CN108557862A - A kind of rare-earth-based light absorbing material, preparation method and application - Google Patents
A kind of rare-earth-based light absorbing material, preparation method and application Download PDFInfo
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- CN108557862A CN108557862A CN201810523863.5A CN201810523863A CN108557862A CN 108557862 A CN108557862 A CN 108557862A CN 201810523863 A CN201810523863 A CN 201810523863A CN 108557862 A CN108557862 A CN 108557862A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/003—Light absorbing elements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The present invention relates to a kind of rare-earth-based light absorbing material, preparation method and applications.Light absorbent is the cerium oxide for adulterating lanthanum element, absorbs blue light and ultraviolet light in visible light, and absorption threshold value is 490nm.Preparation method is easy to operate, easy, at low cost, can largely be produced.Rare-earth-based light absorbing material provided by the invention, the electromagnetic wave of 200 490nm is absorbed, which can effectively absorb blue light and ultraviolet light in visible light, and the absorbent that can be used as blue light or ultraviolet light is used for coating, the product manufacturings such as skin care item, screen and glass field.
Description
Technical field
The present invention relates to a kind of preparation methods of rare-earth-based light absorbing material, belong to technical field of material.
Background technology
Between 200nm-800nm, wherein wave-length coverage of the ultraviolet light in visible light is the electromagnetic wavelength of visible light
The wave-length coverage of 200nm-350nm, purple light are 350nm-455nm, and the wave-length coverage of blue light is in 455nm-492nm.Ultraviolet light
It is larger to the harm of human skin, a variety of skin diseases can be induced, therefore, are required for addition every ultraviolet in many skin-protection products
Agent；Further, since ultraviolet light can induce the functional groups such as carbon-carbon double bond or carbon-oxygen bond in organic coating to degrade, and therefore, big portion
It is also required to completely cut off ultraviolet dose of addition in the organic coating divided.Purple light and blue light are to injure larger one to human eye in visible light
Point electromagnetic wave, current video screen are required for addition isolation blue light and purple in mobile phone screen and windscreen for vehicle pad pasting
The material of light.
Common cerium oxide preparation process is acid-base neutralization method and oxalate precipitation method etc. in current industrial production.First, chlorine
Change cerium solution and generates cerous carbonate precipitation or cerium oxalate precipitation respectively with carbonate or oxalic acid；Second step is will by the way of filtering
Precipitate separated from the water, generation sediment presoma；Third step is will to precipitate to carry out high temperature sintering, and sintering temperature is generally 800
Between DEG C -900 DEG C, cerium oxide is generated.
The large cerium oxide product appearance color industrially produced is white powder, and the energy gap of cerium oxide is about 3.2-
3.4eV, UV-Visible absorption collection of illustrative plates, CeO2Electro-magnetic wave absorption threshold value be 388nm or so, when there are trivalent cerium doppings
In the case of, the extinction threshold value of cerium oxide is 450nm or so, therefore can absorb a part of blue light.In addition, being limited by purity, knot
The influence of brilliant degree and preparation process, the absorption threshold value of cerium oxide will appear the trend of red shift or blue shift.But how to obtain stablize it is red
The material of shifting, yet there are no.
Invention content
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of rare-earth-based light absorbing material, and expression formula is
(La0.05-0.15Ce0.85-0.95)xOy, can absorb the electromagnetic wave of 200-490nm ranges, can effectively absorb blue light in visible light and
Ultraviolet light, the absorbent that can be used as blue light or ultraviolet light use.The present invention also provides the preparation sides of the rare-earth-based light absorbing material
Method, it is easy to operate.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of rare-earth-based light absorbing material, it is the cerium oxide for adulterating lanthanum element that the light, which inhales material,.
Signified rare-earth-based light absorbing material refers to the light absorbing material using rare earth oxide as base material in the present invention.
Rare-earth-based light absorbing material as described above, the light inhale the blue light and ultraviolet light in visible light absorbing material,
Absorption threshold value is 490nm.
Rare-earth-based light absorbing material as described above, described in lanthanum element be to enter the cerium oxide in a manner of solid solution
Lattice in.
The present invention also provides a kind of preparation method of rare-earth-based light absorbing material, preparation method includes the following steps：
S1, the re chloride for configuring cerium chloride and lanthanum chloride；
S2, saturated oxalic acid solution is added into the re chloride, precipitated, wherein in the precipitation process
Temperature be maintained between 20 DEG C~40 DEG C, filtered later；
S3, the filtered obtained oxalic rare earth precipitates object is subjected to high temperature sintering, obtains the oxidation for mixing lanthanum element
Cerium powder.
Preparation method as described above, it is preferable that in step sl, the matter of lanthanum, Ce elements in the re chloride
Amount is than being 1~3:17~19.
Preparation method as described above, it is preferable that in step sl, the re chloride can be by lanthanum carbonate and carbonic acid
It is prepared in the concentrated hydrochloric acid that cerium is dissolved in.
It is further preferred that the mass ratio of the lanthanum, Ce elements is 1:6~15.
Preparation method as described above, it is preferable that in step s3, the temperature of the sintering is 700 DEG C~950 DEG C, is burnt
The knot time is 1~3h.
Further, the temperature of the preferably described sintering is 750 DEG C~900 DEG C.
The cerium oxide powder that lanthanum element is mixed made from preparation method as described above is represented by (La0.05-0.15Ce0.85-0.95)xOy, lanthanum element forms solid solution after being entered in a manner of being dissolved in the lattice of cerium oxide, absorption threshold value is 490nm,
The electromagnetic wave of absorbable 200~490nm.It is expressed as (La0.05-0.15Ce0.85-0.95)xOyRefer to the lanthanum for mixing lanthanum cerium oxide, Ce elements
Mass ratio 0.05~0.15:0.85~0.95 changes within the scope of this, i.e., when La dopings are 5%, Ce 95%, and
When La dopings are 15%, Ce 85%.
The rare-earth-based light absorbing material that rare-earth-based light absorbing material as described above and preparation method prepare is for making
Application in standby fiber, film, coating, skin care item, screen and glass.
(3) advantageous effect
The beneficial effects of the invention are as follows：
Rare-earth-based light absorbing material prepared by the present invention is the cerium oxide powder material for adulterating lanthanum element, expression formula
Can be (La0.05-0.15Ce0.85-0.95)xOy.The apparent red shift for realizing UV-Visible absorption threshold value, absorbs the electricity of 200-490nm
Magnetic wave, the powder body material can effectively absorb blue light and ultraviolet light in visible light, can be used as the absorbent of blue light or ultraviolet light
For fiber, film, coating, skin care item, the product manufacturings such as screen and glass field.
The preparation method of the present invention is easy to operate, easy, at low cost, can largely be produced.What is prepared mixes lanthanum element
Cerium oxide powder material can absorb blue light and ultraviolet light, and then reduce injury of the visible light for human eye or skin.
The powder body material further can be used as auxiliary agent and be widely used in video screen, the fields such as mobile phone screen or vehicle glass.
Description of the drawings
Fig. 1 is that the cerium oxide of doping lanthanum element prepared by the method for the present invention compares collection of illustrative plates with the XRD of pure cerium oxide；
Fig. 2 is the SEM results of the cerium oxide of doping lanthanum element prepared by the method for the present invention；
Fig. 3 is the XPS collection of illustrative plates of the cerium oxide of doping lanthanum element prepared by the method for the present invention；
Fig. 4 is the Raman collection of illustrative plates of the cerium oxide of doping lanthanum element prepared by the method for the present invention；
Fig. 5 is cerium oxide-doped level structure figure；
Fig. 6 is the UV-Visible absorption pair of the cerium oxide and pure zirconia cerium of doping lanthanum element prepared by the method for the present invention
Compare collection of illustrative plates.
Fig. 7 is the cerium oxide and TiO of doping lanthanum element prepared by the method for the present invention2(P25) absorption spectrum comparison diagram.
Fig. 8 is the outside drawing of the cerium oxide (right side) and pure zirconia cerium (left side) of doping lanthanum element prepared by the method for the present invention.
Specific implementation mode
Existing pure CeO2Electro-magnetic wave absorption threshold value be 388nm or so, in the case of there are trivalent cerium dopping, oxidation
The extinction threshold value of cerium is 450nm or so.The present invention is introduced by the doping of lanthanum element in the intrinsic energy level track of cerium oxide
The impurity energy level of lanthanum, absorption threshold value are 490nm, realize the red shift for absorbing threshold value, can absorb 200nm-490nm wave bands
Electromagnetic wave, can be used as production ring of the auxiliary agent for the products such as fiber, film, coating, glass, video screen and mobile phone screen
Section.
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific implementation mode, to this hair
It is bright to be described in detail.
Embodiment 1
The step of cerium oxide powder material of lanthanum is mixed in preparation is as follows：
1, it is equipped with re chloride according to certain lanthanum Ce elements mass ratio, lanthanum element is made to account for the quality of lanthanum Ce elements
5%~15%.It is made of cerium chloride and lanthanum chloride with the re chloride postponed.
2, the preparation of oxalic rare earth precipitates object is carried out：The saturated oxalic acid solution configured is added into re chloride
Add, liquidus temperature is maintained between 20 DEG C~40 DEG C in precipitation process, after the rare earth element in solution all precipitation, is taken out
Filter.
3, by the oxalic rare earth precipitates object obtained after suction filtration carry out high temperature sintering, sintering temperature be 700 DEG C~950 DEG C it
Between, sintering time is generally between 1h~3h.
The powder obtained after sintering is subjected to physical and chemical performance characterization, according to XRD as shown in Figure 1 as a result, powder material
The main phase of material is CeO2, while the characteristic peak of lanthana object phase is not observed, the main peak to cerium oxide in (111) position carries out
Analysis finds that compared with the XRD characteristic peaks of pure zirconia cerium, the characteristic peak positions of 111,220 and 311 crystal faces are all to smaller angle
It is deviated, illustrates that lanthanum element is possible to be entrained in CeO in a manner of solid solution2Lattice in.In order to further confirm that powder
The crystal structure of body carries out morphology observation under Electronic Speculum to sample and EDS energy spectrum analysis and backscattered electron imaging is combined to find
Only a kind of presence of main phase, as shown in Figure 2, wherein mix lanthanum cerium oxide pattern under a, the visual field；B, lanthanum cerium oxide is mixed under the visual field
Elemental redistribution；C, Ce elements are distributed；D, lanthanum element is distributed；E, oxygen element is distributed.But lanthanum element is but equal together with Ce elements
Even is distributed in crystal, has further proved lanthanum element and has been possible to be entrained in the lattice of cerium oxide in the form of solid solution.
In order to further confirm that lanthanum element is in the lattice for entered in a manner of solid solution cerium oxide, while excluding in sample
Lanthana presence, inventor has carried out XPS and Raman energy spectrum to sample again and has analyzed, as shown in figure 3, being analyzed in xps energy spectrum
In, the power spectrum of La3d5/2 orbital electron is detected, the position at power spectrum middle orbit peak is respectively 833.5eV and 838eV.In Fig. 4
Raman test result in, be not found 395cm-1La2O3Characteristic peak, while with pure CeO2It compares, 460cm-1Place
Characteristic peak is deviated, while strength reduction, illustrates that the doping of La changes CeO2Lattice structure, cause lattice vibration
The offset of characteristic peak, while strength reduction.In conjunction with above-mentioned characterization result, the powder that the present invention synthesizes is the oxygen of lanthanum element doping
Change cerium powder, i.e., in the lattice of cerium oxide, part cerium atom is replaced by lanthanum atom, and expression formula is (La0.05- 0.15Ce0.85-0.95)xOy.Lanthanum atom is entered in a manner of being dissolved in the lattice of cerium oxide, and then changes the energy level of cerium oxide
Structure, as shown in figure 5, realizing the apparent red shift of absorption spectrum.
Embodiment 2
Specifically, using the lanthanum carbonate containing the crystallization water and cerous carbonate as raw material, the configuration of re chloride is carried out.First
Lanthanum carbonate and cerous carbonate are dissolved in the concentrated hydrochloric acid of 10mol/L, determine that lanthanum chloride and cerium chloride are molten using EDTA titration methods
The concentration of lanthanum Ce elements in liquid.
Mass ratio according to lanthanum Ce elements is 1:The mixed solution of 10 allotment lanthanum Ce elements, into mixed chlorinated rare earth solution
Oxalic acid solution is added, after the rare earth element in solution all precipitation, is filtered.
Sediment is sintered at 800 DEG C, sintering time 2h.After sintering, the sediment of taking-up is mesh
Mark product.
The UV-Visible absorption of the cerium oxide and pure zirconia cerium of doping lanthanum element manufactured in the present embodiment is compared into collection of illustrative plates
As shown in fig. 6, it is 490nm that the cerium oxide for mixing lanthanum element prepared by the present invention, which absorbs threshold value, and pure cerium oxide absorption threshold value is
388nm。
By the cerium oxide and TiO of doping lanthanum element manufactured in the present embodiment2(P25) absorption spectrum comparison, such as Fig. 7 institutes
Show, it is seen that the cerium oxide of doping lanthanum element prepared by the present invention can absorb the electromagnetic wave of 200-490nm.Doped lanthanum member in all figures
The cerium oxide of element is abbreviated as mixing lanthanum CeO2。
As shown in figure 8, the cerium oxide (right side) for doping lanthanum element manufactured in the present embodiment and large cerium oxide powder material
The outside drawing on (left side), it is seen that the cerium oxide of the doping lanthanum element of index of the present invention is pale green powder.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art can be changed or be modified as the equivalence enforcement of equivalent variations using technology contents disclosed above
Example.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to appointing made by above example
What simple modification, equivalent variations and remodeling, still falls within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of rare-earth-based light absorbing material, which is characterized in that it is the cerium oxide for adulterating lanthanum element that the light, which inhales material,.
2. rare-earth-based light absorbing material as described in claim 1, which is characterized in that its described light is inhaled in visible light absorbing material
Blue light and ultraviolet light, absorption threshold value be 490nm.
3. rare-earth-based light absorbing material as described in claim 1, which is characterized in that the lanthanum element be in a manner of solid solution into
In the lattice for entering the cerium oxide.
4. a kind of preparation method of rare-earth-based light absorbing material, which is characterized in that preparation method includes the following steps：
S1, the re chloride for configuring cerium chloride and lanthanum chloride；
S2, saturated oxalic acid solution is added into the re chloride, precipitated, wherein the temperature in the precipitation process
Degree is maintained between 20 DEG C~40 DEG C, is filtered later；
S3, the filtered obtained oxalic rare earth precipitates object is subjected to high temperature sintering, obtains the cerium oxide powder for mixing lanthanum element
Body.
5. preparation method as claimed in claim 4, which is characterized in that in step sl, lanthanum, cerium in the re chloride
The mass ratio of element is 1~3:17~19.
6. preparation method as claimed in claim 4, which is characterized in that in step sl, the lanthanum, Ce elements mass ratio be
1:6~15.
7. preparation method as claimed in claim 4, which is characterized in that in step s3, the temperature of the sintering is 700 DEG C~
950 DEG C, sintering time is 1~3h.
8. preparation method as claimed in claim 7, which is characterized in that the temperature of the sintering is 750 DEG C~900 DEG C.
9. preparation method as claimed in claim 4, which is characterized in that in step sl, the re chloride can be by carbon
It is prepared in the concentrated hydrochloric acid that sour lanthanum and cerous carbonate are dissolved in.
10. the preparation method described in any one of rare-earth-based light absorbing material as claimed in any one of claims 1-3 and 4-9
Rare-earth-based light absorbing material the answering in being used to prepare fiber, film, coating, skin care item, screen and glass prepared
With.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040760A (en) * | 2019-05-09 | 2019-07-23 | 常州大学 | A kind of method of controllable preparation cerium lanthanum-oxides solid solution nanometer rods |
| CN114344955A (en) * | 2021-12-01 | 2022-04-15 | 大连大平油脂化学有限公司 | Defoaming agent containing rare earth oxide and preparation method thereof |
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| CN107033387A (en) * | 2015-12-11 | 2017-08-11 | 厦门稀土材料研究所 | Nano lanthanum oxide cerium, the ultraviolet ray-resistant material containing it and their preparation method and application |
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2018
- 2018-05-28 CN CN201810523863.5A patent/CN108557862A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107033387A (en) * | 2015-12-11 | 2017-08-11 | 厦门稀土材料研究所 | Nano lanthanum oxide cerium, the ultraviolet ray-resistant material containing it and their preparation method and application |
Non-Patent Citations (1)
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| 杨晓丹等: ""两步法制备镧掺杂氧化铈纳米粉体"", 《稀有金属材料与工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040760A (en) * | 2019-05-09 | 2019-07-23 | 常州大学 | A kind of method of controllable preparation cerium lanthanum-oxides solid solution nanometer rods |
| CN114344955A (en) * | 2021-12-01 | 2022-04-15 | 大连大平油脂化学有限公司 | Defoaming agent containing rare earth oxide and preparation method thereof |
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Application publication date: 20180921 |