CN103964486B - Control the method that yttrium carbonate precipitation digestion time prepares needle-like yttrium oxide - Google Patents
Control the method that yttrium carbonate precipitation digestion time prepares needle-like yttrium oxide Download PDFInfo
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Abstract
The present invention relates to a kind of method controlling yttrium carbonate precipitation digestion time and prepare needle-like yttrium oxide, belong to a kind of material preparation process.The present invention is with YCl
3feed liquid, as feed liquid, is heated to 93 DEG C by solution, adds precipitation agent ammonium bicarbonate soln, and at room temperature, by yttrium carbonate precipitation and the common still aging 0-28 hour of mother liquor, calcination at 1100 DEG C, obtains yttrium oxide powder; Digestion time is 0-18 hour, and yttrium oxide pattern is random granulometric composition; Digestion time is 24 hours, and the yttrium oxide pattern of preparation is single needle-like crystal particle and forms almost spherical particle by needle-like crystal; Digestion time is 28 hours, and the yttrium oxide pattern of preparation forms spheroidal particle by needle-like crystal; Digestion time is 18-24 hour, yttrium oxide pattern by random particle to the complete conversion process of needle-like crystal.
Description
Technical field
The present invention relates to a kind of method controlling yttrium carbonate precipitation digestion time and prepare needle-like yttrium oxide, belong to a kind of material preparation process.
Background technology
Yttrium oxide (Y
2o
3) be a kind of important rare earth compound, there is unique thermotolerance, erosion resistance, high-temperature stability, high-k and a series of excellent optical property, be widely used in the fields such as advanced ceramic, photoelectronics, catalyzer and functional composite material efficient additive.
Along with the development of science and technology, constantly particular requirement is proposed to yttrium oxide pattern, yttrium oxide pattern is different also different to its range of application, and yttrium oxide pattern major influence factors is the many factors such as precipitation agent, ageing process, feed concentration, feed acidity, precipitation endpoint pH, precipitation temperature.The water heat transfer different-shape nano yttrium oxide powder that document face rainbow cloud is shown, material heat treatment technology, 2010,39 (20): 66-69, provide with Y (NO
3)
3as feed liquid, allocate initial material liquid pH value by saturated NaOH solution, react under hydrothermal method condition, obtain yttrium oxide through filtration, washing, calcination, the pH value of starting soln is to presoma and Y
2o
3morphology microstructure has significant impact, and along with the increase of initial soln pH value, the pattern of presoma changes club shaped structure into by hexagonal sheet structure, and pH value increases further, and the nanometer rod of generation is thicker and be easy to reunite together.The carbonate precipitation method that document news thunder is shown prepares Y
2o
3nano powder and crystalline ceramics, China YouSe Acta Metallurgica Sinica, 2006,16 (2): 235-240, provide with 0.5 mol/L Y (NO
3)
3as feed liquid, bicarbonate of ammonia, as precipitation agent, precipitates after terminating, continue stirring 2 days, precipitation, through filtering, washing, obtains needle-like yttrium oxide crystal 700 DEG C of calcinations, 900 DEG C of calcinations obtain spherical yttrium oxide crystal, obtain soilless sticking yttria particles 1100 DEG C of calcinations.Shown the suddenly preparation technology of document on the impact of Ultrafine Yttrium Oxides Powders form and coking property, China rare earth journal, 2007,25 (5): 566-572, provide with Y (NO
3)
3as feed liquid, bicarbonate of ammonia is as precipitation agent, at precipitation temperature 15 DEG C, precipitin reaction endpoint pH is respectively 7.0,7.8,8.3, at pH=7.0, in the aged solution environment of 7.8, along with the increase of digestion time, powder granule is evenly grown up gradually and is calcined rear superfine powder almost spherical, ageing in pH=8.3 solution, along with the time increases, powder granule is grown up obviously and is irregularly shaped.
Summary of the invention
The object of the present invention is to provide a kind of method controlling yttrium carbonate precipitation digestion time and prepare needle-like yttrium oxide, the method is after yttrium carbonate precipitation, in still aging process, the yttrium oxide pattern prepared is converted into the digestion time needed for elongated piece by random particle, reduces the yttrium carbonate precipitation production cycle.
Technical solution:
The present invention take concentration as the YCl of 0.35 mol/L
3solution is as feed liquid, feed liquid is heated to 93 DEG C, adding concentration is 2 mol/L ammonium bicarbonate solns, Yttrium trichloride and bicarbonate of ammonia mol ratio are 1:2.3, at room temperature, by yttrium carbonate precipitation and the common still aging 0-28 hour of mother liquor, through filtering, washing, calcination at 1100 DEG C, obtain yttrium oxide powder, digestion time is 0-18 hour, yttrium oxide pattern is small-particle or large coacervate is all by the many small-particles of bar-shaped upper growth, sheet and random granulometric composition, digestion time is 24-28 hour, the yttrium oxide pattern obtained is single needle-like crystal particle and forms spheroidal particle by needle-like crystal, digestion time is 18-24 hour, yttrium oxide pattern by random particle to the complete conversion process of needle-like crystal.
Optimal selection yttrium carbonate precipitation digestion time of the present invention is 28 hours, and the yttrium oxide pattern of preparation forms spheroidal particle by needle-like crystal.
Invention effect
In the present invention, yttrium carbonate precipitates still aging Time dependent and prepares the key factor that yttrium oxide pattern is needle-like crystal; Digestion time is 24 hours, and the yttrium oxide pattern of preparation is single needle-like crystal particle and forms almost spherical particle by needle-like crystal; Digestion time is 28 hours, and the yttrium oxide pattern of preparation forms spheroidal particle by needle-like crystal; Digestion time extends again, and the depositing technology cycle is oversize, is unfavorable for suitability for industrialized production; As digestion time reaches 60 hours, the yttria particles of preparation is even, and pattern is reunited by multiple needle-like crystal and formed brachyplast strip together and adhere to many small-particles; Digestion time is 24-28 hour is the Best Times preparing needle-like crystal yttria particles, is convenient to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 yttrium oxide SEM schemes;
Fig. 2 is that the embodiment of the present invention 2 yttrium oxide SEM schemes;
Fig. 3 is that the embodiment of the present invention 3 yttrium oxide SEM schemes;
Fig. 4 is that the embodiment of the present invention 4 yttrium oxide SEM schemes.
Embodiment
embodiment 1
The YCl that 2000 L concentration are 0.35 mol/L is added in setting tank
3solution; solution is heated to 93 DEG C; adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, then stirs 30 minutes, stops stirring; at room temperature; yttrium carbonate precipitation was through still aging 6 hours, and yttrium carbonate precipitation is through filtering, washing, calcination at 1100 DEG C; obtaining yttrium oxide pattern is small-particle and large spherical agglomerates granulometric composition, is that small-particle or large coacervate are all by the many small-particles of bar-shaped upper growth, sheet and random granulometric composition.
embodiment 2
The YCl that 2000 L concentration are 0.35 mol/L is added in setting tank
3solution; solution is heated to 93 DEG C; adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, then stirs 30 minutes, stops stirring; at room temperature; yttrium carbonate precipitation was through still aging 18 hours, and yttrium carbonate precipitation is through filtering, washing, calcination at 1100 DEG C; obtaining yttrium oxide pattern is small-particle and large agglomerate particle composition, is that small-particle or large coacervate are all by bar-shaped, sheet and random granulometric composition.
embodiment 3
The YCl that 2000 L concentration are 0.35 mol/L is added in setting tank
3solution, solution is heated to 93 DEG C, adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, stir 30 minutes again, stop stirring, at room temperature, yttrium carbonate precipitation was through still aging 24 hours, yttrium carbonate precipitation is through filtering, washing, and calcination at 1100 DEG C, the yttrium oxide pattern obtained is single needle-like crystal particle and forms almost spherical particle by needle-like crystal.
embodiment 4
The YCl that 2000 L concentration are 0.35 mol/L is added in setting tank
3solution, solution is heated to 93 DEG C, adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, stir 30 minutes again, stop stirring, at room temperature, yttrium carbonate precipitation was through still aging 28 hours, yttrium carbonate precipitation is through filtering, washing, and calcination at 1100 DEG C, the yttrium oxide pattern of preparation forms spheroidal particle by needle-like crystal.
Claims (2)
1. control the method that yttrium carbonate precipitation digestion time prepares needle-like yttrium oxide, it is characterized in that, take concentration as the YCl of 0.35 mol/L
3solution is as feed liquid, feed liquid is heated to 93 DEG C, adding concentration is 2 mol/L ammonium bicarbonate solns, Yttrium trichloride and bicarbonate of ammonia mol ratio are 1:2.3, at room temperature, by yttrium carbonate precipitation and the common still aging 24-28 hour of mother liquor, through filtering, washing, calcination at 1100 DEG C, to obtain yttrium oxide pattern be single needle-like crystal particle and form spheroidal particle by needle-like crystal.
2. control yttrium carbonate precipitation digestion time according to claim 1 prepares the method for needle-like yttrium oxide, it is characterized in that, optimal selection yttrium carbonate precipitation digestion time is 28 hours, and the yttrium oxide pattern of preparation forms spheroidal particle by needle-like crystal.
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| CN108946788A (en) * | 2018-09-03 | 2018-12-07 | 吴秀碧 | A kind of preparation method of needle-shaped yttrium oxide |
| CN109468684B (en) * | 2018-12-27 | 2020-12-01 | 东北大学 | Preparation method of yttrium oxide nano-beam whisker |
| CN109467434B (en) * | 2018-12-27 | 2022-04-12 | 东北大学 | High-fracture toughness and high-thermal shock resistance yttrium oxide material and preparation method thereof |
| CN111017976A (en) * | 2019-12-27 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano yttrium oxide for dielectric ceramic capacitor |
| CN113104880A (en) * | 2021-05-07 | 2021-07-13 | 江西理工大学 | Yttrium oxide microsphere composed of nano rod-shaped structure and preparation method thereof |
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