CN104710168A - Dysprosium-doped hexagonal yttrium aluminate ceramic powder and preparation method thereof - Google Patents
Dysprosium-doped hexagonal yttrium aluminate ceramic powder and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of ceramic materials, and particularly relates to a dysprosium-doped hexagonal yttrium aluminate ceramic powder and a preparation method thereof. The preparation method comprises the following steps: mixing dysprosium nitrate pentahydrate, yttrium nitrate hexahydrate, aluminum nitrate nonahydrate and citric acid monohydrate, dissolving in deionized water, adding ammonia water to regulate the pH value to 1-2, sufficiently stirring, evaporating water, and drying to obtain xerogel; carrying out heat treatment, ball milling and drying on the xerogel to obtain a precursor powder; and (2) putting the precursor powder into a graphite reactor, sintering in a discharge plasma sintering unit, cooling to room temperature after finishing sintering, and grinding to obtain the dysprosium-doped hexagonal yttrium aluminate ceramic powder. The method can obtain the Dy:YAH powder with uniform and small particle size of which the crystalline phase is single-phase YAH. The Dy:YAH powder has favorable sintering activity, and can be used for preparing fine-crystalline Dy:YAH powder or Dy:YAH ceramic at low temperature.
Description
Technical field
The invention belongs to the preparing technical field of stupalith, be specifically related to a kind of dysprosium doped six side yttrium aluminate ceramic powder and preparation method thereof.
Background technology
Y
2o
3-Al
2o
3system material obtains extensive research because having excellent optical property.Y
2o
3-Al
2o
3system material comprises YAlO
3(hexagonal system YAH or rhombic system YAP), Y
3al
5o
12(isometric system YAG) and Y
4al
2o
9(oblique system YAM).
The chemical formula of yttrium aluminum garnet (Yttrium aluminum garnet, YAG) is Y
3al
5o
12, fusing point is 1950 DEG C, belongs to isometric system, has garnet structure.YAG pottery has good thermostability, chemical stability, can be used as high-temperature structural material.Yttrium aluminum garnet has optical isotropy because of its centrosymmetric cubic crystal structure, and its theoretical optics transmitance can reach more than 84%, thus can be used as laser host material or fluorescence host material.YAG pottery is as laser gain material, and comparatively to have doping high for YAG monocrystalline, is easy to preparation, can the advantage such as production large size, complex-shaped product.Nineteen ninety-five, Ikesue utilizes the method for reaction sintering to prepare Nd:YAG crystalline ceramics, and first achieves Laser output.After this, YAG laser ceramics is widely studied, and current YAG laser ceramics maximum laser power reaches 67kW.In fluorescence ceramics, YAG fluorescence ceramics stable chemical nature at high temperature, overcomes conventional LED package material (mainly epoxy resin) and is easy to aging shortcoming, and packaging process is simple, is the potential equivalent material of LED encapsulation material.The Nishiura of Japan has prepared Ce:YAG crystalline ceramics, can excite lower generation sodium yellow at blue light, and the blue light of transmission is mixed to form white light with the sodium yellow inspired, and the LED luminous efficiency utilizing this pottery to assemble reaches 73.5lm/W.Dy:YAG pottery can under the exciting of UV-light generation blue light and sodium yellow, the two mixing and form white light, be fine ultraviolet excitation an illuminating material.
Preparation Dy:YAG pottery can have two kinds of methods, and one is raw material with oxide compound, utilizes the method for reaction sintering to prepare Dy:YAG pottery; Another kind prepares Dy:YAG powder with coprecipitation method or sol-gel combustion method, then prepares Dy:YAG pottery with Dy:YAG powder sintering.Prepare in the process of Dy:YAG powder in a kind of rear method, usually have the appearance of mesophase spherule YAH.
Gandhi etc. apply coprecipitation method and have prepared a series of Y
2o
3-Al
2o
3architecture compound, and have studied Y
3al
5o
12the powder phase transition process kinetics of proportioning raw materials.It thinks that YAG and YAH has two kinds of crystallization driving forces of vying each other, and the difference of preparation method determines and crystallization can form YAG or YAH; In addition, preparation method can affect the structure of unformed phase, and then affects the formation of YAH.Kakade utilizes sol-gel method to prepare in the process of YAG, and the powder obtained 930 DEG C of thermal treatments is the mixed phase of YAH and YAG, is converted into YAG phase at 1050 DEG C.Guo Xianzhong etc. prepares YAG powder with sol-gel method, and the powder obtained 830-905 DEG C of thermal treatment is the mixed phase of YAH and YAG, and the powder that thermal treatment obtains more than 905 DEG C is YAG phase.It thinks that the generation of YAH is the result of positively charged ion segregation, and in raw material, the mole ratio of citric acid and nitrate can affect the formation temperature of YAH.Hess also studied the phase in version process of YAG powder sol-gel method building-up process, and presoma is YAH and YAG mixed phase at the powder that 800-925 DEG C of short period of time thermal treatment obtains by it, extends soaking time or raise thermal treatment temp all can obtain YAG phase.With YAlO in its research
3and Y
3al
5o
12for the lattice parameter of the YAH phase of raw material ratio appearance is suitable, thus with Y
3al
5o
12in the YAH of the raw material appearance of proportioning, Al
2o
3independently exist with the form of unformed phase.
The research of comprehensive above document shows: YAH is the metastable state phase often occurred when wet chemistry method synthesis YAG, there is the Al of unformed phase in YAH
2o
3, be easy to transform to YAG, under given conditions, YAH only short period of time insulation appearance in narrow temperature range, thus needs strictly to control preparation condition.But these researchs often adopt traditional temperature-rising method, temperature rate is slow, long reaction time, and the powder obtained is the mixed phase of YAH and YAG, be difficult to obtain pure phase YAH powder, and rear-earth-doped YAH also rare report.Thus, the Dy:YAH powder that synthesize, needs to explore new preparation method.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, object is to provide a kind of dysprosium doped six side yttrium aluminate ceramic powder and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
A preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium are mixed, be dissolved in deionized water, add ammoniacal liquor and regulate pH to be 1 ~ 2, after fully stirring, after transpiring moisture, drying, obtain xerogel; Xerogel obtains precursor after thermal treatment, ball milling drying;
(2) precursor is put in graphiote reactor, be placed in discharging plasma sintering equipment and sinter, terminate rear powder and be cooled to room temperature, then obtain dysprosium doped six side yttrium aluminate ceramic powder through grinding.
By such scheme, the mol ratio of described five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium is 3 × x%:3 × (1-x%): 5:4, and wherein the span of x is: 0.5≤x≤6.
By such scheme, described in be sintered to: the temperature being warmed up to 800 DEG C ~ 840 DEG C with the temperature rise rate of 50 ~ 200 DEG C/min, insulation 1 ~ 10min.
By such scheme, described in be sintered to: the temperature being warmed up to 810 DEG C ~ 830 DEG C with the temperature rise rate of 100 ~ 150 DEG C/min, insulation 3 ~ 5min.
By such scheme, in sintering process, in described graphiote reactor, keep nonoxidizing atmosphere.
By above-mentioned aspect, the heat treated temperature of described xerogel is 700 DEG C ~ 740 DEG C.
By such scheme, the particle diameter of the dysprosium doped six side yttrium aluminate ceramic powder obtained after described grinding is less than 3 microns.
The dysprosium doped six side yttrium aluminate ceramic powder that above-mentioned preparation method prepares.
Beneficial effect of the present invention is as follows: the present invention with five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium for raw material (Dy
3 × x%y
3 × (1-x%)al
5o
12proportioning raw materials), adopt the method for discharge plasma sintering, prepared by controlling the condition such as thermal treatment temp, temperature rise rate, soaking time the metastable phase powder Dy:YAH powder that prior heat treatment method cannot obtain, described Dy:YAH powder is that uniform particle sizes is tiny, crystallization phases is single-phase YAH (YAlO
3) Dy:YAH powder, this Dy:YAH powder has good sintering activity, can be applied to the thin brilliant Dy:YAG powder of low-temperature growth or Dy:YAG pottery.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of the dysprosium doped six side yttrium aluminate ceramic powder (Dy:YAH powder) that the invention process example 1 ~ 4 obtains, and wherein 1 is embodiment 1, and 2 is embodiment 2, and 3 is embodiment 3, and 4 is embodiment 4.
Fig. 2 is the SEM shape appearance figure of the dysprosium doped six side yttrium aluminate ceramic powder (Dy:YAH powder) that the invention process example 1 obtains.
Fig. 3 is the SEM shape appearance figure of the dysprosium doped six side yttrium aluminate ceramic powder (Dy:YAH powder) that the invention process example 2 obtains.
Fig. 4 is the SEM shape appearance figure of the dysprosium doped six side yttrium aluminate ceramic powder (Dy:YAH powder) that the invention process example 3 obtains.
Fig. 5 is the SEM shape appearance figure of the dysprosium doped six side yttrium aluminate ceramic powder (Dy:YAH powder) that the invention process example 4 obtains.
Fig. 6 is the XRD diffracting spectrum of dysprosium doped yttrium aluminum garnet (Dy:YAG) pottery that the invention process example 1 ~ 4 obtains, and wherein 1 is embodiment 1, and 2 is embodiment 2, and 3 is embodiment 3, and 4 is embodiment 4.
Fig. 7 is the SEM shape appearance figure of the dysprosium doped yttrium aluminum garnet pottery (Dy:YAG pottery) that the invention process example 1 obtains.
Fig. 8 is the SEM shape appearance figure of the dysprosium doped yttrium aluminum garnet pottery (Dy:YAG pottery) that the invention process example 2 obtains.
Fig. 9 is the SEM shape appearance figure of the dysprosium doped yttrium aluminum garnet pottery (Dy:YAG pottery) that the invention process example 3 obtains.
Figure 10 is the SEM shape appearance figure of the dysprosium doped yttrium aluminum garnet pottery (Dy:YAG pottery) that the invention process example 4 obtains.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
A preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) by five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium according to mol ratio be 0.5%:3 (1-0.5%): 5:4 mixing, be dissolved in deionized water, adding ammoniacal liquor regulates pH to be 1, after fully stirring, obtains xerogel after transpiring moisture, drying; Xerogel is placed in retort furnace 700 DEG C of thermal treatments, after ball milling drying, obtains precursor;
(2) precursor is placed in graphiote reactor, graphiote reactor is placed in big current reaction unit (discharging plasma sintering equipment), the atmosphere in graphiote reactor is kept to be nonoxidizing atmosphere, pulsed current is applied to graphiote reactor, it is made to be warmed up to the temperature of 800 DEG C with the temperature rise rate of 50 DEG C/min, insulation 1min, cools to room temperature with the furnace; Ground by above-mentioned powder, milling time is 10min, obtains dysprosium doped six side yttrium aluminate ceramic powder.
The XRD diffracting spectrum of dysprosium doped six side yttrium aluminate ceramic powder prepared by the present invention, see accompanying drawing 1, is six side YAH phases, and the median size of sem analysis display powder is 3 μm, see accompanying drawing 2, namely obtains the Dy:YAH powder that crystallization phases is single-phase YAH.
Take the above-mentioned Dy:YAH powder of 2.45g, be placed in the graphite jig that diameter is 15mm, adopt the method for discharge plasma sintering, be warming up to 950 DEG C with the temperature rise rate of 100 DEG C/min, in vacuum environment, be incubated 3min, obtain Dy:YAG pottery.Its XRD diffracting spectrum is shown in Fig. 7 see accompanying drawing 6, SEM shape appearance figure, Fig. 6 show Dy:YAG pottery for cube YAG phase, SEM figure show pottery average grain size be 300nm.
Embodiment 2
A preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) by five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium according to mol ratio be 2%:3 (1-2%): 5:4 mixing, be dissolved in deionized water, adding ammoniacal liquor regulates pH to be 1.5, after fully stirring, obtains xerogel after transpiring moisture, drying; Xerogel is placed in retort furnace 740 DEG C of thermal treatments, after ball milling drying, obtains precursor;
(2) precursor is placed in graphiote reactor, graphiote reactor is placed in big current reaction unit (discharging plasma sintering equipment), the atmosphere in graphiote reactor is kept to be nonoxidizing atmosphere, pulsed current is applied to graphiote reactor, it is made to be warmed up to the temperature of 840 DEG C with the temperature rise rate of 200 DEG C/min, insulation 10min, cools to room temperature with the furnace; Ground by above-mentioned powder, milling time is 20min, obtains dysprosium doped six side yttrium aluminate ceramic powder.
The XRD diffracting spectrum of dysprosium doped six side yttrium aluminate ceramic powder prepared by the present invention, see accompanying drawing 1, is six side YAH phases, and the median size of sem analysis display powder is 3 μm, see accompanying drawing 3, namely obtains the Dy:YAH powder that crystallization phases is single-phase YAH.
Take the above-mentioned Dy:YAH powder of 2.45g, be placed in the graphite jig that diameter is 15mm, adopt the method for discharge plasma sintering, be warming up to 1000 DEG C with the temperature rise rate of 100 DEG C/min, in vacuum environment, be incubated 3min, obtain Dy:YAG pottery.Its XRD diffracting spectrum is shown in Fig. 8 see accompanying drawing 6, SEM shape appearance figure, Fig. 6 show Dy:YAG pottery for cube YAG phase, SEM figure show pottery average grain size be 600nm.
Embodiment 3
A preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) by five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium according to mol ratio be 4%:3 (1-4%): 5:4 mixing, be dissolved in deionized water, adding ammoniacal liquor regulates pH to be 2, after fully stirring, obtains xerogel after transpiring moisture, drying; Xerogel is placed in retort furnace 720 DEG C of thermal treatments, after ball milling drying, obtains precursor;
(2) precursor is placed in graphiote reactor, graphiote reactor is placed in big current reaction unit (discharging plasma sintering equipment), the atmosphere in graphiote reactor is kept to be nonoxidizing atmosphere, pulsed current is applied to graphiote reactor, it is made to be warmed up to the temperature of 810 DEG C with the temperature rise rate of 100 DEG C/min, insulation 3min, cools to room temperature with the furnace; Ground by above-mentioned powder, milling time is 15min, obtains dysprosium doped six side yttrium aluminate ceramic powder.
The XRD diffracting spectrum of dysprosium doped six side yttrium aluminate ceramic powder prepared by the present invention, see accompanying drawing 1, is six side YAH phases, and the median size of sem analysis display powder is 1 μm, see accompanying drawing 4, namely obtains the Dy:YAH powder that crystallization phases is single-phase YAH.
Take the above-mentioned Dy:YAH powder of 2.45g, be placed in the graphite jig that diameter is 15mm, adopt the method for discharge plasma sintering, be warming up to 950 DEG C with the temperature rise rate of 100 DEG C/min, in vacuum environment, be incubated 3min, obtain Dy:YAG pottery.Its XRD diffracting spectrum is shown in Fig. 9 see accompanying drawing 6, SEM shape appearance figure, Fig. 6 show Dy:YAG pottery for cube YAG phase, SEM figure show pottery average grain size be 480nm.
Embodiment 4
A preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) by five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium according to mol ratio be 6%:3 (1-6%): 5:4 mixing, be dissolved in deionized water, adding ammoniacal liquor regulates pH to be 2, after fully stirring, obtains xerogel after transpiring moisture, drying; Xerogel is placed in retort furnace 740 DEG C of thermal treatments, after ball milling drying, obtains precursor;
(2) precursor is placed in graphiote reactor, graphiote reactor is placed in big current reaction unit (discharging plasma sintering equipment), the atmosphere in graphiote reactor is kept to be nonoxidizing atmosphere, pulsed current is applied to graphiote reactor, it is made to be warmed up to the temperature of 830 DEG C with the temperature rise rate of 150 DEG C/min, insulation 5min, cools to room temperature with the furnace; Ground by above-mentioned powder, milling time is 20min, obtains dysprosium doped six side yttrium aluminate ceramic powder.
The XRD diffracting spectrum of dysprosium doped six side yttrium aluminate ceramic powder prepared by the present invention, see accompanying drawing 1, is six side YAH phases, and the median size of sem analysis display powder is 1 μm, see accompanying drawing 5, namely obtains the Dy:YAH powder that crystallization phases is single-phase YAH.
Take the above-mentioned Dy:YAH powder of 2.45g, be placed in the graphite jig that diameter is 15mm, adopt the method for discharge plasma sintering, be warming up to 1000 DEG C with the temperature rise rate of 100 DEG C/min, in vacuum environment, be incubated 3min, obtain Dy:YAG pottery.Its XRD diffracting spectrum is shown in Figure 10 see accompanying drawing 6, SEM shape appearance figure, Fig. 6 show Dy:YAG pottery for cube YAG phase, SEM figure show pottery average grain size be 500nm.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And therefore amplified apparent change or variation are still within the protection domain of the invention.
Claims (8)
1. a preparation method for dysprosium doped six side yttrium aluminate ceramic powder, is characterized in that, comprise the steps:
(1) five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium are mixed, be dissolved in deionized water, add ammoniacal liquor and regulate pH to be 1 ~ 2, after fully stirring, after transpiring moisture, drying, obtain xerogel; Xerogel obtains precursor after thermal treatment, ball milling drying;
(2) precursor is put in graphiote reactor, be placed in discharging plasma sintering equipment and sinter, terminate rear powder and be cooled to room temperature, then obtain dysprosium doped six side yttrium aluminate ceramic powder through grinding.
2. preparation method according to claim 1, is characterized in that, the mol ratio of described five water Dysprosium trinitrates, six water Yttrium trinitrates, nine water aluminum nitrates and monohydrate potassium is 3 × x%:3 × (1-x%): 5:4, wherein 0.5≤x≤6.
3. preparation method according to claim 1, is characterized in that, described in be sintered to: the temperature being warmed up to 800 DEG C ~ 840 DEG C with the temperature rise rate of 50 ~ 200 DEG C/min, insulation 1 ~ 10min.
4. preparation method according to claim 3, is characterized in that, described in be sintered to: the temperature being warmed up to 810 DEG C ~ 830 DEG C with the temperature rise rate of 100 ~ 150 DEG C/min, insulation 3 ~ 5min.
5. preparation method according to claim 1, is characterized in that, in sintering process, keeps nonoxidizing atmosphere in described graphiote reactor.
6. preparation method according to claim 1, is characterized in that, the heat treated temperature of step (1) described xerogel is 700 DEG C ~ 740 DEG C.
7. preparation method according to claim 1, is characterized in that, the particle diameter of the dysprosium doped six side yttrium aluminate ceramic powder obtained after step (2) described grinding is less than 3 microns.
8. the dysprosium doped six side yttrium aluminate ceramic powder prepared by the arbitrary described preparation method of claim 1 ~ 7.
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| CN107335442A (en) * | 2017-06-23 | 2017-11-10 | 常州大学 | Composite photocatalyst material and its preparation method and application is changed on a kind of Er ions yttrium aluminate/concave convex rod |
| CN110734285A (en) * | 2019-11-06 | 2020-01-31 | 常州大学 | liquid phase combustion for preparing multi-principal-element ABO3Method for producing perovskite-structured ceramic |
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| CN107335442A (en) * | 2017-06-23 | 2017-11-10 | 常州大学 | Composite photocatalyst material and its preparation method and application is changed on a kind of Er ions yttrium aluminate/concave convex rod |
| CN110734285A (en) * | 2019-11-06 | 2020-01-31 | 常州大学 | liquid phase combustion for preparing multi-principal-element ABO3Method for producing perovskite-structured ceramic |
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Application publication date: 20150617 |