CN103113106A - Preparation method of pyrochlore-type A2B2O7 transparent ceramics - Google Patents
Preparation method of pyrochlore-type A2B2O7 transparent ceramics Download PDFInfo
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Abstract
The invention discloses a preparation method of pyrochlore-type A2B2O7 transparent ceramics, relating to A2B2O7-series nano powder preparation by a sol-gel process and belonging to the field of ceramic material preparation. The preparation method comprises the following steps: at room temperature, weighing RE2O3 and ZrOCl2.8H2O or TiCl4 according to the stoichiometric proportion, dissolving the rare earth oxide in nitric acid, adding the ZrOCl2.8H2O or TiCl4 to be dissolved, adding a mixed solution containing a dispersing agent (NH4)2SO4 and PAA (polyacrylic acid), slowly and dropwisely adding into an ammonium bicarbonate solution to obtain a precursor, and drying; adding a certain amount of sintering assistant ethyl orthosilicate or silicon dioxide sol into the precursor, carrying out ball milling, drying, screening and calcining to obtain nano powder; and carrying out compression molding, isostatic cool pressing, vacuum sintering, annealing and polishing treatment to finally obtain the transparent A2B2O7-series ceramics. By adopting the self-made high-activity nano powder to prepare the transparent A2B2O7-series ceramics at low temperature, the technique is simple and feasible.
Description
Technical field
The present invention relates to ceramic preparation field, be specifically related to a kind of preparation method of pyrochlore-type A2B2O7 crystalline ceramics
Technical background
Pyrochlore-type A2B2O7 series (A:REE rare earth element; B:Ti or Zr), in Ti system, two kinds of compounds of La2Ti2O7 and Nd2Ti2O7 belong to oblique system, and other product (A=Sm-Lu) is pyrochlore constitution, belong to isometric system, in Zr system, work as A=La, Nd, Sm, Eu, during Gd, form pyrochlore constitution, belong to isometric system, and, when A=Tb-Lu, form fluorite structure, belong to isometric system.The pyrochlore-type oxide compound is a series of compounds with analog structure, they have unique crystalline structure, and there is a lot of functional alternative in lattice, therefore, have more special performance at aspects such as heat, electricity, magnetic and catalysis, they have been widely used in the fields such as ionophore, catalyzer, luminous substrate material, hard fire colour, solidification of radwaste and large-scale magnetoresistor.
Yet pyrochlore-type A2B2O7 series compound is a kind of more difficult synthetic material, mainly containing of reported literature is following several:
1) pressureless sintering method, i.e. traditional solid state reaction: rare earth oxide and titanium oxide or zirconium white are mixed to grinding by a certain percentage, at high temperature long-time calcination, it is inhomogeneous that this kind of preparation method's raw material mixes, and sintering temperature is high, and crystallization degree is low;
2) High Temperature High Pressure is synthetic: take Gd2O3 and ZrO2 as raw material, it is mixed according to stoichiometric ratio, being placed in dehydrated alcohol grinds, mixed powder is become to green compact through the dry-pressing of 25MPa pressure, it is dried in baking oven, put into the assembling cavity of high-pressure sinter sample, heat up and boost in building-up process and carry out simultaneously, under the pressure and 1600 of 5.2GPa is spent, Gd2Zr2O7 has been synthesized in reaction in 5 minutes, and this synthetic method time is short, and efficiency is high.But it is very harsh that the method requires conversion unit, and certain danger is arranged in reaction process, same crystallization degree is not high;
3) coprecipitation method: by Gd(NO3) 3 and ZrOCl2.8H2O mix after being dissolved in respectively deionized water, this solution is dropwise joined in the excessive ammonia of vigorous stirring, obtain presoma, through suction filtration, washing, drying, calcination at a certain temperature, the powder made is pressed into to base under 100MPa pressure, and under 1550 degree, sintering makes pyrrhite Gd2Zr2O7 pottery in 20 hours;
4) sol-gel method: be dissolved in respectively in Virahol by a certain amount of zirconium iso-propoxide and rare earth nitrate, the latter is slowly dropped in the former and forms colloid, and under 80 degree aging 24 hours, and then the lower Rotary Evaporators drying of using of 80 degree, by this powder transfer in sintering oven under 1200 degree sintering 2 hours;
5) flux method: by rare earth nitrate, zirconium nitrate and fusing assistant are even by certain proportioning ground and mixed, then are transferred in crucible, and insulation 1-2 hour after the fusing of intensification raw material, close stove and be cooled to room temperature, by the deionized water washing and drying, obtains product.
Above-mentioned 5 kinds of methods have all obtained powder or the pottery of pyrochlore-type A2B2O7 series compound, but crystallization degree is not high, hindered the application of some aspect, as Tb2Ti2O7 is used in the magneto-optic memory technique aspect, Dy2Ti2O7 and Ho2Ti2O7 are the Spin Ice materials with height anti-frustration.And the single crystal growing of these materials is all more difficult, therefore the material preparation method of exploring new high-efficiency could promote their widespread use, the invention provides a kind of method of synthetic pyrochlore-type A2B2O7 series compound crystalline ceramics, there is synthetic method simple, the crystallization degree advantages of higher.
Summary of the invention
The problem to be solved in the present invention is to find a kind of method of synthetic pyrochlore-type A2B2O7 crystalline ceramics, first by coprecipitation method, prepare highly active pyrochlore-type A2B2O7 nano-powder, prepare high-quality pyrochlore-type A2B2O7 crystalline ceramics by operations such as moulding, vacuum sintering and annealing afterwards.
Concrete technical scheme is as follows:
A kind of preparation method of pyrochlore-type A2B2O7 crystalline ceramics has step as follows:
Step 1) takes rare earth oxide and ZrOCl2.8H2O or TiCl4 according to stoichiometric ratio, with 1:1 nitric acid, under heated condition, rare earth oxide is dissolved, after dissolve complete and remove unnecessary acid, ZrOCl2.8H2O or TiCl4 deionized water dissolving, then be made into mixing solutions,, add (NH4) simultaneously
2sO
4with PAA, as composite dispersing agent, be dissolved in mixing solutions, ammonium bicarbonate soln is as precipitation agent, and doubly, the 1-5 that liquor capacity is the metallic ion mixed liquor volume doubly for the 4-10 that wherein bicarbonate of ammonia is the total molar mass of metal ion;
Step 2) adopt the mode of back titration, at room temperature, speed by mixing solutions with≤10ml/min, slowly be added drop-wise in the precipitation agent ammonium bicarbonate soln and go, and constantly stir, after titration completes, continue to stir 1-6 hour, make it to react completely, precipitation 24-48 hour, then with the deionized water throw out that washing and filtering obtains repeatedly, with the NH except in dereaction
4nO
3and remaining NH
4hCO
3, then use dehydrated alcohol washing and precipitating thing, the moisture in disgorging as far as possible, to reduce the reunion of powder;
The throw out that step 3) will be cleaned with dehydrated alcohol is dry 24-48 hour under 50-65 ℃, and dry presoma is ground, and then with tetraethoxy or silicon dioxide gel, mixes, and with dehydrated alcohol, makees the ball milling solvent, carries out ball milling.Presoma after ball milling is dry 12-24 hour under 65-85 ℃, then cross the 100-200 mesh sieve, the 0.5-2wt% that wherein tetraethoxy or silicon dioxide gel are precursor powder, the 100-250% that ball-milling medium and dehydrated alcohol quality are presoma, ball milling 4-6h, rotating speed 200-300r/min
Step 4) is carried out calcination processing by the presoma after sieving, and prior to 600-750 ℃ of lower constant temperature 3-6 hour, is being warmed up to 900-1200 ℃ of interval constant temperature 8-12 hour, wherein from room temperature to 600 ℃ this interval in the binder removal stage, heat-up rate is less than 150 ℃/h
Powder after the step 5) calcining continued the 100-200 mesh sieve, and the compression moulding in punching block of the powder after sieving, then, through the further densification of 150-300MPa isostatic cool pressing, obtain biscuit.Biscuit in vacuum tightness higher than 10
-3be heated to 1400-1550 ℃ in the environment of Pa, the insulation certain hour, then annealing, finally obtain pyrochlore-type A2B2O7 crystalline ceramics after polishing, if improve the vacuum tightness of sintering link, vacuum tightness is higher than 10
-4pa, after ceramic post sintering, temperature drops to 1200-1350 ℃, directly in air, anneals more than 10 hours.
The pyrochlore-type A2B2O7 crystalline ceramics that adopts preparation method of the present invention to prepare can be widely used in the fields such as ionophore, catalyzer, luminous substrate material, hard fire colour, solidification of radwaste and large-scale magnetoresistor.The present invention has adopted the back titration mode to prepare pyrochlore-type A2B2O7 nano-powder, adopts (NH in preparation process
4)
2sO
4with PAA as composite dispersing agent, reduced presoma and the presoma agglomeration in calcination process, adopt tetraethoxy or silicon dioxide gel as sintering aid simultaneously, by ball milling, they are mixed with presoma equably, calcined again, the powder specific-surface area detection prepared is large, reunite few, without dephasign, there is higher sintering activity, adopt afterwards the vacuum sintering mode, prepared transparent pyrochlore-type A2B2O7 pottery at lower temperature, technical process is simple, easy handling, and the crystalline ceramics of preparation has good optical property.
Embodiment
embodiment mono-: the stoichiometric ratio according to Tb2Ti2O7 takes Tb
4o
7and TiCl4, with the nitric acid of 1:1, their are dissolved to wiring solution-forming and remove unnecessary acid, add 10% ammonium sulfate of metal ion mole total amount and 0.5% PAA as dispersion agent simultaneously; By bicarbonate of ammonia deionized water wiring solution-forming, bicarbonate of ammonia is 8 times of metal ion integral molar quantity, and volume is 3 times of the metallic ion mixed liquor volume, and makes its dissolve complete; Adopt the mode of back titration, at room temperature, the speed by the solution that configures with≤10ml/min slowly is added drop-wise in bicarbonate of ammonia and goes, and is stirred.The presoma that back titration generates is flocks, has larger specific surface area, owing to having added ammonium sulfate and PAA makes dispersion agent, this presoma is after calcining, can obtain the less particle of reuniting, there is higher activity, be conducive to the preparation of crystalline ceramics.After titration completes, continue to stir 4 hours, make to react completely, then precipitate 24 hours, with the centrifugal throw out obtained of deionized water rinsing 5 times, except the by product ammonium nitrate in dereaction and may remain bicarbonate of ammonia, then use dehydrated alcohol washing and precipitating thing 3 times, moisture in disgorging, reduce the hard aggregation that may occur in drying process as far as possible.To clean the throw out of 3 times under 50 ℃ dry 48 hours with dehydrated alcohol, the tetraethoxy that is presoma 1.0wt% by dry presoma and mass ratio mixes, then make the ball milling solvent with dehydrated alcohol, the dehydrated alcohol quality is 150% of precursor powder, ratio of grinding media to material 4:1, the abrading-ball filling ratio is 40%, ball milling 4 hours, rotating speed is 250r/min, presoma after ball milling under 60 ℃ dry 24 hours, then cross 200 mesh sieves, presoma after sieving is carried out to calcination processing, be warmed up to 700 ℃ with the speed that is less than 150 ℃/min, be incubated 4 hours, then be warming up to 1200 ℃, be incubated 8 hours, after calcining, powder is crossed 100 mesh sieves, powder after sieving is just molded in punching block, then pass through the further densification of 300MPa isostatic cool pressing, obtain biscuit, by biscuit in vacuum tightness higher than 10
-3pa, 1550 ℃ of lower constant temperature 10 hours, then anneal 30 hours, after polishing, finally obtains crystalline ceramics.
embodiment bis-: take Ho2O3 and TiCl4 according to chemical constitution Ho2TiO7, with the nitric acid of 1:1, their are dissolved to wiring solution-forming and remove unnecessary acid, add 15% ammonium sulfate of metal ion mole total amount and 0.4%PAA as dispersion agent simultaneously; By bicarbonate of ammonia deionized water wiring solution-forming, bicarbonate of ammonia is 6 times of metal ion integral molar quantity, and volume is 2 times of the metallic ion mixed liquor volume, and makes its dissolve complete; Adopt the mode of back titration, at room temperature, the speed by the solution that configures with≤10ml/min slowly is added drop-wise in bicarbonate of ammonia and goes, and is stirred.The presoma that back titration generates is flocks, has larger specific surface area, owing to having added ammonium sulfate and PAA as dispersion agent, this presoma is after calcining, can obtain the less particle of reuniting, there is higher activity, be conducive to the preparation of crystalline ceramics.After titration completes, continue to stir 4 hours, make to react completely, then precipitate 24 hours, with the centrifugal throw out obtained of deionized water rinsing 4 times, except the by product ammonium nitrate in dereaction and may remain bicarbonate of ammonia, then use dehydrated alcohol washing and precipitating thing 2 times, moisture in disgorging, reduce the hard aggregation that may occur in drying process as far as possible.To clean the throw out of 2 times under 60 ℃ dry 48 hours with dehydrated alcohol, the tetraethoxy that is presoma 1.0wt% by dry presoma and mass ratio mixes, then do ball-milling medium with dehydrated alcohol, the dehydrated alcohol mass ratio is 150% of precursor powder, ratio of grinding media to material 4:1, the abrading-ball filling ratio is 40%, ball milling 4 hours, rotating speed is 200r/min, presoma after ball milling under 65 ℃ dry 24 hours, then cross 200 mesh sieves, presoma after sieving is carried out to calcination processing, be warmed up to 700 ℃ with the speed that is less than 150 ℃/min, be incubated 4 hours, then be warming up to 1000 ℃, be incubated 8 hours, after calcining, powder continued 100 mesh sieves, powder after sieving is just molded in punching block, then pass through the further densification of 300MPa isostatic cool pressing, obtain biscuit, by biscuit in vacuum tightness higher than 10
-3pa, 1500 ℃ of lower constant temperature 10 hours, then anneal 24 hours, after polishing, finally obtains crystalline ceramics.
embodiment tri-: take Gd2O3 and ZrOCl2.8H2O according to chemical constitution Gd2Zr2O7, with the nitric acid of 1:1, their are dissolved to wiring solution-forming and remove unnecessary acid, add 20% ammonium sulfate of metal ion mole total amount and 0.3% PAA as dispersion agent simultaneously; By bicarbonate of ammonia deionized water wiring solution-forming, bicarbonate of ammonia is 5 times of metal ion integral molar quantity, and volume is 1.5 times of the metallic ion mixed liquor volume, and makes its dissolve complete; Adopt the mode of back titration, at room temperature, the speed by the solution that configures with≤5ml/min slowly is added drop-wise in bicarbonate of ammonia and goes, and is stirred.The presoma that back titration generates is flocks, has larger specific surface area, and owing to having added ammonium sulfate as dispersion agent, this presoma, after calcining, can obtain the less particle of reuniting, and has higher activity, is conducive to the preparation of crystalline ceramics.After titration completes, continue to stir 4 hours, make to react completely, then precipitate 24 hours, with the centrifugal throw out obtained of deionized water rinsing 4 times, except the by product ammonium nitrate in dereaction and may remain bicarbonate of ammonia, then use dehydrated alcohol washing and precipitating thing 2 times, moisture in disgorging, reduce the hard aggregation that may occur in drying process as far as possible.To clean the throw out of 2 times under 60 ℃ dry 48 hours with dehydrated alcohol, the tetraethoxy that is presoma 1.0wt% by dry presoma and mass ratio mixes, then do ball-milling medium with dehydrated alcohol, the dehydrated alcohol mass ratio is 150% of precursor powder, ratio of grinding media to material 4:1, the abrading-ball filling ratio is 40%, ball milling 4 hours, rotating speed is 200r/min, presoma after ball milling under 65 ℃ dry 24 hours, then cross 200 mesh sieves, presoma after sieving is carried out to calcination processing, be warmed up to 700 ℃ with the speed that is less than 150 ℃/min, be incubated 4 hours, then be warming up to 900 ℃, be incubated 8 hours, after calcining, powder continued 100 mesh sieves, powder after going to sieve is just molded in punching block, then pass through the further densification of 300MPa isostatic cool pressing, obtain biscuit, by biscuit in vacuum tightness higher than 10
-3pa, 1450 ℃ of lower constant temperature 10 hours, then anneal 24 hours, after polishing, finally obtains crystalline ceramics.
Claims (5)
1. the preparation method of a pyrochlore-type A2B2O7 crystalline ceramics, is characterized in that the preparation process of pyrochlore-type A2B2O7 nano-powder and the sintering process of crystalline ceramics, has step as follows:
Step 1) takes rare earth oxide and ZrOCl2.8H2O or TiCl4 according to stoichiometric ratio, with 1:1 nitric acid, under heated condition, rare earth oxide is dissolved, after dissolve complete and remove unnecessary acid, ZrOCl2.8H2O or TiCl4 deionized water dissolving, then be made into mixing solutions,, add (NH4) simultaneously
2sO
4with PAA, as composite dispersing agent, be dissolved in mixing solutions, ammonium bicarbonate soln is as precipitation agent;
Step 2) adopt the mode of back titration, at room temperature, speed by mixing solutions with≤10ml/min, slowly be added drop-wise in the precipitation agent ammonium bicarbonate soln and go, and constantly stir, after titration completes, continue to stir 1-6 hour, make it to react completely, precipitation 24-48 hour, then with the deionized water throw out that washing and filtering obtains repeatedly, with the NH except in dereaction
4nO
3and remaining NH
4hCO
3, then use dehydrated alcohol washing and precipitating thing, the moisture in disgorging as far as possible, to reduce the reunion of powder;
The throw out that step 3) will be cleaned with dehydrated alcohol is dry 24-48 hour under 50-65 ℃, and dry presoma is ground, and then with tetraethoxy or silicon dioxide gel, mixes, and with dehydrated alcohol, makees the ball milling solvent, carries out ball milling;
Presoma after ball milling is dry 12-24 hour under 65-85 ℃, then crosses the 100-200 mesh sieve;
Step 4) is carried out calcination processing by the presoma after sieving, and prior to 600-750 ℃ of lower constant temperature 3-6 hour, is being warmed up to 900-1200 ℃ of interval constant temperature 8-12 hour;
Powder after the step 5) calcining continued the 100-200 mesh sieve, and the compression moulding in punching block of the powder after sieving, then, through the further densification of 150-300MPa isostatic cool pressing, obtain biscuit;
Biscuit in vacuum tightness higher than 10
-3be heated to 1400-1550 ℃ in the environment of Pa, the insulation certain hour, then annealing, finally obtain pyrochlore-type A2B2O7 crystalline ceramics after polishing.
2. according to the preparation method of a kind of pyrochlore-type A2B2O7 crystalline ceramics described in claim 1, it is characterized in that, step 1) takes rare earth oxide and ZrOCl2.8H2O or TiCl4 by stoichiometric ratio, then with nitric acid dissolve, mix, doubly, the 1-5 that liquor capacity is the metallic ion mixed liquor volume doubly for the 4-10 that bicarbonate of ammonia is the total molar mass of metal ion.
3. according to the preparation method of a kind of pyrochlore-type A2B2O7 crystalline ceramics described in claim 1, it is characterized in that in step 3) that tetraethoxy or silicon dioxide gel are precursor powder 0.5-2wt%, the 100-250% that ball-milling medium and dehydrated alcohol quality are presoma, ball milling 4-6h, rotating speed 200-300r/min.
4. according to the preparation method of a kind of pyrochlore-type A2B2O7 crystalline ceramics described in claim 1, it is characterized in that in step 4) that from room temperature to 600 ℃ this interval, in the binder removal stage, heat-up rate is less than 150 ℃/h.
5. according to the preparation method of the described a kind of pyrochlore-type A2B2O7 crystalline ceramics of claim 1, it is characterized in that in step 5), improve the vacuum tightness of sintering link, vacuum tightness is higher than 10
-4pa, after ceramic post sintering, temperature drops to 1200-1350 ℃, directly in air, anneals more than 10 hours.
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| CN105905944A (en) * | 2016-04-20 | 2016-08-31 | 陕西科技大学 | Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method |
| CN110372384A (en) * | 2019-07-30 | 2019-10-25 | 华东师范大学重庆研究院 | A kind of preparation method of transparent stealth material |
| CN110790571A (en) * | 2019-12-10 | 2020-02-14 | 湖南工学院 | Preparation of Gd2Zr2O7Method for making transparent ceramics |
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| CN105905944A (en) * | 2016-04-20 | 2016-08-31 | 陕西科技大学 | Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method |
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| CN111116199A (en) * | 2020-01-18 | 2020-05-08 | 湖南工学院 | Preparation of Gd by vacuum pressureless sintering2Zr2O7Method for making transparent ceramics |
| CN114685158A (en) * | 2022-05-05 | 2022-07-01 | 闽都创新实验室 | Magneto-optical ceramic and preparation method and application thereof |
| CN116283271A (en) * | 2023-03-07 | 2023-06-23 | 宁波大学 | Gd with high refractive index and high optical quality 2 Sn 2 O 7 Method for preparing pyrochlore type transparent ceramic |
| CN116283271B (en) * | 2023-03-07 | 2024-03-12 | 宁波大学 | Gd with high refractive index and high optical quality 2 Sn 2 O 7 Method for preparing pyrochlore type transparent ceramic |
| CN116514541A (en) * | 2023-05-09 | 2023-08-01 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of composite ceramic absorber material and application of material |
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Application publication date: 20130522 |