CN109608188A - Anti- sintering zirconium pyrophosphate porous ceramics of one kind and preparation method thereof - Google Patents
Anti- sintering zirconium pyrophosphate porous ceramics of one kind and preparation method thereof Download PDFInfo
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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
- C04B35/01—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
- C04B35/447—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 phosphates, e.g. hydroxyapatite
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- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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Abstract
The present invention relates to a kind of anti-sintering zirconium pyrophosphate porous ceramics and preparation method thereof, more particularly to a kind of low-density, lower thermal conductivity, anti-sintering zirconium pyrophosphate porous ceramics and using high temperature template removal method and partially sinter the method for preparing zirconium pyrophosphate porous ceramics, belong to high temperature porous heat-proof coating material technical field, the low-density refers to density no more than 1.3g/cm3, lower thermal conductivity is not higher than 0.2W/ (mK).
Description
Technical field
The present invention relates to a kind of anti-sintering zirconium pyrophosphate porous ceramics and preparation method thereof more particularly to a kind of low-density,
Lower thermal conductivity, anti-sintering zirconium pyrophosphate porous ceramics and using high temperature template removal method and partially sinter that prepare zirconium pyrophosphate porous
The method of ceramics, belongs to high temperature porous heat-proof coating material technical field, and the low-density refers to density no more than 1.3g/
cm3, lower thermal conductivity is not higher than 0.2W/ (mK).
Background technique
The high temperature insulating ceramic material of existing hypersonic aircraft is with silica (SiO2), aluminium oxide (Al2O3) and oxygen
Change zirconium (ZrO2) etc. based on systems, applied in practical application with the porous form of these systems.But these systems all exist
Apparent sintering phenomenon can occur at high temperature for obvious deficiency, the i.e. porous material of these systems, lead to porous material
Thermal conductivity have apparent rising at high temperature, this temperature, pressure that will be improved matrix and born, and finally cause aircraft
Failure.
Summary of the invention
Technology of the invention solves the problems, such as: overcome the deficiencies in the prior art, proposes that a kind of anti-sintering zirconium pyrophosphate is porous
Ceramics and preparation method thereof.
The technical solution of the invention is as follows:
A kind of anti-sintering zirconium pyrophosphate porous ceramics, the raw material of the porous ceramics includes zirconium pyrophosphate powder, and raw material may be used also
To include flour, when raw material includes flour, the volume content of flour is not more than the 40% of raw material volume；Wherein flour is averaged grain
Diameter is 10 microns；The group of the porous ceramics becomes zirconium pyrophosphate, and the porosity of the porous ceramics is 44%-60%, and this is porous
Ceramics thermal conductivity within the scope of 0-1500 DEG C is not more than 0.2W/ (mK).It is heat-treated 4-8 hours within the scope of 1000-1500 DEG C
Cubical contraction less than 2.5%.
A kind of preparation method of anti-sintering zirconium pyrophosphate porous ceramics, the step of this method include:
(1) raw material and mixing medium are mixed in the ball mill, incorporation time is 6-24 hours, and mixing medium is nothing
Water-ethanol obtains mixture；
(2) mixture that step (1) obtains is dried to obtain powder, and the powder after drying is compressed to piece
The green compact of shape, the pressure of compacting are 1-10MPa；
(3) step (2) pressed green compact are put into cold isostatic press and are formed, briquetting pressure 150-
300MPa, the green compact densified；
(4) green compact for the densification for obtaining step (3) carry out high-temperature heat treatment, and high-temperature heat treatment is in high temperature air furnace
It carries out, the purpose of high-temperature heat treatment is to remove and partially sinter process for template, and the temperature of high-temperature heat treatment is 1000-1500
DEG C, the time of high-temperature heat treatment is 1-10 hours, obtains zirconium pyrophosphate porous ceramics, porosity 44%-60%.
Heating rate in the step (4) is 5-30 DEG C/minute.
The invention has the following beneficial effects:
(1) present invention is for the first time using zirconium pyrophosphate powder and fabric as raw material, in air through high temperature template removal and part
Sintering directly obtains high porosity, low-heat is led, the zirconium pyrophosphate porous ceramics of anti-sintering, and warp is analysis shows the porous pottery of zirconium pyrophosphate
Porcelain has the characteristics that purity is high and porosity are high.
(2) present invention prepares high porosity, low-heat is led, anti-sintering zirconium pyrophosphate porous ceramics technical process is simple, raw material
It is low in cost, it does not need that foaming agent and surface dispersant is added；Meanwhile high temperature template removal and high-temperature part sintering process are continuous
It carries out, centre does not need to cool down.
(3) high-purity that is prepared of the present invention, low-heat lead, porosity, the intensity of anti-sintering zirconium pyrophosphate porous ceramics
It is good with thermal conductivity controllability, the density or high-sintering process adjustment apertures rate, intensity and thermal conductivity of adjusting green compact can be passed through
Rate, preparation process are flexibly controllable.
(4) the preparation method simple process, low in cost for the anti-sintering zirconium pyrophosphate porous ceramics that the present invention is prepared,
Long heat treatment cubical contraction is small at high temperature for porous ceramics, hence it is evident that is better than existing high temperature insulating porous ceramics, can apply
In mass production, there is stronger practicability.
(5) a kind of low-density, lower thermal conductivity, anti-sintering zirconium pyrophosphate porous ceramics and its preparation side are designed to provide
Method, to solve the problems, such as current insulating porous material easy-sintering at high temperature.The preparation method simple process, practical, system
Standby obtained zirconium pyrophosphate porous ceramics has the advantages that purity is high, porosity are high, thermal conductivity is low etc..
(6) the object of the present invention is to provide a kind of low-heat to lead, anti-sintering zirconium pyrophosphate porous ceramic film material and its preparation side
Method belongs to high temperature porous heat-barrier material field.This method is mixed using zirconium pyrophosphate and flour as raw material by physical mechanical method
6-24 hours, be cold-pressed into column under the pressure of 1-10MPa after drying process, under the pressure of 150-300MPa isostatic cool pressing at
Type is heated to 1000-1500 DEG C in air and removes removing template and partially sinter to prepare zirconium pyrophosphate high temperature porous ceramics.
It is the preparation method simple process, practical, have the advantages that (1) purity is high, the phase content 100wt% of zirconium pyrophosphate, nothing
Impurity phase；(2) porosity is high, and the range of porosity is 44-60%；(3) compressive strength is high, strength range 3-14MPa；(4)
Thermal conductivity is low, and does not vary with temperature；(5) anti-agglutinatting property is strong, is heat-treated 4-8 hours within the scope of 1000-1500 DEG C, and volume is received
Shrinkage is less than 2.5%.The zirconium pyrophosphate porous ceramics of this method preparation is suitable for high temperature thermal insulation coating Material Field.
Detailed description of the invention
Fig. 1 is that the phase constituent for the zirconium pyrophosphate porous ceramic skeleton that the embodiment of the present invention 1 is prepared contains with flour volume
The X-ray diffracting spectrum of magnitude relation；
The final consistency and porosity of the zirconium pyrophosphate porous ceramics that Fig. 2 is prepared for the embodiment of the present invention 2 and face
The relation curve of powder volume content；
Fig. 3 is the microstructure photograph for the zirconium pyrophosphate porous ceramics that the embodiment of the present invention 3 is prepared；
Fig. 4 is the thermal conductivity variation with temperature relationship for the zirconium pyrophosphate porous ceramics that the embodiment of the present invention 4 is prepared；
Fig. 5 is fine and close after the zirconium pyrophosphate porous ceramics that the embodiment of the present invention 5 is prepared is heat-treated at different temperatures
The change curve of degree and cubical contraction.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments:
Embodiment 1
Using zirconium pyrophosphate powder and flour as raw material, wherein flour volume content variation range is 0-40%, with anhydrous second
Alcohol is medium, is mixed 16 hours with planetary ball mill, uniformly mixed raw material is vacuum dried obtain zirconium pyrophosphate powder and
Flour mixed-powder is pressed into the disk of 8 millimeters of 15 millimeters thick of diameter with the method for dry-pressing, and the pressure of dry-pressing is 2MPa, will be done
The green compact of pressure, which are put into cold isostatic press, to be formed, briquetting pressure 200MPa.Molding sample is put into high temperature air furnace
In, 1300 DEG C are heated to 15 DEG C/minute of the rate of heat addition, 3 hours is kept the temperature, obtains zirconium pyrophosphate porous ceramics.Different sides powder
The phase composition of the porous ceramics obtained under product content is as shown in Figure 1, the result shows that obtained porous ceramics is pure pyrophosphoric acid
Zirconium porous ceramics.
Embodiment 2
Using zirconium pyrophosphate powder and flour as raw material, wherein flour volume content variation range is 0-40%, with anhydrous second
Alcohol is medium, is mixed 24 hours with planetary ball mill, uniformly mixed raw material is vacuum dried obtain zirconium pyrophosphate powder and
Flour mixed-powder is pressed into the disk of 10 millimeters of 20 millimeters thick of diameter with the method for dry-pressing, and the pressure of dry-pressing is 5MPa, will be done
The green compact of pressure, which are put into cold isostatic press, to be formed, briquetting pressure 250MPa.Molding sample is put into high temperature air furnace
In, 1400 DEG C are heated to 10 DEG C/minute of the rate of heat addition, 1.5 hours is kept the temperature, obtains zirconium pyrophosphate porous ceramics, porosity
It is distributed as 44-60%.Fig. 2 show 1400 DEG C heat preservation 1.5 hours zirconium pyrophosphate porous ceramics being prepared porosity and
The relationship of density and flour volume content, it can be seen that, obtained zirconium pyrophosphate porous ceramics lower with flour volume content
Porosity it is higher, therefore can pass through control material rate control zirconium pyrophosphate porous ceramics porosity.
Embodiment 3
Using zirconium pyrophosphate powder and flour as raw material, wherein zirconium pyrophosphate powder 17.0g, flour 3.0g, flour volume contain
Amount is 26%, using dehydrated alcohol as medium, is mixed 12 hours with planetary ball mill, and uniformly mixed raw material is vacuum dried to be obtained
To zirconium pyrophosphate powder and flour mixed-powder, the disk of 15 millimeters of 30 millimeters thick of diameter, dry-pressing are pressed into the method for dry-pressing
Pressure be 4MPa, the green compact of dry-pressing are put into cold isostatic press and are formed, briquetting pressure 150MPa.By molding sample
Product are put into high temperature air furnace, are heated to 1350 DEG C with 20 DEG C/minute of the rate of heat addition, are kept the temperature 2.5 hours, it is more to obtain zirconium pyrophosphate
Hole ceramics, porosity 54%.Microstructure as shown in figure 3, wherein (a) be gas cell distribution microstructure photograph, wherein
The large aperture stomata being evenly distributed is the stomata for removing flour particle and leaving, and the stomata of smaller aperture due is zirconium pyrophosphate particle part
It is sintered the spilehole formed, is (b) microstructure photograph of amplification, from can be significantly found out between zirconium pyrophosphate particle in (b)
Necking down.
Embodiment 4
Using zirconium pyrophosphate powder and flour as raw material, wherein zirconium pyrophosphate powder 15.0g, flour 5.0g, flour volume contain
Amount is 40%, using dehydrated alcohol as medium, is mixed 18 hours with planetary ball mill, and uniformly mixed raw material is vacuum dried to be obtained
To zirconium pyrophosphate powder and flour mixed-powder, the disk of 2 millimeters of 15 millimeters thick of diameter is pressed into the method for dry-pressing, dry-pressing
Pressure is 6MPa, and the green compact of dry-pressing are put into cold isostatic press and are formed, briquetting pressure 240MPa.By molding sample
It is put into high temperature air furnace, is heated to 1320 DEG C with 12 DEG C/minute of the rate of heat addition, keeps the temperature 2 hours, obtain the porous pottery of zirconium pyrophosphate
Porcelain, porosity 60%.Porous ceramics is as shown in Figure 4 from the thermal conductivity measurement result within the scope of 0-1500 DEG C, the results showed that
Its thermal conductivity is respectively less than 0.2W/ (mK) over the entire temperature range, and variation with temperature is unobvious.
Embodiment 5
Using zirconium pyrophosphate powder and flour as raw material, wherein zirconium pyrophosphate powder 15.0g, flour 5.0g, flour volume contain
Amount is 40%, using dehydrated alcohol as medium, is mixed 20 hours with planetary ball mill, and uniformly mixed raw material is vacuum dried to be obtained
To zirconium pyrophosphate powder and flour mixed-powder, the disk of 12 millimeters of 25 millimeters thick of diameter, dry-pressing are pressed into the method for dry-pressing
Pressure be 3MPa, the green compact of dry-pressing are put into cold isostatic press and are formed, briquetting pressure 220MPa.By molding sample
Product are put into high temperature air furnace, are heated to 1450 DEG C with 8 DEG C/minute of the rate of heat addition, are kept the temperature 1 hour, it is porous to obtain zirconium pyrophosphate
Ceramics, porosity 59%.Obtained porous ceramics is kept the temperature 6 hours at a temperature of 1000-1500 DEG C, consistency and body
Product shrinking percentage is as shown in Figure 5, the results showed that its consistency and cubical contraction variation after porous ceramics keeps the temperature 6 hours at high temperature
Unobvious, maximum volume shrinking percentage shows that the zirconium pyrophosphate porous ceramics being prepared has excellent anti-sintering less than 2.5%
Performance.
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (10)
1. a kind of anti-sintering zirconium pyrophosphate porous ceramics, it is characterised in that: the raw material of the porous ceramics is zirconium pyrophosphate powder, should
The group of porous ceramics becomes zirconium pyrophosphate, and the porosity of the porous ceramics is 44%-60%.
2. the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 1, it is characterised in that: the original of the porous ceramics
Material further includes flour, and the volume content of flour is not more than the 40% of raw material volume.
3. the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 1 or 2, it is characterised in that: the porous ceramics
Thermal conductivity is not more than 0.2W/ (mK) within the scope of 0-1500 DEG C, and 4-8 hours bodies are heat-treated within the scope of 1000-1500 DEG C
Product shrinking percentage is less than 2.5%.
4. the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 2, it is characterised in that: wherein flour is averaged grain
Diameter is 10 microns.
5. a kind of preparation method of anti-sintering zirconium pyrophosphate porous ceramics, it is characterised in that the step of this method includes:
(1) raw material and mixing medium are mixed in the ball mill, obtains mixture；
(2) mixture that step (1) obtains is dried to obtain powder, and the powder after drying is compressed to sheet
Green compact；
(3) step (2) pressed green compact are put into cold isostatic press the green compact for forming, being densified；
(4) densification for obtaining step (3) green compact carry out high-temperature heat treatment, high-temperature heat treatment in high temperature air furnace into
Row, obtains zirconium pyrophosphate porous ceramics.
6. the preparation method of the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 5, it is characterised in that: described
The step of (1) in, incorporation time be 6-24 hour, mixing medium be dehydrated alcohol.
7. the preparation method of the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 5, it is characterised in that: described
The step of (2) in, the pressure of compacting is 1-10MPa.
8. the preparation method of the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 5, it is characterised in that: described
The step of (3) in, briquetting pressure 150-300MPa.
9. the preparation method of the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 5, it is characterised in that: described
The step of (4) in, the temperature of high-temperature heat treatment is 1000-1500 DEG C, and the time of high-temperature heat treatment is 1-10 hours.
10. the preparation method of the anti-sintering zirconium pyrophosphate porous ceramics of one kind according to claim 5, it is characterised in that: institute
In the step of stating (4), heating rate is 5-30 DEG C/minute.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417669A (en) * | 2022-09-30 | 2022-12-02 | 武汉科技大学 | High silica glass fiber reinforced zirconium pyrophosphate-based composite material and preparation method thereof |
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| CN115417669A (en) * | 2022-09-30 | 2022-12-02 | 武汉科技大学 | High silica glass fiber reinforced zirconium pyrophosphate-based composite material and preparation method thereof |
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