A kind of pucherite function ceramics and preparation method thereof
Technical field
The invention belongs to ceramic material field, be specifically related to a kind of pucherite function ceramics and preparation method thereof.
Background technology
Functional materials is the core of field of new, plays important promotion and supporting role to the development of new and high technology.In global field of new, functional materials accounts for 85%.Ceramic material is the important component part of functional materials, has the characteristic of many excellences, is subject to the great attention of scientific and technological circle and business circles.
Pucherite (be called for short 184 yellow) is a kind of important Inorganic yellow pigment, has the characteristics such as nontoxic, bright color, stable chemical nature.Pucherite as the narrower semiconductor material of a kind of band gap (
e g=2.4eV), having good product oxygen activity under visible light illumination, is a kind of novel photocatalyst.At present, pucherite is more and more extensive in the application of pigment and photocatalysis field.
According to document, utilize high temperature solid phase synthesis, chemical bath deposition method, sol-gel method, hydrothermal method, the precipitator method etc., pucherite powder can be prepared; Utilize crystal pulling method, can pucherite monocrystal be prepared.But, in document, lack the report about pucherite pottery up to now.This is because pucherite fusing point lower (~ 940 DEG C), highly volatile in sintering procedure, makes the product burnt till be vesicular structure.Utilize solid reaction process, very difficultly sinter out fine and close solid pucherite pottery, thus make pucherite become blank in function ceramics research field.In view of pucherite is a kind of important semiconductor material, in the widespread use of photochemical catalysis and pigment art, there is the physical propertys such as ionic conductivity, ferroelasticity, photochromic, be necessary to develop a kind of preparation method, prepare the pucherite pottery of excellent property, develop its distinctive functional attributes.
Summary of the invention
Technical problem to be solved by this invention overcomes the problem that pucherite is difficult to sinter into porcelain, provides a kind of pucherite function ceramics and preparation method thereof.
The present invention for solving the problems of the technologies described above adopted technical scheme is: a kind of pucherite function ceramics, and its chemical composition is BiVO
4, density more than 97%, specific inductivity is 60, dielectric loss <0.005.
The preparation method of described pucherite function ceramics is, with Bi
2o
3and V
2o
5powder is raw material, once fire putting into airtight mould after raw material mixed pressuring plate, fire rear grinds and compressing tablet again, again put into airtight mould afterwards to carry out secondary and fire, fire control cooling rate after terminating and be not more than 3.3 DEG C/min, after being down to room temperature, namely obtain pucherite function ceramics.
The described method once fired is: be directly warming up to 890 DEG C of pre-burnings 12 hours.
Heating curve in described secondary sintering procedure is: first rise to 500 DEG C with the temperature rise rate of 2 DEG C/min by room temperature, keep after 2 hours, be warming up to 890 DEG C, keep 12 hours more afterwards with the temperature rise rate of 3.25 DEG C/min.
Temperature lowering curve in described secondary sintering procedure is: be down to 800 DEG C with the rate of temperature fall of 1.5 DEG C/min by 890 DEG C, 700 DEG C are down to again with the rate of temperature fall of 1.7 DEG C/min, 550 DEG C are down to afterwards with the rate of temperature fall of 2.5 DEG C/min, be down to 350 DEG C with the rate of temperature fall of 3.3 DEG C/min again, finally naturally cool to room temperature.
Described airtight mould is quartz molds, and the size of mould and tightness thereof ensure that pressure inner in sintering procedure can stop the composition in raw material to volatilize.
Through once firing and after grinds, carrying out compressing tablet with oil press under the pressure of 6Mpa, be pressed into diameter 15mm, the base substrate of thickness 2mm.
The invention has the beneficial effects as follows:
1, when firing, compressing tablet being placed in airtight mould, making around compressing tablet, to form higher vapour pressure, effectively can suppress the volatilization of composition, thus avoid the formation of vesicular structure, make to fire through secondary the pucherite pottery made and there is higher density.
2, the product in order to avoid causing because cooling rate is too fast after firing end shrinks too fast and ununiform shrinkage, cooling rate is limited to not higher than 3.3 DEG C/min, can prevent product from cooling contraction process, occurring hole thus, ensure the high-compactness of product further.
3, by the control to the processing condition such as firing temperature, time and parameter, ensured that raw material is to the transformation efficiency of pucherite pottery and production efficiency, makes the final product supported be the pure monoclinic phase pucherite existed without other dephasigns.
4, the pucherite ceramic dense degree prepared by described method can reach more than 97%, specific inductivity is about 60, dielectric loss is less than 0.005, and this pottery has the physical propertys such as ionic conductivity, ferroelasticity, photochromic, is a kind of potential high dielectric function stupalith.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of pucherite pottery of the present invention;
Fig. 2 is the sample photo of pucherite pottery of the present invention;
Fig. 3 is the XRD figure of pucherite pottery of the present invention.
Embodiment
A kind of pucherite function ceramics, its chemical composition is BiVO
4, density more than 97%, specific inductivity is 60, dielectric loss <0.005.This pottery has the physical propertys such as ionic conductivity, ferroelasticity, photochromic, and has good dielectric properties, is a kind of desirable functional materials.
The preparation method of described pucherite function ceramics is, with Bi
2o
3and V
2o
5powder is raw material, by Bi
2o
3and V
2o
5powder is according to after the molar ratio ingredient of 1:1, and mixing loaded grinding plant, with underhand polish 5 hours, be solvent with dehydrated alcohol when grinding, can keep uniform particles, be also unlikely to produce powder airborne dust, added dehydrated alcohol amount is about 5% of joined powder quality.Ensure to volatilize after ground complete, can not remain in powder.By compressing tablet after ground powder drying; Compressing tablet is put into quartz molds, and by quartz molds sealing with the volatilization suppressing composition, the size of mould and tightness thereof ensure that pressure inner in sintering procedure can stop the composition in raw material to volatilize.In order to avoid composition volatilization in follow-up sintering procedure as far as possible, after loading compressing tablet in quartz molds, remaining space is the smaller the better, and the volume size of quartz molds is advisable can just load compressing tablet; Quartz molds after sealing is put into retort furnace once fire, firing temperature is preferably 890 DEG C, and the firing time is 12 hours.Fired rear grinds and compressing tablet again, tablet forming technique can be adopted with the following method: after grinds, carries out compressing tablet with oil press under the pressure of 6Mpa, is pressed into diameter 15mm, the base substrate of thickness 2mm.The quartz molds again putting into sealing after compressing tablet is carried out secondary and is fired, the top temperature fired of secondary with once fire identical.890 DEG C of sintering 12-14 hours can be directly warming up to according to usual method, but preferably carry out according to following heating curve, heating curve is: first rise to 500 DEG C with the temperature rise rate of 2 DEG C/min by room temperature, keep after 2 hours, be warming up to 890 DEG C with the temperature rise rate of 3.25 DEG C/min, keep 12 hours more afterwards.Adopt this speed to heat up gradually, while products quality guarantee, also can at utmost save the consumed energy.Will lower the temperature after firing end, cooling rate is not easily too fast, and excessive velocities can cause hole to produce to a certain extent.Therefore, cooling rate to be controlled after firing end and be not more than 3.3 DEG C/min.Preferably carry out according to following temperature lowering curve, temperature lowering curve is: be down to 800 DEG C with the rate of temperature fall of 1.5 DEG C/min by 890 DEG C, 700 DEG C are down to again with the rate of temperature fall of 1.7 DEG C/min, 550 DEG C are down to afterwards with the rate of temperature fall of 2.5 DEG C/min, be down to 350 DEG C with the rate of temperature fall of 3.3 DEG C/min again, finally naturally cool to room temperature.
After testing, the pucherite ceramic dense degree more than 97% obtained.Shown in accompanying drawing 3, it is pucherite pottery XRD figure prepared by the present embodiment.Contrast with standard P DF card (No.75-1866), can determine that the present embodiment gained pottery is pure monoclinic phase pucherite, exist without other dephasigns.Under room temperature and 1MHz test condition, impedance analysis result shows, and pucherite ceramic dielectric constant prepared by the present embodiment is about 60, and dielectric loss is less than 0.005, is a kind of potential high dielectric ceramic material.