CN103553596A - Preparation method of zirconic acid lanthanum ceramic fiber - Google Patents
Preparation method of zirconic acid lanthanum ceramic fiber Download PDFInfo
- Publication number
- CN103553596A CN103553596A CN201310521491.XA CN201310521491A CN103553596A CN 103553596 A CN103553596 A CN 103553596A CN 201310521491 A CN201310521491 A CN 201310521491A CN 103553596 A CN103553596 A CN 103553596A
- Authority
- CN
- China
- Prior art keywords
- ceramic fiber
- zirconic acid
- lanthanum
- acid lanthanum
- fiber
- 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.)
- Granted
Links
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a preparation method of a zirconic acid lanthanum ceramic fiber. The method comprises the following steps: preparing a gel fiber through a colloidal sol centrifugal fiber forming technology by using zirconium nitrate as a zirconium source, lanthanum nitrate as a lanthanum source, citric acid as a chelating agent, and water as a solvent, and calcining the gel fiber to form the zirconic acid lanthanum ceramic fiber. A precursor prepared by the invention has stable colloidal sol property and is good in filamentation property with no need of adding a polymer spinning additive. The prepared zirconic acid lanthanum ceramic fiber is good in flexibility, compact in microstructure, good in phase stability an low in heat conductivity coefficient and can be used for high-temperature thermal-insulation material, and the crystal form of the zirconic acid lanthanum ceramic fiber is pyrochlore form.
Description
Technical field
The preparation method who the present invention relates to a kind of zirconic acid lanthanum ceramic fiber, belongs to field of inorganic nonmetallic material.
Background technology
In recent years, along with the needs of develop rapidly and the energy-saving and emission-reduction of aeronautical and space technology, more and more higher to the requirement of lagging material.In existing various lagging materials, ceramic fiber is with its outstanding lightweight and high-temperature stability and become the first-selection of lagging material, it is the high-temperature stability of organic and/or inorganic materials both, there are again the features such as low heat conductivity, low density, high heat capacity and the goods of filamentary material are various informative, as high temperature insulating material, have been widely used in all kinds of thermal protection engineerings.
The high-temperature heat insulation fiber material of widespread use at present mainly contains pure aluminium silicate base ceramic fibre, alumina base and zirconia-based ceramics fiber.Aluminosilicate refractory fiber has solved the heat-insulating problem of spacecraft substantially, but because the thermal conductivity of this material is relatively large, therefore must reduce thermal conduction with thicker size, and increase transmitting and the manufacturing cost of all kinds of aircraft; In addition, aluminosilicate refractory fiber goods are considered to two class carcinogenss and by American-European countries, are forbidden just gradually.Ceramic alumina fiber has good heat-insulating property as lagging material, can significantly reduce thermosteresis, but the upper limit temperature of heat tolerance can only reach 1700 ℃.The high temperature that zirconia ceramics fiber ability is 2000 ℃, during high temperature, can resistance to acid corrode, but zirconia-based ceramics fiber has 8% volumetric expansion when tetragonal is cooled to monocline, the accumulation that recycles stress in process can cause thermofin to destroy, and even loses efficacy.
For meeting the requirement of the high use temperature of high temperature insulating material, low thermal conductivity, anti-sintering and thermal distortion, it is found that the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) material property is better.La
2zr
2o
7there is good high-temperature-phase stability, fusing point (2300 ℃) before crystalline structure remain unchanged.In addition, its intrinsic thermal conductivity is lower than zirconium white (La
2zr
2o
7, 1.56W/ (mK); ZrO
2, 2.3W/ (mK)).ZrO
2oxygen infiltration type material, and La
2zr
2o
7oxygen ionic conductivity is very low, can be described as not infiltration type material of oxygen.With ZrO
2compare La
2zr
2o
7in room temperature, to nothing between fusing point, change mutually, thermostability is higher, and thermal conductivity, thermal expansivity and Young's modulus are lower, more anti-sintering.Based on La
2zr
2o
7the above-described outstanding advantages of material, La
2zr
2o
7fiber is in the application prospect widely that has in high temperature insulating field.
Current La
2zr
2o
7the preparation method of powder mainly contains the precipitator method, solid reaction process, hydrothermal synthesis method, sol-gel method, self-propagating combustion etc., and CN101407336A provides a kind of method that adopts solution coprecipitation method to prepare lanthanum zirconate powder.But the preparation of zirconic acid lanthanum ceramic fiber there is not yet patent report.Due to zirconic acid lanthanum La
2zr
2o
7the fusing point of material own is very high, be difficult to sintering, with traditional melt-spinning, is difficult to realize.If prepare gelled fibre by electrostatic spinning technique, then zirconic acid lanthanum (La is prepared in calcining
2zr
2o
7) nanofiber, due to La
2zr
2o
7itself is difficult to sintering material, adds in spinning solution and has a large amount of chlorions, and causing fiber is to be connected and composed by irregular nanometer sheet, and the poor fiber snappiness that makes of compactness is poor, hinders it in the practical application in high temperature insulating field.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of zirconic acid lanthanum ceramic fiber.
Technical scheme of the present invention is as follows:
A kind of zirconic acid lanthanum (La
2zr
2o
7) preparation method of ceramic fiber, comprise that step is as follows:
(1) preparation of spinning property precursor sol
Zirconium nitrate, lanthanum nitrate and citric acid are joined respectively in suitable quantity of water, stir to clarify transparent; Under room temperature, three kinds of solution are mixed, after stirring, 40～70 ℃ of water-baths, being aged to viscosity is 60～100Pas, obtains spinning property precursor sol;
Wherein, the mol ratio of zirconium nitrate and lanthanum nitrate is 1:0.87～1.15, presses metal ion (La
3++ Zr
4+) with the mol ratio of citric acid be that citric acid is added in 1:0.3～1.2.
(2) centrifugal fibroblast is prepared gelled fibre
Spinning property precursor sol prepared by step (1) carries out centrifugal fibroblast, and processing condition are: getting rid of a bore dia is 0.2～0.5mm, and getting rid of a revolution is 3000～12000r/min, and getting rid of temperature in silk bucket is 10～40 ℃, and relative humidity is 10～40%; Obtain gelled fibre;
(3) calcining gelled fibre carries out ceramic
Ceramic is carried out in gelled fibre calcining prepared by step (2), processing condition are: the heat-up rate with 0.5～3 ℃/min rises to 550～650 ℃ from room temperature, at this temperature insulation 0.5～2h, heat-up rate with 5～10 ℃/min rises to 800～1000 ℃ again, at this temperature insulation 0.5～3h, obtain the zirconic acid lanthanum ceramic fiber of fluorite structure again; Finally with the heat-up rate of 10～20 ℃/min, rise to 1100～1400 ℃ again, and at this temperature insulation 0.5～2h, obtain the zirconic acid lanthanum ceramic fiber of pyrochlore type structure.
According to the present invention, optimum condition is as follows:
In step (1), zirconium nitrate (Zr (NO
3)
43H
2o) with lanthanum nitrate (La (NO
3)
36H
2o) mol ratio is 1:0.95～1.05; Citric acid (C
6h
8o
7h
2o) press metal ion (La
3++ Zr
4+) being 1:0.6～1.0 with the mol ratio of citric acid, amount is added.
The zirconium nitrate, the lanthanum nitrate that use are respectively Zr (NO
3)
43H
2o, La (NO
3)
36H
2o.
In step (1), water-bath aging temperature is 40～60 ℃, and being aged to viscosity is 70～90Pas, obtains the spinning property precursor sol that ropiness is good, under room temperature, with glass stick, can pull out long filament.Viscosity of the present invention all adopts rotational viscosimeter at room temperature to measure.
In step (2), getting rid of a bore dia is 0.2～0.3mm, and getting rid of temperature in silk bucket is 20～40 ℃, and getting rid of a rotating speed is 6000～9000r/min, and relative humidity is 10～30%.
Calcining gelled fibre in step (3) carries out ceramic processing condition: the heat-up rate with 0.5～1 ℃/min rises to 600～650 ℃ from room temperature, at this temperature insulation 1～2h, heat-up rate with 5～8 ℃/min rises to 800～900 ℃ again, obtains the zirconic acid lanthanum (La of fluorite type structure at this temperature insulation 0.5～1h
2zr
2o
7) ceramic fiber, finally with the heat-up rate of 10～20 ℃/min, rise to 1100～1300 ℃ again, and at this temperature insulation 0.5～2h, obtain the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) ceramic fiber.
The pyrochlore-type zirconic acid lanthanum (La that utilizes the inventive method to prepare
2zr
2o
7) ceramic fiber diameter is little and be evenly distributed, diameter Distribution scope is 1～7 μ m; Fiber outward appearance is fluffy, has snappiness, and thermal conductivity 0.054～0.082W/ (mK) is applicable to being applied to high temperature insulating field very much.
The method that the present invention prepares zirconic acid lanthanum ceramic fiber is, with zirconium nitrate (Zr (NO
3)
43H
2o) be zirconium source, lanthanum nitrate (La (NO
3)
36H
2o) be lanthanum source, citric acid (C
6h
8o
7h
2o) be sequestrant, water is solvent, by the centrifugal fibroblast technology of colloidal sol, obtains gelled fibre, after calcining, forms zirconic acid lanthanum (La
2zr
2o
7) ceramic fiber.Technical characterstic of the present invention and excellent results are as follows:
1. adopt sol-gel method to prepare ceramic fiber, technological process temperature is low, and because gel particles is less, specific surface area is large, greatly reduces sintering temperature, reduces by 200～400 ℃, thereby reduced energy consumption than conventional sintering temperature.
2. sol-gel process is through solution, colloidal sol, gel three phases, each component of raw material can reach molecular level and mix in solution, the microstructure of fiber is easy to control, and purity is decided by material purity, by controlling crystalline structure and the physical and chemical performance that raw material and component proportion can controlled material.
3. the sol-gel presoma homogeneous transparent that prepared by the present invention, stable in properties can long-term storage, without adding polymer spin finish aid just to have good ropiness.Adopt centrifugal drying silk fibroblast, equipment is simple.According to the adjustable conditions such as a bore dia, rotating speed of getting rid of of colloidal sol viscosity, technique is simple and easy to adjust.
4. gelled fibre ceramic processing condition of the present invention are: the heat-up rate with 0.5～3 ℃/min rises to 550～650 ℃ from room temperature, at this temperature insulation 0.5～2h, slowly remove water in gelled fibre, organism, acid etc., gelled fibre is evenly shunk, avoid organism and moisture evaporation too fast and cause hole, affect the compactness of ceramic fiber; Heat-up rate with 5～10 ℃/min rises to 800～1000 ℃ again, at this temperature insulation 0.5～3h, forms the zirconic acid lanthanum (La of fluorite type structure
2zr
2o
7) ceramic fiber; Finally with the heat-up rate of 10～20 ℃/min, rise to 1100～1400 ℃ again, and at this temperature insulation 0.5～2h, obtain the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) ceramic fiber (as accompanying drawing 3).
5. the zirconic acid lanthanum (La that prepared by the present invention
2zr
2o
7) ceramic fiber outward appearance is fluffy, has snappiness (as accompanying drawing 1); Microstructure fiber is fine and close, diameter Distribution average (as accompanying drawing 4); Crystal formation is pyrochlore-type, and phase stability is good, before fusing point, do not change mutually, and thermal conductivity 0.054～0.082W/ (mK), very suitable to high temperature insulating material.
Accompanying drawing explanation
Fig. 1 is the optical photograph of embodiment 1 gained zirconic acid lanthanum ceramic fiber.
Fig. 2 is that embodiment 1 gained gelled fibre is fired to the XRD spectra of 900 ℃.
Fig. 3 is that embodiment 1 gained gelled fibre is fired to the XRD spectra of 1200 ℃.
Fig. 4 is the SEM photo of embodiment 4 gained zirconic acid lanthanum ceramic fibers.
Fig. 5 is the high power SEM photo of embodiment 6 gained zirconic acid lanthanum ceramic fibers.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described, but be not limited to this.
Embodiment 1
(1) preparation of spinning property precursor sol
By 78.6g zirconium nitrate (Zr (NO
3)
43H
2o), 86.6g lanthanum nitrate (La (NO
3)
36H
2o) and 42.0g citric acid (C
6h
8o
7h
2o) join respectively in suitable quantity of water, stir to clarify transparent; Under room temperature, three kinds of solution are mixed, stir to clarify after transparent and be aged to viscosity 80Pas 60 ℃ of water-baths, obtain spinning property colloidal sol;
(2) centrifugal fibroblast is prepared gelled fibre
Colloidal sol prepared by step (1) carries out centrifugal fibroblast, and processing condition are: getting rid of a bore dia is 0.3mm, and getting rid of a rotating speed is 9000r/min, and getting rid of temperature in silk bucket is 25 ℃, and relative humidity is 25%;
(3) the gelled fibre ceramic of being prepared by step (2), processing condition are: the heat-up rate with 3 ℃/min rises to 600 ℃ from room temperature, at this temperature insulation 2h, then rise to 900 ℃ with the heat-up rate of 10 ℃/min, at this temperature insulation 1h, obtain the zirconic acid lanthanum (La of fluorite phase structure
2zr
2o
7) ceramic fiber, finally with the heat-up rate of 15 ℃/min, rise to 1200 ℃ again, and at this temperature insulation 2h, obtain the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) ceramic fiber.
When gained gelled fibre is fired to 900 ℃, be the zirconic acid lanthanum (La of fluorite type structure
2zr
2o
7) fiber, XRD spectra is as shown in Figure 2; While being fired to 1200 ℃, be the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) fiber, XRD spectra is as shown in Figure 3.
Zirconic acid lanthanum (the La of gained pyrochlore type structure
2zr
2o
7) fiber outward appearance is fluffy, porosity is high, as shown in Figure 1; Diameter 2～5 μ m, thermal conductivity is 0.054W/ (mK).
Embodiment 2
As described in Example 1, difference is:
Citric acid (C in step (1)
6h
8o
7h
2o) be 50.2g; Step (2) is with embodiment 1.
In step (3), gelled fibre ceramic processing condition are: the heat-up rate with 1 ℃/min rises to 600 ℃ from room temperature, at this temperature insulation 2h, heat-up rate with 5 ℃/min rises to 900 ℃ again, obtains the zirconic acid lanthanum (La of fluorite phase structure at this temperature insulation 1h
2zr
2o
7) ceramic fiber, finally with the heat-up rate of 15 ℃/min, rise to 1100 ℃ again, and at this temperature insulation 2h, obtain the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) ceramic fiber.
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, diameter is 2～5 μ m, and fiber outward appearance is fluffy, and thermal conductivity is 0.062W/ (mK).
Embodiment 3
As described in Example 1, difference is: lanthanum nitrate (La (NO in step (1)
3)
36H
2o) be 82.2g; Step (2) is with embodiment 1.
In step (3), obtain the zirconic acid lanthanum (La of fluorite phase structure
2zr
2o
7) ceramic fiber finally rises to 1200 ℃ with the heat-up rate of 15 ℃/min again, and at this temperature insulation 1h, obtain the zirconic acid lanthanum (La of pyrochlore type structure
2zr
2o
7) ceramic fiber.
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, Fibre diameter 2～5 μ m, thermal conductivity is 0.059W/ (mK).
Embodiment 4
As described in Example 1, difference is: step (1) zirconium nitrate (Zr (NO
3)
43H
2o) in, be 70.7g; In step (2), getting rid of a bore dia is 0.5mm, and getting rid of a rotating speed is 6000r/min.Step (3) is with embodiment 1;
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, diameter is 3～7 μ m, SEM photo as shown in Figure 4, the smooth densification of fiber surface, size distribution is even, product thermal conductivity is 0.069W/ (mK).
Embodiment 5
As described in Example 1, difference is: citric acid (C in step (1)
6h
8o
7h
2o) be 50.2g, it is 90Pas that colloidal sol is aged to viscosity; Step (2), (3) are with embodiment 1.
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, diameter is 4～7 μ m, and fiber outward appearance is fluffy, and snappiness is good, and product thermal conductivity is 0.082W/ (mK).
Embodiment 6
As described in Example 1, difference is: in step (2), getting rid of temperature in silk bucket is 35 ℃, and relative humidity is 30%, and getting rid of a rotating speed is 11000r/min;
Zirconic acid lanthanum (the La of fluorite phase structure in step (3)
2zr
2o
7) ceramic fiber finally rises to the heat-up rate of 15 ℃/min the zirconic acid lanthanum (La that 1400 ℃ of insulation 1h obtain pyrrhite phase structure again
2zr
2o
7) ceramic fiber;
Step (1) is with embodiment 1.
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, diameter is 1～5 μ m, and fiber outward appearance is fluffy, and porosity is high, the smooth densification of fiber surface, size distribution is even, and as shown in Figure 5, thermal conductivity is 0.058W/ (mK) on single fiber surface.
Embodiment 7
As described in Example 1, difference is: in step (2), getting rid of temperature in silk bucket is 25 ℃, and relative humidity is 30%;
Step (1), (3) are with embodiment 1.
Gained ceramic fiber is the zirconic acid lanthanum (La of pyrochlore constitution
2zr
2o
7) fiber, diameter is 2～5 μ m, fiber outward appearance is fluffy, and the smooth densification of fiber surface, thermal conductivity is 0.073W/ (mK).
Claims (5)
1. a zirconic acid lanthanum (La
2zr
2o
7) preparation method of ceramic fiber, comprise that step is as follows:
(1) preparation of spinning property precursor sol
Zirconium nitrate, lanthanum nitrate and citric acid are joined respectively in suitable quantity of water, stir to clarify transparent; Under room temperature, three kinds of solution are mixed, after stirring, 40～70 ℃ of water-baths, being aged to viscosity is 60～100Pas, obtains spinning property precursor sol;
Wherein, the mol ratio of zirconium nitrate and lanthanum nitrate is 1:0.87～1.15, presses metal ion (La
3++ Zr
4+) with the mol ratio of citric acid be that citric acid is added in 1:0.3～1.2.
(2) centrifugal fibroblast is prepared gelled fibre
Spinning property precursor sol prepared by step (1) carries out centrifugal fibroblast, and processing condition are: getting rid of a bore dia is 0.2～0.5mm, and getting rid of a revolution is 3000～12000r/min, and getting rid of temperature in silk bucket is 10～40 ℃, and relative humidity is 10%～40%; Obtain gelled fibre;
(3) calcining gelled fibre carries out ceramic
Ceramic is carried out in gelled fibre calcining prepared by step (2), and processing condition are: the heat-up rate with 0.5～3 ℃/min rises to 550～650 ℃ from room temperature, at this temperature insulation 0.5～2h.Heat-up rate with 5～10 ℃/min rises to 800～1000 ℃ again, then at this temperature insulation 0.5～3h, obtains the zirconic acid lanthanum ceramic fiber of fluorite structure; Finally with the heat-up rate of 10～20 ℃/min, rise to 1100～1400 ℃ again, and at this temperature insulation 0.5～2h, obtain the zirconic acid lanthanum ceramic fiber of pyrochlore type structure.
2. the preparation method of zirconic acid lanthanum ceramic fiber as claimed in claim 1, is characterized in that, in step (1), the mol ratio of zirconium nitrate and lanthanum nitrate is 1:0.95～1.05; Citric acid is pressed metal ion (La
3++ Zr
4+) being 1:0.6～1.0 with the mol ratio of citric acid, amount is added.
3. the preparation method of zirconic acid lanthanum ceramic fiber as claimed in claim 1, is characterized in that, in step (1), water-bath aging temperature is 40～60 ℃, and being aged to viscosity is 70～90Pas.
4. the preparation method of zirconic acid lanthanum ceramic fiber as claimed in claim 1, it is characterized in that, in step (2), getting rid of a bore dia is 0.2～0.3mm, and getting rid of temperature in silk bucket is 20～40 ℃, getting rid of a rotating speed is 6000～9000r/min, and relative humidity is 10～30%.
5. the preparation method of zirconic acid lanthanum ceramic fiber as claimed in claim 1, it is characterized in that, calcining gelled fibre in step (3) carries out ceramic processing condition: the heat-up rate with 0.5～1 ℃/min rises to 600～650 ℃ from room temperature, at this temperature insulation 1～2h, heat-up rate with 5～8 ℃/min rises to 800～900 ℃ again, at this temperature insulation 0.5～1h, obtain the zirconic acid lanthanum ceramic fiber of fluorite type structure, finally with the heat-up rate of 10～20 ℃/min, rise to 1100～1300 ℃ again, and at this temperature insulation 0.5～2h, obtain the zirconic acid lanthanum ceramic fiber of pyrochlore type structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310521491.XA CN103553596B (en) | 2013-10-29 | 2013-10-29 | Preparation method of zirconic acid lanthanum ceramic fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310521491.XA CN103553596B (en) | 2013-10-29 | 2013-10-29 | Preparation method of zirconic acid lanthanum ceramic fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103553596A true CN103553596A (en) | 2014-02-05 |
| CN103553596B CN103553596B (en) | 2014-09-10 |
Family
ID=50008015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310521491.XA Active CN103553596B (en) | 2013-10-29 | 2013-10-29 | Preparation method of zirconic acid lanthanum ceramic fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103553596B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624834A (en) * | 2016-01-30 | 2016-06-01 | 山东大学 | Barium zirconate fiber and method for preparing same |
| CN107267148A (en) * | 2017-07-26 | 2017-10-20 | 齐齐哈尔大学 | A kind of terbium ion doping zirconic acid lanthanum fluorescent material and preparation method thereof |
| CN108410170A (en) * | 2018-04-21 | 2018-08-17 | 郭平 | A kind of ceramic fibre enhancing polyimides electrical insulating property composite material |
| CN108505145A (en) * | 2018-04-11 | 2018-09-07 | 山东大学 | A kind of calcium zirconate fiber and preparation method thereof |
| CN113087729A (en) * | 2021-04-01 | 2021-07-09 | 山东大学 | Lanthanum complex precursor, lanthanum oxide fiber and preparation method and application of lanthanum zirconate fiber derived from lanthanum oxide fiber |
| CN113370549A (en) * | 2021-06-08 | 2021-09-10 | 山东大学 | Lanthanum zirconate fiber reinforced aerogel composite material, and continuous production method and device |
| CN115094544A (en) * | 2022-07-28 | 2022-09-23 | 中国人民解放军国防科技大学 | Lanthanum zirconate nano ceramic fiber and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792170A (en) * | 2010-02-10 | 2010-08-04 | 长春理工大学 | Method for preparing cerium dioxide polycrystal nanobelt |
| CN102786307A (en) * | 2011-05-20 | 2012-11-21 | 钡泰电子陶瓷股份有限公司 | Method for manufacturing piezoelectric ceramic fiber |
| CN102864397A (en) * | 2012-09-23 | 2013-01-09 | 西北有色金属研究院 | Preparation method of fiber-reinforced titanium matrix composite precursors |
-
2013
- 2013-10-29 CN CN201310521491.XA patent/CN103553596B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792170A (en) * | 2010-02-10 | 2010-08-04 | 长春理工大学 | Method for preparing cerium dioxide polycrystal nanobelt |
| CN102786307A (en) * | 2011-05-20 | 2012-11-21 | 钡泰电子陶瓷股份有限公司 | Method for manufacturing piezoelectric ceramic fiber |
| CN102864397A (en) * | 2012-09-23 | 2013-01-09 | 西北有色金属研究院 | Preparation method of fiber-reinforced titanium matrix composite precursors |
Non-Patent Citations (2)
| Title |
|---|
| HUIJUAN TANG ET.AL.: "Fabrication and characterization of nanostructured La2Zr2O7 fibers", 《MATERIALS LETTERS》, vol. 70, 3 December 2011 (2011-12-03), pages 48 - 50 * |
| 刘树信，王海滨: "稀土镧添加氧化锆的合成与物相分析研究", 《无机盐工业》, vol. 43, no. 12, 31 December 2011 (2011-12-31), pages 26 - 28 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624834A (en) * | 2016-01-30 | 2016-06-01 | 山东大学 | Barium zirconate fiber and method for preparing same |
| CN105624834B (en) * | 2016-01-30 | 2018-04-06 | 山东大学 | A kind of barium zirconate fiber and preparation method thereof |
| CN107267148A (en) * | 2017-07-26 | 2017-10-20 | 齐齐哈尔大学 | A kind of terbium ion doping zirconic acid lanthanum fluorescent material and preparation method thereof |
| CN108505145A (en) * | 2018-04-11 | 2018-09-07 | 山东大学 | A kind of calcium zirconate fiber and preparation method thereof |
| CN108410170A (en) * | 2018-04-21 | 2018-08-17 | 郭平 | A kind of ceramic fibre enhancing polyimides electrical insulating property composite material |
| CN113087729A (en) * | 2021-04-01 | 2021-07-09 | 山东大学 | Lanthanum complex precursor, lanthanum oxide fiber and preparation method and application of lanthanum zirconate fiber derived from lanthanum oxide fiber |
| CN113370549A (en) * | 2021-06-08 | 2021-09-10 | 山东大学 | Lanthanum zirconate fiber reinforced aerogel composite material, and continuous production method and device |
| CN115094544A (en) * | 2022-07-28 | 2022-09-23 | 中国人民解放军国防科技大学 | Lanthanum zirconate nano ceramic fiber and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103553596B (en) | 2014-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103553596B (en) | Preparation method of zirconic acid lanthanum ceramic fiber | |
| CN102181962B (en) | Method for preparing thin-diameter zirconium oxide fibers and fiber board thereof | |
| CN108511793B (en) | Solid lithium lanthanum zirconium oxygen ceramic nano fiber electrolyte film and preparation thereof | |
| CN102557628B (en) | Flexible yttrium stable zirconium oxide ceramic fiber and preparation method thereof | |
| CN103183513B (en) | Preparation method of proton conductive ceramic electrolyte film | |
| KR101572545B1 (en) | Oxide electrode materials composite fibers internal mixing electrolyte materials and method for preparation thereof | |
| CN104141181B (en) | A kind of containing SiO2the ZrO of doping2the preparation method of fiber | |
| CN104496469A (en) | Method for preparing dense micro/nano ceramic fiber by virtue of coaxial electrospinning technology | |
| CN106178981B (en) | A kind of method of low temperature preparation titanium oxide ceramics ultrafiltration membrane | |
| CN104086200A (en) | Preparation method of mullite fiber | |
| CN102965764A (en) | Preparation method of aluminum oxide ceramic continuous fiber | |
| CN103408292A (en) | Preparation method for alumina-zirconia ceramic fiber | |
| CN102380321A (en) | Method for preparing coating of alumina ceramic membrane | |
| CN103643402B (en) | A kind of preparation method of lanthanum zirconate ceramic fiber blanket | |
| CN104987115A (en) | Method for preparing heat-insulation heat-preservation ceramic by utilizing potassium hexatitanate whiskers | |
| WO2018094860A1 (en) | Manufacturing process of spiral ceramic spring | |
| CN104032412A (en) | Preparation method for zirconium oxide ceramic fibers | |
| CN108505145A (en) | A kind of calcium zirconate fiber and preparation method thereof | |
| CN103114352A (en) | Preparation method of sol gel of alumina fiber | |
| CN102775143A (en) | Method for preparing fully-stabilized tetragonal-phase zirconia crystal fibers | |
| CN103757751B (en) | A kind of preparation method of super high temperature zirconia ceramic fiber | |
| CN101767819B (en) | Preparation method of BaTi2O5 nano wire | |
| CN1203025C (en) | Rare earth-doped srstrontium cerate nano crystal ceramic preparing method | |
| CN103556305A (en) | Method for preparing magnesium oxide fiber via sol-gel method | |
| CN105778109A (en) | Barium titanate ceramic polymer precursor and preparation method of barium titanate ceramic polymer precursor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |