CN101602944B - Method for producing rare earth ion doped yttrium aluminum garnet nano phosphor powder - Google Patents

Abstract

The invention discloses a method for producing a rare earth ion doped yttrium aluminum garnet nano phosphor powder. The general formula of the nano powder is (Y1-xLnx)3Al5O12, wherein Ln is one of rare earth elements Ce and Eu, x is more than or equal to 0.0 and less than or equal to 0.1, mixed solution of nitrates or acetates of Al, Y and Ln is used as a mother liquor of salt, and mixed solution of NH4HCO3 and NH3.H2O is used as solution of compound precipitator; the ammonia water is used for adjusting the pH value of the solution of compound precipitator to 10; and the mother liquor of salt undergoes ultrasonic atomization and then is sprayed in the solution of compound precipitator which is continuously stirred, and after complete reaction, the mixed solution if filtered, washed, dried, repeatedly ball-milled and calcined to obtain uniform and dispersed rare earth ion doped YAG nano phosphor powder. The method has the advantages that the produced nano phosphor powder is uniform and dispersed, the granularity is small (between 50 and 70 nanometers), and the generated phase is unitary; and the high-concentration uniform doping of the rare earth ions is realized, so that the rare earth ion doped yttrium aluminum garnet nano phosphor powder can be obtained in high efficiency.

Description

A kind of working method of rare earth ion doped yttrium aluminum garnet nano phosphor powder

Technical field

The present invention relates to the working method of a kind of yttrium aluminum garnet (YAG) fluorescent powder, particularly a kind of working method of rare earth ion doped yttrium aluminum garnet (YAG) nano phosphor powder.

Background technology

The fluorescent material that with the rare earth ion is luminescence center has obtained number of applications in a lot of fields, like lamp phosphor, medical fluorescent material, TV fluorescent material etc., because this added value of product is high, remarkable benefit, has become the key areas of rare earth high-tech development.Though the consumption of fluorescent RE powder is less than 4% of the rare earth total quantity consumed, the output value accounts for 41% of rare earth application market total sales volume, is the most popular industry of rare-earth trade ^[1,2]

Yttrium aluminum garnet (yttrium aluminum garnet), chemical formula is Y ₃Al ₅O ₁₂, be called for short YAG, have excellent optical property and good mechanical and thermal property, be widely used in laser and luminous host material.Rare earth ion doped YAG fluorescent material is important a kind of in the fluorescent material, YAG as the substrate material of fluorescent material have that transparency height, chemicalstability are good, advantage such as good, the anti-high intensity radiation of thermal conductivity and electron-bombardment ^[3]So rare earth ion doped YAG fluorescent material has obtained extensive studies in recent years.

The preparation method of rare earth ion doped YAG fluorescent material mainly contains high-temperature solid phase reaction method ^[4], sol-gel method ^[5], polymer-network gel method ^[6], solvent-thermal method ^[7], combustion method ^[8], spray pyrolysis ^[9], coprecipitation method ^[10]Deng, still, all there is certain shortcoming in these methods, and like high-temperature solid phase reaction method, the gained powder needs ball mill pulverizing, and particle is big and size distribution is wide; Sol-gel method needs expensive starting material, cost height; Metal alkoxide in the polymer-network gel method generally is difficult to obtain, and cost is higher, and in reaction process, wants strict control moisture, severe reaction conditions; Solvent-thermal method needs higher synthesis temperature and pressure; The powder out-of-shape that combustion method generates; Coprecipitation method is compared with other chemical processes, and that its advantage is is with low cost, equipment simple and be easy to scale operation, but preparing method's process is loaded down with trivial details, processing requirement is harsh, the time is longer.Except that there was certain shortcoming in processing condition, aforesaid method like sol-gel method, was worked as Eu aspect the high-concentration dopant of realizing rare earth ion certain deficiency being arranged also ³⁺When content reaches 0.06mol, Eu ³⁺Luminously reach the strongest, then along with Eu ³⁺The concentration quenching phenomenon takes place in the increase of content and reducing ^[11]Use coprecipitation method, work as Ce ³⁺Doping content in YAG is 4.8% o'clock, and it is maximum that fluorescence intensity reaches, Ce ³⁺When doping content further increases, because Ce ³⁺Between radiationless relaxation and concentration quenching has taken place ^[12]

Reference:

[1] Lido, river, Yang Yuchun. rare-earth luminescent material new development [J]. rare metal, 1996,20 (2): 129～133.

[2] Wang Yong, Li Ping, Wang Jieqiang. rear-earth-doped YAG fluorescent material preparing method's progress [J]. Shandong chemical industry, 2007,36 (2): 22～27.

[3]CHEN?Teng-Ming，Chen?S?C，Yu?Chao-Jung.Preparation?and?characterization?ofgarnet?phosphor?nanoparticles?derived?from?oxalate?coprecipitation[J].Journal?of?solidstate?chemistry，1999，144：437～441.

[4]Pan?Y?X，Wu?M?M，Su?Q.Tailored?photo-luminescence?of?YAG:Ce?phosphor?thoughvarious?methods[J].J.Phys.Chem.Solids，2000，65：845-850.

[5]H.M.H.Fadlalla，C.C.Tang，E.M.Elssfah，F.Shi.Synthesis?and?characterization?of?singlecrystalline?YAG:Eu?nano-sized?powder?by?sol-gel?method.Materials?Chemistry?andPhysics?109(2008)436-439.

[6]Li?Q，Gao?L，Yan?D?S.Preparation?and?spectra?characterization?of?YAG:Ce ³⁺?ultrafinepowders.J.Inorg.Mater，1997，12(4)：575-578.

[7]Xia?Li，Qiang?Li，Jiyang?Wang，Shunliang?Yang.Synthesis?of?YAG:Eu?phosphors?withspherical?morphology?by?solvo-thermal?method?and?their?luminescent?property.MaterialsScience?and?Engineering?B?131(2006)32-35

[8] Xia Guodong, Zhou Shengming, Zhang Junji, Zhang Lianhan, Jia Guangqiang Xu Jun. gel-combustion method is synthesized YAG:Eu ³⁺The structure of nano-luminescent material and luminescent properties. Chinese Journal of Inorganic Chemistry, 2005,21 (8): 1203-1207.

[9]Y.H.Zhou，J.Lin，M.Yu，S.M.Han，S.B.Wang，H.J.Zhang.Morphology?control?andluminescence?properties?of?YAG:Eu?phosphors?prepared?by?spray?pyrolysis.MaterialsResearch?Bulletin?38(2003)1289-1299.

[10]J.Su，Q.L.Zhang，S.F.Shao，W.P.Liu，S.M.Wan，S.T.Yin.Phase?transition，structureand?luminescence?of?Eu:YAG?nanophosphors?by?co-precipitation?method.Journal?ofAlloys?and?Compounds，2008.

[11] the week oath is red, Zhang Siyuan, Zhang Jingjun, Pan Wenge .YAG:Eu ³⁺, Bi ³⁺Sol-gel method synthetic and structure and luminous. SCI .1998,19 (11): 1826-1828.

[12] Zhang Kai, Liu Hezhou, the coroner Asia is graceful, Hu Wenbin. and coprecipitation method prepares nanometer cerium doped yttrium aluminum garnet fluorescent powder and fluorescent characteristic thereof. mechanical engineering material .2007,31 (1): 53-56.

Summary of the invention

Technical problem to be solved by this invention provides a kind of epigranular, dispersion and generates the working method of yttrium aluminum garnet (YAG) nano phosphor powder of mutually single, high-concentration dopant rare earth ion; This method equipment is simple, easy to operate; Combined coefficient is high, and the doping content of particle diameter of nanometer powder narrow distribution range, percent crystallinity and the rare earth ion of production is high.

The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of working method of rare earth ion doped yttrium aluminum garnet nano phosphor powder, and it may further comprise the steps:

The general formula of 1. rare earth ion doped yttrium aluminum garnet is (Y _1-χLn _χ) ₃Al ₅O ₁₂, wherein Ln is a kind of among rare earth element ce, the Eu, its doping χ is 0.01≤χ≤0.1, according to the stoichiometric ratio of general formula, is raw material with their corresponding nitrate salt or acetate, makes mixed aqueous solution as female salts solution, cofabrication NH ₄HCO ₃The aqueous solution is used NH ₃H ₂O regulates NH ₄HCO ₃PH value of aqueous solution to 10 will add NH ₃H ₂NH behind the O ₄HCO ₃Solution is as precipitant solution;

2. be injected to female salts solution in the precipitant solution through behind the ultrasonic atomizatio, the control mist flow makes to be reflected in 1～15h and accomplishes, and in the liquid of hybrid reaction, carries out mechanical stirring simultaneously;

The mixing solutions that 3. will react filters, and then the material after filtering is washed, and uses washed with de-ionized water earlier, cleans with absolute ethyl alcohol again;

4. cleaned material is put into oven drying, drying temperature is 90～130 ℃, time of drying 6～20h;

5. dried material is dispersed in the absolute ethyl alcohol, carries out repetitious wet-milling with the Ceramic Balls of different size size respectively, dry again after the wet-milling, and then repeatedly dry grind with the big or small Ceramic Balls of different size and to obtain powder;

6. the powder after will dry grinding promptly obtains rare earth ion doped nano phosphor powder at 900～1200 ℃ of temperature sintering 1～5h.

The female salts solution of described step in 1. is the nitrate salt of Al, Y and Ln or the mixing solutions of acetate, and its positively charged ion total concn is 0.1～0.5 mol; NH ₄HCO ₃The concentration of the aqueous solution is 0.1～1 mol, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1.

The ultrasonic atomizatio of described step in 2. is at room temperature; After flow was 0.1～0.6 millimeter shower nozzle through internal diameter, it was 40～600 milliliters/hour that regulated valve makes flow rate of liquid, in the 50KHz frequency; Under the ultrasonication of 10～80W continuous output, be transformed into little mist vapour; The distance of regulating nozzle and reaction liquid level makes the contact reacts area of little mist vapour and liquid level at least greater than 15m ², churned mechanically rotating speed is 20～200 rev/mins.

The wet-milling of described step in 5. is to use earlier Φ 25mm; Use Φ 10mm again, with zirconia ball difference ball milling 0.5～8h of Φ 5mm, the add-on of absolute ethyl alcohol is 5～50 milliliters of every gram materials at last; After the described wet-milling again the exsiccant temperature be 110～130 ℃, be 10～20h time of drying; Described dry grinding is the zirconia ball ball milling 0.5～8h with Φ 25mm, uses Φ 10mm again, uses each ball milling 0.5～3h of zirconia ball of Φ 5mm at last.

Compared with prior art, the invention has the advantages that the method that adopts ullrasonic spraying and co-precipitation to combine carries out the production of rare earth ion doped yttrium aluminum garnet nano phosphor powder.

Coprecipitation method is in blended metal salt solution (metals ion that contains two or more), to add suitable precipitation agent, and reaction generates forms deposition uniformly, and precipitation heat obtains high-purity superfine powdery material after decomposing.The maximum characteristics of coprecipitation method are: the solution nucleation is fast, and is easy to control, can make highly purified product, the nano powder that can be uniformly dispersed, size-grade distribution is narrow; This method equipment is simple, is easy to industrialization, has stronger industrial promotional value.But coprecipitation method has following serious defective, promptly in precipitation process, is prone to reunite, and particle diameter is wayward, and particle radius is big.

And ullrasonic spraying is to utilize the ultrasonic cavitation energy to quicken and the control chemical reaction; Improve reaction yield and a kind of new technology that causes new chemical reaction; The inventor utilizes the ultrasonic cavitation energy; Change into the little vaporific drop with certain energy to female salts solution of reaction and big area is sprayed onto in the co-precipitation mixing solutions, transforming the little mist vapour that obtains is a kind of evenly tiny liquid small-particle.The mother liquor of handling through ultrasonic atomizatio, carry out chemical reaction with the composite precipitation agent solution after, be expected to improve the homogeneity of chemical reaction, obtain tiny, dispersive nano-powder.

And having combined the working method of above-mentioned two kinds of technology obviously to have following characteristics: 1. female salts solution is at first handled through ultrasonic atomizatio; Make it become little mist vapour with certain energy; Big area is ejected in the mixed precipitation agent solution, thereby has increased the homogeneity of chemical reaction, has overcome phenomenons such as nanoparticle agglomerates; The particle granularity that obtains after the calcining is merely 50～70 nanometer (see figure 1)s, and powder is single YAG phase (see figure 2); 2. another characteristics of the present invention are rear-earth-doped YAG not to be had the treatment technology of reunion fluorescent powder.Conventional all fairly simple to the processing and the store method of rear-earth-doped YAG fluorescent powder, usually the shelf time not long, cause the particulate hard aggregation easily.We obtain good dispersion through the repeatedly wet-milling and the dry grinding repeatedly of coupling different size Ceramic Balls, seldom reunite evenly in single rear-earth-doped YAG fluorescent powder (see figure 1); 3. the YAG powder that method of the present invention is produced also has beyond thought high concentration rare earth doping characteristic; Has very high concentration quenching effect; In the YAG:Eu powder, quenching of fluorescence phenomenon (Fig. 4) does not appear, apparently higher than the 6mol% of sol-gel method when the Eu doping content reaches 10mol%.In the YAG:Ce powder, when the Ce doping content reached 6～7mol%, fluorescence intensity reached maximum (see figure 6), apparently higher than the 4.8mol% of coprecipitation method.Therefore use this method can realize high efficiency rare earth ion doped YAG nano phosphor powder.

Description of drawings

Fig. 1 is the SEM figure of the YAG:Ln sample of 1000 ℃ of calcining 2h, (a) Ln=Eu; (b) Ln=Ce.;

Fig. 2 is the XRD figure of YAG:Ln (Ln=Eu, Ce) presoma at differing temps calcining 2h;

Fig. 3 is the emmission spectrum of the YAG:Eu powder of different Eu doping contents, (1) 1%Eu; (2) 2%Eu; (3) 4%Eu; (4) 6%Eu; (5) 8%Eu; (6) 10%Eu.;

Fig. 4 is the emissive porwer (λ of different levels of doping Eu:YAG powder _Ex=396nm);

Fig. 5 is the emmission spectrum of the YAG:Ce powder of various ce doping content, (1) 1%Ce; (2) 2%Ce; (3) 4%Ce; (4) 6%Ce; (5) 8%Ce; (6) 10%Ce.;

Fig. 6 is the emissive porwer (λ of different levels of doping Ce:YAG powder _Ex=470nm).

Embodiment

Below in conjunction with specific embodiment the present invention is described in further detail.

Embodiment 1:

(1) at first with Al (NO ₃) ₃, Y (NO ₃) ₃And Eu (NO ₃) ₃Solution is according to general formula (Y _0.98Eu _0.02) ₃Al ₅O ₁₂Stoichiometric ratio, being made into cation concn is female salts solution of 0.2 mol, prepares the ammonium bicarbonate solution of 0.6 mol again with deionized water, and with the pH to 10 of ammoniacal liquor regulator solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1;

(2) regulated valve; Making female salts solution aperture of flowing through is 0.20 millimeter titanium alloy ullrasonic spraying head; Get into ultrasonic atomizing device with 300 milliliters/hour flow velocitys, the control mist flow makes to be reflected in 4 hours and accomplishes, under the continuous ultrasound effect of frequency 50KHz, power 45W; Join behind the ultrasonic atomizatio in the mixed precipitation agent solution of continuous stirring, the spray reaction area is about 35cm ²Mechanical stirring speed is 80 rev/mins;

(3) will mix object and filter, the material that obtains is earlier with washed with de-ionized water 1 time, again with absolute ethyl alcohol cleaning 3 times;

The material that (4) will clean is put into baking oven, and temperature remains on 120 ℃ of dry 12h;

(5) drying is good material is dispersed in the absolute ethyl alcohol, and the add-on of absolute ethyl alcohol is 10 milliliters of every gram materials, uses Φ 25mm earlier, uses Φ 10mm again, uses each ball milling 2h of zirconia ball of Φ 5mm at last; Then that ball milling is good powder is placed on dry 12h in the baking oven that temperature remains on 120 ℃; Use the zirconia ball ball milling 1h of Φ 25mm after the drying again, use Φ 10mm again, use each ball milling 1h of zirconia ball of Φ 5mm at last;

(6) powder after will dry grinding promptly obtains rare earth ion doped YAG nano phosphor powder at 1000 ℃ of temperature lower calcination 2h.

Embodiment 2:

(1) at first with Al (NO ₃) ₃, Y (NO ₃) ₃And Ce (NO ₃) ₃Solution is according to general formula (Y _0.96Ce _0.04) ₃Al ₅O ₁₂Stoichiometric ratio be made into female salts solution that cation concn is 0.3 mol, prepare the ammonium bicarbonate solution of 0.9 mol again with deionized water, and with the pH to 10 of ammoniacal liquor regulator solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1;

(2) regulated valve; Making female salts solution aperture of flowing through is 0.20 millimeter titanium alloy ullrasonic spraying head; Get into ultrasonic atomizing device with 300 milliliters/hour flow velocitys, the control mist flow makes to be reflected in 4 hours and accomplishes, under the continuous ultrasound effect of frequency 50KHz, power 45W; Join behind the ultrasonic atomizatio in the mixed precipitation agent solution of continuous stirring, the spray reaction area is about 35cm ²Mechanical stirring speed is 80 rev/mins;

(3) will mix object and filter, the material that obtains is earlier with washed with de-ionized water 1 time, again with absolute ethyl alcohol cleaning 3 times;

The material that (4) will clean is put into baking oven, and temperature remains on 120 ℃ of dry 12h;

(5) drying is good material is dispersed in the absolute ethyl alcohol, and the add-on of absolute ethyl alcohol is 10 milliliters of every gram materials, uses Φ 25mm earlier, uses Φ 10mm again, uses each ball milling 2h of zirconia ball of Φ 5mm at last; Then that ball milling is good powder is placed on dry 12h in the baking oven that temperature remains on 120 ℃; Use the zirconia ball ball milling 1h of Φ 25mm after the drying again, use Φ 10mm again, use each ball milling 1h of zirconia ball of Φ 5mm at last;

(6) powder after will dry grinding promptly obtains rare earth ion doped YAG nano phosphor powder at 1000 ℃ of temperature sintering 2h.

Embodiment 3:

(1) at first with Al (Ac) ₃, Y (Ac) ₃And Eu (Ac) ₃Solution is according to general formula (Y _0.94Eu _0.06) ₃Al ₅O ₁₂Stoichiometric ratio be made into female salts solution that cation concn is 0.15 mol, prepare the ammonium bicarbonate solution of 0.45 mol again with deionized water, and with the pH to 10 of ammoniacal liquor regulator solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1;

(2) regulated valve; Making female salts solution aperture of flowing through is 0.20 millimeter titanium alloy ullrasonic spraying head; Get into ultrasonic atomizing device with 200 milliliters/hour flow velocitys, the control mist flow makes to be reflected in 4 hours and accomplishes, under the continuous ultrasound effect of frequency 50KHz, power 45W; Join behind the ultrasonic atomizatio in the mixed precipitation agent solution of continuous stirring, the spray reaction area is about 35cm ²Mechanical stirring speed is 80 rev/mins;

(3) will mix object and filter, the material that obtains is earlier with washed with de-ionized water 1 time, again with absolute ethyl alcohol cleaning 3 times;

The material that (4) will clean is put into baking oven, and temperature remains on 120 ℃ of dry 12h;

(5) drying is good material is dispersed in the absolute ethyl alcohol, and the add-on of absolute ethyl alcohol is 15 milliliters of every gram materials, uses Φ 25mm earlier, uses Φ 10mm again, uses each ball milling 2h of zirconia ball of Φ 5mm at last; Then that ball milling is good powder is placed on dry 12h in the baking oven that temperature remains on 120 ℃; Use the zirconia ball ball milling 1h of Φ 25mm after the drying again, use Φ 10mm again, use each ball milling 1h of zirconia ball of Φ 5mm at last;

(6) powder after will dry grinding promptly obtains rare earth ion doped YAG nano phosphor powder at 1000 ℃ of temperature sintering 2h.

Embodiment 4:

(1) at first with Al (NO ₃) ₃, Y (NO ₃) ₃And Eu (NO ₃) ₃Solution is according to general formula (Y _0.96Eu _0.04) ₃Al ₅O ₁₂Stoichiometric ratio be made into female salts solution that cation concn is 0.25 mol, prepare the ammonium bicarbonate solution of 0.75 mol again with deionized water, and with the pH to 10 of ammoniacal liquor regulator solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1;

(2) regulated valve; Making female salts solution aperture of flowing through is 0.15 millimeter titanium alloy ullrasonic spraying head; Get into ultrasonic atomizing device with 100 milliliters/hour flow velocitys, the control mist flow makes to be reflected in 4 hours and accomplishes, under the continuous ultrasound effect of frequency 50KHz, power 20W; Join behind the ultrasonic atomizatio in the mixed precipitation agent solution of continuous stirring, the spray reaction area is about 20cm ²Mechanical stirring speed is 100 rev/mins;

(3) will mix object and filter, the material that obtains is earlier with washed with de-ionized water 1 time, again with absolute ethyl alcohol cleaning 3 times;

The material that (4) will clean is put into baking oven, and temperature remains on 100 ℃ of dry 15h;

(5) drying is good material is dispersed in the absolute ethyl alcohol, and the add-on of absolute ethyl alcohol is 20 milliliters of every gram materials, uses Φ 25mm earlier, uses Φ 10mm again, uses each ball milling 3h of zirconia ball of Φ 5mm at last; Then that ball milling is good powder is placed on dry 15h in the baking oven that temperature remains on 100 ℃; Use the zirconia ball ball milling 1.5h of Φ 25mm after the drying again, use Φ 10mm again, use each ball milling 1h of zirconia ball of Φ 5mm at last;

(6) powder after will dry grinding promptly obtains rare earth ion doped YAG nano phosphor powder at 900 ℃ of temperature sintering 3h.

Embodiment 5:

(1) at first with Al (Ac) ₃, Y (Ac) ₃And Ce (Ac) ₃Solution is according to general formula (Y _0.94Ce _0.06) ₃Al ₅O ₁₂Stoichiometric ratio be made into female salts solution that cation concn is 0.2 mol, prepare the ammonium bicarbonate solution of 0.6 mol again with deionized water, and with the pH to 10 of ammoniacal liquor regulator solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1;

(2) regulated valve; Making female salts solution aperture of flowing through is 0.45 millimeter titanium alloy ullrasonic spraying head; Get into ultrasonic atomizing device with 450 milliliters/hour flow velocitys, the control mist flow makes to be reflected in 4 hours and accomplishes, under the continuous ultrasound effect of frequency 50KHz, power 40W; Join behind the ultrasonic atomizatio in the mixed precipitation agent solution of continuous stirring, the spray reaction area is about 22cm ²Mechanical stirring speed is 90 rev/mins;

(3) will mix object and filter, the material that obtains is earlier with washed with de-ionized water 1 time, again with absolute ethyl alcohol cleaning 3 times;

The material that (4) will clean is put into baking oven, and temperature remains on 130 ℃ of dry 8h;

(5) drying is good material is dispersed in the absolute ethyl alcohol, and the add-on of absolute ethyl alcohol is 30 milliliters of every gram materials, uses Φ 25mm earlier, uses Φ 10mm again, uses each ball milling 4.5h of zirconia ball of Φ 5mm at last; Then that ball milling is good powder is placed on dry 8h in the baking oven that temperature remains on 130 ℃; Use the zirconia ball ball milling 2h of Φ 25mm after the drying again, use Φ 10mm again, use each ball milling 1h of zirconia ball of Φ 5mm at last;

(6) powder after will dry grinding promptly obtains rare earth ion doped YAG nano phosphor powder at 1100 ℃ of temperature sintering 1.5h.

Claims (1)

1. the working method of a rare earth ion doped yttrium aluminum garnet nano phosphor powder is characterized in that it may further comprise the steps:

The general formula of 1. rare earth ion doped yttrium aluminum garnet is (Y _1-χLn _χ) ₃Al ₅O ₁₂Wherein Ln is a kind of among rare earth element ce, the Eu; Its doping χ is 0.01≤χ≤0.1, according to the stoichiometric ratio of general formula, is raw material with nitrate salt or the acetate of Al, Y and Ln; Making the positively charged ion total concn is female salts solution of 0.1～0.5 mol, and cofabrication concentration is the NH of 0.1～1 mol ₄HCO ₃The aqueous solution, NH ₄HCO ₃Molar weight and (Y _1-χLn _χ) ₃Al ₅O ₁₂The ratio of middle positively charged ion integral molar quantity is 3: 1, uses NH ₃H ₂O regulates NH ₄HCO ₃PH value of aqueous solution to 10 will add NH ₃H ₂NH behind the O ₄HCO ₃Solution is as precipitant solution;

2. be injected to female salts solution in the precipitant solution through behind the ultrasonic atomizatio; Ultrasonic atomizatio is at room temperature; After flow was 0.1～0.6 millimeter shower nozzle through internal diameter, it was 40～600 milliliters/hour that regulated valve makes flow rate of liquid, in the 50KHz frequency; Under the ultrasonication of 10～80W continuous output, be transformed into little mist vapour; The distance of regulating nozzle and reaction liquid level makes the contact reacts area of little mist vapour and liquid level at least greater than 15m ², the control mist flow makes to be reflected in 1～15h and accomplishes, and in the liquid of hybrid reaction, carries out mechanical stirring simultaneously, and churned mechanically rotating speed is 20～200 rev/mins;

The mixing solutions that 3. will react filters, and then the material after filtering is washed, and uses washed with de-ionized water earlier, cleans with absolute ethyl alcohol again;

4. cleaned material is put into oven drying, drying temperature is 90～130 ℃, time of drying 6～20h;

5. dried material is dispersed in the absolute ethyl alcohol, carries out repetitious wet-milling with the Ceramic Balls of different size size respectively, dry again after the wet-milling; And then repeatedly dry grind with the Ceramic Balls of different size size and to obtain powder, wet-milling is to use Φ 25mm earlier, uses Φ 10mm again; Distinguish ball milling 0.5～8h with the zirconia ball of Φ 5mm at last; The add-on of absolute ethyl alcohol is 5～50 milliliters of every gram materials, after the described wet-milling again the exsiccant temperature be 110～130 ℃, be 10～20h time of drying; Described dry grinding is the zirconia ball ball milling 0.5～8h with Φ 25mm, uses Φ 10mm again, uses each ball milling 0.5～3h of zirconia ball of Φ 5mm at last;

6. the powder after will dry grinding promptly obtains rare earth ion doped nano phosphor powder at 900～1200 ℃ of temperature sintering 1～5h.

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