CN109133167A - A method of zirconic acid lanthanum powder is prepared using high-temperature machinery force chemistry - Google Patents
A method of zirconic acid lanthanum powder is prepared using high-temperature machinery force chemistry Download PDFInfo
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Abstract
The present invention provides a kind of method for preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry, step includes: to prepare zirconic acid lanthanum precursor powder；Zirconic acid lanthanum precursor powder is added in the ball grinder of high temperature energy ball grinder；Mill ball is added into zirconic acid lanthanum precursor 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 using high-temperature machinery force chemistry provided by the invention, simple process, low energy consumption, obtained powder is uniformly mixed.
Description
Technical field
The present invention relates to heat barrier coat material technical fields, in particular to a kind of to prepare zirconium using high-temperature machinery force chemistry
The method of sour 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 for preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry.
In order to solve the above technical problems, preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry the present invention provides a kind of
Method, include the following steps:
Prepare zirconic acid lanthanum precursor powder；
Zirconic acid lanthanum precursor powder is added in the ball grinder of high temperature energy ball grinder；
Mill ball is added into zirconic acid lanthanum precursor 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, 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.
A kind of method preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry provided by the invention, using heating and calcining
The method carried out simultaneously in same high temperature reaction stove with ball milling, since milling atmosphere temperature is high, in the short period before zirconic acid lanthanum
Enough energy can be obtained by driving body powder, decompose simultaneously aggregation rapidly, and the external heating of the strength of ball milling and system is simultaneously
It carries out, promotes absorption of the zirconic acid lanthanum granular precursor to energy, the temperature of reaction system can be made to be rapidly achieved and be more than synthesis
The critical-temperature of zirconic acid lanthanum accelerates the reaction rate of system, can get the tiny zirconic acid lanthanum powder of granularity in a short time, no
Operating procedure is only simplified, the reaction time is saved, and also reduce energy loss, has saved cost.Also, ball appropriate
It is levigate to have changed crystal grain, increased specific surface area, so as to improve dynamic conditions, so that conventional high temperature solid phase synthesis exists
It just will do it to obtain more complete reaction under 1200-1600 DEG C of hot conditions, it can under 650 DEG C -800 DEG C of lower temperature
It realizes, compared with the high temperature solid phase synthesis used in the routine, temperature reduces 450 DEG C -850 DEG C, to 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
Add uniformly, reactants and products is made to be continuously available refinement, obtains good dispersion, microcosmic to be uniformly mixed, grain size is big, partial size
It is small, the zirconic acid lanthanum powder of the uniform soilless sticking phenomenon of microstructure.Meanwhile the thermal expansion system of zirconic acid lanthanum powder produced by the present invention
Number is higher, with Y2O3Partially stabilized ZrO2The thermal expansion coefficient of material (YSZ) is very close, i.e., with Ni based high-temperature alloy material
Similar thermal expansion coefficient is suitable for use in Ni based high-temperature alloy surface.
Detailed description of the invention
Fig. 1 is the method flow provided in an embodiment of the present invention that zirconic acid lanthanum powder is prepared using high-temperature machinery force chemistry
Figure；
Fig. 2 is prepared made from the method for zirconic acid lanthanum powder to be provided in an embodiment of the present invention using high-temperature machinery force chemistry
The X ray diffracting spectrum of zirconic acid lanthanum powder；
Fig. 3 is prepared made from the method for zirconic acid lanthanum powder to be provided in an embodiment of the present invention using high-temperature machinery force chemistry
The granularity graph of zirconic acid lanthanum powder.
Specific embodiment
Referring to Fig. 1, a kind of side preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry provided in an embodiment of the present invention
Method includes 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:
Zr4+(aq)+4OH-=Zr (OH)4(s)。
Zirconic acid lanthanum precursor powder is added in the ball grinder of high temperature energy ball grinder by step 2；
Stainless steel or zirconium oxide abrasive ball are added into zirconic acid lanthanum precursor powder according to ratio of grinding media to material 15:1-30:1 for step 3,
It closes the lid, and seals ball grinder；
Ball grinder is put into high temperature energy ball grinder burner hearth by step 4, and burner hearth is warming up to 500 DEG C, keeps the temperature 2h；
Step 5 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 6 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, the side provided in an embodiment of the present invention that zirconic acid lanthanum powder is prepared using high-temperature machinery force chemistry
Method, zirconic acid lanthanum powder obtained not only good dispersion, microcosmic to be uniformly mixed, grain size is big, and partial size is small, the uniform nothing of microstructure
Agglomeration, and the thermal expansion coefficient of zirconic acid lanthanum powder obtained is higher, with Y2O3Partially stabilized ZrO2The heat of material (YSZ)
The coefficient of expansion is very close, is suitable for use in Ni based high-temperature alloy material surface.
Below by specific embodiment a kind of zirconic acid lanthanum powder is prepared using high-temperature machinery force chemistry to provided by the invention
The method at end 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) take 100g zirconic acid lanthanum precursor powder as reactant；
(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) take 100g zirconic acid lanthanum precursor powder as reactant；
(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) take 100g zirconic acid lanthanum precursor powder as reactant；
(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 method for preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry, which comprises the steps of:
Prepare zirconic acid lanthanum precursor powder；
Zirconic acid lanthanum precursor powder is added in the ball grinder of high temperature energy ball grinder；
Mill ball is added into zirconic acid lanthanum precursor 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, 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. the method according to claim 1 for preparing zirconic acid lanthanum powder using high-temperature machinery force chemistry, 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.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115536062A (en) * | 2022-11-02 | 2022-12-30 | 中国科学院过程工程研究所 | Solid-phase synthesis method of lanthanum zirconate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003024A (en) * | 2006-09-19 | 2007-07-25 | 东北大学 | High temperature energy ball grinder |
Non-Patent Citations (1)
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| HONGFEI CHEN ET AL.: ""Coprecipitation synthesis and thermal conductivity of La2Zr2O7"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115536062A (en) * | 2022-11-02 | 2022-12-30 | 中国科学院过程工程研究所 | Solid-phase synthesis method of lanthanum zirconate |
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Application publication date: 20190104 |