CN104891572B - A micro-nano potassium yttrium tungstate film and a preparing method thereof - Google Patents
A micro-nano potassium yttrium tungstate film and a preparing method thereof Download PDFInfo
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Abstract
A micro-nano potassium yttrium tungstate film and a preparing method thereof are disclosed. The preparing method includes dissolving a tungstate, a yttrium compound, a potassium compound and citric acid to prepare a precursor solution with the molar ratio of tungstate ion, yttrium ion and potassium ion being 2:1:1; cleaning and drying a quartz glass substrate; putting the quartz glass substrate into the precursor solution; preparing a coating film with a dipping-pulling method; drying; and performing thermal treatment at a thermal treatment temperature of 600-950 DEG C with the temperature maintaining time being 1-3 h. The finally obtained film comprises KY(WO4)2 particles. The particle size of the particles is 500-100 nm. The form of the film is compact particles, irregular particles or columnar particles. According to the film and the preparing method, the equipment cost is low, a preparing process is simple, production is green and the film and the preparing method are prone to industrial application. The potassium yttrium tungstate film as a photoelectric functional material has a wide application prospect in the fields of solid-state lasers, optical fiber, high-definition displays, photocatalysis, solar spectrum selective absorption film materials, and the like.
Description
Technical field
The invention belongs to inorganic functional material preparing technical field is and in particular to a kind of sol-gal process prepares inorganic thin film
The technology of material.
Background technology
In recent decades, the fast development of the high science and technology such as nanosecond science and technology, microelectronics science and technology and microelectromechanical systems,
Size of electronic devices is less and less, and electronic device miniaturization promotes material and develops to low-dimensional yardstick.Low-dimensional materials include two dimension
Micro-/ nano thin-film material, 1-dimention nano pipe/wire material and zero-dimensional quantum dots material.Due to the intrinsic small size of thin-film material and
The feature of low cross scattering, so that inorganic thin film material has the performances such as the light more excellent compared with powder, electricity, magnetic and catalysis, can use
In solid-state laser, fiber optics, high-resolution equipment, electroluminescence device, ionization sub-panel, Flied emission equipment and solar spectrum
The fields such as selective absorbing membrane material.The traditional preparation methods of inorganic thin film material include various vacuum and antivacuum method,
Vacuum method mainly has the physical vapour deposition (PVD) with thermal evaporation, magnetron sputtering, electron beam evaporation, pulsed laser deposition etc. as representative
Method；Antivacuum preparation method refers generally to chemical solution method, including spray-wall interaction, electro-deposition, sol-gel and heat injection
Deng.But different methods has the limitation of oneself, although vacuum production method has, quality of forming film is good, elemental composition is easily controlled
The advantages such as system, but its equipment is complex and expensive and high energy consumption, and when more particularly preparing thin-film material, Volatile Elements are led
The re-evaporation problem causing hinders the lifting further of vacuum method efficiency, hinders the development of its commercial applications；Based on chemical solution
The preparation method of liquid has geneogenous advantage on cost, along between component element, mixed phase ought all hook, without vacuum
Environment, does not have such problems as that element volatilizees again；But still also there are some inevitable defects in chemical solution method, such as poisonous danger
The use of the chemical solvent (additive as hydrazine and heat injection etc.) of danger, the material of preparation includes a certain amount of organic impurities
As c and o (hot injection etc.).Compared with other method for manufacturing thin film, sol-gal process has the advantage that (1) process is simple,
Without expensive device；(2) crystal grain of film is little, the Nomenclature Composition and Structure of Complexes uniformly, the uniformity is up to molecular level or atom level；(3) to base
The size and shape of piece does not have particular/special requirement, can prepare uniform film with large area；(4) reaction temperature is low, and course of reaction is easy to
Control；(5) stoichiometric proportion, accurately it is easy to modified, doping wide ranges, can efficiently control the composition of film and micro- knot
Structure；(6) each component intersolubility of multicomponent mixture film is preferable.
The multiple tungstates ky (wo of rear-earth-doped alkaline earth4)2Crystal is a kind of host material of excellent performance, with other matrix
Material is compared, and has big absorption and launching cross-sectional area, low pumping threshold, the active ions of high-concentration dopant, heavy pumping light is inhaled
Receipts ability, it is adaptable to as micro-slice laser operation material the features such as low amounts sub- defect；On the other hand, matrixGroup
Efficient stoke conversion produced by dither, can realize Raman and multiwavelength laser operating, this makes its range of application simultaneously
Wider, there is potential application in wide spectrums such as remote sensing, medical treatment, scientific research and communications；Simultaneously its Low threshold, high efficiency and with fly
The Third-order nonlinearity that second laser interaction produces, is to manufacture fiber waveguide and the optical waveguides amplifier part with micro pattern
Ideal material.But ky (wo4)2Low-dimensional nanoscale effect, the research of the synthesis technique of micro-nanometer structural material less relate to
And.
Prior art is concentrated mainly on bulk single crystal growth, spectral quality, waveguide properties side to the application of Potassium Yttrium Tungstate
The aspects such as face.So far, the report of patent aspect be related to tungstate single crystal prepare (cn200610123988,
200910067493.x, 200910067492.5) preparation of tungstate nano film (200810032456.0,
200510026632.6) and double tungstates powder luminous material (201410003791,201410216380,
201310583971st, 201310252704,200910114933.2) etc..
Present inventor seminar early stage synthesizes closely spherical ky (wo by hydro-thermal method4)2Particle (zl
201310245935.1), research shows doping with rare-earth ions eu3+When, eu3+: closely spherical ky (wo4)2Particle has excellent glimmering
Luminous effect and photocatalytic effect；But, due to closely spherical ky (wo4)2Particle is powder shaped, leads to powder in preparation, separates and place
Reunite during managing and depositing, micro-nano powder is also easy to produce dust in production, transport and storage link simultaneously, causes ring
Border is polluted；On the other hand, micro-nano powder can be sent out because having the characteristics such as particle diameter is little, specific surface is big, surface-active is high, long-term preservation
Give birth to reunion and oxidation reaction and lose activity, the development of restriction industrial applications.
Content of the invention
It is an object of the invention to provide a kind of micro-nano Potassium Yttrium Tungstate film and preparation method thereof, make thin-film material compared with powder
Body material has the performances such as more excellent light, electricity, magnetic and catalysis, especially film thermophysical property thermal conductive property, can reduce
The harmful effect to device for the fuel factor, is with a wide range of applications in microoptoelectronic device field, and equipment is simple, technique
Simplify, with low cost, reproducible, convenient post-treatment, environmental protection.
In order to solve above technical problem, the present invention combines dip-coating method by sol-gal process, in quartz glass substrate
Micro-nano ky (wo is plated on piece4)2Thin-film material, the concrete technical scheme of employing is as follows:
A kind of preparation method of micro-nano Potassium Yttrium Tungstate film is it is characterised in that comprise the following steps
Step one, prepares precursor solution: after tungstates, yttrium compound and potassium compound are dissolved separately in distilled water
Obtain tungstate solution, yttrium compound solution and potassium compound solution, the mol ratio of tungstate ion, ruthenium ion and potassium ion is 2:
1:1；
By citric acid be separately added in described tungstate solution, yttrium compound solution and potassium compound solution respectively molten
Liquid a, solution b and solution c, the quality of the citric acid being added is respectively the 1 ~ 1.5 of tungstate ion, ruthenium ion and potassium ion
Times；The ph value of allotment solution a, solution b and solution c is for after 1 ~ 3 respectively, then after three is mixed mixed liquor, adjust
Mixed liquor ph value is 1 ~ 3；
Stirring mixed liquor uniformly adds ethylene glycol solution afterwards, stirs that to obtain presoma molten to forming stable transparent liquid
Liquid；Described ethylene glycol solution is identical with mole total amount of described citric acid；
Step 2, the process of quartz glass substrate and plated film: quartz glass substrate is cleaned and puts into step one after being dried
In described precursor solution, with dip-coating method after plated film on quartz glass substrate in drying box 100 DEG C 10min is dried
Obtain intermediate product；
Step 3, heat treatment: described intermediate product is heat-treated, 600 ~ 950 DEG C of heat treatment temperature, temperature retention time
1 ~ 3 hour, finally obtain micro-nano Potassium Yttrium Tungstate film.
Described tungstates is (nh4)10w12o41Or (nh4)10h2(w2o7)6.
Described yttrium compound is y2o3Or y (no3)3.
Described potassium compound is koh or kno3.
Described quartz glass substrate cleaning method is: ultrasonic vibration in acetone, distilled water, alcohol, distilled water successively
Cleaning 10min；Or successively mass fraction be 5% naoh solution in soak 20min and then in the hcl solution of 1mol/l
Soak 10min, finally ultrasonic oscillation cleaning 20min in distilled water and alcohol.
When preparing precursor solution in described step one, by yttrium compound be dissolved in dust technology yttrium compound is molten
Liquid.
A kind of micro-nano Potassium Yttrium Tungstate film it is characterised in that: described micro-nano Potassium Yttrium Tungstate film is by ky (wo4)2Particle
Composition, between 500 ~ 100nm, described film shape is dense granule, irregular particle or column to described grain graininess size
Particle.
The present invention has beneficial effect.The present invention prepares Potassium Yttrium Tungstate film using sol-gal process, by adjusting ph, Re Chu
Manage temperature and quartz glass substrate cleaning way to control product shape, crystal growth orientation and consistency.Sol-gal process
Have its unique advantage in terms of preparing film: without expensive device and complicated experiment condition, and can be in large area various
Film forming on different shape, the substrate of different materials, experimental technique is relatively easy, processing ease, can be by changing experiment condition
Controlling particle diameter, pattern, particle is uniformly dispersed mode simultaneously, and raw material dosage is few, recoverable, it is easy to accomplish continuous prodution
Running, providing for industrialized production may.Gained film product is applied to solid-state laser, fiber optics, high-resolution equipment, electroluminescent
Luminaire, ionization sub-panel, the microoptoelectronic device such as Flied emission equipment, there is extensive popularizing application prospect.
Brief description
Fig. 1 is the scanning electron microscope diagram of the present invention micro-nano Potassium Yttrium Tungstate film；
The X-ray diffraction pattern of the micro-nano Potassium Yttrium Tungstate film that Fig. 2 is prepared for the present invention；
The scanning electron microscope diagram of the micro-nano Potassium Yttrium Tungstate film that Fig. 3 is prepared for the present invention；
The X-ray diffraction pattern of the micro-nano Potassium Yttrium Tungstate film that Fig. 4 is prepared for the present invention；
The scanning electron microscope diagram of the micro-nano Potassium Yttrium Tungstate film that Fig. 5 is prepared for the present invention；
The X-ray diffraction pattern of the micro-nano Potassium Yttrium Tungstate film that Fig. 6 is prepared for the present invention；
The scanning electron microscope diagram of the micro-nano Potassium Yttrium Tungstate film that Fig. 7 is prepared for the present invention；
The X-ray diffraction pattern of the micro-nano Potassium Yttrium Tungstate film that Fig. 8 is prepared for the present invention.
Specific embodiment
With specific embodiment, technical scheme is described in further details below in conjunction with the accompanying drawings.
Embodiment 1
(nh by 1/3mol4)10h2(w2o7)6, y (the no of 2mol3)3Kno with 2mol3It is dissolved separately in distilled water
In, it is configured to tungstate solution, yttrium compound solution and potassium compound solution；Weigh the lemon of 4.8mol, 2.4mol and 2.4mol
Lemon acid sequentially add in above-mentioned tungstate solution, yttrium compound solution and potassium compound solution respectively solution a, solution b and
Solution c, after mixing, the above-mentioned solution of stirring are uniform, allotment solution a, the ph value of solution b and solution c are 1, then three are mixed respectively
Adjust ph value after being combined and obtain mixed liquor for 1, stirring mixed liquor uniformly adds the ethylene glycol solution of 9.6mol afterwards, stirs to shape
Stable transparent liquid is become to obtain precursor solution；By quartz glass substrate successively in acetone, distilled water, alcohol, distilled water
Ultrasonic vibration cleans 10min, puts in above-mentioned precursor solution, plated with dip-coating method on quartz glass substrate after being dried
After film in drying box 100 DEG C 10min be dried obtain intermediate product.Intermediate product is heat-treated, heat treatment temperature is 850
DEG C, temperature retention time is 3 hours, finally obtains micro-nano Potassium Yttrium Tungstate film, as shown in Figure 1.Film is by ky (wo4)2Particle group
Become, between 100～200nm, film shape is dense granule to grain graininess size, and thin film diffraction figure is as shown in Figure 2.
Embodiment 2
(nh by 1/3mol4)10h2(w2o7)6, y (the no of 2mol3)3Kno with 2mol3It is dissolved separately in distilled water
In, it is configured to tungstate solution, yttrium compound solution and potassium compound solution；Weigh the lemon of 4.8mol, 2.4mol and 2.4mol
Lemon acid sequentially add in above-mentioned tungstate solution, yttrium compound solution and potassium compound solution respectively solution a, solution b and
Solution c, after mixing, the above-mentioned solution of stirring are uniform, allotment solution a, the ph value of solution b and solution c are 3, then three are mixed respectively
Adjust ph value after being combined and obtain mixed liquor for 3, stirring mixed liquor uniformly adds the ethylene glycol solution of 9.6mol afterwards, stirs to shape
Stable transparent liquid is become to obtain precursor solution；By quartz glass substrate successively in acetone, distilled water, alcohol, distilled water
Ultrasonic vibration cleans 10min, puts in above-mentioned precursor solution, plated with dip-coating method on quartz glass substrate after being dried
After film in drying box 100 DEG C 10min be dried obtain intermediate product.Intermediate product is heat-treated, heat treatment temperature is 850
DEG C, temperature retention time is 3 hours, finally obtains micro-nano Potassium Yttrium Tungstate film.As shown in Figure 3, film is by ky (wo4)2Particle group
Become, between 100～500nm, film shape is dense granule to grain graininess size, and thin film diffraction figure is as shown in Figure 4.
Embodiment 3
Kno by 2mol3(nh with 1/3mol4)10h2(w2o7)6It is dissolved separately in distilled water, weigh the y of 1mol2o3
It is dissolved in dust technology, be configured to tungstate solution, yttrium compound solution and potassium compound solution；Weigh 4.8mol, 2.4mol
With the citric acid of 2.4mol sequentially add in above-mentioned tungstate solution, yttrium compound solution and potassium compound solution respectively molten
Liquid a, solution b and solution c, after mixing, the above-mentioned solution of stirring are uniform, allotment solution a, the ph value of solution b and solution c are 3 respectively,
Adjust ph value after again three being mixed and obtain mixed liquor for 3, stirring mixed liquor uniformly adds the ethylene glycol of 9.6mol molten afterwards
Liquid, stirs and obtains precursor solution to formation stable transparent liquid；By quartz glass substrate successively in acetone, distilled water, wine
In essence, distilled water, ultrasonic vibration cleaning 10min, puts in above-mentioned precursor solution, with dip-coating method in quartz after being dried
After plated film on glass substrate in drying box 100 DEG C 10min be dried obtain intermediate product.Intermediate product is heat-treated, at heat
Reason temperature is 800 DEG C, and temperature retention time is 2 hours, finally obtains micro-nano Potassium Yttrium Tungstate film.As shown in Figure 5, film is by ky
(wo4)2Particle forms, and between grain graininess size 150～400nm, film shape is irregular particle, thin film diffraction figure such as Fig. 6
Shown in.
Embodiment 4
(nh by 1/3mol4)10h2(w2o7)6, y (the no of 2mol3)3Kno with 2mol3It is dissolved separately in distilled water
In, it is configured to tungstate solution, yttrium compound solution and potassium compound solution；Weigh the lemon of 4.8mol, 2.4mol and 2.4mol
Lemon acid sequentially add in above-mentioned tungstate solution, yttrium compound solution and potassium compound solution respectively solution a, solution b and
Solution c, mixing, stir above-mentioned solution uniform after, allotment solution a, the ph value of solution b and solution c solution are 3 respectively, then by three
Person adjusts ph value and obtains mixed liquor for 3 after mixing, stirring mixed liquor uniformly adds the ethylene glycol solution of 9.6mol, stirring afterwards
Obtain precursor solution to forming stable transparent liquid；Successively mass fraction be 5% naoh solution in soak 20min right
Soak 10min afterwards in the hcl solution of 1mol/l, finally ultrasonic oscillation cleaning 20min in distilled water and alcohol, after being dried
Put in above-mentioned precursor solution, 100 DEG C of dryings in drying box after plated film on quartz glass substrate with dip-coating method
10min obtains intermediate product.Intermediate product is heat-treated, heat treatment temperature is 850 DEG C, temperature retention time is 3 hours, finally obtains
Obtain micro-nano Potassium Yttrium Tungstate film.As shown in fig. 7, film is by ky (wo4)2Cylindrical particle forms, the draw ratio of grain graininess size
50nm*150nm～100nm*400nm, film shape is cylindrical particle, and thin film diffraction figure is as shown in Figure 8.
Claims (4)
1. a kind of preparation method of micro-nano Potassium Yttrium Tungstate film is it is characterised in that comprise the following steps
Step one, prepares precursor solution: obtain tungstates after tungstates, yttrium compound and potassium compound are dissolved respectively molten
Liquid, yttrium compound solution and potassium compound solution, wherein tungstates and potassium compound are dissolved in distilled water, and yttrium compound is nitric acid
Yttrium or yittrium oxide, yttrium nitrate is dissolved in distilled water, and yittrium oxide is dissolved in dust technology, tungstate ion, ruthenium ion and potassium ion
Mol ratio is 2:1:1；
By citric acid be separately added in described tungstate solution, yttrium compound solution and potassium compound solution respectively solution a,
Solution b and solution c, the quality of the citric acid being added is respectively 1～1.5 times of tungstate ion, ruthenium ion and potassium ion；Point
Not Tiao Pei solution a, solution b and solution c ph value for after 1～3, then after three is mixed mixed liquor, adjust mixing
Liquid ph value is 1～3；
Stirring mixed liquor uniformly adds ethylene glycol solution afterwards, stirs and obtains precursor solution to formation stable transparent liquid；Institute
State ethylene glycol solution identical with mole total amount of described citric acid；
Step 2, the process of quartz glass substrate and plated film: quartz glass substrate is cleaned and puts into described in step one after being dried
Precursor solution in, with dip-coating method after plated film on quartz glass substrate in drying box 100 DEG C be dried during 10min obtains
Between product；
Step 3, heat treatment: described intermediate product is heat-treated, 600～950 DEG C of heat treatment temperature, temperature retention time 1～
3 hours, finally obtain micro-nano Potassium Yttrium Tungstate film.
2. a kind of micro-nano Potassium Yttrium Tungstate film according to claim 1 preparation method it is characterised in that: described tungsten
Hydrochlorate is (nh4)10w12o41Or (nh4)10h2(w2o7)6.
3. a kind of micro-nano Potassium Yttrium Tungstate film according to claim 1 preparation method it is characterised in that: described potassium
Compound is koh or kno3.
4. according to a kind of preparation method of micro-nano Potassium Yttrium Tungstate film as claimed in claim 1 it is characterised in that described
Quartz glass substrate cleaning method is: ultrasonic vibration cleaning 10min in acetone, distilled water, alcohol, distilled water successively；Or
Successively mass fraction be 5% naoh solution in soak 20min then in the hcl solution of 1mol/l soak 10min, finally
Ultrasonic oscillation cleaning 20min in distilled water and alcohol.
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| CN109734120B (en) * | 2018-12-24 | 2021-05-25 | 江苏大学 | Flower-like microsphere structure potassium yttrium tungstate material and preparation method thereof |
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