CN105272252B - A kind of fluorite type Eu doping Y2Ce2O7 nano-ceramic pigments and preparation method - Google Patents
A kind of fluorite type Eu doping Y2Ce2O7 nano-ceramic pigments and preparation method Download PDFInfo
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- CN105272252B CN105272252B CN201510820891.XA CN201510820891A CN105272252B CN 105272252 B CN105272252 B CN 105272252B CN 201510820891 A CN201510820891 A CN 201510820891A CN 105272252 B CN105272252 B CN 105272252B
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Abstract
The present invention discloses a kind of fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment has Y2Ce2~xEuxO7Structure, 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.Fluorite type Eu doping Y is also disclosed2Ce2O7The preparation method of nano-ceramic pigment.Compared with prior art, the invention has the advantages that：1, present invention gained pigment have the advantages that thermal stability is good, chemical stability is good and it is bright in colour, high temperature is non-discolouring.2, preparation method of the present invention is simple, and raw material is easy to get, and toxic element is free of in product, environmentally protective.3, products therefrom particle good dispersion of the present invention, even particle size distribution, colour generation are good；Synthesis temperature is low, simple for process controllable, is suitable for large-scale production.
Description
Technical field
The invention belongs to ceramic paint field, more particularly to a kind of fluorite doping type superfine ceramic pigment and its preparation side
Method.
Background technology
With the continuous development of urban construction, urban environment is exacerbated.It is reported that being often only energy caused by construction industry
Loss accounts for 23% or more of gross energy loss, it is contemplated that is up to 35% to the year two thousand twenty.Reduction with urban green space and the strong sun
Radiation, heat are assembled to form " heat island " effect, have been further exacerbated by energy consumption.It can radiate very much and be radiated by ~ 5% UV, 50%
Visible radiation and 45% near-infrared radiation composition.The radiation energy of the sun focuses primarily upon two regions of visible light and near-infrared, face
The attribute of material is the principal element for influencing coating optical properties and near-infrared reflection.In recent years, more and more research interests
Concentrate on exploring the research of the roof Material with high infrared reflection.
Currently on the market apply it is more for some metal composite oxide inorganic pigments for example chrome green, cadmium stannate, plumbous chromate,
Cadmium yellow and metatitanic acid chrome yellow etc. are widely used as near-infrared reflection pigment.However, most of pigment includes toxic metals, institute
To be subject to certain restrictions in application.It is one of the method for preparing colored organic pigments using metal ion mixing.So research and development
New environmental-friendly near-infrared reflection pigment is imperative to substitute existing commercial pigments.
Application No. is a kind of Inorganic yellow pigments of the patent application publication of 201110286954.X and preparation method thereof, are sent out
Bright pigment has Y3~xCexAl5O12Structure, bright in colour, stable structure.But it needs to carry out precipitated liquid in preparation process
It washs repeatedly, and complex for operation step, quality is difficult to ensure if large-scale production, and cost is higher；And synthesis temperature is high,
It needs to calcine at 1000 ~ 1500 DEG C, is unfavorable for industrialized production.
It is reported that due to having unfilled f electronic shell outside the unique electronic structure, that is, core of rare earth element, these are not electric in pairs
Son itself has higher energy, can select to absorb visible light and colour, play chromophore in pigment rare earth elements,
Show the corresponding tone of rare earth element；On the other hand, rare earth element plays change as Doped ions change crystal phase structure to pigment
Color, steady color and the effect for helping color.
Invention content
The present invention be in order to solve the above-mentioned technical problem present in disadvantage, provide fluorite type Eu doping Y2Ce2O7Nanometer
Rare-earth europium doping is entered Y by ceramic paint and preparation method thereof2Ce2O7In lattice, high brightness has been synthesized at a lower temperature
Environment friendly inorganic pigment, be suitable for large-scale production.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment has Y2Ce2-xEuxO7Structure, 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 adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, includes the following steps：
（1）According to Y：Ce：The molar ratio of Eu is 2: (1.7~2):(0.3 ~ 0) takes corresponding yttrium nitrate or nitric acid respectively
Cerium, europium nitrate are dissolved in distilled water and obtain mixed solution；Preferably Y：Ce：The molar ratio of Eu is 2: (1.7~1.95): (0.3~
0.05)；Y:(Ce+Eu) molar ratio is 1：1.15~1；More preferable Y:(Ce+Eu) molar ratio is 1：1；
（2）By above-mentioned steps（1）Obtained mixed solution is added in the aqueous solution of glycine, wherein Gly：（Y+Ce+
Eu）：H2O =2~3: 1: 300~600；
（3）Utilize magnetic stirring apparatus by step at 50 DEG C ~ 70 DEG C（2）In mixed solution stirring 1h or more after, 100
DEG C ~ 120 DEG C at burn concentration, obtain precursor powder；Preferably, utilize magnetic stirring apparatus by step at 60 DEG C（2）In
Mixed solution stir 1.5h ~ 2h, if the reaction time be less than 1 hour, product cannot sufficient diffusion reaction, lead to the phase of product
It is uneven.Mixing speed is 80 revs/min ~ 100 revs/min, in order to make it fully burn, obtains fluffy precursor powder, excellent
Concentration of burning at 120 DEG C is selected, precursor powder is obtained；
（4）Finally by above-mentioned steps（3）Obtained precursor powder is directly calcined with Muffle furnace, calcination temperature be 500~
700 DEG C, calcine 2 hours or more, obtain fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment；Preferred calcination temperature is 700 DEG C, is forged
It burns more preferable 2 ~ 4 hours of time, still more preferably 3 ~ 4 hours, obtains fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment, if
Calcination temperature is too low, and the coloration of product is relatively low, if calcination temperature is more than 700 DEG C, the coloration of product does not have significant change, still
Energy consumption will greatly increase if industrialized production.
In any of the above-described technical solution preferably, the ceramic paint finally obtained is determined according to 1976 colour codes of CIE
Chromaticity coordinate is：At 700 DEG C, L* is 60 ~ 80.
In any of the above-described technical solution preferably, the infrared reflection rate of the ceramic paint finally obtained be 80% with
On.
In any of the above-described technical solution preferably, the ceramic paint granularity finally obtained is at 40 ~ 80 nanometers.
Compared with prior art, the invention has the advantages that：
1, it is excellent to have that thermal stability is good, chemical stability is good and bright in colour, high temperature is non-discolouring for present invention gained pigment
Point.
2, preparation method of the present invention is simple, and raw material is easy to get, and toxic element is free of in product, environmentally protective.
3, products therefrom particle good dispersion of the present invention, even particle size distribution, colour generation are good；Synthesis temperature is low, technique letter
It is single controllable, it is suitable for large-scale production.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is Y2Ce2-xEuxO7The X-ray diffraction spectrogram of pigment, wherein x=0,0.05,0.1,0.15,0.2,0.3, it is horizontal
Coordinate is the angle of diffraction, and ordinate is diffracted intensity；
Fig. 2 is Y under different temperatures2Ce1.9Eu0.1O7The XRD diagram of gained；
Fig. 3 a, 3b, 3c, 3d are Y2Ce1.9Eu0.1O7The scanning electron microscope (SEM) photograph of pigment different amplification；
Fig. 4 is Y2Ce1.9Eu0.1O7EDS collection of illustrative plates after calcining；
Fig. 5 is Y2Ce1.9Eu0.1O7Surface scan collection of illustrative plates after calcining.
Specific implementation mode
Embodiment 1:
A kind of fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment has Y2Ce2-xEuxO7Structure, 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.
Fluorite type Eu adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, includes the following steps：
（1）According to Y：Ce：The molar ratio of Eu is 2: (1.7~2):(0.3 ~ 0) takes corresponding yttrium nitrate or nitric acid respectively
Cerium, europium nitrate are dissolved in distilled water and obtain mixed solution；Preferably Y：Ce：The molar ratio of Eu is 2: (1.7~1.95): (0.3~
0.05)；Y:(Ce+Eu) molar ratio is 1：1.15~1；More preferable Y:(Ce+Eu) molar ratio is 1：1；
（2）By above-mentioned steps（1）Obtained mixed solution is added in the aqueous solution of glycine, wherein Gly：（Y+Ce+
Eu）：H2O =2~3: 1: 300~600；
（3）Utilize magnetic stirring apparatus by step at 50 DEG C ~ 70 DEG C（2）In mixed solution stirring 1h or more after, 100
DEG C ~ 120 DEG C at burn concentration, obtain precursor powder；Preferably, utilize magnetic stirring apparatus by step at 60 DEG C（2）In
Mixed solution stir 1.5h ~ 2h, if the reaction time be less than 1 hour, product cannot sufficient diffusion reaction, lead to the phase of product
It is uneven.Mixing speed is 80 revs/min ~ 100 revs/min, in order to make it fully burn, obtains fluffy precursor powder, excellent
Concentration of burning at 120 DEG C is selected, precursor powder is obtained；
（4）Finally by above-mentioned steps（3）Obtained precursor powder is directly calcined with Muffle furnace, calcination temperature be 500~
700 DEG C, calcine 2 hours or more, obtain fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment；
Preferred calcination temperature is 700 DEG C, and more preferable 2 ~ 4 hours of calcination time still more preferably 3 ~ 4 hours, obtains fluorite
Type Eu adulterates Y2Ce2O7Nano-ceramic pigment, if calcination temperature is too low, the coloration of product is relatively low, if calcination temperature is more than
700 DEG C, the coloration of product does not have significant change, but energy consumption will greatly increase if industrialized production.
Embodiment 2
Glycine 3.603g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 5.081g cerous nitrates,
0.134g europium nitrates are added to respectively in 10ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, it is small with 80 revs/min ~ 100 revs/min of speed stirring 1.5 using magnetic stirring apparatus
When.Then the condensed combustion at 120 DEG C, obtains precursor powder.And calcine precursor powder 4 hours at 600 DEG C, it is stood
Square fluorite doping type Y2Ce1.95Eu0.05O7Inorganic ceramic pigment.
Embodiment 3
Glycine 3.603g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 4.950g cerous nitrates,
0.268g europium nitrates are added to respectively in 10ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, is stirred 1.5 hours with 80 revs/min ~ 100 revs/min of speed.Then at 120 DEG C
Lower condensed combustion, obtains precursor powder.And calcine precursor powder 4 hours at 600 DEG C, obtain cubic fluorite doping type
Y2Ce1.9Eu0.1O7Inorganic ceramic pigment.
Embodiment 4
Glycine 5.4g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 4.820g cerous nitrates,
0.402g europium nitrates are added to respectively in 10ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, is stirred 1.5 hours with 80 revs/min ~ 100 revs/min of speed.Then at 120 DEG C
Lower condensed combustion, obtains precursor powder.And calcine precursor powder 4 hours at 600 DEG C, obtain cubic fluorite doping type
Y2Ce1.85Eu0.15O7Inorganic ceramic pigment.
Embodiment 5
Glycine 3.603g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 4.690g cerous nitrates,
0.535g europium nitrates are added to respectively in 10ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, is stirred 1.5 hours with 80 revs/min ~ 100 revs/min of speed.Then at 120 DEG C
Lower condensed combustion, obtains precursor powder.And calcine precursor powder 4 hours at 600 DEG C, obtain cubic fluorite doping type
Y2Ce1.8Eu0.2O7Inorganic ceramic pigment.
Embodiment 6
Glycine 5.4g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 4.429g cerous nitrates,
0.803g europium nitrates are added to respectively in 10ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, is stirred 1.5 hours with 80 revs/min ~ 100 revs/min of speed.Then at 120 DEG C
Lower condensed combustion, obtains precursor powder.And calcine precursor powder 4 hours at 600 DEG C, obtain cubic fluorite doping type
Y2Ce1.7Eu0.3O7Inorganic ceramic pigment.
Embodiment 7
Glycine 3.603g is added in 50ml water and obtains solution A.By 4.596g yttrium nitrates, 5.081g cerous nitrates,
0.134g europium nitrates are added to respectively in 100ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 60 DEG C, it is small with 80 revs/min ~ 100 revs/min of speed stirring 1.5 using magnetic stirring apparatus
When.Then the condensed combustion at 120 DEG C, obtains precursor powder.And calcine precursor powder 4 hours at 700 DEG C, it is stood
Square fluorite doping type Y2Ce1.95Eu0.05O7Inorganic ceramic pigment.
Embodiment 8
Glycine 7.6056g is added in 180ml water and obtains solution A.By 7.661g yttrium nitrates, 7.38g cerous nitrates,
1.013g europium nitrates are added to respectively in 36ml water.Yttrium nitrate solution, cerous nitrate solution and europium nitrate solution are sequentially added molten
In liquid A, solution C is stirred to clarify at 55 DEG C, is stirred 1.6 hours with 80 revs/min of speed.Then combustion is concentrated at 100 DEG C
It burns, obtains precursor powder.And calcine precursor powder 2 hours at 500 DEG C, obtain cubic fluorite doping type
Y2Ce1.7Eu0.3O7Inorganic ceramic pigment.
Preferably, glycine：Metal ion=2:1
Preferably, using Eu ion dopings, 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 is tested
XRD analysis is carried out to the product prepared by different addition quantity, as shown in Figure 1.As a result known to：When the volume x of Eu exists
When 0.05 ~ 0.15, products therefrom structure and matrix are completely the same, and only the intensity at peak decreases, and are cube of single-phase
Fluorite type structure, and with the increase of volume, diffraction maximum is lower and lower.When other conditions are all identical, different calcining temperature
The XRD diagram of the lower products therefrom of degree is as shown in Figure 2.Can be seen that at four temperature can successful synthetic product, with the raising of temperature,
The crystallinity of product is become better and better, overall economic efficiency select 600 DEG C for preferable calcination temperature.
Test
Micro-structural test is carried out to product by scanning electron microscope, is illustrated in figure 3 Y2Ce1.9Eu0.1O7The SEM of pigment shines
Piece, it is good by the material scatter synthesized by the synthetic method which illustrates, even particle size distribution, and granule size is about 40 to receive
Rice.For pigment, granularity is smaller, and particle specific surface is bigger, and specific surface energy is higher, and material scatter is good in addition, is using
Uniform coating, and strong adhesive force, evenness are easily formed in the process.
Test
Face constituent test, as shown in Figures 4 and 5, Fig. 4 Y have been carried out to product by energy disperse spectroscopy2Ce1.9Eu0.1O7It receives
The Surface scan energy spectrum diagram of rice material, the figure illustrate that the product after doping is made of tetra- kinds of elements of element Y, Eu, Ce, O and surface is divided
Cloth is visibly homogeneous, chemical segregation phenomena does not occur.
Coloration is tested
Coloration test is carried out to pigment prepared in embodiment, the results are shown in Table 1.The result shows that being adulterated when through Eu
Product, before L* values are above doping, illustrate doping after product brightness reduce；A* doping is front and back to change unobvious, b* values
From just becoming negative, illustrate that the blue degree increase of product after doping, yellowing reduce.Different amounts of product coloration is adulterated to change and little,
From the point of view of the energy and economy, it is preferable that doping ratio is 0.05≤x≤0.10.
Y after 1 700 DEG C of calcinings of table2Ce2-xEuxO7The color coordinates of pigment
Claims (4)
1. a kind of fluorite type Eu adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, it is characterised in that：
The fluorite type Eu adulterates Y2Ce2O7Nano-ceramic pigment has Y2Ce2~xEuxO7Structure, wherein：0.05≤x≤
0.30；
The fluorite type Eu adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, includes the following steps：
（1）According to Y：Ce：The molar ratio of Eu is 2: (1.7~1.95):(0.3 ~ 0.05) takes corresponding yttrium nitrate or nitre respectively
Sour cerium, europium nitrate are dissolved in distilled water and obtain mixed solution；
（2）By above-mentioned steps（1）Obtained mixed solution is added in the aqueous solution of glycine, wherein Gly：（Y+Ce+Eu）：H2O
=2~3: 1: 300~600；
（3）Utilize magnetic stirring apparatus by step at 50 DEG C ~ 70 DEG C（2）In mixed solution stirring 1h or more after, 100 DEG C ~
It burns and concentrates at 120 DEG C, obtain precursor powder；
（4）Finally by above-mentioned steps（3）Obtained precursor powder is directly calcined with Muffle furnace, and calcination temperature is 500~700
DEG C, calcine 2 hours or more, obtain fluorite type Eu doping Y2Ce2O7Nano-ceramic pigment.
2. fluorite type Eu according to claim 1 adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, it is characterised in that：
The step（1）Middle Y:(Ce+Eu) molar ratio is 1：1, the step（3）Utilize magnetic stirring apparatus by step at 60 DEG C
（2）In mixed solution stirring 1.5h ~ 2 h after, concentration of burning at 120 DEG C obtains precursor powder, step（4）Middle calcining temperature
Degree is 700 DEG C；The step（4）By step（3）Obtained precursor powder is directly calcined with Muffle furnace, is calcined 2 ~ 4 hours, is obtained
Y is adulterated to fluorite type Eu2Ce2O7Nano-ceramic pigment；Step（3）Middle mixing speed is 80 revs/min ~ 100 revs/min.
3. fluorite type Eu according to claim 1 adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, it is characterised in that：
The step（4）By step（3）Obtained precursor powder is directly calcined with Muffle furnace, is calcined 3 ~ 4 hours, is obtained fluorite type Eu
Adulterate Y2Ce2O7Nano-ceramic pigment.
4. fluorite type Eu according to claim 1 adulterates Y2Ce2O7The preparation method of nano-ceramic pigment, it is characterised in that：
Y:(Ce+Eu) molar ratio is 1：1, utilize magnetic stirring apparatus by step at 60 DEG C（2）In mixed solution stirring 1.5h ~
2h, if the reaction time be less than 1 hour, product cannot sufficient diffusion reaction, lead to the mutually uneven of product；It is fired at 120 DEG C
Concentration is burnt, precursor powder is obtained.
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