CN109369175A - A method of zirconic acid lanthanum powder is prepared by raw material of zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder - Google Patents
A method of zirconic acid lanthanum powder is prepared by raw material of zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder Download PDFInfo
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Abstract
The present invention provides a kind of method for preparing zirconic acid lanthanum powder as raw material using zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder, step includes: to prepare zirconic acid lanthanum precursor powder；The CeO for accounting for zirconic acid lanthanum precursor powder quality 8wt% is separately added into zirconic acid lanthanum precursor powder2Powder and DyO2Powder；By zirconic acid lanthanum precursor powder, CeO2Powder and DyO2The mixed-powder of powder is added in the ball grinder of high temperature energy ball grinder；Mill ball is added into mixed-powder according to ratio of grinding media to material 15:1-30:1, seals ball grinder；Ball grinder is put into high temperature energy ball grinder burner hearth, burner hearth is warming up to 500 DEG C, keeps the temperature 2h；By burner hearth vacuumize process and it is passed through argon atmosphere protection, starts ball mill, and ball mill temperature is raised to 650 DEG C -800 DEG C, keeps the temperature 12-48h；It closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, even-grained ultra-fine zirconic acid lanthanum powder can be obtained.A kind of method preparing zirconic acid lanthanum powder as raw material using zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder provided by the invention, simple process, low energy consumption, obtained zirconic acid lanthanum powder is uniformly mixed.
Description
Technical field
The present invention relates to heat barrier coat material technical fields, in particular to one kind is with zirconic acid lanthanum precursor powder, cerium oxide
Powder and dysprosia powder are the method that raw material prepares zirconic acid lanthanum powder.
Background technique
With the continuous development of aeronautical technology and to flying speed, the demands such as flying distance and security performance are constantly mentioned
It rises, protects aero-engine hot-end component from the ablation, corrosion and oxidation of high-temperature fuel gas, improve its service life, become and work as
The emphasis of preceding research.Current most widely used thermal barrier coating (Thermal barrier coating, TBC) material is Y2O3Portion
Divide and stablizes ZrO2(YSZ), but when temperature is more than 1200 DEG C, YSZ is easy to happen phase transformation and sintering, leads to coating failure.And
Zirconic acid lanthanum (La2Zr2O7, LZ) at high temperature have very high crystal structural stability, when temperature its fusing point (2300 DEG C) below
Shi Buhui is undergone phase transition, and has lower sintering rate and thermal conductivity, is a kind of one of very promising high temperature TBC material.
Thermal expansion coefficient is the primary foundation for selecting thermal barrier coating ceramic material close to metallic matrix, and the thermal expansion system of LZ
Number is 8.91-9.1 × 10–6/ K, it is lower than YSZ material, this be restrict LZ be used in Ni based high-temperature alloy surface it is main because
Element, but the thermal expansion coefficient of LZ can be significantly increased by modification by ion-doping.
Industrially preparing zirconic acid lanthanum with more method at present is high temperature solid phase synthesis, and this method is with ZrO2And La2O3
For raw material, by ZrO2And La2O3Powder is placed is dried 1h at 1000 DEG C in phase batch-type furnace, remove ZrO2And La2O3Powder
The H of middle absorption2O and CO2, the ZrO after drying is then weighed by the ratio between amount of substance 2: 12And La2O3Powder adds in ball grinder
Enter twice of mixed-powder gross mass of ZrO2Mill ball adds twice of mixed-powder gross mass of ultrapure water in ball grinder,
Mixing ball milling 48h together.It is dried after the complete slurry of ball milling is crossed 200 mesh sieve again, finally takes mixture to be put into crucible and be placed in
In batch-type furnace, synthesized in 1200 DEG C -1600 DEG C of temperature lower calcinations, and soaking time 12h.This method needs when synthesizing zirconic acid lanthanum
Synthesis is calcined at a high temperature of 1200-1600 DEG C, not only production procedure is complicated, but also energy consumption is high, and it is at high cost, and this method obtains
The microcosmic mixing of powder it is uneven, have component segregation, microstructure uneven and reunite the problems such as serious.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of simple process, low energy consumption, obtained powder is uniformly mixed
The method that zirconic acid lanthanum powder is prepared as raw material using zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder.
In order to solve the above technical problems, the present invention provides one kind with zirconic acid lanthanum precursor powder, ceria oxide powder and oxygen
Changing dysprosium powder is the method that raw material prepares zirconic acid lanthanum powder, is included the following steps:
Prepare zirconic acid lanthanum precursor powder；
The CeO for accounting for zirconic acid lanthanum precursor powder quality 8wt% is separately added into zirconic acid lanthanum precursor powder2Powder and
DyO2Powder；
By zirconic acid lanthanum precursor powder, CeO2Powder and DyO2The mixed-powder of powder is added to the ball of high temperature energy ball grinder
In grinding jar；
According to ratio of grinding media to material 15:1-30:1 to zirconic acid lanthanum precursor powder, CeO2Powder and DyO2Add in the mixed-powder of powder
Enter mill ball, seals ball grinder；
Ball grinder is put into high temperature energy ball grinder burner hearth, burner hearth is warming up to 500 DEG C, keeps the temperature 2h；
By burner hearth vacuumize process and it is passed through argon atmosphere protection, starts ball mill, and ball mill temperature is raised to 650
DEG C -800 DEG C, keep the temperature 12-48h；
It closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, even-grained ultra-fine zirconic acid lanthanum powder can be obtained.
Further, the preparation method of the zirconic acid lanthanum precursor powder includes the following steps:
By La2O3It is dissolved in hydrochloric acid and matches to obtain La3+Concentration is the La of 0.5mol/L3+Solution, ZrOCl2·8H2O is dissolved in water and matches
Zr4+Concentration is the Zr of 0.5mol/L4+Solution；
By La3+Solution and Zr4+Solution mixing generates precipitating to mixed solution and dripping ammonium hydroxide, then solid-liquid system exists
Heating stirring under 60 DEG C of bath temperature, and it is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant；
After heating stirring 25-40min, solid-liquid system is filtered, by washing of precipitate, until the pH=7 of cleaning solution；
11-13h will be dried at a temperature of 110-130 DEG C being deposited in, and then be ground, 200 mesh sieve excessively obtain zirconic acid lanthanum forerunner
Body powder.
One kind provided by the invention prepares zirconium using zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder as raw material
The method of sour lanthanum powder, the method carried out simultaneously in same high temperature reaction stove using heating and calcining and ball milling, due to ball milling ring
Border temperature is high, and zirconic acid lanthanum precursor powder can obtain enough energy in the short period, decomposes simultaneously aggregation, and ball milling rapidly
Strength and system external heating and meanwhile carry out, promote absorption of the zirconic acid lanthanum granular precursor to energy, reactant can be made
The temperature of system is rapidly achieved and is more than the critical-temperature for synthesizing zirconic acid lanthanum, accelerates the reaction rate of system, in a short time may be used
The tiny zirconic acid lanthanum powder of granularity is obtained, operating procedure is not only simplified, saves the reaction time, and also reduces energy damage
Consumption, has saved cost.Also, ball milling appropriate has refined crystal grain, has increased specific surface area, so as to improve dynamic conditions,
So that conventional high temperature solid phase synthesis just will do it to obtain more complete reaction under 1200-1600 DEG C of hot conditions, 650
It can be realized as under DEG C -800 DEG C of lower temperature, compared with the high temperature solid phase synthesis used in the routine, temperature reduces 450
DEG C -850 DEG C, so that further reduced energy consumption has saved cost.Due to the presence of ball milling, reduce the generation of agglomeration,
So that powder further refines and disperse more uniform, so that reactants and products is continuously available refinement, obtains good dispersion,
Microcosmic to be uniformly mixed, grain size is big, and partial size is small, the zirconic acid lanthanum powder of the uniform soilless sticking phenomenon of microstructure.Meanwhile the present invention
The thermal expansion coefficient of zirconic acid lanthanum powder obtained is higher, with Y2O3Partially stabilized ZrO2The thermal expansion coefficient very phase of material (YSZ)
Closely, i.e., the similar thermal expansion coefficient with Ni based high-temperature alloy material is suitable for use in Ni based high-temperature alloy surface.
Detailed description of the invention
It with zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder is former that Fig. 1, which is provided in an embodiment of the present invention,
Material prepares the method flow diagram of zirconic acid lanthanum powder；
It with zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder is former that Fig. 2, which is provided in an embodiment of the present invention,
Material prepares the X ray diffracting spectrum of zirconic acid lanthanum powder made from the method for zirconic acid lanthanum powder；
It with zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder is former that Fig. 3, which is provided in an embodiment of the present invention,
Material prepares the granularity graph of zirconic acid lanthanum powder made from the method for zirconic acid lanthanum powder.
Specific embodiment
Referring to Fig. 1, one kind provided in an embodiment of the present invention is with zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder
End is the method that raw material prepares zirconic acid lanthanum powder, is included the following steps:
Step 1 prepares zirconic acid lanthanum precursor powder: by La2O3It is dissolved in hydrochloric acid and matches to obtain La3+Concentration is the La of 0.5mol/L3+It is molten
Liquid, ZrOCl2·8H2O is dissolved in water and matches to obtain Zr4+Concentration is the Zr of 0.5mol/L4+Solution；Then by La3+Solution and Zr4+Solution is mixed
Merging be stirred in constant temperature blender with magnetic force, precipitating reagent such as ammonium hydroxide is added dropwise into mixed solution, immediately generate white,
Lilac or light yellow flocculent deposit, then the heating stirring under 60 DEG C of bath temperature of the solid-liquid system after precipitating will be generated, and
It is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant；After 25-40min, to solid-liquid system filter, will precipitating constantly with distilled water repeatedly
Washing, until the pH=7 of cleaning solution；Finally obtained precipitated filter cakes are fitted into culture dish dry at a temperature of 110-130 DEG C
11-13h, then grind, cross 200 mesh sieve zirconic acid lanthanum precursor powder can be obtained.The chemical reaction occurred during this is as follows:
Step 2 is separately added into the CeO for accounting for zirconic acid lanthanum precursor powder quality 8wt% into zirconic acid lanthanum precursor powder2
Powder and DyO2Powder；
Step 3 is by zirconic acid lanthanum precursor powder, CeO2Powder and DyO2The mixed-powder of powder is added to high temperature energy ball grinder
Ball grinder in；
Step 4 is according to ratio of grinding media to material 15:1-30:1 to zirconic acid lanthanum precursor powder, CeO2Powder and DyO2The mixed powder of powder
Stainless steel or zirconium oxide abrasive ball are added in end, closes the lid, and seal ball grinder；
Ball grinder is put into high temperature energy ball grinder burner hearth by step 5, and burner hearth is warming up to 500 DEG C, keeps the temperature 2h；
Step 6 is by burner hearth vacuumize process and is passed through argon atmosphere protection, starts ball mill, adjusts drum's speed of rotation, and
Ball mill temperature is raised to 650 DEG C -800 DEG C simultaneously, keeps the temperature 12-48h；
Step 7 closes ball mill and waits for that burner hearth is cooled to room temperature, and takes out ball grinder, even-grained ultra-fine zirconic acid lanthanum can be obtained
Powder.
Referring to figs. 2 and 3, provided in an embodiment of the present invention with zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia
Powder is the raw material method for preparing zirconic acid lanthanum powder, zirconic acid lanthanum powder obtained not only good dispersion, microcosmic to be uniformly mixed, crystal grain
Degree is big, and partial size is small, the uniform soilless sticking phenomenon of microstructure, and the thermal expansion coefficient of zirconic acid lanthanum powder obtained is higher, with
Y2O3Partially stabilized ZrO2The thermal expansion coefficient of material (YSZ) is very close, is suitable for use in Ni based high-temperature alloy material surface.Together
When, ultra-fine La produced by the present invention2Zr2O7In powder, Ce is dissolved into zirconic acid lanthanum lattice substitution Zr atom site, and Dy and
The doping of Ce will not change the crystal structure of zirconic acid lanthanum in a certain range.
Below by specific embodiment to one kind provided by the invention with zirconic acid lanthanum precursor powder, ceria oxide powder and oxygen
Changing dysprosium powder is that the method that raw material prepares zirconic acid lanthanum powder illustrates.
Embodiment 1
Ultra-fine La2Zr2O7The preparation process of powder, includes the following steps:
(1) by La2O3It is dissolved in hydrochloric acid, ZrOCl2·8H2O is dissolved in water, is configured to cationic La respectively3+And Zr4+Concentration is
The solution of 0.5mol/L, is mixed in constant temperature blender with magnetic force, and ammonium hydroxide reaction is added dropwise into mixed liquor and generates cotton-shaped sink
It forms sediment, is stirred continuously after bath temperature is then adjusted to 60 DEG C, while it is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant.Lasting stirring
It after 30min, filters, washs precipitating repeatedly with distilled water, until the pH=7 of cleaning solution, will finally filter obtained filter cake and be packed into
In 120 DEG C of dry 12h in culture dish, zirconic acid lanthanum precursor powder is can be obtained in ground 200 mesh.
(2) 100g zirconic acid lanthanum precursor powder is uniformly mixed to be used as with 8g ceria oxide powder and 8g dysprosia powder and is reacted
Object；
(3) it puts the powder into stainless steel jar mill, stainless steel steel ball, ratio of grinding media to material 15:1 is added；
(4) ball grinder is put into high temperature energy ball grinder；
(5) ball mill is warming up to 500 DEG C, keeps the temperature 2h；
(6) using ball mill vacuumize process and argon gas is passed through as protective gas；
(7) start ball mill, it is lasting to rotate, while burner hearth is warming up to 800 DEG C, keep the temperature 12h；
(8) it closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, obtain even-grained zirconic acid lanthanum powder.
Embodiment 2
Ultra-fine La2Zr2O7The preparation process of powder, includes the following steps:
(1) by La2O3It is dissolved in hydrochloric acid, ZrOCl2·8H2O is dissolved in water, is configured to cationic La respectively3+And Zr4+Concentration is
The solution of 0.5mol/L, is mixed in constant temperature blender with magnetic force, and ammonium hydroxide reaction is added dropwise into mixed liquor and generates cotton-shaped sink
It forms sediment, is stirred continuously after bath temperature is then adjusted to 60 DEG C, while it is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant.Lasting stirring
It after 25min, filters, washs precipitating repeatedly with distilled water, until the pH=7 of cleaning solution, will finally filter obtained filter cake and be packed into
In 110 DEG C of dry 13h in culture dish, zirconic acid lanthanum precursor powder is can be obtained in ground 200 mesh.
(2) 100g zirconic acid lanthanum precursor powder is uniformly mixed to be used as with 8g ceria oxide powder and 8g dysprosia powder and is reacted
Object；
(3) it puts the powder into stainless steel jar mill, zirconia ball, ratio of grinding media to material 25:1 is added；
(4) ball grinder is put into high temperature energy ball grinder；
(5) ball mill is warming up to 500 DEG C, keeps the temperature 2h；
(6) using ball mill vacuumize process and argon gas is passed through as protective gas；
(7) start ball mill, it is lasting to rotate, while burner hearth is warming up to 750 DEG C, heat preservation is for 24 hours；
(8) it closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, obtain even-grained zirconic acid lanthanum powder.
Embodiment 3
Ultra-fine La2Zr2O7The preparation process of powder, includes the following steps:
(1) by La2O3It is dissolved in hydrochloric acid, ZrOCl2·8H2O is dissolved in water, is configured to cationic La respectively3+And Zr4+Concentration is
The solution of 0.5mol/L, is mixed in constant temperature blender with magnetic force, and ammonium hydroxide reaction is added dropwise into mixed liquor and generates cotton-shaped sink
It forms sediment, is stirred continuously after bath temperature is then adjusted to 60 DEG C, while it is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant.Lasting stirring
It after 40min, filters, washs precipitating repeatedly with distilled water, until the pH=7 of cleaning solution, will finally filter obtained filter cake and be packed into
In 130 DEG C of dry 11h in culture dish, zirconic acid lanthanum precursor powder is can be obtained in ground 200 mesh.
(2) 100g zirconic acid lanthanum precursor powder is uniformly mixed to be used as with 8g ceria oxide powder and 8g dysprosia powder and is reacted
Object；
(3) it puts the powder into stainless steel jar mill, stainless steel steel ball, ratio of grinding media to material 30:1 is added；
(4) ball grinder is put into high temperature energy ball grinder；
(5) ball mill is warming up to 500 DEG C, keeps the temperature 2h；
(6) using ball mill vacuumize process and argon gas is passed through as protective gas；
(7) start ball mill, it is lasting to rotate, while burner hearth is warming up to 650 DEG C, keep the temperature 48h；
(8) it closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, obtain even-grained zirconic acid lanthanum powder.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it,
Although being described the invention in detail referring to example, those skilled in the art should understand that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention, should all cover
In the scope of the claims of the present invention.
Claims (2)
1. a kind of side for preparing zirconic acid lanthanum powder using zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder as raw material
Method, which comprises the steps of:
Prepare zirconic acid lanthanum precursor powder；
The CeO for accounting for zirconic acid lanthanum precursor powder quality 8wt% is separately added into zirconic acid lanthanum precursor powder2Powder and DyO2
Powder；
By zirconic acid lanthanum precursor powder, CeO2Powder and DyO2The mixed-powder of powder is added to the ball grinder of high temperature energy ball grinder
In；
According to ratio of grinding media to material 15:1-30:1 to zirconic acid lanthanum precursor powder, CeO2Powder and DyO2It is added and grinds in the mixed-powder of powder
Abrading-ball seals ball grinder；
Ball grinder is put into high temperature energy ball grinder burner hearth, burner hearth is warming up to 500 DEG C, keeps the temperature 2h；
By burner hearth vacuumize process and it is passed through argon atmosphere protection, starts ball mill, and ball mill temperature is raised to 650 DEG C -800
DEG C, keep the temperature 12-48h；
It closes ball mill and waits for that burner hearth is cooled to room temperature, take out ball grinder, even-grained ultra-fine zirconic acid lanthanum powder can be obtained.
2. according to claim 1 prepare by raw material of zirconic acid lanthanum precursor powder, ceria oxide powder and dysprosia powder
The method of zirconic acid lanthanum powder, it is characterised in that: the preparation method of the zirconic acid lanthanum precursor powder includes the following steps:
By La2O3It is dissolved in hydrochloric acid and matches to obtain La3+Concentration is the La of 0.5mol/L3+Solution, ZrOCl2·8H2O is dissolved in water and matches to obtain Zr4+It is dense
Degree is the Zr of 0.5mol/L4+Solution；
By La3+Solution and Zr4+Solution mixing generates precipitating to mixed solution and dripping ammonium hydroxide, then by solid-liquid system at 60 DEG C
Bath temperature under heating stirring, and it is 10 that ammonium hydroxide, which is added dropwise, to keep the pH value of system constant；
After heating stirring 25-40min, solid-liquid system is filtered, by washing of precipitate, until the pH=7 of cleaning solution；
11-13h will be dried at a temperature of 110-130 DEG C being deposited in, and then be ground, 200 mesh sieve excessively obtain zirconic acid lanthanum precursor
End.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811185242.7A CN109369175B (en) | 2018-10-11 | 2018-10-11 | Method for preparing lanthanum zirconate powder by taking lanthanum zirconate precursor powder, cerium oxide powder and dysprosium oxide powder as raw materials |
Applications Claiming Priority (1)
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| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
| CN101200375A (en) * | 2007-11-16 | 2008-06-18 | 北京矿冶研究总院 | Preparation method of nano zirconium-containing series thermal barrier coating material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
| CN101200375A (en) * | 2007-11-16 | 2008-06-18 | 北京矿冶研究总院 | Preparation method of nano zirconium-containing series thermal barrier coating material |
Non-Patent Citations (3)
| Title |
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| HONGFEI CHEN ET AL.: "Coprecipitation synthesis and thermal conductivity of La2Zr2O7", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 周宏明等: "稀土Dy和Ce共掺杂La2Zr2O7新型热障涂层用陶瓷材料", 《无机材料学报》 * |
| 祁康成等: "《发光原理与发光材料》", 29 February 2012, 电子科技大学出版社 * |
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