CN107585787B - Tri- rare earth ion tantalates of Sm-Eu-Dy and the preparation method and application thereof - Google Patents
Tri- rare earth ion tantalates of Sm-Eu-Dy and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of tri- rare earth ion tantalates of Sm-Eu-Dy and the preparation method and application thereof, the chemical general formula of the tri- rare earth ion tantalates of Sm-Eu-Dy is SmaEubDycTaO7, wherein a+b+c=3, a, b, c=0.8~1.2.Preparation method includes the following steps: 1) stoichiometrically to weigh Europium chloride, samaric nitrate, dysprosium nitrate and tantalum oxalate, and mechanical mixture is carried out under heat-retaining condition with the citric acid of set amount, in mixed process be added concentrated ammonia liquor in and solution, then under heat-retaining condition carry out mechanical mixture promote chemical reaction progress.2) acquired solution is dried, then calcining removes carbon impurity to get tri- rare earth ion tantalic acid salt powder of Sm-Eu-Dy at high temperature.The tri- rare earth ion tantalates of Sm-Eu-Dy, high high-temp stability is good, and thermal conductivity coefficient is low, can be used as heat barrier coat material and is applied.
Description
Technical field
The present invention relates to a kind of tantalates, a kind of tri- rare earth ion tantalates of Sm-Eu-Dy and preparation method thereof is particularly related to
With application.
Background technique
With the development of Aeronautics and Astronautics and civilian technology, hot-end component uses temperature requirement higher and higher, has reached height
The extreme condition of temperature alloy and monocrystal material.By taking the heating part of gas turbine such as nozzle, blade, combustion chamber as an example, at them
In the adverse circumstances such as high-temperature oxydation and high temperature gas flow erosion, bearing temperature is up to 1100 DEG C, has been more than that high temperature nickel alloy makes
Limiting temperature (1075 DEG C).The high intensity of metal, high tenacity are combined with the advantage resistant to high temperature of ceramics prepared
Thermal barrier coating out can solve the above problem, it can play the role of it is heat-insulated, anti-oxidant, etch-proof, steam turbine, diesel oil send out
Certain application is obtained on the material of the hot ends such as motor, jet engine, and extends the service life of hot-end component.
Currently, the ceramic material for being most suitable as thermal barrier coating mainly has yttria-stabilized zirconia (YSZ), rare earth zirconic acid
Salt (RE2Zr2O7), rare earth silicate (RE2SiO5), RE phosphate (REPO4), rare earth cerate (RE2Ce2O7) and rare earth
Stannate (RE2Sn2O7) etc..Wherein most widely used is yttria-stabilized zirconia (YSZ), with high-melting-point, low-heat
It leads, high thermal expansion coefficient and good mechanical property, but lower using temperature, only 1200 DEG C, this is because at 1200 DEG C
The above YSZ, which can be undergone phase transition, to be led to volume change and causes coating failure.Other than YSZ, the thermal barrier coating material applied at present
Material has La2Zr2O7, belong to one kind of rare earth zirconate, there is lower thermal conductivity compared to YSZ, and be up to using temperature
1600 DEG C, this is because rare earth zirconate is burnt green stone and defect fluorite type structure, have a large amount of crystal defect can be effective
Phonon is scattered, to reduce thermal conductivity, and the problems such as phase transformation is not present at high temperature.It follows that finding novel thermal boundary
When coating material the low thermal conducting material with good high temperature phase stability can be explored from crystal structure.
Rare earth tantalate RE3TaO7It is a kind of novel heat barrier coat material, the result of study of Yoshiyuki shows
(Yoshiyuki Yokogawa,Masahiro Yoshimura and Shigeyuki Somiya；Order-disorder in
R3TaO7(R=rare earth) Phases, Solid State ionics:28-30 (1988) 1250-1253), in RE3TaO7
In with the variation of ionic radius of rare earth occur to be changed by Jiao Lvshi to defect fluorite structure it is orderly -- unordered variation, this with it is dilute
Native zirconates (RE2Zr2O7) similar.Therefore it can guess that the two oxides ceramics with analogous crystalline structure may have phase
Same characteristic, such as high-melting-point, lower thermal conductivity, high thermal expansion coefficient etc., and RE is shown according to previous investigation3TaO7For
Ferroelasticity material, this is identical as YSZ, therefore has good mechanical property at high temperature.
Summary of the invention
The tri- rare earth ion tantalic acid of Sm-Eu-Dy that the purpose of the present invention is to provide a kind of thermal conductivity coefficients is low, thermal stability is good
Salt and the preparation method and application thereof.
To achieve the above object, tri- rare earth ion tantalates of Sm-Eu-Dy provided by the present invention, chemical general formula are
SmaEubDycTaO7, wherein a+b+c=3, a, b, c=0.8~1.2.Preferably, a=b=c=1, at this point, the Sm-Eu-Dy
The chemical formula of three rare earth ion tantalates is SmEuDyTaO7。
Preferably, which has the property that 1) average grain size is 1~10 μ
m；2) at 100~800 DEG C of temperature, thermal conductivity is 1.2~1.9Wm-1·K-1, and reduced as temperature increases；3) XRD diagram
In spectrum, diffraction maximum is successively decreased by relative intensity arranges the angle at place are as follows: and 29.9 ± 1 °, 49.3 ± 1 °, 58.2 ± 1 °, 34.7 ±
1 °, 79.1 ± 1 °, 61.2 ± 1 °, 71.5 ± 1 °.
Invention also provides a kind of preparation methods of above-mentioned tri- rare earth ion tantalates of Sm-Eu-Dy, including walk as follows
It is rapid:
1) samaric nitrate, Europium chloride, dysprosium nitrate and tantalum oxalate are stoichiometrically weighed, and is being protected with the citric acid of set amount
It carries out mechanical mixture under the conditions of temperature, is added in mixed process in concentrated ammonia liquor and solution, then carry out mechanical mixture under heat-retaining condition
Promote the progress of chemical reaction:
In the above reaction, the sum of the amount of substance of three kinds of rare earth elements: tantalum oxalate: citric acid=6: 1: 8, each rare earth element
Substance amount stoichiometrically coefficient determine；Citric acid then can be calcined out, therefore can be slightly excessive；Ammonium hydroxide additional amount with
So that solution is reached near neutral is advisable.
2) acquired solution is dried, then at high temperature calcining removal carbon impurity to get tri- rare earth of Sm-Eu-Dy from
Sub- tantalic acid salt powder.
Preferably, in step 1), when first time mechanical mixture, temperature is 120~160 DEG C, 40~60min of time；Second
When secondary mechanical mixture, temperature is 170~190 DEG C, 30~50min of time.
Preferably, in step 2), drying temperature is 250~300 DEG C, 6~10h of drying time；Calcination temperature be 700~
1000 DEG C, 6~10h of calcination time.
Above-mentioned tri- rare earth ion tantalates of Sm-Eu-Dy has the low low and higher thermal expansion coefficient of thermal conductivity coefficient, can make
It is applied for heat barrier coat material.Its a kind of application mode as heat barrier coat material are as follows: the Sm-Eu-Dy tri- is dilute
Native ion tantalates is sent into atmospheric plasma spraying equipment with powder morphology, carries out air plasma spraying to matrix surface,
Prepare tri- rare earth ion tantalates thermal barrier coating of Sm-Eu-Dy.Atmospheric plasma spraying (APS) and electron beam-physical vapor
Deposition (EB-PVD) is the main method currently used for preparing thermal barrier coating.Compared with air plasma spraying, EB-PVD thermal boundary
Its deposition efficiency of coating is lower, and coating layer thickness is uncontrollable, that surface clean is complicated, the device is complicated is expensive, deposition rate is relatively low,
Process flow is cumbersome, and specimen size cannot be too big, therefore prepares high temperature using air plasma spraying mode in the present invention
Ceramic coating.
Preferably, atmospheric plasma spraying equipment is re-fed into after the tri- rare earth ion tantalates of Sm-Eu-Dy being granulated
It is sprayed；The step of granulation includes: 1) to be mixed into binder in tri- rare earth ion tantalic acid salt powder of Xiang Suoshu Sm-Eu-Dy,
Be made pureed liquid, 2) it is re-fed into spray drier and is sprayed, spherical prilling powder, the powder obtained after sieving is made
Granularity is 40~50 μm.The binder is preferably high viscosity agar solution of the viscosity in 900~1200MPaS.
Preferably, when carrying out atmospheric plasma spraying, the ionized gas that uses is Ar and He, and the flow of Ar gas
For 50~100L/min, the flow of He gas is 6~20L/min；Arc voltage be 50~80V, arc current be 500~
800A；Powder feed rate is 20~110g/min, and powder feeding angle is 60~90 °, and spray distance is 90~130mm.
Beneficial effects of the present invention are as follows:
1) the tri- rare earth ion tantalates Sm of Sm-Eu-DyaEubDycTaO7It can get than existing rare earth tantalate
RE3TaO7Better thermal property, such as better high high-temp stability (using without phase-change at 1600 DEG C), lower thermal conductivity
Coefficient (1.3~1.9W.m-1.K-1, 100~800 DEG C) and higher thermal expansion coefficient (~12.5 × 10-6K-1, 1200 DEG C), energy
Enough effectively reduce the thermal mismatching with alloy substrate.With double rare earth ion tantalates (number of patent application: CN201610597143.4)
It compares, tri- rare earth ion tantalates of Sm-Eu-Dy is defect fluorite type crystal structure in the present invention, and oxygen vacancy concentration is big, Neng Gouyou
Effect reduces thermal conductivity, and at high temperature without phase-change；And double rare earth ion tantalates are monoclinic phase (m) structure, are deposited at high temperature
In m-t phase transformation, volume change is big, and possible volume change, which generates huge internal stress, in practical applications leads to the failure etc. of coating.
2) preparation method uses liquid-phase reaction system, is sufficiently mixed three kinds of rare earth ions, and mechanical mixed using heat preservation
Conjunction and the addition of concentrated ammonia liquor, promote the abundant reaction between raw material, and obtained tri- rare earth ion tantalates of Sm-Eu-Dy is pure
The defects of degree is high, and impurity content is few, and consistency is high, and crystallite dimension is small, stomata, crackle is few, has good mechanical property.
3) the tri- rare earth ion tantalates of Sm-Eu-Dy is tested, the results show that its crystallite dimension is 1~10 μm；
At 100~800 DEG C of temperature, thermal conductivity is 1.2~1.9Wm-1·K-1, and reduced as temperature increases；In XRD spectrum, spread out
Penetrate peak by relative intensity successively decrease arrangement where angle are as follows: 29.9 ± 1 °, 49.3 ± 1 °, 58.2 ± 1 °, 34.7 ± 1 °, 79.1 ±
1 °, 61.2 ± 1 °, 71.5 ± 1 °.
5) the tri- rare earth ion tantalates of Sm-Eu-Dy has good high temperature phase stability, and greater hardness is lower
Thermal conductivity, higher thermal expansion coefficient are used as novel heat barrier coat material, have good heat insulation.
Detailed description of the invention
Fig. 1 is tri- rare earth ion tantalates SmEuDyTaO of Sm-Eu-Dy provided by embodiment 17Refractory ceramics block
X-ray diffractogram (XRD spectrum)；
Fig. 2 is tri- rare earth ion tantalates SmEuDyTaO of Sm-Eu-Dy provided by embodiment 17Refractory ceramics block
Picture in kind；
Fig. 3 is tri- rare earth ion tantalates SmEuDyTaO of Sm-Eu-Dy provided by embodiment 17Refractory ceramics block
Electron scanning micrograph (SEM)；
Fig. 4 is tri- rare earth ion tantalates SmEuDyTaO of Sm-Eu-Dy provided by embodiment 17Refractory ceramics block
Thermal conductivity and yttria-stabilized zirconia (7YSZ), samarium tantalate (Sm3TaO7) and rare earth zirconate (La2Zr2O7) comparison diagram.
Specific embodiment
1~8 the present invention is described in further detail in the following with reference to the drawings and specific embodiments.
Tri- rare earth ion tantalates of Sm-Eu-Dy provided by the present invention, chemical general formula SmaEubDycTaO7, wherein
A+b+c=3, a, b, c=0.8~1.2.In each embodiment, see Table 1 for details for the coefficient of Eu, Sm, Dy.
The preparation step of above-mentioned tri- rare earth ion tantalates of Sm-Eu-Dy is as follows:
(1) Europium chloride (EuCl is stoichiometrically weighed3), samaric nitrate (Sm (NO3)3), dysprosium nitrate (Dy (NO3)3) and grass
Sour tantalum (Ta2(C2O4)5), it is added to citric acid (C6H8O7) in, each specific additional amount of embodiment, which is shown in Table 1, (to be needed to convert when weighing
It at quality, indicates stoichiometric ratio in the present invention therefore uses mole to be measured).50min is kept the temperature at 135 DEG C to go forward side by side
The violent mechanical stirring of row mixes them thoroughly, and is added dropwise in concentrated ammonia liquor in whipping process with the speed of 1mL/min and solution is (with guarantor
Ammonium hydroxide is added dropwise until solution is neutrality in warm time consistency 50min), 30min and vigorous mechanical agitation are then kept the temperature at 180 DEG C
Promote the progress of reaction.
2) obtained solution is heated to 290 DEG C, heat preservation is dried for 7 hours.Obtained solid powder is placed in sintering
It is heated to 1000 DEG C in furnace, keeps the temperature 10 hours progress carbon removal treatments.
3) tabletting is carried out to the powder that step 2) obtains.Dwell pressure 5MPa, dwell time 2min, finally at 1690 DEG C
Sintering obtains fine and close tri- rare earth ion tantalates ceramic block of Sm-Eu-Dy for 10 hours, and photo is as shown in Figure 2, it can be seen that
Block surface pore-free, crackle, surface quality are good.
Each embodiment raw material proportioning of table 1 and test data
4) X-ray diffraction is carried out to ceramic block obtained, is as shown in Figure 1 SmEuDyTaO obtained by embodiment 17
The XRD spectrum of block, diffraction maximum is successively decreased by relative intensity arranges the angle at place are as follows: and 29.9 ± 1 °, 49.3 ± 1 °, 58.2 ±
1 °, 34.7 ± 1 °, 79.1 ± 1 °, 61.2 ± 1 °, 71.5 ± 1 °.The XRD spectrum of other embodiments is substantially the same manner as Example 1,
Only the intensity of part diffraction maximum is different.With Sm3TaO7Standard PDF card PDF Number:38-1412 be compared, in addition to compared with
Lower 15 ° of the diffraction maximum of low angle is unobvious outer, and the ceramic of compact X-ray diffraction result of tri- rare earth ion tantalates of Sm-Eu-Dy is aobvious
The diffraction maximum shown is consistent with the quantity of standard PDF card, and corresponds with it, this illustrates the crystal structure class of obtained sample
Type and standard card it is consistent, and miscellaneous phase is not present.The object of gained sample is mutually cubic phase, tri- axis of abc in crystal structure
Angle is 90 degree, and a, b, c are equal in length in crystal structure, space group Fd-3m.In addition, gained sample
All diffraction maximums all deviate to the right compared with standard card, this is because the rare earth ion Eu of doping3+、Dy3+With than Sm3+It is smaller
Ionic radius reduces the mean radius of rare earth ion, leads to the diminution of lattice constant and the shortening of atomic distance.
5) ceramic block is made to each embodiment using scanning electron microscope (SEM) to shoot, is illustrated in figure 3 reality
Apply SmEuDyTaO obtained by example 17The SEM photograph of block, it can be seen from the figure that tri- rare earth of Sm-Eu-Dy being prepared
Ion tantalates ceramic structure is fine and close, and crystal grain is tiny (1~5 μm), and flawless, which exists, only has micro stomata, and test result shows it
Consistency reaches 93%.See Table 1 for details for the average grain size range that each embodiment measures.
6) SmEuDyTaO obtained by embodiment 1 is continuously measured7(laser is anti-for thermal conductivity of the block at 100~800 DEG C
Penetrate method, LFA 457), it is as a result plotted in Fig. 4, gives the thermal barrier coating material being widely used at present in figure simultaneously as a comparison
Expect 7YSZ, Sm3TaO7And La2Zr2O7Thermal conductivity.It will be seen from figure 1 that SmEuDyTaO obtained by embodiment 17Block exists
Thermal conductivity in 100~800 DEG C of temperature is 1.3~1.9Wm-1·K-1, it is far below 7YSZ and La2Zr2O7, and heat insulation is made
For the main function of thermal barrier coating, lower thermal conductivity is exactly the performance of its most critical, it may thus be appreciated that SmEuDyTaO7Ceramics can be made
For heat barrier coat material popularization and application.See Table 1 for details for the thermal conductivity range that each embodiment measures, and smaller value is 100 DEG C of measured values, compared with
Big value is 800 DEG C of measured values.
An application examples of the tri- rare earth ion tantalates of Sm-Eu-Dy is given below.
In the application example, tri- rare earth ion tantalates of Sm-Eu-Dy is sprayed to by Ni-based conjunction using atmospheric plasma spraying
Golden steel matrix surface, the specific steps of which are as follows:
1) by preparation step 2) obtained tri- rare earth ion tantalic acid salt powder of Sm-Eu-Dy is added dissolved adhesiveness in concentration and is
It is the high viscosity agar solution of 1200MPaS when 2%, 60 DEG C nearby keep the temperature, and are stirred simultaneously, pureed liquid is made.
2) pureed liquid is carried out using the spray drier of 25000rpm, 160 DEG C of inlet temperature, 78 DEG C of outlet temperature
It is spraying, 30~60 μm of spherical prilling powder is made.
3) spherical prilling powder grinding (grinding is needed not move through when powder diameter is suitable to be sieved) is placed on 50 μm again
With 40 μm of the upper and lower sieve being disposed vertically, intermediate powder is taken, 40~50 μm of particle can be obtained.
4) it is sprayed using air plasma spraying equipment (Sluzer Metco UniCoat), spray gun type 9MB.Spray
It is 80L/min, He flow is 12L/min that apply gaseous environment, which be Ar/He:Ar flow,；Arc voltage is 80V, arc current is
500A, powder feed rate 110g/min, powder feeding angle be 90 °, spray distance 130mm.In spraying process, using recirculated water
Cooling method cools down matrix, and the flow of cooling water flow is 200L/min.It is cooled to room temperature and is applied to get to required refractory ceramics thermal boundary
Layer (1.2~1.8W.m-1.K-1)。
Claims (9)
1. a kind of tri- rare earth ion tantalates of Sm-Eu-Dy, it is characterised in that: the chemical general formula of the tantalates is
SmaEubDycTaO7, wherein a+b+c=3, a, b, c=0.8~1.2；And the crystal structure of the tantalates is defect fluorite type.
2. tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 1, it is characterised in that: a=b=c=1.
3. tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 1, it is characterised in that: tri- rare earth of Sm-Eu-Dy
Ion tantalates has the property that 1) its crystallite dimension is 1~10 μm；2) at 100~800 DEG C of temperature, thermal conductivity be 1.2~
1.9W·m-1·K-1, and reduced as temperature increases；3) in XRD spectrum, diffraction maximum is successively decreased by relative intensity arranges place
Angle are as follows: 29.9 ± 1 °, 49.3 ± 1 °, 58.2 ± 1 °, 34.7 ± 1 °, 79.1 ± 1 °, 61.2 ± 1 °, 71.5 ± 1 °.
4. a kind of preparation method of tri- rare earth ion tantalates of Sm-Eu-Dy according to any one of claims 1 to 3, special
Sign is: including the following steps:
1) Europium chloride, samaric nitrate, dysprosium nitrate and tantalum oxalate are stoichiometrically weighed, and with the citric acid of set amount in heat preservation strip
It carries out mechanical mixture under part, is added in mixed process in concentrated ammonia liquor and solution, then carry out mechanical mixture promotion under heat-retaining condition
Complex reaction,
2) acquired solution is dried, then calcining removes carbon impurity to get tri- rare earth ion tantalum of Sm-Eu-Dy at high temperature
Hydrochlorate,
In step 1), when first time mechanical mixture, temperature is 120~160 DEG C, 40~60min of time；Second of mechanical mixture
When, temperature is 170~190 DEG C, 30~50min of time；In step 2), drying temperature is 250~300 DEG C, drying time 6~
10h；Calcination temperature is 700~1000 DEG C, 6~10h of calcination time.
5. the preparation method of tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 4, it is characterised in that: step 1)
In, the sum of the amount of substance of three kinds of rare earth elements: tantalum oxalate: citric acid=6: 1: 8.
6. a kind of tri- rare earth ion tantalates of Sm-Eu-Dy according to any one of claims 1 to 3 is as thermal barrier coating material
The application of material.
7. application of the tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 6 as heat barrier coat material, special
Sign is: the tri- rare earth ion tantalates of Sm-Eu-Dy being sent into atmospheric plasma spraying equipment with powder morphology, to base
Body surface face carries out air plasma spraying, prepares high-temperature ceramic coating.
8. application of the tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 7 as heat barrier coat material, special
Sign is: being re-fed into atmospheric plasma spraying equipment after the tri- rare earth ion tantalates of Sm-Eu-Dy is granulated and sprays
It applies；The step of granulation includes: 1) to be mixed into binder in tri- rare earth ion tantalic acid salt powder of Xiang Suoshu Sm-Eu-Dy, and mud is made
Shape liquid, 2) it is re-fed into spray drier and is sprayed, spherical prilling powder is made, the powder size obtained after sieving is
40~50 μm.
9. application of the tri- rare earth ion tantalates of Sm-Eu-Dy according to claim 7 or 8 as heat barrier coat material,
Be characterized in that: when carrying out atmospheric plasma spraying, the ionized gas that uses is Ar and He, and the flow of Ar gas be 50~
The flow of 100L/min, He gas is 6~20L/min；Arc voltage is 50~80V, and arc current is 500~800A；Powder feeding
Speed is 20~110g/min, and powder feeding angle is 60~90 °, and spray distance is 90~130mm.
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Address after: 710000 building B5, No. 175, Biyuan Second Road, Xiliu Street office, Xi'an high tech Zone, Shaanxi Province Patentee after: Shaanxi Tianxuan Coating Technology Co., Ltd Address before: 650000 No. 9218-1, building B, building B, Science Park, Kunming University of Science and Technology, Kunming, Kunming, Yunnan Patentee before: KUNMING GONGJIANG COATING TECHNOLOGY Co.,Ltd. |