chloride solution, after removing the unnecessary zirconium salt solution between fiber surface and fiber, passes through Fiber after calcination dipping obtains zirconia ceramics fiber.This method is used till today, simple with method, can be mass produced The features such as.But, content of organics is high in this method precursor fiber, there is large quantity of moisture and hydrochloric acid and organic matter row during calcination Remove, cause fiber loose porous, intensity is very low.Co-blended spinning method is the polymer adhesive using Linear Polymer chain and dispersion Agent mixes with zirconium oxide micro mist, and adds resin as bonding agent, and slurry is obtained, and is extruded into silk by micropore high pressure and is used as forerunner Body, by this presoma fiber is directly fired into.In the method for ensure presoma into silk, still used substantial amounts of adhesive and Resinoid bond, and zirconium oxide grain size of micropowder is larger, presoma is thicker, and the fibre structure after firing is undesirable, it is impossible to meets and protects The heat-insulated needs of temperature.Meanwhile, this method needs Jing complicated technologies to prepare the zirconium oxide and zirconates particle of sub-meter grade, relatively costly, no It is suitable to large-scale production.Colloidal sol spin processes be with organic or inorganic zirconates as raw material, it is anti-in a solvent with complexing agent by zirconates Should, prepare and be suitable to the macromolecular colloidal sol of spinning, then prepare zirconia ceramics fiber through spinning and high-temperature process.This method institute The zirconium content for obtaining colloidal sol fiber is higher, reduces the large amount of organic in heat treatment process and decomposes the defect for causing, and can prepare The zirconia ceramics fibrous material of good mechanical performance.
The preparation of the poly- zirconium colloidal sol of spinnability is the key that colloidal sol spin processes prepare zirconia ceramics material.Conventional colloidal sol network Mixture mainly has beta-diketon class, organic carboxyl acid class alcohols and alcamines complexing agent.For example:Patent ZL200410024264.7 is utilized Zirconium oxychloride, acetylacetone,2,4-pentanedione, ethanol, triethylamine etc. prepare acetylacetone,2,4-pentanedione zirconium, then acetylacetone,2,4-pentanedione zirconium and yttrium nitrate are dissolved in Zirconium colloidal sol spinning solution is prepared in methyl alcohol.Substantial amounts of volatile organic solvent and triethylamine etc. are directed in this method poisonous inflammable Quick-fried material, causes control of product quality unstable and industrialization is difficult.Patent CN102181962B adopts zirconium oxycarbonate, ice Acetic acid and water prepare poly- zirconium colloidal sol spinning solution, although process route with respect to environmental protection, but by colloidal sol spinning obtain it is solidifying Glue fiber is sensitive to ambient temperature and humidity so that the fibre-forming performance of colloidal sol spinning solution is poor, obtains easy moisture absorption bonding after gelatinous fibre, Cause the Zirconium oxide fibre pattern and intensity of preparation not good.Therefore, development technology is simple, and environmental protection is cheap, can be used for The poly- zirconium spinning colloidal sols for preparing high-performance zirconia fibrous material have great importance.
The content of the invention
To overcome serious prior art processes complexity, environmental pollution, spinning colloidal sols and gelatinous fibre property stable in the air The defect such as poor, the invention provides a kind of preparation method of Zirconium oxide fibre.
The preparation method of Zirconium oxide fibre of the present invention, is as core technology including as follows with the poly- zirconium spinning colloidal sols of acrylic acid Step:
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
Acrylic acid is added to the water and is uniformly mixed, zirconium carbonate is added after being warming up to 45-75 DEG C, continue to stir to thing Expect transparent clarification, obtain final product the poly- zirconium solution of acrylic acid;Zirconium oxide crystalline phase stabilizer is added in the poly- zirconium solution of gained acrylic acid and is had Machine additive, continues the stirring at 45-75 DEG C and is concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide in system When mass concentration reaches 45-60%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
The mol ratio fed intake according to zirconium oxide, water and acrylic acid in reaction system is 1:5-15:The ratio of 0.5-3, weighs The zirconium carbonate of corresponding weight, water and acrylic acid.
The zirconium oxide crystalline phase stabilizer is yttrium nitrate, according to zirconium oxide in reaction system and Y2O3The mol ratio for feeding intake is 90-95:The ratio of 10-5, weighs the zirconium carbonate and yttrium nitrate of corresponding weight.
The organic additive is one or two in acetic acid, citric acid, according to zirconium oxide in reaction system and acetic acid The mol ratio for feeding intake is 1:The mol ratio that 0.5-2.5, zirconium oxide and citric acid feed intake is 1:The ratio of 0.1-0.3, weighs corresponding The zirconium carbonate of weight, acetic acid and citric acid.
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, in high speed centrifugation effect Under power by getting rid of wire tray aperture by obtain gelatinous fibre containing zirconium into fine;The rotating speed of high speed centrifugation tumbling machine is 10000- per second 13000 turns.
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h, then raises temperature to 1000-1600 DEG C simultaneously Insulation 1h, obtains the Zirconium oxide fibre of a diameter of 3-6 microns by being cooled to after room temperature.
The heating rate for being warming up to 550 DEG C is 0.5-1.5 DEG C/min;The heating rate for being warming up to 1000-1600 DEG C is 1-5 ℃/min。
Beneficial effects of the present invention are embodied in:
1st, the poly- zirconium colloidal sol of acrylic acid of the invention is prepared in a simple way using conventional reaction vessel, is not related to electrolysis Deng complicated technology, and solvent is made using water, it is to avoid the use of a large amount of organic solvents, cost is relatively low, is suitable to large-scale production.
2nd, the poly- zirconium colloidal sol spinning solution of acrylic acid of the invention overcomes shortcoming of the acetic acid zirconium colloidal sol to humidity sensitive, can press down The apparent infiltration and absorption to moisture of gelatinous fibre processed, so that the poly- zirconium colloidal sol of acrylic acid possesses preferable fibre forming property and life Produce controllability.
3rd, prepared by the poly- zirconium colloidal sol spinning solution Jing high speed centrifugations dry spinning of acrylic acid of the invention and subsequent heat treatment Zirconium oxide fibre is a diameter of 3-6 μm, and apparent smooth, uniform diameter, high-temperature behavior is excellent.
Description of the drawings
Fig. 1 is the digital camera photo of the poly- zirconium colloidal sol spinning solution of acrylic acid of the present invention.
Fig. 2 is the digital camera photo of Zirconium oxide fibre of the present invention.
Fig. 3 is the stereoscan photograph of Zirconium oxide fibre of the present invention.
Specific embodiment
Embodiment 1:
The preparation method of Zirconium oxide fibre is as follows in the present embodiment:
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
11.7g acrylic acid is added in 29.2g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 45 DEG C Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs You are than being 1:5:0.5);Zirconium oxide crystalline phase stabilizer yttrium nitrate 27.6g is added in the poly- zirconium solution of gained acrylic acid and organic is added Plus agent acetic acid 48.8g, continue the stirring at 45 DEG C and be concentrated by evaporation, progressively moisture content unnecessary in removing system, when oxidation in system When zirconium mass concentration reaches 45%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 10000 turns per second Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium;
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 0.5 DEG C/min, with It is warming up to 1000 DEG C with the heating rate of 1 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature Zirconium oxide fibre.Using SEM sem tests its average diameters be 3.6 μm, fibre diameter it is uniform and apparent smooth, compared with The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566- 1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1100MPa.
Embodiment 2:
The preparation method of Zirconium oxide fibre is as follows in the present embodiment:
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
23.4g acrylic acid is added in 46.7g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 55 DEG C Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs You are than being 1:8:1);Zirconium oxide crystalline phase stabilizer yttrium nitrate 21.6g and organic addition are added in the poly- zirconium solution of gained acrylic acid Agent acetic acid 39g, citric acid 6.2g, continue the stirring at 55 DEG C and are concentrated by evaporation, and progressively moisture content unnecessary in removing system, works as system When middle zirconium oxide mass concentration reaches 50%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 11000 turns per second Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium;
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.0 DEG C/min, with It is warming up to 1100 DEG C with the heating rate of 2 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature Zirconium oxide fibre.Using SEM sem tests its average diameters be 4.0 μm, fibre diameter it is uniform and apparent smooth, compared with The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566- 1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1200MPa.
Embodiment 3:
The preparation method of Zirconium oxide fibre is as follows in the present embodiment:
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
46.8g acrylic acid is added in 70g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 65 DEG C Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs You are than being 1:12:2);Zirconium oxide crystalline phase stabilizer yttrium nitrate 21.6g and organic addition are added in the poly- zirconium solution of gained acrylic acid Agent acetic acid 19.5g, continues the stirring at 65 DEG C and is concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide in system When mass concentration reaches 55%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 12000 turns per second Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium;
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.2 DEG C/min, with It is warming up to 1200 DEG C with the heating rate of 3.5 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature Zirconium oxide fibre.Using SEM sem tests its average diameters be 4.5 μm, fibre diameter it is uniform and apparent smooth, compared with The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566- 1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1100MPa.
Embodiment 4:
The preparation method of Zirconium oxide fibre is as follows in the present embodiment:
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
70.2g acrylic acid is added in 87.5g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 75 DEG C Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs You are than being 1:15:3);Zirconium oxide crystalline phase stabilizer yttrium nitrate 13.1g and organic addition are added in the poly- zirconium solution of gained acrylic acid Agent acetic acid 9.75g, citric acid 18.6g, continue the stirring at 75 DEG C and are concentrated by evaporation, progressively moisture content unnecessary in removing system, when When zirconium oxide mass concentration reaches 60% in system, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 13000 turns per second Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium;
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.5 DEG C/min, with It is warming up to 1600 DEG C with the heating rate of 5 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature Zirconium oxide fibre.Using SEM sem tests its average diameters be 5.5 μm, fibre diameter it is uniform and apparent smooth, compared with The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566- 1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 350MPa.

Claims (6)

1. a kind of preparation method of Zirconium oxide fibre, it is characterised in that comprise the steps:
(1) preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
Acrylic acid is added to the water and is uniformly mixed, zirconium carbonate is added after being warming up to 45-75 DEG C, continue to stir saturating to material Bright clarification, obtains final product the poly- zirconium solution of acrylic acid;Zirconium oxide crystalline phase stabilizer is added in the poly- zirconium solution of gained acrylic acid and organic is added Plus agent, continue the stirring at 45-75 DEG C and be concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide quality in system When concentration reaches 45-60%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained;
(2) shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step (1) is obtained is placed in high speed centrifugation tumbling machine, in high speed centrifugation active force Under by getting rid of wire tray aperture by obtain gelatinous fibre containing zirconium into fine;
(3) it is heat-treated
The gelatinous fibre containing zirconium that step (2) is obtained is warming up to 550 DEG C and is incubated 1h, 1000-1600 DEG C is then raised temperature to and is protected Warm 1h, obtains the Zirconium oxide fibre of a diameter of 3-6 microns by being cooled to after room temperature.
2. preparation method according to claim 1, it is characterised in that:
In step (1), the mol ratio fed intake according to zirconium oxide, water and acrylic acid in reaction system is 1:5-15:The ratio of 0.5-3 Example, weighs zirconium carbonate, water and the acrylic acid of corresponding weight.
3. preparation method according to claim 1, it is characterised in that:
In step (1), the zirconium oxide crystalline phase stabilizer is yttrium nitrate, according to zirconium oxide in reaction system and Y2O3What is fed intake rubs You are than being 90-95:The ratio of 10-5, weighs the zirconium carbonate and yttrium nitrate of corresponding weight.
4. preparation method according to claim 1, it is characterised in that:
In step (1), the organic additive is one or two in acetic acid, citric acid, according to zirconium oxide in reaction system It is 1 with the mol ratio that acetic acid feeds intake:The mol ratio that 0.5-2.5, zirconium oxide and citric acid feed intake is 1:The ratio of 0.1-0.3, claims Take zirconium carbonate, acetic acid and the citric acid of corresponding weight.
5. preparation method according to claim 1, it is characterised in that:
In step (2), the rotating speed of high speed centrifugation tumbling machine turns for 10000-13000 per second.
6. preparation method according to claim 1, it is characterised in that:
In step (3), the heating rate for being warming up to 550 DEG C is 0.5-1.5 DEG C/min;It is warming up to 1000-1600 DEG C of intensification speed Rate is 1-5 DEG C/min.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108467549A (en) * 2018-03-29 2018-08-31 平顶山学院 A kind of Electric insulation material and preparation method thereof that high temperature resistant is anti-aging
CN111792933A (en) * 2020-07-30 2020-10-20 安徽同和晶体新材料股份有限公司 Method for preparing environment-friendly zirconia crystal fiber by alkaline process
CN113023775A (en) * 2021-04-08 2021-06-25 齐鲁工业大学 Preparation method of ligand-modified zirconia sol and zirconia polycrystalline fiber
CN113620705A (en) * 2021-08-17 2021-11-09 山东鲁阳浩特高技术纤维有限公司 Zirconia fiber and preparation method thereof, zirconia fiber filter material and preparation method thereof
CN113716970A (en) * 2021-09-23 2021-11-30 中钢集团洛阳耐火材料研究院有限公司 Preparation method of zirconia fiber heat insulation product

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503417A (en) * 2011-10-11 2012-06-20 武汉钢铁(集团)公司 Preparation method for yttria-partially-stabilized zirconia powder
CN103193480A (en) * 2013-03-11 2013-07-10 绍兴市圣诺超高温晶体纤维材料有限公司 Preparation method of high-performance zirconia ceramic fibers
CN103757749A (en) * 2013-12-17 2014-04-30 安徽同和晶体新材料股份有限公司 Preparation method for zirconia crystal fiber
CN104032412A (en) * 2014-06-25 2014-09-10 东华大学 Preparation method for zirconium oxide ceramic fibers
CN104987124A (en) * 2015-07-22 2015-10-21 南京理工宇龙新材料科技有限公司 Cubic-phase zirconia fiber reinforced zirconia foamed ceramics and preparation method therefor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503417A (en) * 2011-10-11 2012-06-20 武汉钢铁(集团)公司 Preparation method for yttria-partially-stabilized zirconia powder
CN103193480A (en) * 2013-03-11 2013-07-10 绍兴市圣诺超高温晶体纤维材料有限公司 Preparation method of high-performance zirconia ceramic fibers
CN103757749A (en) * 2013-12-17 2014-04-30 安徽同和晶体新材料股份有限公司 Preparation method for zirconia crystal fiber
CN104032412A (en) * 2014-06-25 2014-09-10 东华大学 Preparation method for zirconium oxide ceramic fibers
CN104987124A (en) * 2015-07-22 2015-10-21 南京理工宇龙新材料科技有限公司 Cubic-phase zirconia fiber reinforced zirconia foamed ceramics and preparation method therefor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108467549A (en) * 2018-03-29 2018-08-31 平顶山学院 A kind of Electric insulation material and preparation method thereof that high temperature resistant is anti-aging
CN111792933A (en) * 2020-07-30 2020-10-20 安徽同和晶体新材料股份有限公司 Method for preparing environment-friendly zirconia crystal fiber by alkaline process
CN113023775A (en) * 2021-04-08 2021-06-25 齐鲁工业大学 Preparation method of ligand-modified zirconia sol and zirconia polycrystalline fiber
CN113620705A (en) * 2021-08-17 2021-11-09 山东鲁阳浩特高技术纤维有限公司 Zirconia fiber and preparation method thereof, zirconia fiber filter material and preparation method thereof
CN113716970A (en) * 2021-09-23 2021-11-30 中钢集团洛阳耐火材料研究院有限公司 Preparation method of zirconia fiber heat insulation product

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