CN101698609B - Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder - Google Patents
Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder Download PDFInfo
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Abstract
The invention provides a method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder, which comprises the steps of adding urea into solution containing yttrium ions and adopting the homogeneous precipitation method for preparing spherical and monodisperse rare earth ion-doped yttrium oxide nano-powder. Monodisperse and single-size nano-ceramic powder is a key for preparing transparent ceramics with high transmittance. The slow decomposition of the urea in water by heating is utilized for changing the pH value of the solution, thereby leading the rare earth ion-doped yttrium salt solution to precipitate monodisperse and single-size spherical particles; and single-size spherical nano-powder which is suitable for sintering of the transparent ceramics is prepared by calcining, and the rare earth ion-doped yttrium oxide transparent ceramics is prepared by shaping and sintering.
Description
Technical field
The present invention relates to the preparation method of a kind of sphere, monodisperse and single-size yttrium oxide nano-powder.
Background technology
Crystalline ceramics has had practical application at aspects such as photoelectric ceramics and high-pressure mercury lamp fluorescent tubes at present as the optical material of a new generation.In laser ceramics and scintillating ceramic field, polycrystalline transparent ceramic also relies on its excellent performance, progressively plays the effect that substitutes monocrystal material.The yttrium oxide transparent ceramic material of (like neodymium, ytterbium, holmium, the erbium etc.) of doping with rare-earth ions has fabulous laser applications prospect.
The yttrium oxide transparent ceramic that is called Yttralox is at first succeeded in developing by AM General company, with 10%ThO
2As sinter additives, sintering temperature is about 2170 ℃.USP 3873657 and 4115134 has been introduced respectively with BeO and La
2O
3Prepare the method for yttrium oxide transparent ceramic as sinter additives, but its sintering temperature is usually all more than 2000 ℃.
The crystalline ceramics that obtains high permeability just must have well behaved powder as raw materials for sintering.At first higher purity must be arranged, the normally transparent ceramic powder requires its purity greater than 99.99%, and is opaque even exist a small amount of second phase impurity also can make the inner a large amount of scatterings of generation of pottery in the system.Secondly must be scattered superfine powder, granularity be usually between tens to 500nm.If occur in the powder reuniting, the pore that will in the agglomerating process, occur getting rid of etc.Further, in order to get rid of pore as much as possible in the sintering later stage, powder preferably has single size monodispersity ability, disperses powder but present crystalline ceramics preparation method still can't prepare suitable crystalline ceramics agglomerating list.
Traditional nanopowder preparation method mainly contains solid reaction process, chemical precipitation method, sol-gel method and auto-combustion method etc.It is monodispersed alumina powder jointed that Sacks equals to utilize the urea homogeneous precipitation method to prepare in 1984, but the particle size distribution broad is not applied in the crystalline ceramics sintering.Development along with powder technology; Japan scientist Noriko Saito and Takayasu Ikegami have proposed to prepare with bicarbonate of ammonia and ammonia water titration yttrium salts solution the method for yttrium oxide transparent ceramic powder respectively at 1998 and 2002, realized the low-temperature sintering (1700 ℃) of yttrium oxide transparent ceramic.Prepared powder is thinner, less than 100nm, be fit to the sintering of crystalline ceramics, but powder has certain reunion, and is dispersed bad, may produce the pore that can't get rid of in the sintering later stage.Afterwards, Chen Jiyang, Shi Jianlin etc. have introduced the method for utilizing bicarbonate of ammonia and the compound titration of ammoniacal liquor to prepare the yttrium oxide transparent ceramic powder in the Chinese patent 03129648.3 of application.
Summary of the invention
The present invention is based on the powder shape irregularity that present crystalline ceramics powder preparation method commonly used obtains, be prone to reunion, be unfavorable for characteristics such as sintering, proposed the preparation method of a kind of sphere, monodisperse and single-size doped yttrium oxide transparent ceramic powder.This method utilizes the evenly slow release hydroxide ion of urea to come the rare earth ion doped yttrium oxide nano-powder of precipitation from homogeneous solution(PFHS).
One aspect of the present invention; The preparation method of a kind of sphere, monodisperse and single-size yttrium oxide nano-powder is provided; It is characterized in that; In containing the solution of ruthenium ion, add urea, adopt homogeneous precipitation method to prepare the yttrium oxide nano-powder or the unadulterated yttrium oxide nano-powder of the doping with rare-earth ions of spherical monodisperse and single-size.
Preferably, said rare earth ion element is selected from one or more the combination among Nd, Yb, Ho, Er, Sm, Pr, Ce, the Eu.In the yttrium oxide nano-powder of said doping with rare-earth ions, the doping of rare earth ion is for this rare earth ion accounts for 0～10% of ruthenium ion and rare earth ion integral molar quantity in the powder, is preferably more than 0 and smaller or equal to 10%, most preferably is greater than 0 and smaller or equal to 5%.
Method of the present invention is different from general stirring titration method; Its principle is: slowly discharge the pH value that hydroxide ion improves solution evenly, lentamente through urea; Prepare the rare earth ion doped yttrium oxide nano-powder that is fit to crystalline ceramics agglomerating monodisperse and single-size, prepared particle diameter of nanometer powder is 50～500 nanometers.
Be meant that powder granule is separated from one another, be not entangled to together that single size is meant that the size of powder granule is the same single the dispersion.The nano-ceramic powder that singly disperses and have single size is the key of preparation high permeability crystalline ceramics; The nano-ceramic powder that adopts method preparation of the present invention singly to disperse and have single size, key are the use of urea precipitation from homogeneous solution(PFHS) performance and control for the strictness of conditions such as homogeneous reaction condition (like temperature, time etc.), ruthenium ion concentration and urea concentration.
The contriver finds through lot of experiments, when the ratio of control urea concentration and ruthenium ion concentration during in certain limit, and spherical single dispersion powder that can obtain having single size; When the ratio of urea concentration and ruthenium ion concentration hour, can not make nucleation of all ruthenium ions but repeatedly nucleation takes place, so the particle that forms has size, be not single size; When the large percentage of urea concentration and ruthenium ion concentration,, not monodispersed owing to the particle of the too much nucleation of urea is entangled to the powder that obtains pasty state together.As shown in Figure 4: when the ratio of urea concentration and ruthenium ion concentration reduced, because nucleation repeatedly, it is big that particulate size difference becomes, and it is big that standard deviation becomes.
Repeatedly the nucleation principle is as shown in Figure 5: along with the pH value rises, nucleation takes place, but become the certain pH value of karyophthisis, so hydroxide radical concentration is lower than the nucleation threshold value again, wait until that urea decomposes pH value nucleation once more when reaching threshold value again once more.Like this nucleation can take place repeatedly, thereby cause particle size variant.Therefore, the pH value of control solution is promptly controlled urea concentration and ruthenium ion concentration in the solution, singly disperses and has the nano-powder of single size most important for preparing.
Preferably, said precipitation from homogeneous solution(PFHS) reacts on to heat in the baking oven to carry out or in microwave oven, heat and carries out; Be preferable over 90～100 ℃ of following constant temperature 2～10 hours, perhaps in microwave oven, heated 5～30 minutes, the power of said microwave oven can be 200～1200W; When adopting the microwave heating reaction, can obtain the ultrafine nanometer powder below the 100nm.
Preferably, the concentration of ruthenium ion is 0.005～0.04mol/L in the said solution, is preferably 0.01～0.04mol/L, most preferably is 0.015～0.04mol/L; Said urea add-on is 40～120 times of ruthenium ion molar weight, is preferably 105～120 times.
Preferably, when the unadulterated yttrium oxide transparent ceramic powder of preparation, described solution can be the nitrate soln of ruthenium ion, also can be the chloride soln of ruthenium ion.
Preferably, when preparing the yttrium oxide transparent ceramic powder of doping with rare-earth ions, described solution can be the nitrate salt of ruthenium ion and the nitrate soln of rare earth ion, also can be the muriate of ruthenium ion and the chloride soln of rare earth ion.
Further, among the present invention, said employing homogeneous precipitation method prepares the yttrium oxide nano-powder or the unadulterated yttrium oxide nano-powder of the doping with rare-earth ions of sphere, monodisperse and single-size, specifically may further comprise the steps:
A. prepare mixing solutions: yttrium oxide powder or yttrium oxide and RE oxide powder are dissolved in nitric acid or the hydrochloric acid; Boil after the dissolving and evaporate unnecessary nitric acid or hydrochloric acid, add deionized water then and process the solution that ruthenium ion concentration is 0.005～0.04mol/L; Be incorporated in the urea of 40～120 times of ruthenium ion molar weights again, stir, be made into mixing solutions;
B. precipitation from homogeneous solution(PFHS) reaction: steps A gained solution in 90～100 ℃ of following constant temperature 2～10 hours, was perhaps heated in microwave oven 5～30 minutes; Then the washing, drying;
C. dried powder was calcined 2～5 hours down in 700～1000 ℃.
Preferably, in the steps A, the consumption of RE oxide powder accounts for 0～10% of ruthenium ion and rare earth ion integral molar quantity by rare earth ion and adds, and is preferably by greater than 0 and add smaller or equal to 10%, most preferably is by greater than 0 and add smaller or equal to 5%; The concentration of ruthenium ion is preferably 0.01～0.04mol/L, most preferably is 0.015～0.04mol/L; Said urea add-on is preferably 105～120 times.
Further, in the steps A, the nitrate soln of ruthenium ion or the chloride soln of ruthenium ion also can directly be dissolved in the deionized water formulated by Yttrium trinitrate or Yttrium trichloride; The nitrate soln of rare earth ion or the chloride soln of rare earth ion also can directly be dissolved in the deionized water formulated by the nitrate salt or the muriate of rare earth ion.
Preferably, among the step B, the power of said microwave oven is 200～1200W; Said washing can repeatedly be washed by water, also can repeatedly repeatedly wash with ethanol after the washing again; Said drying can be lyophilize, also can be that low temperature is slowly dry in baking oven, for example 60 ℃ of dryings in baking oven.
The present invention provides a kind of purposes that adopts the nano-powder of method for preparing on the other hand, promptly adopts the powder of method for preparing to be fit to the pressureless sintering of crystalline ceramics under 1600～1850 ℃ of vacuum conditions.
The present invention utilizes urea in water, to heat the pH value that slowly decomposition changes solution; Make the yttrium salts solution that is mixed with rare earth ion be settled out the spheroidal particle that singly disperses and have single size; Prepare suitable crystalline ceramics agglomerating list size ball shaped nano powder through calcining, through preparing rare earth ion doped yttrium oxide transparent ceramic behind moulding and the sintering.Compared with prior art, beneficial effect of the present invention is:
1. can prepare and singly disperse and have single size rare earth ion doped and a doped yttrium oxide powder not, prepared diameter of particle is at 50～500nm, and can make the superfine powder below the 100nm.
2. adopt the prepared diameter of particle homogeneous of method of the present invention, help complete densification.
3. adopt the prepared powder granule of method of the present invention to be the sphere of rule, size distribution is very even, and particle size distribution is narrower, and no agglomeration occurs.
4. equipment used is simple, uses raw material to have no special requirements, and high-purity yttrium oxide and rare earth oxide are commercial powder.
Description of drawings
Fig. 1 is that diameter of particle is about 400nm according to the micrograph of single size powder of instance 1 preparation
Fig. 2 is that diameter of particle is about 70nm according to the micrograph of single size powder of instance 2 preparations
Fig. 3 is that diameter of particle is about 500nm according to the micrograph of single size powder of instance 3 preparations
The ratio of Fig. 4 urea concentration and ruthenium ion concentration is to the influence (recording under the precipitation from homogeneous solution(PFHS) reaction conditions by embodiment 1) of particulate size
Fig. 5 is the nucleation principle repeatedly
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
The preparation mixing solutions, wherein Yttrium trinitrate 2.5 * 10
-2Mol/L, neodymium nitrate 5 * 10
-4Mol/L, urea 1.2mol/L placed 7 hours for 90 ℃ in baking oven, took out then, washed lyophilize then (20Pa ,-50 degree) 5 times.Dried powder in 850 ℃ of calcinings 4 hours, can obtain the dispersion of neodymium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.See accompanying drawing 1.
Embodiment 2
The preparation mixing solutions, wherein Yttrium trichloride 1 * 10
-2Mol/L, Neodymium trichloride 2 * 10
-4Mol/L, urea 0.8mol/L, power placed 5 minutes in the microwave oven of 700W, took out then, washs lyophilize then (20Pa ,-50 spend) 5 times.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of neodymium doped yttrium oxide list, single size powder in retort furnace.See accompanying drawing 2.
Embodiment 3
The preparation mixing solutions, wherein Yttrium trinitrate 3 * 10
-2Mol/L, ytterbium nitrate 2.5 * 10
-4Mol/L, urea 1.8mol/L placed 4 hours for 90 ℃ in baking oven, took out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of ytterbium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.See accompanying drawing 3
Embodiment 4
The preparation mixing solutions, wherein Yttrium trinitrate 4 * 10
-2Mol/L, urea 4mol/L placed 10 hours for 90 ℃ in baking oven, took out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.In 700 ℃ of calcinings calcining in 5 hours, can obtaining not, the doped yttrium oxide list disperses dried powder, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
The preparation mixing solutions, wherein Yttrium trinitrate 0.5 * 10
-2Mol/L, holmium nitrate 2.3 * 10
-4Mol/L, urea 0.6mol/L placed 2 hours for 100 ℃ in baking oven, took out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 1000 ℃ of calcinings calcining in 2 hours, can obtain the dispersion of holmium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Embodiment 6
The preparation mixing solutions, wherein Yttrium trichloride 4 * 10
-2Mol/L, Erbium trichloride 2 * 10
-4Mol/L, urea 2mol/L placed 10 hours for 90 ℃ in baking oven, took out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of erbium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Embodiment 7
The preparation mixing solutions, wherein Yttrium trichloride 1.5 * 10
-2Mol/L, samarium trichloride 15 * 10
-4Mol/L, urea 0.6mol/L is to place 30 minutes in the microwave oven of 700W at power, takes out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of samarium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Embodiment 8
The preparation mixing solutions, wherein Yttrium trichloride 0.6 * 10
-2Mol/L, praseodymium chloride 3 * 10
-4Mol/L, urea 0.63mol/L is to place 15 minutes in the microwave oven of 700W at power, takes out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of praseodymium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Embodiment 9
The preparation mixing solutions, wherein Yttrium trichloride 0.6 * 10
-2Mol/L, Cerium II Chloride 3 * 10
-4Mol/L, urea 0.63mol/L is to place 30 minutes in the microwave oven of 200W at power, takes out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of cerium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Embodiment 10
The preparation mixing solutions, wherein Yttrium trichloride 0.6 * 10
-2Mol/L, Europium trichloride 3 * 10
-4Mol/L, urea 0.63mol/L is to place 5 minutes in the microwave oven of 1200W at power, takes out then, wash 5 times after, wash 2 times with alcohol again, place slowly dryings of 60 ℃ in baking oven.Dried powder in 850 ℃ of calcinings calcining in 4 hours, can obtain the dispersion of europium doped yttrium oxide list, single size powder in retort furnace.Good through ceramic transmitance after moulding and the vacuum sintering.
Claims (5)
1. the preparation method of a spherical monodisperse and single-size yttrium oxide nano-powder; It is characterized in that; In containing the solution of ruthenium ion, add urea, adopt homogeneous precipitation method to prepare the yttrium oxide nano-powder or the unadulterated yttrium oxide nano-powder of the doping with rare-earth ions of spherical monodisperse and single-size; Specifically may further comprise the steps:
A. prepare mixing solutions: yttrium oxide powder or yttrium oxide and RE oxide powder are dissolved in nitric acid or the hydrochloric acid; Boil after the dissolving and evaporate unnecessary nitric acid or hydrochloric acid, add deionized water then and process the solution that ruthenium ion concentration is 0.005～0.04mol/L; Be incorporated in the urea of 40～120 times of ruthenium ion molar weights again, stir, be made into mixing solutions;
B. precipitation from homogeneous solution(PFHS) reaction: steps A gained solution in 90～100 ℃ of following constant temperature 2～10 hours, was perhaps heated steps A gained solution 5～30 minutes in microwave oven; Then the washing, drying;
C. dried powder was calcined 2～5 hours down in 700～1000 ℃.
2. the preparation method of spherical monodisperse and single-size yttrium oxide nano-powder as claimed in claim 1 is characterized in that, said rare earth ion element is selected from one or more the combination among Nd, Yb, Ho, Er, Sm, Pr, Ce, the Eu.
3. the preparation method of spherical monodisperse and single-size yttrium oxide nano-powder as claimed in claim 1 is characterized in that, said precipitation from homogeneous solution(PFHS) reacts on to heat in the baking oven to carry out or in microwave oven, heat and carries out.
4. the preparation method of spherical monodisperse and single-size yttrium oxide nano-powder as claimed in claim 1; It is characterized in that; When preparing the yttrium oxide nano-powder of doping with rare-earth ions; Described solution is the nitrate salt of ruthenium ion and the nitrate soln of rare earth ion, or the chloride soln of the muriate of ruthenium ion and rare earth ion; When the unadulterated yttrium oxide nano-powder of preparation, described solution is the nitrate soln of ruthenium ion, or the chloride soln of ruthenium ion.
5. the preparation method of spherical monodisperse and single-size yttrium oxide nano-powder as claimed in claim 1 is characterized in that, dry described in the step B is lyophilize or heat drying.
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| CN104003432B (en) * | 2014-06-12 | 2015-02-11 | 全南县新资源稀土有限责任公司 | Method for preparing low apparent density rare earth oxide |
| CN105645959B (en) * | 2015-12-25 | 2018-06-19 | 江苏师范大学 | Y2O3The spraying codepostion preparation method of base transparent ceramic powder |
| CN106044835A (en) * | 2016-06-08 | 2016-10-26 | 广西科技大学 | Preparation method of nanoscale spherical yttrium oxide powder |
| CN107188214B (en) * | 2017-01-24 | 2018-10-12 | 徐州盛唐光电科技有限公司 | A kind of preparation method of yttrium oxide nano-powder and nanostructure |
| CN109665868A (en) * | 2018-12-27 | 2019-04-23 | 东北大学 | A kind of preparation method of yttrium oxide functionally gradient material (FGM) |
| 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 |
| CN112125663B (en) * | 2020-08-14 | 2022-06-28 | 广东省科学院稀有金属研究所 | Preparation method of monodisperse yttria-stabilized zirconia nano powder |
| CN112645378B (en) * | 2021-03-01 | 2022-09-30 | 广州建丰五矿稀土有限公司 | Preparation process of gadolinium oxide powder |
| CN113737040A (en) * | 2021-08-09 | 2021-12-03 | 西安交通大学 | Nano yttrium oxide dispersion strengthening molybdenum alloy and preparation method thereof |
| CN114656963B (en) * | 2022-03-31 | 2023-02-28 | 北京化工大学 | Surface hydrophobic modification method of yttrium europium oxide fluorescent powder |
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| 霍地等.超细粉体制备Nd：Y2O3透明陶瓷.《中国稀土学报》.2008,第26卷(第1期),第56-60页. * |
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