CN108383524A - A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials and preparation method thereof - Google Patents
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials and preparation method thereof Download PDFInfo
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
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- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Abstract
The invention discloses a kind of Gd2O3、Yb2O3The preparation method of modified YSZ nano-powder materials and preparation method thereof, the YSZ nano-powder materials includes：Multicomponent co-precipitation is first passed through to be made with Gd2O3Nanometer powder, Yb2O3Nanometer powder is the cladded type presoma of kernel, then carries out ultrasonic atomizatio to the cladded type presoma cleaned up, is re-fed into fast reaction in the superelevation temperature-heat-source of induction plasma line, you can generates Gd2O3、Yb2O3Modified YSZ nano-powder materials.The present invention can make the mean free path of YSZ material molecules reduce, reduce the thermal coefficient of material, and the phase structure of YSZ materials is made more to stablize, stability of the electrical and optical performance of material when higher than 1100 DEG C of high temperature is promoted, and preparation method can effectively avoid multicomponent from being co-precipitated the problems such as lack of homogeneity, granularity control ability are poor, technological process is excessively complicated, low production efficiency technology.
Description
Technical field
The present invention relates to YSZ (yttria-stabilized zirconia) field of powder material more particularly to a kind of Gd2O3、Yb2O3Change
The YSZ nano-powder materials and preparation method thereof of property.
Background technology
YSZ powder material is a kind of fine ceramics material being widely used, it has unique calorifics, electricity, optics
Characteristic, therefore it is widely used in the necks such as insulating moulding coating/coating, features ceramic structures, material of giving out light, fuel cell
Domain.But YSZ powder material, during being recycled for a long time at higher than 1100 DEG C, there are phase transformation, crystal grain are long for material itself
Phenomena such as big, this can cause material phenomena such as thermal coefficient increases, electric conductivity declines, optical property is unstable occur, seriously
Affect the application performance of YSZ powder material.
Invention content
It is existing relatively steady during existing YSZ powder material recycles for a long time at higher than 1100 DEG C in order to solve
The problems such as qualitative difference, calorifics, optics, unstable electrical application performance, the present invention provides a kind of Gd2O3、Yb2O3Modified YSZ
Nano-powder material and preparation method thereof can make the mean free path of YSZ material molecules reduce, reduce the heat conduction system of material
Number, and the phase structure of YSZ materials is made more to stablize, promote stabilization of the electrical and optical performance of material when higher than 1100 DEG C of high temperature
Property, and the preparation method of modification YSZ nano-powder materials can effectively avoid multicomponent co-precipitation lack of homogeneity, granularity control
Can the problems such as force difference, subsequent process flow be excessively complicated, low production efficiency technology, realization efficiently and rapidly prepares high-quality
Gd2O3、Yb2O3Modified YSZ nano-powder materials, have a good application prospect.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of Gd2O3、Yb2O3The preparation method of modified YSZ nano-powder materials, including：
Step 1, by Gd2O3Nanometer powder, Yb2O3Nanometer powder is added to the water to obtain the first mixed liquor, is then added and accounts for
The polyethylene glycol of first mixed liquor gross mass 0.2~5%, and be uniformly mixed, to obtain the first suspension；Wherein, Gd2O3It receives
Rice flour end and Yb2O3The mass ratio of nanometer powder is 1:1~3:1 or 1:1~1:3；Gd2O3Nanometer powder and Yb2O3Nanometer powder
Primary particle degree be 5~15nm；
Step 2 mixes aqueous solution and first suspension of the aqueous solution of zirconates, yttrium salt, to obtain
Then second mixed liquor is added and accounts for the polyethylene glycol of the second mixed liquor gross mass 0.2~5%, and is uniformly mixed, to obtain the
Three mixed liquors；Wherein, the molar ratio of zirconates and yttrium salt is 1:7~1:19, Gd2O3Nanometer powder and Yb2O3Nanometer powder always rubs
The molar ratio of that number and zirconates is 1:5~1:23.5；
Step 3 carries out the third mixed liquor with the rotating speed of 60~240r/min to continue high-speed stirred, while to described
Lye is added in third mixed liquor, the pH value of the third mixed liquor is made to be adjusted to 8~11, not medium well in the third mixed liquor
K is added into the third mixed liquor when the white precipitate in the third mixed liquor is not further added by white precipitate2CO3
Catalyst, and high-speed stirred is continued 4 hours with the rotating speed of 60~240r/min, to obtain with Gd2O3Nanometer powder, Yb2O3It receives
Rice flour end is the cladded type presoma of kernel；
Step 4 washs the cladded type presoma, until it can't detect chlorion using silver nitrate, so
After carry out water removal press filtration, to obtain presoma filter cake；
Step 5, by the presoma filter cake and predetermined medium according to mass ratio 1:0.4~1:5 are mixed, and are added poly-
Ethylene glycol obtains forerunner's liquid suspension；Then forerunner's liquid suspension is sent into ultrasonic mist with the conveying speed of 0.1~15Kg/h
Change nozzle and carry out ultrasonic atomizatio, the frequency of ultrasonic atomizatio shower nozzle is 0~2.4MHz, then using induction of induction coil excitation etc. from
Beamlet stream is sent into as superelevation temperature-heat-source, by forerunner's liquid suspension after atomization using the inert gas that air pressure is 0.1~1.2MPa
Fast reaction is carried out in the superelevation temperature-heat-source that temperature is 8000~12000 DEG C, to which powder size ranging from 30nm~105 be made
μm be Gd2O3、Yb2O3Modified YSZ nano-powder materials.
Preferably, by the frequency of the conveying speed, ultrasonic atomizatio shower nozzle of forerunner's liquid suspension, indifferent gas in step 5
The air pressure of body is adjusted, and controls final Gd obtained2O3、Yb2O3The powder size of modified YSZ nano-powder materials.
Preferably, in step 1, ultrasonic disperse is carried out using ultrasonic disperser and is allowed to uniformly mixed.
Preferably, in step 2, high-speed stirred is carried out with the rotating speed of 60~240r/min and is allowed to uniformly mixed.
Preferably, in step 3, the volumetric concentration of the lye is 10~80%, and the addition speed of the lye is 0.1
~10kg/min, the K2CO3The addition of catalyst is the 1% of the lye gross mass.
Preferably, in step 4, using at least one of pure water, alcohol or methanol to the cladded type presoma
It is washed.
Preferably, in steps of 5, the predetermined medium is alcohol or water, the polyethylene glycol in forerunner's liquid suspension
Weight percentage be 0.1~2%, the working media of the induction plasma line of induction coil excitation is argon gas, work(
Rate is 10~80KW.
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, using above-mentioned Gd2O3、Yb2O3Modified YSZ nanometers
The preparation method of dusty material is prepared.
As seen from the above technical solution provided by the invention, Gd provided by the invention2O3、Yb2O3Modified YSZ receives
The method that rice flour powder material first passes through nanometer powder nucleus guiding chemical synthesis presoma is prepared with Gd2O3Nanometer powder,
Yb2O3Nanometer powder is the cladded type presoma of kernel, has then carried out ultrasonic atomizatio to the cladded type presoma, and be sent to
Fast reaction is carried out in the superelevation temperature-heat-source of induction plasma line, to can rapidly and efficiently prepare powder size ranging from
30nm~105 μm are Gd2O3、Yb2O3Modified YSZ nano-powder materials；The Gd2O3、Yb2O3Modified YSZ nano-powder materials
In, Gd2O3And Yb2O3YSZ nanometer powders are modified according to the aforementioned proportion relationship proposed in the present invention, this can make YSZ materials
Expect that the mean free path of molecule reduces, reduces the thermal coefficient of material, and the phase structure of YSZ materials is made more to stablize, promotes material
Expect stability of electrical and optical performance when higher than 1100 DEG C of high temperature, has a good application prospect.With conventional preparation techniques
In chemical coprecipitation process compare, preparation method provided by the present invention can effectively avoid multicomponent be co-precipitated uniformity
The technical problems such as difference, granularity control ability difference, and evaded the sintering of subsequent technique high temperature, coarse crushing, essence of the prior art
The technical problems such as conventional process flows are excessively complicated, production efficiency is low such as fine crushing, agglomeration granulation, secondary high-temperature sintering, can
High-quality Gd is efficiently and rapidly prepared in realization2O3、Yb2O3Modified YSZ nano-powder materials.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 is the Gd that the powder size that the embodiment of the present invention 1 provides is 30~60nm2O3、Yb2O3Modified YSZ nano powders
The electron microscope photo scanning of powder material.
Fig. 2 is the Gd that the powder size that the embodiment of the present invention 2 provides is 5~20 μm2O3、Yb2O3Modified YSZ nano powders
The electron microscope photo scanning of powder material.
Fig. 3 is the Gd that the powder size that the embodiment of the present invention 3 provides is 30~100 μm2O3、Yb2O3Modified YSZ nanometers
The electron microscope photo scanning of dusty material.
Specific implementation mode
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
Below to Gd provided by the present invention2O3、Yb2O3Modified YSZ nano-powder materials and preparation method thereof carry out detailed
Thin description.The content not being described in detail in the present invention belongs to the prior art well known to professional and technical personnel in the field.
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, preparation method include the following steps：
Step 1, by Gd2O3Nanometer powder, Yb2O3Nanometer powder is added to the water to obtain the first mixed liquor, is then added and accounts for
The polyethylene glycol of first mixed liquor gross mass 0.2~5% is made as dispersant, and using ultrasonic disperser progress ultrasonic disperse
It is to be uniformly mixed, to obtain the first suspension.Wherein, Gd2O3Nanometer powder and Yb2O3The mass ratio of nanometer powder is 1:1~
3:1 or 1:1~1:3；Gd2O3Nanometer powder and Yb2O3The primary particle degree of nanometer powder is 5~15nm.
Yttrium salt, is made the aqueous solution of yttrium salt by step 2, the aqueous solution that zirconates is made to zirconates, then by the aqueous solution of zirconates,
The aqueous solution of yttrium salt is mixed with first suspension, to obtain the second mixed liquor, is then added and is accounted for the second mixing
The polyethylene glycol of liquid gross mass 0.2~5% carries out high-speed stirred with the rotating speed of 60~240r/min and is allowed to mixed as dispersant
It closes uniformly, to obtain third mixed liquor.Wherein, the molar ratio of zirconates and yttrium salt is 1:7~1:19, Gd2O3Nanometer powder and
Yb2O3The total mole number of nanometer powder and the molar ratio of zirconates are 1:5~1:23.5.
Step 3 persistently carries out high-speed stirred with the rotating speed of 60~240r/min to the third mixed liquor, and with 0.1~
The lye that volumetric concentration is 10~80% is added into the third mixed liquor for the addition speed of 10kg/min, and (lye can be adopted
With strong base solution, weak caustic solution can also be used), so that the pH value of the third mixed liquor is adjusted to 8~11, zirconates and yttrium salt meeting
Chemical precipitation reaction occurs, high-speed stirred is persistently carried out in this whole process, white is continuously generated in the third mixed liquor
Precipitation is added into the third mixed liquor when the white precipitate in the third mixed liquor is not further added by and accounts for the lye
The K of gross mass 1%2CO3Catalyst, and high-speed stirred is continued 4 hours with the rotating speed of 60~240r/min, to obtain with Gd2O3
Nanometer powder, Yb2O3Nanometer powder is the cladded type presoma of kernel.
Step 4 washs the cladded type presoma using at least one of pure water, alcohol or methanol, directly
Until it can't detect chlorion using silver nitrate, water removal press filtration is then carried out, to obtain presoma filter cake.
Step 5, by the presoma filter cake and predetermined medium (the predetermined medium can be alcohol or water) according to mass ratio
1:0.4~1:5 are mixed, and polyethylene glycol is added as dispersant, are 0.1 to obtain polyethylene glycol weight percentage
~2% forerunner's liquid suspension；Then by suspension feed appliance by forerunner's liquid suspension with the conveying of 0.1~15Kg/h
Speed is sent into ultrasonic atomizatio shower nozzle and carries out ultrasonic atomizatio, and the frequency of ultrasonic atomizatio shower nozzle is 0~2.4MHz, atomized rear forerunner
Liquid suspension；It uses the induction plasma line of induction coil excitation as superelevation temperature-heat-source again, presoma after atomization is suspended
The inert gas that liquid is 0.1~1.2MPa using air pressure is sent into the superelevation temperature-heat-source that temperature is 8000~12000 DEG C and is carried out soon
The working media of speed reaction, the induction plasma line of induction coil excitation is argon gas, and power is 10~80KW, to which powder be made
Last granularity is that 30nm~105 μm are Gd2O3、Yb2O3Modified YSZ nano-powder materials.
Specifically, Gd provided by the present invention2O3、Yb2O3Modified YSZ nano-powder materials and preparation method thereof are at least
Has following advantages：
(1) Gd provided by the present invention2O3、Yb2O3In modified YSZ nano-powder materials, it is using primary particle degree
The Gd of 5~15nm2O3And Yb2O3YSZ nanometer powders are modified, Gd therein2O3And Yb2O3With higher chemical stabilization
Property, higher fusing point, larger atomic radius, as these Gd2O3And Yb2O3According to the aforementioned proportion relationship proposed in the present invention
After being modified to YSZ nanometer powders, the mean free path of YSZ material molecules can be made to reduce, reduce the thermal coefficient of material, and
So that the phase structure of YSZ materials is more stablized, promotes stability of the electrical and optical performance of material when higher than 1100 DEG C of high temperature, because
This Gd2O3、Yb2O3Modified YSZ nano-powder materials can be used for heat-insulated protection, solid fuel cell, it is extraordinary shine etc. it is numerous
Field has a good application prospect.
(2) Gd provided by the present invention2O3、Yb2O3One is provided in the preparation method of modified YSZ nano-powder materials
The method of kind nanometer powder nucleus guiding chemical synthesis presoma, to prepare with Gd2O3Nanometer powder, Yb2O3Nanometer powder is interior
The cladded type presoma of core, and ultrasonic atomizatio has been carried out to the cladded type presoma, it is then fed into induction plasma line
Superelevation temperature-heat-source in carry out fast reaction, to can rapidly and efficiently prepare above-mentioned Gd2O3、Yb2O3Modified YSZ nanometers
Dusty material；Compared with the chemical coprecipitation process in conventional preparation techniques, preparation method provided by the present invention can be effective
The technical problems such as multicomponent co-precipitation lack of homogeneity, granularity control ability difference are avoided, and have evaded the follow-up work of the prior art
Conventional process flows are excessively complicated, produce for the sintering of skill high temperature, coarse crushing, fine broken, agglomeration granulation, secondary high-temperature sintering etc.
The technical problems such as efficiency is low, can realize and efficiently and rapidly prepare high-quality Gd2O3、Yb2O3Modified YSZ nanometer powder materials
Material.
(3) Gd provided by the present invention2O3、Yb2O3In the preparation method of modified YSZ nano-powder materials, by step
The frequency of conveying speed, ultrasonic atomizatio shower nozzle of forerunner's liquid suspension, the air pressure of inert gas are effectively adjusted in rapid 5, energy
Enough final Gd obtained of control2O3、Yb2O3The powder size of modified YSZ nano-powder materials, thus it is provided by the present invention
Gd2O3、Yb2O3The preparation method of modified YSZ nano-powder materials is strong to the granularity control ability of final products, disclosure satisfy that
Various occasions are to Gd2O3、Yb2O3The Grained Requirements of modified YSZ nano-powder materials.
To sum up, the embodiment of the present invention can make the mean free path of YSZ material molecules reduce, reduce the heat conduction of material
Coefficient, and the phase structure of YSZ materials is made more to stablize, it is steady when higher than 1100 DEG C of high temperature to promote the electrical and optical performance of material
It is qualitative, and the preparation method of modification YSZ nano-powder materials can effectively avoid multicomponent co-precipitation lack of homogeneity, granularity control
High-quality is efficiently and rapidly prepared in the problems such as making excessively complicated energy force difference, subsequent process flow, low production efficiency technology, realization
Gd2O3、Yb2O3Modified YSZ nano-powder materials, have a good application prospect.
In order to more clearly from show technical solution provided by the present invention and generated technique effect, below with tool
Body embodiment is provided for the embodiments of the invention Gd2O3、Yb2O3Modified YSZ nano-powder materials and preparation method thereof carry out
Detailed description.
Embodiment 1
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, preparation method may include following steps：
Step a1, by the Gd of 3.17kg2O3The Yb of nanometer powder, 3.45kg2O3Nanometer powder is added in the water of 70kg and obtains
To the first mixed liquor, the polyethylene glycol of 3.5kg is then added and carries out ultrasonic disperse as dispersant, and using ultrasonic disperser
It is allowed to uniformly mixed, to obtain the first suspension.Wherein, Gd2O3Nanometer powder and Yb2O3The primary particle degree of nanometer powder
It is 5~15nm.
Step a2, the six water yttrium chlorides of the zirconium oxychloride of 50kg, 4.255kg are added in 500kg deionized waters, are stirred
Uniformly, first suspension is then added, to obtain the second mixed liquor, the polyethylene glycol of 9kg is then added as dispersion
Agent, and high-speed stirred is carried out with the rotating speed of 200r/min and is allowed to uniformly mixed, to obtain third mixed liquor.
Step a3, high-speed stirred is persistently carried out to the third mixed liquor with the rotating speed of 200r/min, be used in combination 70 minutes to
The ammonium hydroxide that 45kg volumetric concentrations are 40% is added in the third mixed liquor, make the pH value of the third mixed liquor be adjusted to 8~
11, chemical precipitation reaction can occur for zirconates and yttrium salt, continue to carry out high-speed stirring with the rotating speed of 200r/min in this whole process
It mixes, white precipitate is continuously generated in the third mixed liquor, when the white precipitate in the third mixed liquor is not further added by, to
The K of 450g is added in the third mixed liquor2CO3Catalyst, and high-speed stirred is continued 4 hours with the rotating speed of 200r/min, to
It obtains with Gd2O3Nanometer powder, Yb2O3Nanometer powder is the cladded type presoma of kernel.
Step a4, the cladded type presoma is washed using at least one of pure water, alcohol or methanol, directly
Until it can't detect chlorion using silver nitrate, water removal press filtration is then carried out, to obtain presoma filter cake.
Step a5, according to the presoma filter cake:Pure water:Polyethylene glycol=1:1:0.01 mass ratio, to before described
It drives and pure water and polyethylene glycol is added in body filter cake, after stirring evenly, obtain uniform and stable forerunner's liquid suspension；Then pass through
Forerunner's liquid suspension is sent into ultrasonic atomizatio shower nozzle with the conveying speed of 8Kg/h and carries out ultrasonic atomizatio by suspension feed appliance,
The frequency of ultrasonic atomizatio shower nozzle is 2.4MHz, atomized rear forerunner's liquid suspension；The induction etc. of induction coil excitation is used again
Ion beam current is sent into temperature as superelevation temperature-heat-source, by the inert gas that forerunner's liquid suspension is 1MPa using air pressure after atomization
Fast reaction is carried out in 8000~10000 DEG C of superelevation temperature-heat-source, the work of the induction plasma line of induction coil excitation is situated between
Matter is argon gas, and power 60KW is Gd to which obtained powder size as shown in Figure 1 is 30~60nm2O3、Yb2O3Modified
YSZ nano-powder materials.
Embodiment 2
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, preparation method may include following steps：
Step b1, by the Gd of 1.25kg2O3The Yb of nanometer powder, 1.36kg2O3Nanometer powder is added in the water of 70kg and obtains
To the first mixed liquor, the polyethylene glycol of 3.5kg is then added and carries out ultrasonic disperse as dispersant, and using ultrasonic disperser
It is allowed to uniformly mixed, to obtain the first suspension.Wherein, Gd2O3Nanometer powder and Yb2O3The primary particle degree of nanometer powder
It is 5~15nm.
Step b2, the six water yttrium chlorides of the zirconium oxychloride of 50kg, 7.90kg are added in 500kg deionized waters, are stirred
Uniformly, first suspension is then added, to obtain the second mixed liquor, then the polyethylene glycol of addition 8.5kg, which is used as, divides
Powder, and high-speed stirred is carried out with the rotating speed of 200r/min and is allowed to uniformly mixed, to obtain third mixed liquor.
Step b3, high-speed stirred is persistently carried out to the third mixed liquor with the rotating speed of 200r/min, be used in combination 70 minutes to
The ammonium hydroxide that 40kg volumetric concentrations are 50% is added in the third mixed liquor, make the pH value of the third mixed liquor be adjusted to 8~
11, chemical precipitation reaction can occur for zirconates and yttrium salt, continue to carry out high-speed stirring with the rotating speed of 200r/min in this whole process
It mixes, white precipitate is continuously generated in the third mixed liquor, when the white precipitate in the third mixed liquor is not further added by, to
The K of 450g is added in the third mixed liquor2CO3Catalyst, and high-speed stirred is continued 4 hours with the rotating speed of 200r/min, to
It obtains with Gd2O3Nanometer powder, Yb2O3Nanometer powder is the cladded type presoma of kernel.
Step b4, the cladded type presoma is washed using at least one of pure water, alcohol or methanol, directly
Until it can't detect chlorion using silver nitrate, water removal press filtration is then carried out, to obtain presoma filter cake.
Step b5, according to the presoma filter cake:Pure water:Polyethylene glycol=1:1:0.01 mass ratio, to before described
It drives and pure water and polyethylene glycol is added in body filter cake, after stirring evenly, obtain uniform and stable forerunner's liquid suspension；Then pass through
Forerunner's liquid suspension is sent into ultrasonic atomizatio shower nozzle with the conveying speed of 5Kg/h and carries out ultrasonic atomizatio by suspension feed appliance,
The frequency of ultrasonic atomizatio shower nozzle is 0MHz, atomized rear forerunner's liquid suspension；Use again induction etc. of induction coil excitation from
Beamlet stream is sent into temperature as superelevation temperature-heat-source, by the inert gas that forerunner's liquid suspension is 0.5MPa using air pressure after atomization
Fast reaction is carried out in 8000~10000 DEG C of superelevation temperature-heat-source, the work of the induction plasma line of induction coil excitation is situated between
Matter is argon gas, and power 50KW is Gd to which obtained powder size is 5~20 μm2O3、Yb2O3Modified YSZ nanometer powder materials
Material.
Embodiment 3
A kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, preparation method may include following steps：
Step c1, by the Gd of 1.25kg2O3The Yb of nanometer powder, 1.36kg2O3Nanometer powder is added in the water of 70kg and obtains
To the first mixed liquor, the polyethylene glycol of 3.5kg is then added and carries out ultrasonic disperse as dispersant, and using ultrasonic disperser
It is allowed to uniformly mixed, to obtain the first suspension.Wherein, Gd2O3Nanometer powder and Yb2O3The primary particle degree of nanometer powder
It is 5~15nm.
Step c2, the six water yttrium chlorides of the zirconium oxychloride of 50kg, 7.9kg are added in 500kg deionized waters, stirring is equal
It is even, first suspension is then added, to obtain the second mixed liquor, the polyethylene glycol of 8.5kg is then added as dispersion
Agent, and high-speed stirred is carried out with the rotating speed of 200r/min and is allowed to uniformly mixed, to obtain third mixed liquor.
Step c3, high-speed stirred is persistently carried out to the third mixed liquor with the rotating speed of 200r/min, be used in combination 70 minutes to
The ammonium hydroxide that 40kg volumetric concentrations are 50% is added in the third mixed liquor, make the pH value of the third mixed liquor be adjusted to 8~
11, chemical precipitation reaction can occur for zirconates and yttrium salt, continue to carry out high-speed stirring with the rotating speed of 200r/min in this whole process
It mixes, white precipitate is continuously generated in the third mixed liquor, when the white precipitate in the third mixed liquor is not further added by, to
The K of 450g is added in the third mixed liquor2CO3Catalyst, and high-speed stirred is continued 4 hours with the rotating speed of 200r/min, to
It obtains with Gd2O3Nanometer powder, Yb2O3Nanometer powder is the cladded type presoma of kernel.
Step c4, the cladded type presoma is washed using at least one of pure water, alcohol or methanol, directly
Until it can't detect chlorion using silver nitrate, water removal press filtration is then carried out, to obtain presoma filter cake.
Step c5, according to the presoma filter cake:Pure water:Polyethylene glycol=1:1:0.01 mass ratio, to before described
It drives and pure water and polyethylene glycol is added in body filter cake, after stirring evenly, obtain uniform and stable forerunner's liquid suspension；Then pass through
Forerunner's liquid suspension is sent into ultrasonic atomizatio shower nozzle with the conveying speed of 4Kg/h and carries out ultrasonic atomizatio by suspension feed appliance,
The frequency of ultrasonic atomizatio shower nozzle is 0MHz, atomized rear forerunner's liquid suspension；Use again induction etc. of induction coil excitation from
Beamlet stream is sent into temperature as superelevation temperature-heat-source, by the inert gas that forerunner's liquid suspension is 0.2MPa using air pressure after atomization
Fast reaction is carried out in 8000~10000 DEG C of superelevation temperature-heat-source, the work of the induction plasma line of induction coil excitation is situated between
Matter is argon gas, and power 45KW is Gd to which obtained powder size is 30~100 μm2O3、Yb2O3Modified YSZ nanometer powders
Material.
To sum up, the embodiment of the present invention can make the mean free path of YSZ material molecules reduce, reduce the heat conduction of material
Coefficient, and the phase structure of YSZ materials is made more to stablize, it is steady when higher than 1100 DEG C of high temperature to promote the electrical and optical performance of material
It is qualitative, and preparation method can be avoided effectively that multicomponent co-precipitation lack of homogeneity, granularity control ability be poor, subsequent process flow
The problems such as excessively complicated, low production efficiency technology, realization efficiently and rapidly prepares high-quality Gd2O3、Yb2O3Modified YSZ receives
Rice flour powder material, has a good application prospect.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (8)
1. a kind of Gd2O3、Yb2O3The preparation method of modified YSZ nano-powder materials, which is characterized in that including：
Step 1, by Gd2O3Nanometer powder, Yb2O3Nanometer powder is added to the water to obtain the first mixed liquor, is then added and accounts for first
The polyethylene glycol of mixed liquor gross mass 0.2~5%, and be uniformly mixed, to obtain the first suspension；Wherein, Gd2O3Nano powder
End and Yb2O3The mass ratio of nanometer powder is 1:1~3:1 or 1:1~1:3；Gd2O3Nanometer powder and Yb2O3The one of nanometer powder
Secondary granularity is 5~15nm；
Step 2 mixes aqueous solution and first suspension of the aqueous solution of zirconates, yttrium salt, to obtain second
Then mixed liquor is added the polyethylene glycol for accounting for the second mixed liquor gross mass 0.2~5%, and is uniformly mixed, mixed to obtain third
Close liquid；Wherein, the molar ratio of zirconates and yttrium salt is 1:7~1:19, Gd2O3Nanometer powder and Yb2O3The total mole number of nanometer powder
Molar ratio with zirconates is 1:5~1:23.5；
Step 3 carries out the third mixed liquor with the rotating speed of 60~240r/min to continue high-speed stirred, while to the third
Lye is added in mixed liquor, so that the pH value of the third mixed liquor is adjusted to 8~11, is continuously generated in the third mixed liquor white
Color precipitates, and when the white precipitate in the third mixed liquor is not further added by, K is added into the third mixed liquor2CO3Catalysis
Agent, and high-speed stirred is continued 4 hours with the rotating speed of 60~240r/min, to obtain with Gd2O3Nanometer powder, Yb2O3Nano powder
End is the cladded type presoma of kernel；
Step 4 washs the cladded type presoma, until it can't detect chlorion using silver nitrate, then into
Row water removal press filtration, to obtain presoma filter cake；
Step 5, by the presoma filter cake and predetermined medium according to mass ratio 1:0.4~1:5 are mixed, and poly- second two is added
Alcohol obtains forerunner's liquid suspension；Then forerunner's liquid suspension is sent into ultrasonic atomizatio spray with the conveying speed of 0.1~15Kg/h
Head carries out ultrasonic atomizatio, and the frequency of ultrasonic atomizatio shower nozzle is 0~2.4MHz, then the induction plasma beam using induction coil excitation
Stream is used as superelevation temperature-heat-source, and forerunner's liquid suspension after atomization is sent into temperature using the inert gas that air pressure is 0.1~1.2MPa
To carry out fast reaction in 8000~12000 DEG C of superelevation temperature-heat-source, it is to which powder size ranging from 30nm~105 μm be made
Gd2O3、Yb2O3Modified YSZ nano-powder materials.
2. Gd according to claim 12O3、Yb2O3The preparation method of modified YSZ nano-powder materials, which is characterized in that
By being adjusted to the frequency of conveying speed, ultrasonic atomizatio shower nozzle of forerunner's liquid suspension, the air pressure of inert gas in step 5
It is whole, control final Gd obtained2O3、Yb2O3The powder size of modified YSZ nano-powder materials.
3. Gd according to claim 1 or claim 22O3、Yb2O3The preparation method of modified YSZ nano-powder materials, feature exist
In, in step 1, using ultrasonic disperser carry out ultrasonic disperse be allowed to uniformly mixed.
4. Gd according to claim 1 or claim 22O3、Yb2O3The preparation method of modified YSZ nano-powder materials, feature exist
In in step 2, carrying out high-speed stirred with the rotating speed of 60~240r/min and be allowed to uniformly mixed.
5. Gd according to claim 1 or claim 22O3、Yb2O3The preparation method of modified YSZ nano-powder materials, feature exist
In, in step 3, the volumetric concentration of the lye is 10~80%, and the addition speed of the lye is 0.1~10kg/min,
The K2CO3The addition of catalyst is the 1% of the lye gross mass.
6. Gd according to claim 1 or claim 22O3、Yb2O3The preparation method of modified YSZ nano-powder materials, feature exist
In in step 4, being washed to the cladded type presoma using at least one of pure water, alcohol or methanol.
7. Gd according to claim 1 or claim 22O3、Yb2O3The preparation method of modified YSZ nano-powder materials, feature exist
In in steps of 5, the predetermined medium is alcohol or water, and the weight percent of polyethylene glycol contains in forerunner's liquid suspension
Amount is 0.1~2%, and the working media of the induction plasma line of the induction coil excitation is argon gas, and power is 10~80KW.
8. a kind of Gd2O3、Yb2O3Modified YSZ nano-powder materials, which is characterized in that appoint using in the claims 1 to 7
Gd described in one2O3、Yb2O3The preparation method of modified YSZ nano-powder materials is prepared.
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