CN106747538A - Phosphate strengthens the preparation method of Zirconium oxide fibre effectively insulating composite - Google Patents
Phosphate strengthens the preparation method of Zirconium oxide fibre effectively insulating composite Download PDFInfo
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- CN106747538A CN106747538A CN201611077640.8A CN201611077640A CN106747538A CN 106747538 A CN106747538 A CN 106747538A CN 201611077640 A CN201611077640 A CN 201611077640A CN 106747538 A CN106747538 A CN 106747538A
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- C04B35/803—
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
- C04B35/6306—Binders based on phosphoric acids or phosphates
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Abstract
The present invention relates to the preparation method that a kind of phosphate strengthens Zirconium oxide fibre effectively insulating composite, belong to the preparing technical field of inorganic composite materials.The present invention is comprised the following steps：(1) pretreatment of Zirconium oxide fibre；(2) preparation of phosphate binders；(3) prepared by heat-insulation composite material shaping slurry；(4) suction filtration shaping；(5) it is heat-treated, obtains the phosphate enhancing Zirconium oxide fibre effectively insulating composite.Operation is simple for the present invention, and gained target product can be in 1500 DEG C of long-term uses, and with the good characteristic such as low-density, high-temperature stability be good, the mechanical property of composite is also greatly improved.
Description
Technical field
The present invention relates to the preparation method that a kind of phosphate strengthens Zirconium oxide fibre effectively insulating composite, belong to inorganic
The preparing technical field of composite.
Background technology
High temperature insulating material is one of hypersonic aircraft thermal protection key technology, as flying speed is improved, flight
Time lengthening, the flight environment of vehicle of aircraft is harsher, and requirement higher is proposed to heat-barrier material.
China Patent Publication No. CN101691138A discloses a kind of preparation method of thermal insulation tile, and it is mainly fine using quartz
Dimension, mixing small amounts aluminum fiber and boron nitride powder prepare low temperature thermal insulation tile, but the patent disclosure thermal insulation tile coating formula
There are a large amount of alkali metal ions, limit its temperature in use.China Patent Publication No. CN102199042A announces a kind of light rigidity
The preparation method of ceramic insulation watt, the patent adds a small amount of boron nitride also mainly with quartz fibre and mullite fiber as matrix
And carborundum powder, because carborundum density is big, the skewness in base substrate causes thermal insulation tile poor mechanical property, and is also to answer
Used in low temperature environment.
The heat-barrier material for being prepared using fibre at present is main used below at 1500 DEG C, the high temperature more than 1500 DEG C every
Hot material is primarily present density and the big problem of thermal conductivity factor, and influence of the density to aerospace applications is very big.Zirconium oxide is fine
Dimension have both the advantage of zirconia ceramics and the advantage of fibrous material, with density it is small, thermal conductivity factor is low, corrosion-resistant, heat-resisting quantity
Can be good, can be for a long time using the characteristic such as indeformable the optimal selection of rigid heat-barrier material more than 1500 DEG C.
But because Zirconium oxide fibre heat-barrier material firing temperature is high, common bond is difficult to meet and requires, can only select resistance to
The inorganic binder of high temperature, inorganic binder low intensity, the heat-barrier material mechanical property of preparation is poor, and is difficult to uniform compound.
The content of the invention
It is an object of the invention to provide the preparation side that a kind of phosphate strengthens Zirconium oxide fibre effectively insulating composite
Method, operation is simple for it, and gained target product can be in 1500 DEG C of long-term uses and good with low-density, high-temperature stability
Deng good characteristic, the mechanical property of composite is also greatly improved.
Phosphate of the present invention strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, including following step
Suddenly：
(1) pretreatment of Zirconium oxide fibre：The treatment that is chopped is carried out to Zirconium oxide fibre；
(2) preparation of phosphate binders：By quality proportioning, chloride monohydrate, phosphoric acid and deionized water are 3~6:2~
4:10~30, stir after powder is completely dissolved, 5~90min is stirred using mini-sized blender, stood after solution is thoroughly mixed
4~48h；
(3) prepared by heat-insulation composite material shaping slurry：The fiber that step (1) treatment is obtained and phosphorus obtained in step (2)
Hydrochlorate in mass ratio 1:1~1:15 mixing, 5~90min is stirred with mini-sized blender；
(4) suction filtration shaping：Step (3) is obtained into slurry carries out suction filtration shaping, the demoulding after shaping, moves to thermostatic drying chamber,
Drying system is 50~70 DEG C of insulations 1~24h, 120~140 DEG C of 1~24h of insulation, and base substrate is obtained；
(5) it is heat-treated：The base substrate that step (4) is obtained is placed in high temperature sintering furnace, with the heating rate of 10 DEG C/min from
Room temperature rises to 1000 DEG C, is incubated 10~60min, then is warming up to 1500~1600 DEG C from 1000 DEG C with 5 DEG C/min, and it is incubated 30~
300min, the phosphate enhancing Zirconium oxide fibre effectively insulating composite is obtained after furnace cooling through processing.
In step (1), a diameter of 1-5 μm before Zirconium oxide fibre treatment；Be chopped treatment rear oxidation zirconium fibre length be
30-150μm。
In step (1), the handling process that is chopped is as follows：By Zirconium oxide fibre, deionized water in mass ratio 1：20~50 mixing
After be placed in fiber shearing machine, fiber shearing machine rotating speed be 4000~6000r/min, shear time be 1~10min, shearing knot
Thermostatic drying chamber will be placed in after beam after fiber filter, drying system is 100~120 DEG C of 24~48h of insulation.
Preferably, Zirconium oxide fibre, deionized water quality ratio are 1:40, fiber cutting and rotating speed are 6000r/min, shearing
Time is 5min.
In step (2), the preparation process of phosphate binders is as follows：LaCl3·6H2O and deionized water in mass ratio 4~
5:20~25 mixing, after particle is completely dissolved, add H3PO4, 30~45min is stirred with mini-sized blender, treat that solution is mixed completely
12~24h is stood after conjunction, binding agent lanthanum orthophosphate is obtained, wherein, LaCl3·6H2O and H3PO4Mass ratio be 4~5:2~3.
In step (3), it is preferred that fiber is 1 according to mass ratio with phosphate:2~1:8 mixing, mixing time be 30~
40min。
In step (4), the vacuum of suction filtration shaping is -0.06~-0.1MPa, and suction filtration process time is 3~10 minutes,
It is 70 DEG C of insulations 12~15h, 140 DEG C of 4~6h of insulation that body drying system is preferably.
In step (5), Technology for Heating Processing is preferably：1000 DEG C, insulation are risen to from room temperature with the heating rate of 10 DEG C/min
10~20min, then 1500~1550 DEG C are warming up to from 1000 DEG C with 5 DEG C/min, it is incubated 90~120min, furnace cooling.
The present invention compared with prior art, has the advantages that：
(1) Zirconium oxide fibre has excellent high-temperature stability, can be used at 1500 DEG C for a long time, and selection is suitable to be bonded
Agent turns into key, and the present invention utilizes the resistant to elevated temperatures characteristic of phosphate, at high temperature as the binding agent of Zirconium oxide fibre matrix, no
It is only compound with matrix uniform, and the mechanical behavior under high temperature of fibrous thermal composite is effectively improved.
(2) binding agent synthetic method of the present invention is simple, scientific and reasonable, it is easy to implement and with short production cycle, can
Disposable a large amount of productions；Obtained binding agent has certain viscosity at low temperature, can well disperse fiber and keep certain
Time not coagulation.
(3) the obtained heat-insulation composite material density of the present invention is controllable, and density is 0.4~1.3g/cm3, not only with higher
Mechanical property and excellent effect of heat insulation, but also with good high-temperature stability, have non-under various hot conditions
Often wide application prospect.
Brief description of the drawings
Fig. 1 is the unprocessed preceding original SEM pictures of Zirconium oxide fibre；
Fig. 2 is the Zirconium oxide fibre SEM pictures of the product of embodiment 1.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but it is not intended to limit implementation of the invention.
In raw materials used：
Zirconium oxide fibre：Shandong fiber Co., Ltd, cellucotton, 1-3 μm of diameter, ZrO2>=90%；
Phosphoric acid：Tianjin chemical inc, analyzes pure, content >=85%；
Six water lanthanum chlorides：Shandong Co., Ltd, analyzes pure, and >=45%.
Embodiment 1
Weigh 2000gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (30 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 200%, Zirconium oxide fibre quality 3000%
Deionized water mixing, using mini-sized blender stir 40min be made me fibrous slurry.The vacuum of vacuum tank is maintained at-
0.1MPa, is added to slurry mould and collects, and vacuum filtration process time is 10 minutes, and suction filtration shaping is made wet base.By wet base
Thermostatic drying chamber is placed in, drying process is 70 DEG C of insulations 12h, 140 DEG C of insulation 4h.Wet base after drying is loaded on high temperature sintering furnace
Burnt till in 1500 DEG C under middle normal pressure, insulation 2h is cooled to room temperature, the density 0.43g/cm of the composite for obtaining3, compressive strength
0.4MPa, 1100 DEG C of thermal conductivity 0.134W/mK.
Embodiment 2
Weigh 2000gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (150 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 500%, Zirconium oxide fibre quality
2500% deionized water mixing, stirs 40min and is made me fibrous slurry using mini-sized blender.The vacuum of vacuum tank keeps
In -0.06MPa, slurry is added to mould and is collected, vacuum filtration process time is 10 minutes, suction filtration shaping is made wet base.
Wet base is placed in thermostatic drying chamber, drying process is 50 DEG C of insulations 24h, 140 DEG C of insulation 4h.Wet base after drying is loaded on high temperature
Burnt till in 1500 DEG C under normal pressure in sintering furnace, insulation 2h is cooled to room temperature, the density 0.47g/cm of the composite for obtaining3, pressure
Contracting intensity 0.7MPa, 1100 DEG C of thermal conductivity 0.141W/mK.
Embodiment 3
Weigh 2500gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (30 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 100%, Zirconium oxide fibre quality 3000%
Deionized water mixing, using mini-sized blender stir 40min be made me fibrous slurry.The vacuum of vacuum tank is maintained at-
0.05MPa, is added to slurry mould and collects, and vacuum filtration process time is 10 minutes, and suction filtration shaping is made wet base.Will be wet
Base is placed in thermostatic drying chamber, and drying process is 70 DEG C of insulations 12h, 140 DEG C of insulation 4h.Wet base after drying is loaded on high temperature sintering
Burnt till in 1550 DEG C under normal pressure in stove, insulation 5h is cooled to room temperature, the density 0.44g/cm of the composite for obtaining3, compression is by force
Degree 0.47MPa, 1100 DEG C of thermal conductivity 0.138W/mK.
Embodiment 4
Weigh 2500gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (50 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 500%, Zirconium oxide fibre quality 2500%
Deionized water mixing, using mini-sized blender stir 40min be made me fibrous slurry.The vacuum of vacuum tank is maintained at-
0.1MPa, is added to slurry mould and collects, and vacuum filtration process time is 10 minutes, and suction filtration shaping is made wet base.By wet base
Thermostatic drying chamber is placed in, drying process is 60 DEG C of insulations 12h, 140 DEG C of insulation 1h.Wet base after drying is loaded on high temperature sintering furnace
Burnt till in 1550 DEG C under middle normal pressure, insulation 3h is cooled to room temperature, the density 0.57g/cm of the composite for obtaining3, compressive strength
0.72MPa, 1100 DEG C of thermal conductivity 0.145W/mK.
Embodiment 5
Weigh 2500gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (80 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 800%, Zirconium oxide fibre quality 2500%
Deionized water mixing, using mini-sized blender stir 40min be made me fibrous slurry.The vacuum of vacuum tank is maintained at-
0.1MPa, is added to slurry mould and collects, and vacuum filtration process time is 10 minutes, and suction filtration shaping is made wet base.By wet base
Thermostatic drying chamber is placed in, drying process is 70 DEG C of insulations 1h, 120 DEG C of insulation 24h.Wet base after drying is loaded on high temperature sintering furnace
Burnt till in 1600 DEG C under middle normal pressure, insulation 0.5h is cooled to room temperature, the density 0.74g/cm of the composite for obtaining3, compression is by force
Degree 0.75MPa, 1100 DEG C of thermal conductivity 0.147W/mK.
Embodiment 6
Weigh 2500gLaCl3·6H2O, is added in 10000g deionized waters, stirs after powder is completely dissolved, and adds
1000gH3PO4, 30min is stirred with mini-sized blender, stand 12h after solution is well mixed.By the zirconium oxide after chopped treatment
Fiber (30 μm of average length), the binding agent lanthanum orthophosphate solution of Zirconium oxide fibre quality 1500%, Zirconium oxide fibre quality
3000% deionized water mixing, stirs 40min and is made me fibrous slurry using mini-sized blender.The vacuum of vacuum tank keeps
In -0.1MPa, slurry is added to mould and is collected, vacuum filtration process time is 10 minutes, suction filtration shaping is made wet base.Will
Wet base is placed in thermostatic drying chamber, and drying process is 70 DEG C of insulations 12h, 130 DEG C of insulation 8h.Wet base after drying burns loaded on high temperature
Burnt till in 1550 DEG C under normal pressure in freezing of a furnace, insulation 2h is cooled to room temperature, the density 0.77g/cm of the composite for obtaining3, compression
Intensity 0.77MPa, 1100 DEG C of thermal conductivity 0.151W/mK.
Claims (8)
1. a kind of phosphate strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, it is characterised in that including following step
Suddenly：
(1) pretreatment of Zirconium oxide fibre：The treatment that is chopped is carried out to Zirconium oxide fibre；
(2) preparation of phosphate binders：By quality proportioning, chloride monohydrate, phosphoric acid and deionized water are 3~6:2~4:10
~30, stirring stirs 5~90min after after powder dissolving, after 4~48h of standing after solution mixing；
(3) prepared by heat-insulation composite material shaping slurry：The fiber that step (1) treatment is obtained and phosphate obtained in step (2)
In mass ratio 1:1~1:15 mixing, stir 5~90min；
(4) suction filtration shaping：Step (3) is obtained into slurry carries out suction filtration shaping, the demoulding after shaping, moves to thermostatic drying chamber, dries
System is 50~70 DEG C of insulations 1~24h, 120~140 DEG C of 1~24h of insulation, and base substrate is obtained；
(5) it is heat-treated：The base substrate that step (4) is obtained is placed in high temperature sintering furnace, with the heating rate of 10 DEG C/min from room temperature
Rise to 1000 DEG C, be incubated 10~60min, then 1500~1600 DEG C are warming up to from 1000 DEG C with 5 DEG C/min, and it is incubated 30~
300min, the phosphate enhancing Zirconium oxide fibre effectively insulating composite is obtained after furnace cooling through processing.
2. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (1), a diameter of 1-5 μm before Zirconium oxide fibre treatment；Be chopped treatment rear oxidation zirconium fibre length be
30-150μm。
3. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (1), the handling process that is chopped is as follows：By Zirconium oxide fibre, deionized water in mass ratio 1：After 20~50 mixing
It is placed in fiber shearing machine, fiber shearing machine rotating speed is 4000~6000r/min, shear time is 1~10min, and shearing terminates
Thermostatic drying chamber will be placed in after fiber filter afterwards, drying system is 100~120 DEG C of 24~48h of insulation.
4. phosphate according to claim 3 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：Zirconium oxide fibre, deionized water quality ratio are 1:20-30, fiber cutting and rotating speed are 6000r/min, shear time
It is 5min.
5. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (2), the preparation process of phosphate binders is as follows：LaCl3·6H2O and deionized water in mass ratio 4~5:
20~25 mixing, after after grain dissolution, add H3PO4, 30~45min is stirred, after 12~24h is stood after solution mixing, glued
Knot agent lanthanum orthophosphate, wherein, LaCl3·6H2O and H3PO4Mass ratio be 4~5:2~3.
6. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (3), fiber is 1 according to mass ratio with phosphate:2~1:8 mixing, mixing time is 30~40min.
7. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (4), the vacuum of suction filtration shaping is -0.06~-0.1MPa, and suction filtration process time is 3~10 minutes,
Body drying system is 70 DEG C of insulations 12~15h, 140 DEG C of 4~6h of insulation.
8. phosphate according to claim 1 strengthens the preparation method of Zirconium oxide fibre effectively insulating composite, and it is special
Levy and be：In step (5), Technology for Heating Processing is：With the heating rate of 10 DEG C/min 1000 DEG C are risen to from room temperature, insulation 10~
20min, then 1500~1550 DEG C are warming up to from 1000 DEG C with 5 DEG C/min, it is incubated 90~120min, furnace cooling.
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| CN201611077640.8A CN106747538A (en) | 2016-11-30 | 2016-11-30 | Phosphate strengthens the preparation method of Zirconium oxide fibre effectively insulating composite |
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| CN201611077640.8A CN106747538A (en) | 2016-11-30 | 2016-11-30 | Phosphate strengthens the preparation method of Zirconium oxide fibre effectively insulating composite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110983757A (en) * | 2019-12-04 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Method for modifying fiber interface of alumina fiber cloth and modified alumina fiber cloth prepared by method |
| CN114045671A (en) * | 2021-11-18 | 2022-02-15 | 航天特种材料及工艺技术研究所 | Continuous oxide fiber fabric with lanthanum phosphate layer and preparation method thereof |
| CN115572183A (en) * | 2022-11-09 | 2023-01-06 | 航天特种材料及工艺技术研究所 | High-strength high-temperature-resistant heat-insulating material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110983757A (en) * | 2019-12-04 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Method for modifying fiber interface of alumina fiber cloth and modified alumina fiber cloth prepared by method |
| CN110983757B (en) * | 2019-12-04 | 2022-04-29 | 航天特种材料及工艺技术研究所 | Method for modifying fiber interface of alumina fiber cloth and modified alumina fiber cloth prepared by method |
| CN114045671A (en) * | 2021-11-18 | 2022-02-15 | 航天特种材料及工艺技术研究所 | Continuous oxide fiber fabric with lanthanum phosphate layer and preparation method thereof |
| CN114045671B (en) * | 2021-11-18 | 2024-01-09 | 航天特种材料及工艺技术研究所 | Continuous oxide fiber fabric with lanthanum phosphate layer and preparation method thereof |
| CN115572183A (en) * | 2022-11-09 | 2023-01-06 | 航天特种材料及工艺技术研究所 | High-strength high-temperature-resistant heat-insulating material and preparation method thereof |
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