CN106635007B - A kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor - Google Patents

A kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor Download PDF

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CN106635007B
CN106635007B CN201610830199.XA CN201610830199A CN106635007B CN 106635007 B CN106635007 B CN 106635007B CN 201610830199 A CN201610830199 A CN 201610830199A CN 106635007 B CN106635007 B CN 106635007B
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yttrium oxide
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CN106635007A (en
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陈智慧
李志伟
邱建华
朱媛媛
丁建宁
袁宁
袁宁一
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Changzhou University
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    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The present invention provides a kind of preparation methods of extra small scale rare earth doped yttrium oxide base nano-phosphor, its step includes: to make rare-earth salt solution and precipitating reagent that continuous dynamic coprecipitation reaction occur with vigorous stirring using continuous dynamic precipitation method, generate extra small scale rare earth doped yttrium oxide base nano-phosphor presoma, through suction filtration, washing, dehydration, drying, calcining obtains rare earth doped yttrium oxide base nano-phosphor.The average grain diameter for the rare earth doped yttrium oxide base nano-phosphor presoma that this method provides is 2-3nm, and after being fired processing, the particle size of nano-phosphor is less than 10nm.The method of the present invention preparation rare earth doped yttrium oxide base nano-phosphor scale is extra small, monodisperse；Simple process, at low cost, the period is short, can satisfy the demand of industrialization.

Description

A kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor
Technical field
The present invention relates to a kind of preparation method of the yttria-base luminescent material of doping with rare-earth ions, more particularly to one kind are super The preparation method of the rare earth doped yttrium oxide base nano-phosphor of small scale.
Background technique
Yttrium oxide and gadolinium oxide have many advantages, such as that luminous intensity is high, stability is good, are common luminous substrate materials.Rare earth Doped yttrium oxide/gadolinium oxide material be widely used in high-quality show with illuminating device in.Rare earth doped yttrium oxide original washing powder body At present mainly based on the precipitation method, sol-gel method and solid phase method.Sol-gel method prepares powder and is easy to reunite, and prepares week Phase is long, higher cost, is not suitable for batch production.Chinese patent (201010201596.1, containing the rear-earth-doped of metal nanoparticle Yttrium oxide luminescent material and preparation method thereof) it discloses a kind of sol-gal process and prepares rear earth-doped yttrium oxide luminescent material, it should Reaction time, digestion time was 40-60 hours, and drying time is up to 48-96 hours at 4-6 hours.Prolonged ageing is with after Treatment process is easy that powder is made to reunite, and forms bulky grain.Influence of the granularity to luminous intensity leads to metal nanoparticle It is unobvious to the improvement of yttrium oxide luminous intensity.The rare earth doping fluorescent powder of solid sintering technology preparation is micron particles, And bad dispersibility.Chinese patent (200810061448.9, gadolinium lutetium oxide fluorescent powder and preparation method thereof) uses solid sintering technology It is prepared for gadolinium lutetium oxide fluorescent powder, but without the micro-structural feature of report gained powder.The forerunner of conventional precipitation method preparation Body is easy to happen reunion in drying, calcining and other processes, so that powder granularity is bigger than normal, bad dispersibility.Chinese patent (CN201510630997.3) a kind of precipitation method are disclosed and prepare yttrium oxide powder, this method joined crystalline substance after precipitating reagent is added The big inhibitor of grain length, powder average grain diameter are 70nm.Chinese patent (200910198286.8) discloses a kind of microwave and homogeneously sinks Shallow lake method introduces dispersing agent in preparation process twice, and the yttrium oxide powder partial size of preparation is in 100nm or more.Although dispersibility is Improve, diameter of particle still tens even several hundred nanometers.Therefore, if there is a kind of technique that can obtain extra small scale, monodispersed Rare earth doped yttrium oxide base nano-phosphor fundamentally improves the microstructure of powder, improves the performance of powder, and then improve The luminous intensity of powder, and the demand that can satisfy industrialization will be greatly promoted the long term growth in rare earth material field.
Summary of the invention
The technical scheme is that in order to overcome the shortcomings of prior art, propose a kind of to be able to satisfy the super of industrialization demand The preparation method of small scale, monodispersed rare earth doped yttrium oxide base nano-phosphor.
The invention proposes extra small scale rare earth doped yttrium oxide base nano-phosphor preparation method, including following step It is rapid:
A, according to chemical composition Eu2xGd2yY2(1-x-y)O3(x=0.01-0.1, y=0-0.5) weigh micron order europium oxide, Yttrium oxide, gadolinium oxide powder, are dissolved in boiling in nitric acid or hydrochloric acid and evaporate extra nitric acid or hydrochloric acid, match deionized water is added It is set to certain density rare-earth salt solution；Or match by same chemical composition using rare earth nitrades, sulfate, chloride as raw material It is set to rare-earth salt solution.
B, rare-earth salt solution is added in dispersing agent dehydrated alcohol；Dehydrated alcohol and ammonium hydroxide are mixed, constant volume, form ammonia Aqueous solution；At room temperature, rare-earth salt solution and ammonia spirit are continuously injected into reactor, mixed solution and ammonium hydroxide with identical speed Precipitation reaction occurs solution for moment in the presence of vigorous stirring；Precipitating is flowed out from reactor outlet dynamic immediately after being formed；It will Precipitating filtering, dehydrated alcohol washing, drains, obtains solid sediment；
C, solid sediment is mixed with n-amyl alcohol, carries out decompression co-boiling distiling；Solid state powder after distillation is in horse Not 900 DEG C of -1250 DEG C of roastings obtain extra small scale rare earth doped yttrium oxide base nano-phosphor powder in 30 minutes in furnace.
Wherein, the concentration of rare-earth salt solution described in step a is 0.5mol/L-2.0mol/L.The dehydrated alcohol Amount is respectively the 10-30% of rare-earth salt solution and ammonia spirit volume.
Reactor described in step b is using the import of multiple groups reaction solution and generates liquid outlet, and inlet and outlet is alternately placed；Institute The speed for rare-earth salt solution and ammonia spirit the injection reactor stated is 40L/h-200L/h；The mixing speed is 800rpm-4000rpm；The precipitation reaction pH value adjusts pH value in reaction between 8-9, with ammonia spirit.
The process that solid sediment is generated described in step b is injected into white slurry from reactant and generates, intermediate without ageing, Whole process orderly, is dynamically rapidly completed.
Wherein, preferably:
The concentration of rare-earth salt solution used is between 0.8-1.2mol/1；
The amount of dispersing agent dehydrated alcohol is respectively the 20% of rare-earth salt solution and ammonia spirit volume；
The speed of rare-earth salt solution and ammonia spirit injection reactor is 80L/h-120L/h；
Mixing speed during precipitation reaction is 2000rpm-4000rpm；
The present invention prepares extra small scale rare earth doped yttrium oxide base nano-phosphor using continuous dynamic precipitation method, specific side Method includes following several key components.Between 0.5-2.0mol/1, solution high concentration has the concentration of rare-earth salt solution used Help quickly generate a large amount of small grains.In second step, used reactor uses the import of multiple groups reaction solution and generation Liquid outlet, inlet and outlet are alternately placed, and solid granulates have just generated just from nearest reactor outlet outflow reactor, are reacting Residence time is very short in device, greatly reduces the probability that same container is in previous stage nanoparticle generated, Guarantee that obtained nanoparticle has good monodispersity.Rare-earth salt solution and ammonia spirit are continuously quick with identical speed Reactor is injected, the speed for injecting reactor is 40L/h-200L/h, and the mixing speed during precipitation reaction is 800rpm- 4000rpm.When mixed solution and ammonia spirit mix under high-intensitive mechanical stirring, dispersed by convective motion, turbulent motion At the solution micelle being mutually mutually separated, precipitation reaction is to roll into a ball interface in micro- liquid group of rare-earth salt solution and micro- liquid of ammonia spirit Upper generation.Therefore, churned mechanically intensity is bigger, then the number of fast nucleation is also bigger, and it is smaller to be formed by grain diameter.
The present invention also provides the rare earth doped yttrium oxide base nano-phosphors of this method preparation.Wherein, the rare earth of preparation The partial size of doped yttrium oxide base nano-phosphor presoma is in 2-3nm；Rare earth doped yttrium oxide base nano-phosphor after roasting Average grain diameter be less than 10nm.
Beneficial effects of the present invention: this method prepares the rare earth doped yttrium oxide of extra small scale by continuous dynamic precipitation method Base nano-phosphor is injected into white depositions from reactant and generates, and whole process is continuous, is dynamically completed.It is not required to be aged, not make With surfactant, rapid reaction, the period is short, and simple and convenient is at low cost, is suitble to produce extra small scale in enormous quantities, be uniformly dispersed Rare earth doped yttrium oxide base nano-phosphor.
Detailed description of the invention
Fig. 1 is Eu prepared by embodiment 10.08Y1.92O3The XRD diagram of nano-phosphor presoma.
Fig. 2 is Eu prepared by embodiment 10.08Y1.92O3TEM figure after 1050 DEG C of nano-phosphor roastings.
Fig. 3 is Eu prepared by embodiment 20.08(Y 0.5Gd0.5)1.92O3TEM figure after 1050 DEG C of nano-phosphor roastings.
Fig. 4 is Eu prepared by embodiment 10.08Y1.92O3Nano-phosphor luminous intensity with Eu content relationship.
Fig. 5 is Eu prepared by embodiment 10.08Y1.92O3Nano-phosphor luminous intensity with maturing temperature relationship.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1
According to chemical composition Eu2xY2(1-x)O3(x=0.04) weigh micron order europium oxide, yttrium oxide powder is dissolved in nitric acid, boil Boiling evaporates extra nitric acid, adds the Eu (NO that deionized water is configured to 0.8mol/L3)3/Y(NO3)3Rare-earth salt solution；It will Dehydrated alcohol is separately added into rare-earth salt solution and ammonia spirit according to 20% volume ratio, respectively stirring, constant volume.At room temperature, Rare-earth salt solution and ammonia spirit are continuously injected into reactor from reactor inlet with the speed of 80L/h, at the same blender with The revolution of 2000rpm is vigorously stirred, and controls precipitation reaction pH value between 8.5-9.0；Sediment formed after immediately from reactor Outlet dynamic flows out, and obtains precursor pulp；Slurry is filtered, dehydrated alcohol washing drains, obtains solid sediment. Solid sediment is mixed with n-amyl alcohol, carries out decompression co-boiling distiling, the extra small scale europium that average grain diameter is 2-3nm is obtained and adulterates Yttrium oxide rare earth phosphor precursor powder；Precursor powder is Muffle kiln roasting obtains monodisperse, particle size is less than The europium doped yttrium oxide nano-phosphor of 10nm.
Embodiment 2
According to chemical composition Eu0.08(Y 0.5Gd0.5)1.92O3It is molten to weigh micron order europium oxide, gadolinium oxide and yttrium oxide powder It in nitric acid, boils and evaporates extra nitric acid, add the Eu (NO that deionized water is configured to 0.8mol/L3)3/Gd(NO3)3/Y (NO3)3Rare-earth salt solution；Dehydrated alcohol is separately added into rare-earth salt solution and ammonia spirit according to volume ratio 20%, is stirred respectively It mixes, constant volume.At room temperature, rare-earth salt solution and ammonia spirit are continuously injected from reactor inlet with the speed of 80L/h and is reacted Device, while blender is vigorously stirred with the revolution of 3000rpm, controls precipitation reaction pH value between 8.5-9.0；Sediment is formed It is flowed out immediately from reactor outlet dynamic afterwards, obtains precursor pulp；Slurry is filtered, dehydrated alcohol washing is drained, obtained To solid sediment.Solid sediment is mixed with n-amyl alcohol, carries out decompression co-boiling distiling, obtaining average grain diameter is 2-3nm's Extra small scale Eu0.08(Y0.5Gd0.5)1.92O3Rare earth phosphor precursor powder；Precursor powder obtains list in Muffle kiln roasting Dispersion, particle size are less than the Eu of 10nm0.08(Y0.5Gd0.5)1.92O3Nano-phosphor.
Embodiment 3
According to chemical composition Eu0.08Gd0.4Y1.52O3It weighs micron order europium oxide, gadolinium oxide, yttrium oxide powder and is dissolved in nitric acid, It boils and evaporates extra nitric acid, add the mischmetal salting liquid that deionized water is configured to 0.8mol/L；By dehydrated alcohol It is separately added into rare-earth salt solution and ammonia spirit according to 20% volume ratio, respectively stirring, constant volume.At room temperature, by rare-earth salts Solution and ammonia spirit continuously inject reactor from reactor inlet with the speed of 80L/h, while blender is turned with 3000rpm Number is vigorously stirred, and controls precipitation reaction pH value between 8.5-9.0；Sediment formed after immediately from reactor outlet dynamic stream Out, precursor pulp is obtained；Slurry is filtered, dehydrated alcohol washing drains, obtains solid sediment.Solid is precipitated Object is mixed with n-amyl alcohol, carries out decompression co-boiling distiling, obtains the extra small scale Eu that average grain diameter is 2-3nm0.08Gd0.4Y1.52O3It is dilute Native fluorescent powder precursor powder；Precursor powder obtains monodisperse, particle size less than 10nm's in Muffle kiln roasting Eu0.08Gd0.4Y1.52O3Nano-phosphor.
Comparative example 1
According to chemical composition Eu0.08Gd0.4Y1.52O3It weighs micron order europium oxide, gadolinium oxide, yttrium oxide powder and is dissolved in nitric acid, It boils and evaporates extra nitric acid, add the mischmetal salting liquid that deionized water is configured to 0.8mol/L；By dehydrated alcohol It is separately added into rare-earth salt solution and ammonia spirit according to 20% volume ratio, respectively stirring, constant volume.At room temperature, by rare-earth salts Solution and ammonia spirit instill reactor, are vigorously stirred with the revolution of 800rpm, control precipitation reaction pH value 8.5-9.0 it Between；Sediment is aged 1 hour after being formed, and is diluted sediment with a large amount of deionized waters, is obtained precursor pulp；Slurry was carried out Filter, dehydrated alcohol washing, drains, obtains solid sediment.Solid sediment is mixed with n-amyl alcohol, decompression azeotropic is carried out and steams It evaporates, obtains Eu0.08Gd0.4Y1.52O3Rare earth phosphor precursor powder；Precursor powder is obtained in Muffle kiln roasting Eu0.08Gd0.4Y1.52O3Nano-phosphor.Powder has reunion, and particle size is greater than 30nm.

Claims (5)

1. a kind of preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor, it is characterised in that: the preparation side Method includes the following steps:
A, micron order RE oxide powder is dissolved in nitric acid or hydrochloric acid, boils and evaporates extra nitric acid or hydrochloric acid, then plus Enter deionized water and is configured to rare-earth salt solution；Or using rare earth nitrades, sulfate, chloride as raw material to be configured to rare-earth salts molten Liquid；
The concentration of the rare-earth salt solution is 0.5mol/L-2.0mol/L；
B, dispersing agent dehydrated alcohol is separately added into above-mentioned rare-earth salt solution and ammonia spirit, stirring, constant volume；At room temperature, will Rare-earth salt solution and ammonia spirit continuously rapidly inject reactor, rare-earth salt solution and ammonia from reactor inlet with identical speed Aqueous solution is inscribed after touch in reactor, and moment forms white depositions in the presence of vigorous stirring；After white depositions are formed It is flowed out immediately from reactor outlet dynamic；White precipitate is filtered, dehydrated alcohol washing drains, obtains solid sediment；
The reactor is using the import of multiple groups reaction solution and generates liquid outlet, and inlet and outlet is alternately placed；
The process of the generation solid sediment orderly, is dynamically rapidly completed, and sediment is cleaned immediately after generating, filtered, nothing Ageing process；
C, solid sediment is mixed with n-amyl alcohol, carries out decompression co-boiling distiling, heating steams moisture completely, continues to distill To the extra small scale rare earth doped yttrium oxide base nano-phosphor precursor powder of white；Rare earth doped yttrium oxide base nano-phosphor Precursor powder obtains rare earth doped yttrium oxide base nano-phosphor in Muffle kiln roasting；
Solid state powder after the distillation maturing temperature in Muffle furnace are as follows: 900 DEG C -1250 DEG C, calcining time are as follows: 30 points Clock.
2. the preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor as described in claim 1, feature exist In: the chemical composition of micron order rare earth oxide described in step (a) is Eu2xGd2yY2(1-x-y)O3, wherein x=0.01-0.1, y =0-0.5；The amount of the dispersing agent dehydrated alcohol is respectively the 10-30% of rare-earth salt solution and ammonia spirit volume.
3. the preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor as described in claim 1, feature exist In: the concentration of rare-earth salt solution described in step (a) is between 0.8-1.2mol/1；The amount of dispersing agent dehydrated alcohol is respectively dilute The 20% of earth salt solution and ammonia spirit volume.
4. the preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor as described in claim 1, feature exist In: the speed of rare-earth salt solution described in step (b) and ammonia spirit injection reactor is 40L/h-200L/h；The stirring Speed is 800rpm-4000rpm；The precipitation reaction pH value is between 8-9.
5. the preparation method of extra small scale rare earth doped yttrium oxide base nano-phosphor as claimed in claim 4, feature exist In: the speed of rare-earth salt solution described in step (b) and ammonia spirit injection reactor is 80L/h-120L/h；Precipitation reaction Mixing speed in journey is 2000rpm-4000rpm.
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CN111017978A (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 holmium oxide for dielectric ceramic capacitor
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