CN105272252A - Fluorite-type Eu-doped Y2Ce2O7 nano ceramic pigment and preparation method - Google Patents

Fluorite-type Eu-doped Y2Ce2O7 nano ceramic pigment and preparation method Download PDF

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CN105272252A
CN105272252A CN201510820891.XA CN201510820891A CN105272252A CN 105272252 A CN105272252 A CN 105272252A CN 201510820891 A CN201510820891 A CN 201510820891A CN 105272252 A CN105272252 A CN 105272252A
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doping
ceramic pigment
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fluorite
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CN105272252B (en
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仝玉萍
杨中正
王慧贤
马军涛
韩爱红
符静
霍洪媛
王贝贝
程龄贺
严亮
张海龙
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North China University of Water Resources and Electric Power
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Abstract

The invention discloses a fluorite-type Eu-doped Y2Ce2O7 nano ceramic pigment with the structure of Y2Ce(2-x)EuxO7, wherein 0.05<=x<=0.30, preferably, 0.05<=x<=0.20, more preferably, 0.05<=x<=0.15, and most preferably, 0.05<=x<=0.10. The invention further discloses a preparation method of the fluorite-type Eu-doped Y2Ce2O7 nano ceramic pigment. Compared with the prior art, the fluorite-type Eu-doped Y2Ce2O7 nano ceramic pigment has the advantages of being good in heat stability and chemical stability, bright in color, changeless in color at high temperature; the preparation method has the advantages that the method is simple, the raw materials are easy to obtian, no toxic element is contained in products, and green and environmental protection are achieved; the obtained pigment is good in particle dispersibility, uniform in size distribution and good in color generation property; the synthesizing temperature is low, the technology is simple and controllable, and the pigment is suitable for scale production.

Description

A kind of fluorite type Eu doping Y2Ce2O7 nano-ceramic pigment and preparation method
Technical field
The invention belongs to beramic color field, particularly a kind of fluorite doping type superfine ceramic pigment and preparation method thereof.
Background technology
Along with the development of urban construction, urban environment exacerbated.It is reported, be often only the energy waste that construction industry causes and account for more than 23% of total energy loss, expecting the year two thousand twenty will reach 35%.Along with minimizing and the strong solar radiation of urban green space, heat accumulation forms " heat island " effect, exacerbates energy consumption further.Too can radiation by ~ 5% UV radiation, the visible radiation of 50% and 45% near-infrared radiation composition.The radiating capacity of the sun mainly concentrates on visible ray and near infrared two regions, and the attribute of pigment is the principal element affecting coating optical properties and near-infrared reflection.In recent years, increasing research interest concentrates on the research explored and have the roof Material of high infrared reflection.
Apply more for some complex metal oxides mineral dyes are as chrome green, cadmium stannate, lead chromate, cadmium yellow and metatitanic acid chrome yellow etc. in the market, be widely used as near-infrared reflection pigment.But most of pigment includes noxious metals, so be subject to a definite limitation when applying.Metal ion mixing is utilized to be one of method preparing colored organic pigments.So research and develop new environment-friendly near-infrared reflection pigment, to carry out alternative existing commercial pigments imperative.
Application number is that the patent application of 201110286954.X discloses a kind of Inorganic yellow pigment and preparation method thereof, and institute's invention pigment has Y 3 ~ xce xal 5o 12structure, bright in colour, Stability Analysis of Structures.But need in preparation process to carry out repetitive scrubbing to precipitated liquid, and complex operation step, the words of scale operation are difficult to ensure the quality of products, and cost is higher; And synthesis temperature is high, needs to calcine at 1000 ~ 1500 DEG C, be unfavorable for suitability for industrialized production.
It is reported, owing to having the f electronic shell of not filling up outside the electronic structure of rare earth element uniqueness and core, these unpaired electrons self have higher energy, can Selective absorber visible ray and painted, chromophoric effect is played, the corresponding tone of display rare earth element at pigment rare earth elements; On the other hand, rare earth element changes crystal phase structure as dopant ion and plays a part variable color, steady look to pigment and help look.
Summary of the invention
The present invention is the shortcoming in order to solve the problems of the technologies described above middle existence, provides fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment and preparation method thereof, enters Y by rare-earth europium doping 2ce 2o 7in lattice, synthesize the environment friendly inorganic pigment of high brightness at a lower temperature, be suitable for scale operation.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment, has Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.30, preferably 0.05≤x≤0.20, more preferably 0.05≤x≤0.15, optimally 0.05≤x≤0.10.
Above-mentioned fluorite type Eu doping Y 2ce 2o 7the preparation method of nano-ceramic pigment, comprises the following steps:
(1) be 2:(1.7 ~ 2 according to the mol ratio of Y:Ce:Eu): (0.3 ~ 0), get corresponding Yttrium trinitrate or cerous nitrate respectively, europium nitrate is dissolved in distilled water and obtains mixing solutions; Preferably the mol ratio of Y:Ce:Eu is 2:(1.7 ~ 1.95): (0.3 ~ 0.05); Y:(Ce+Eu) mol ratio is 1:1.15 ~ 1; More preferably Y:(Ce+Eu) mol ratio be 1:1;
(2) mixing solutions that above-mentioned steps (1) obtains is joined in the aqueous solution of glycine, wherein Gly:(Y+Ce+Eu): H 2o=2 ~ 3:1:300 ~ 600;
(3), after utilizing magnetic stirring apparatus that the mixing solutions in step (2) is stirred more than 1h at 50 DEG C ~ 70 DEG C, at 100 DEG C ~ 120 DEG C, burning is concentrated, obtains precursor powder; Preferably, utilize magnetic stirring apparatus that the mixing solutions in step (2) is stirred 1.5h ~ 2h at 60 DEG C, if the reaction times is less than 1 hour, product can not diffusion reaction fully, causes the mutually uneven of product.Stirring velocity is 80 revs/min ~ 100 revs/min, in order to make its Thorough combustion, obtains fluffy precursor powder, and preferably burning is concentrated at 120 DEG C, obtains precursor powder;
(4) precursor powder finally above-mentioned steps (3) obtained is directly with retort furnace calcining, and calcining temperature is 500 ~ 700 DEG C, calcines more than 2 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment; Preferred calcination temperature is 700 DEG C, and calcination time more preferably 2 ~ 4 hours, is also more preferably 3 ~ 4 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment, if calcining temperature is too low, the colourity of product is lower, if calcining temperature is more than 700 DEG C, the colourity of product does not have considerable change, but the words energy consumption of suitability for industrialized production will increase greatly.
In above-mentioned arbitrary technical scheme preferably, the tristimulus coordinates that the final beramic color obtained is determined according to CIE1976 colour code is: 700 DEG C time, L* is 60 ~ 80.
In above-mentioned arbitrary technical scheme preferably, the infrared reflection rate of the final beramic color obtained is more than 80%.
In above-mentioned arbitrary technical scheme preferably, the final beramic color granularity obtained is in 40 ~ 80 nanometers.
Compared with prior art, the present invention has actively useful effect:
1, gained pigment of the present invention has that Heat stability is good, chemical stability are good and bright in colour, the non-discoloring advantage of high temperature.
2, preparation method of the present invention is simple, and raw material is easy to get, not containing toxic element in product, and environmental protection.
3, good, the even particle size distribution of products therefrom particle dispersion of the present invention, colour generation is good; Synthesis temperature is low, and technique is simply controlled, is suitable for large-scale production.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is Y 2ce 2 ~ xeu xo 7the X-ray diffraction spectrogram of pigment, wherein, x=0,0.05,0.1,0.15,0.2,0.3, X-coordinate is diffraction angle, and ordinate zou is diffracted intensity;
Fig. 2 is Y under differing temps 2ce 1.9eu 0.1o 7the XRD figure of gained;
Fig. 3 a, 3b, 3c, 3d are Y 2ce 1.9eu 0.1o 7the scanning electron microscope (SEM) photograph of pigment different amplification;
Fig. 4 is Y 2ce 1.9eu 0.1o 7eDS collection of illustrative plates after calcining;
Fig. 5 is Y 2ce 1.9eu 0.1o 7surface scan collection of illustrative plates after calcining.
Embodiment
Embodiment 1:
A kind of fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment, has Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.30, preferably 0.05≤x≤0.20, more preferably 0.05≤x≤0.15, optimally 0.05≤x≤0.10.
This fluorite type Eu adulterates Y 2ce 2o 7the preparation method of nano-ceramic pigment, comprises the following steps:
(1) be 2:(1.7 ~ 2 according to the mol ratio of Y:Ce:Eu): (0.3 ~ 0), get corresponding Yttrium trinitrate or cerous nitrate respectively, europium nitrate is dissolved in distilled water and obtains mixing solutions; Preferably the mol ratio of Y:Ce:Eu is 2:(1.7 ~ 1.95): (0.3 ~ 0.05); Y:(Ce+Eu) mol ratio is 1:1.15 ~ 1; More preferably Y:(Ce+Eu) mol ratio be 1:1;
(2) mixing solutions that above-mentioned steps (1) obtains is joined in the aqueous solution of glycine, wherein Gly:(Y+Ce+Eu): H 2o=2 ~ 3:1:300 ~ 600;
(3), after utilizing magnetic stirring apparatus that the mixing solutions in step (2) is stirred more than 1h at 50 DEG C ~ 70 DEG C, at 100 DEG C ~ 120 DEG C, burning is concentrated, obtains precursor powder; Preferably, utilize magnetic stirring apparatus that the mixing solutions in step (2) is stirred 1.5h ~ 2h at 60 DEG C, if the reaction times is less than 1 hour, product can not diffusion reaction fully, causes the mutually uneven of product.Stirring velocity is 80 revs/min ~ 100 revs/min, in order to make its Thorough combustion, obtains fluffy precursor powder, and preferably burning is concentrated at 120 DEG C, obtains precursor powder;
(4) precursor powder finally above-mentioned steps (3) obtained is directly with retort furnace calcining, and calcining temperature is 500 ~ 700 DEG C, calcines more than 2 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment;
Preferred calcination temperature is 700 DEG C, and calcination time more preferably 2 ~ 4 hours, is also more preferably 3 ~ 4 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment, if calcining temperature is too low, the colourity of product is lower, if calcining temperature is more than 700 DEG C, the colourity of product does not have considerable change, but the words energy consumption of suitability for industrialized production will increase greatly.
embodiment 2
Glycine 3.603g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 5.081g cerous nitrate, 0.134g europium nitrate are added in 10ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, utilize magnetic stirring apparatus to stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 600 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.95eu 0.05o 7inorganic ceramic pigment.
embodiment 3
Glycine 3.603g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 4.950g cerous nitrate, 0.268g europium nitrate are added in 10ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 600 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.9eu 0.1o 7inorganic ceramic pigment.
embodiment 4
Glycine 5.4g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 4.820g cerous nitrate, 0.402g europium nitrate are added in 10ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 600 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.85eu 0.15o 7inorganic ceramic pigment.
embodiment 5
Glycine 3.603g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 4.690g cerous nitrate, 0.535g europium nitrate are added in 10ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 600 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.8eu 0.2o 7inorganic ceramic pigment.
embodiment 6
Glycine 5.4g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 4.429g cerous nitrate, 0.803g europium nitrate are added in 10ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 600 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.7eu 0.3o 7inorganic ceramic pigment.
embodiment 7
Glycine 3.603g is added in 50ml water and obtains solution A.4.596g Yttrium trinitrate, 5.081g cerous nitrate, 0.134g europium nitrate are added in 100ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 60 DEG C, stir to clarify solution C, utilize magnetic stirring apparatus to stir 1.5 hours with the speed of 80 revs/min ~ 100 revs/min.Then condensed combustion at 120 DEG C, obtains precursor powder.And by precursor powder 700 DEG C of calcinings 4 hours, obtain cubic fluorite doping type Y 2ce 1.95eu 0.05o 7inorganic ceramic pigment.
embodiment 8
Glycine 7.6056g is added in 180ml water and obtains solution A.7.661g Yttrium trinitrate, 7.38g cerous nitrate, 1.013g europium nitrate are added in 36ml water respectively.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are added in solution A successively, at 55 DEG C, stir to clarify solution C, stir 1.6 hours with the speed of 80 revs/min.Then condensed combustion at 100 DEG C, obtains precursor powder.And by precursor powder 500 DEG C of calcinings 2 hours, obtain cubic fluorite doping type Y 2ce 1.7eu 0.3o 7inorganic ceramic pigment.
Preferably, glycine: metal ion=2:1
Preferably, adopt Eu ion doping, doping ratio is 0.05≤x≤0.15.
Its structure of inorganic ceramic pigment synthesized by the present invention is cubic fluorite doping type.
test example
xRD tests
XRD analysis is carried out to the product prepared by different addition quantity, as shown in Figure 1.Result is known: when the volume x of Eu is 0.05 ~ 0.15 time, products therefrom structure and matrix completely the same, being only that the intensity at peak decreases, is the cubic fluorite structure of single-phase, and along with the increase of volume, its diffraction peak is more and more lower.When other conditions are all identical, under different calcining temperatures, the XRD figure of products therefrom as shown in Figure 2.Can find out at four temperature all can successful synthetic product, and along with the rising of temperature, the crystallinity of product is become better and better, and overall economic efficiency selects 600 DEG C for better calcining temperature.
test
By scanning electron microscope, micro-structural test is carried out to product, be illustrated in figure 3 Y 2ce 1.9eu 0.1o 7the SEM photo of pigment, it is good by the material scatter synthesized by this synthetic method that this photo illustrates, even particle size distribution, globule size is about 40 nanometers.For pigment, granularity is less, and particle specific surface is larger, and specific surface energy is higher, and material scatter is good in addition, in use easily forms uniform coating, and strong adhesion, evenness.
test
Carried out face moiety test by energy spectrometer to product, as shown in Figures 4 and 5, Fig. 4 is Y 2ce 1.9eu 0.1o 7the Surface scan energy spectrogram of nano material, the product after this figure illustrates doping is made up of element Y, Eu, Ce, O tetra-kinds of elements and surface arrangement is very even, does not occur chemical segregation phenomena.
colourity is tested
Carry out colourity test to pigment prepared in embodiment, result is as shown in table 1.Result shows, when the product adulterated through Eu, its L* value, all higher than before doping, illustrates that the brightness of doping after product reduces; Before and after a* doping, change is not obvious, and b* value is negative from just becoming, and illustrate that the blue degree of doping after product increases, yellowing reduces.The product colourity of the different amount of doping changes also little, and consider from the energy and economic angle, preferably, doping ratio is 0.05≤x≤0.10.
Y after table 1700 DEG C calcining 2ce 2 ~ xeu xo 7the color coordinates of pigment

Claims (9)

1. a fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment, is characterized in that: have Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.30.
2. the fluorite type Eu doping Y according to the claims 1 2ce 2o 7nano-ceramic pigment, is characterized in that: have Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.20.
3. the fluorite type Eu doping Y according to the claims 2 2ce 2o 7nano-ceramic pigment, is characterized in that, has Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.15.
4. the fluorite type Eu doping Y according to the claims 3 2ce 2o 7nano-ceramic pigment, is characterized in that: have Y 2ce 2 ~ xeu xo 7structure, wherein: 0.05≤x≤0.10.
5. the fluorite type Eu doping Y according to any one of claim 1 ~ 4 2ce 2o 7the preparation method of nano-ceramic pigment, comprises the following steps:
(1) be 2:(1.7 ~ 2 according to the mol ratio of Y:Ce:Eu): (0.3 ~ 0), get corresponding Yttrium trinitrate or cerous nitrate respectively, europium nitrate is dissolved in distilled water and obtains mixing solutions;
(2) mixing solutions that above-mentioned steps (1) obtains is joined in the aqueous solution of glycine, wherein Gly:(Y+Ce+Eu): H 2o=2 ~ 3:1:300 ~ 600;
(3), after utilizing magnetic stirring apparatus that the mixing solutions in step (2) is stirred more than 1h at 50 DEG C ~ 70 DEG C, at 100 DEG C ~ 120 DEG C, burning is concentrated, obtains precursor powder;
(4) precursor powder finally above-mentioned steps (3) obtained is directly with retort furnace calcining, and calcining temperature is 500 ~ 700 DEG C, calcines more than 2 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment.
6. fluorite type Eu doping Y according to claim 5 2ce 2o 7the preparation method of nano-ceramic pigment, it is characterized in that: described step (1) is 2:(1.7 ~ 1.95 according to the mol ratio of Y:Ce:Eu): (0.3 ~ 0.05), get corresponding Yttrium trinitrate or cerous nitrate respectively, europium nitrate is dissolved in distilled water and obtains mixing solutions.
7. fluorite type Eu doping Y according to claim 5 2ce 2o 7the preparation method of nano-ceramic pigment, is characterized in that: Y:(Ce+Eu in step (1)) mol ratio be 1 ~ 1.15:1.
8. fluorite type Eu doping Y according to claim 5 2ce 2o 7the preparation method of nano-ceramic pigment, it is characterized in that: Y:(Ce+Eu in step (1)) mol ratio be 1:1, after described step (3) utilizes magnetic stirring apparatus that the mixing solutions in step (2) is stirred 1.5h ~ 2h at 60 DEG C, at 120 DEG C, burning is concentrated, obtain precursor powder, in step (4), calcining temperature is 700 DEG C
Fluorite type Eu doping Y according to claim 5 2ce 2o 7the preparation method of nano-ceramic pigment, is characterized in that: the precursor powder that step (3) obtains by described step (4) directly with retort furnace calcining, is calcined 2 ~ 4 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment.
9. fluorite type Eu doping Y according to claim 5 2ce 2o 7the preparation method of nano-ceramic pigment, is characterized in that: in step (3), stirring velocity is 80 revs/min ~ 100 revs/min, and the precursor powder that step (3) obtains by described step (4) directly with retort furnace calcining, is calcined 3 ~ 4 hours, obtains fluorite type Eu doping Y 2ce 2o 7nano-ceramic pigment.
CN201510820891.XA 2015-11-24 2015-11-24 A kind of fluorite type Eu doping Y2Ce2O7 nano-ceramic pigments and preparation method Expired - Fee Related CN105272252B (en)

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CN107987558A (en) * 2017-12-05 2018-05-04 华北水利水电大学 A kind of flowers shape LaFexEu1-xO3/TiO2The preparation method of compound superfine red ceramic paint
CN107987559A (en) * 2017-12-05 2018-05-04 华北水利水电大学 A kind of spherical compound superfine red ceramic paint and preparation method thereof
CN108946818A (en) * 2018-08-23 2018-12-07 华北水利水电大学 A kind of preparation method of black inorganic ceramic paint
CN109401361A (en) * 2018-11-05 2019-03-01 郑州成功财经学院 A kind of preparation method of the white inorganic ceramic paint of pyrochlore constitution

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CN107987558A (en) * 2017-12-05 2018-05-04 华北水利水电大学 A kind of flowers shape LaFexEu1-xO3/TiO2The preparation method of compound superfine red ceramic paint
CN107987559A (en) * 2017-12-05 2018-05-04 华北水利水电大学 A kind of spherical compound superfine red ceramic paint and preparation method thereof
CN107987558B (en) * 2017-12-05 2020-03-31 华北水利水电大学 Flower cluster-shaped LaFexEu1-xO3/TiO2Preparation method of composite superfine red ceramic pigment
CN107987559B (en) * 2017-12-05 2020-04-07 华北水利水电大学 Spherical composite superfine red ceramic pigment and preparation method thereof
CN108946818A (en) * 2018-08-23 2018-12-07 华北水利水电大学 A kind of preparation method of black inorganic ceramic paint
CN109401361A (en) * 2018-11-05 2019-03-01 郑州成功财经学院 A kind of preparation method of the white inorganic ceramic paint of pyrochlore constitution

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