CN103936051A

CN103936051A - Method for preparing large-grained yttria by virtue of adding NH4Cl into material liquid

Info

Publication number: CN103936051A
Application number: CN201410185738.XA
Authority: CN
Inventors: 张瑞祥; 郝先库; 李健; 赵永志; 刘海旺; 王士智; 马显东; 许宗泽; 斯琴毕力格
Original assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU; Baotou Rare Earth Research Institute
Current assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU; Baotou Rare Earth Research Institute; Santoku Corp
Priority date: 2014-05-05
Filing date: 2014-05-05
Publication date: 2014-07-23

Abstract

The invention relates to a method for preparing large-grained yttria by virtue of adding NH4Cl into a material liquid and belongs to a material preparation process. The method comprises the following steps: adding NH4Cl into a YCl3 solution so as to prepare the material liquid, heating the material liquid to 93 DEG C, adding a precipitant, namely an ammonium bicarbonate solution, so as to prepare yttrium carbonate precipitates, carrying out standing ageing, filtrating and washing on the prepared yttrium carbonate precipitates, and burning at the temperature of 1,100 DEG C, thereby obtaining the large-grained yttria of which the center grain diameter D50 is 29-43 microns, the grains are uniform, the fluidity is good and the morphology is formed by needle-like crystals.

Description

Feed liquid is added NH 4cl prepares macrobead yttrium oxide method

Technical field

The present invention relates to a kind of feed liquid and add NH ₄cl prepares macrobead yttrium oxide method, belongs to a kind of material preparation process.

Background technology

Along with scientific and technical development, macrobead yttrium oxide is applied to the fields such as coating, sputter, vacuum plating, more and more to macrobead yttrium oxide demand.CN102992382A discloses a kind of method of preparing macrobead yttrium oxide, Yttrium trinitrate is joined in the mixing solutions of bicarbonate of ammonia and ammoniacal liquor, then adds hydrogen peroxide to obtain peroxide yttrium carbonate precipitation, through calcination, prepares D ₅₀for 200-220 μ m yttrium oxide product; CN101381092B discloses the preparation method of a kind of macrobead, large specific surface area spherical yttrium oxide, with inorganic salt solution and the ammonium bicarbonate soln direct reaction of yttrium, generate the slurries containing yttrium carbonate, add a certain amount of solubility ammonium salt, ageing, calcining obtain granularity D ₅₀at 20-100 μ m yttrium oxide product; CN101182207A discloses a kind of dusty spray containing yttrium oxide and preparation method thereof, carry out ball milling with nanometer or micron yttria particles and water, ethanol or acetone, the Conglobation type spherical yttrium oxide powder that spraying is dry and thermal treatment is made, granularity is in 10-100 μ m scope; Synthetic and the sign of the volume particle size yttrium oxide that document horse jade-like stone is shown, the 6th both sides of the Straits ultrafine particle scientific seminar collection of thesis, 2009, provides macrobead yttrium oxide preparation method, prepare yttrium oxalate precipitation with oxalic acid and Yttrium trinitrate, after yttrium oxalate calcination, obtain granularity D ₅₀for 45.8-66.4 μ m yttrium oxide product; The oxalate precipitation method that document horse jade-like stone is shown is prepared macrobead yttrium oxide technical study, rare metal, 2010,34 (6): 950-954, macrobead yttrium oxide preparation method is provided, prepare yttrium oxalate precipitation with oxalic acid and Yttrium trinitrate, and regulate acidity with nitric acid, obtain obtaining granularity D after yttrium oxalate calcination ₅₀for >50 μ m yttrium oxide product.

Summary of the invention

The object of the present invention is to provide a kind of uniform particles, good fluidity, medium particle diameter D ₅₀for 29-43 μ m, the macrobead yttrium oxide preparation method that pattern is made up of needle-like crystal.

Technical solution:

The present invention is at YCl ₃in solution, add NH ₄cl is as feed liquid, YCl in feed liquid ₃concentration is 0.35 mol/L, YCl ₃with NH ₄cl mol ratio is 1:0.6-1.1, and feed liquid is heated to 93 DEG C, and adding concentration is 2 mol/L ammonium bicarbonate solns, Yttrium trichloride and bicarbonate of ammonia mol ratio are 1:2.3, yttrium carbonate precipitation is through still aging, filtration, washing, and calcination at 1100 DEG C, obtains medium particle diameter D ₅₀for 29-43 μ m, the macrobead yttrium oxide that uniform particles, good fluidity, pattern are made up of needle-like crystal.

Invention effect

Yttrium carbonate precipitation temperature and NH in the present invention ₄cl addition is to prepare macrobead yttrium oxide key; When precipitation temperature is 93 DEG C, precipitation is easily filtered, is washed, and technique is easy to control; Along with NH ₄cl addition increases, and the yttrium oxide granularity of preparation also increases, and controls YCl ₃nH in solution ₄cl addition, can prepare varigrained yttrium oxide product, and this technique is convenient to realize suitability for industrialized production; The NH adding in feed liquid ₄cl is that yttrium carbonate mother liquor of precipitation of ammonium process is concentrated, crystalline, and in mother liquor, ammonium chloride has been realized recycle.

Brief description of the drawings

Fig. 1 is the XRD figure of macrobead yttrium oxide of the present invention;

Fig. 2 is the particle size distribution figure of macrobead yttrium oxide of the present invention;

Fig. 3 is the SEM figure of macrobead yttrium oxide of the present invention.

Embodiment

embodiment 1

In setting tank, adding 2000 L concentration is the YCl of 0.35 mol/L ₃solution, then add 24 kg solid NH ₄cl, stirs solid NH ₄cl is heated to 93 DEG C by solution after dissolving, and adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, then stirs 30 minutes, stops stirring, and yttrium carbonate precipitation is through still aging, filtration, washing, and calcination at 1100 DEG C, obtains medium particle diameter D ₅₀be 29.89 μ m, the macrobead yttrium oxide that uniform particles, good fluidity, pattern are made up of needle-like crystal.

embodiment 2

In setting tank, adding 2000 L concentration is the YCl of 0.35 mol/L ₃solution, then add 32 kg solid NH ₄cl, stirs solid NH ₄cl is heated to 93 DEG C by solution after dissolving, and adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, then stirs 30 minutes, stops stirring, and yttrium carbonate precipitation is through still aging, filtration, washing, and calcination at 1100 DEG C, obtains medium particle diameter D ₅₀be 34.43 μ m, the macrobead yttrium oxide that uniform particles, good fluidity, pattern are made up of needle-like crystal.

embodiment 3

In setting tank, adding 2000 L concentration is the YCl of 0.35 mol/L ₃solution, then add 32 kg solid NH ₄cl, stirs solid NH ₄cl is heated to 93 DEG C by solution after dissolving, and adding 810 L concentration is 2 mol/L ammonium bicarbonate solns, then stirs 30 minutes, stops stirring, and yttrium carbonate precipitation is through still aging, filtration, washing, and calcination at 1100 DEG C, obtains medium particle diameter D ₅₀be 42.54 μ m, the macrobead yttrium oxide that uniform particles, good fluidity, pattern are made up of needle-like crystal.

Claims

1. feed liquid is added NH ₄cl prepares macrobead yttrium oxide method, it is characterized in that, at YCl ₃in solution, add NH ₄cl is as feed liquid, YCl in feed liquid ₃concentration is 0.35 mol/L, YCl ₃with NH ₄cl mol ratio is 1:0.6-1.1, and feed liquid is heated to 93 DEG C, and adding concentration is 2 mol/L ammonium bicarbonate solns, Yttrium trichloride and bicarbonate of ammonia mol ratio are 1:2.3, yttrium carbonate precipitation is through still aging, filtration, washing, and calcination at 1100 DEG C, obtains medium particle diameter D ₅₀for 29-43 μ m, the macrobead yttrium oxide that uniform particles, good fluidity, pattern are made up of needle-like crystal.