CN102643089A - High-temperature and high-pressure rapid synthesis method of Gd2Zr2O7 pyrochlore ceramic - Google Patents

High-temperature and high-pressure rapid synthesis method of Gd2Zr2O7 pyrochlore ceramic Download PDF

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CN102643089A
CN102643089A CN2012100914013A CN201210091401A CN102643089A CN 102643089 A CN102643089 A CN 102643089A CN 2012100914013 A CN2012100914013 A CN 2012100914013A CN 201210091401 A CN201210091401 A CN 201210091401A CN 102643089 A CN102643089 A CN 102643089A
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hthp
pyrrhite
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唐敬友
谢华
卢喜瑞
易发成
罗学刚
肖正学
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Southwest Jiaotong University
Southwest University of Science and Technology
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Abstract

The invention discloses a high-temperature and high-pressure rapid synthesis method of Gd2Zr2O7 pyrochlore ceramic, which comprises the five steps of: batching, grinding, drying, dry pressing and high-temperature and high-pressure synthesis. The high-temperature and high-pressure rapid synthesis method has the beneficial effects that within the wide pressure and temperature scope, a multi-component oxide mixture is taken as a raw material, the synthesis of a Gd2-xAxZr2-yByO7 (x is more than or equal to 0 but less than or equal to 2, and y is more than or equal to 0 but less than or equal to 2) compound with a pyrochlore structure and the dense sintering of the ceramic is realized at the same time, and the time required is only 15-30 minutes, so that the preparation time of the pyrochlore ceramic is greatly shortened; and compared with the prior art, the time used is shortened by 100 times at least, the efficiency is improved, and the practicability is strong.

Description

Gd 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery
Technical field
The present invention relates to Gd 2Zr 2O 7Pyrrhite base pottery Gd 2-xA xZr 2-yB yO 7The HTHP fast synthesis method of (0≤x≤2,0≤y≤2), wherein A, B position are respectively trivalent and quadrivalent cation, all can be REE or actinoid.If A, B all are REE, then Gd 2-xA xZr 2-yB yO 7(0＜x＜2,0＜y＜2) type stupalith has the ability of ionic conduction, electronic conduction under External Electrical Field, can be used for the electrolyte of high temperature solid oxide fuel cell; If A, B all are actinoids, Gd 2-xA xZr 2-yB yO 7(0≤x≤2,0≤y≤2) type stupalith has contained the actinium series nucleic, becomes the cured body of actinium series nucleic, thereby can be used for the solidification treatment of higher chain product and α refuse, can also be the oxide solid solution of U and Pu to Gd 2Zr 2O 7Processing the MOX element in the pyrrhite base pottery is used for fast reactor or processes inactive ceramic base material (IFM) being used for following long lifetime nuclide transmutation technology.
Background technology
Nuclear disarmament mainly refers to the weapongrade excess stock that produces 235U with 239Two kinds of easy fissioners of Pu utilize the nuclear technique generating also will produce a large amount of spent fuels, wherein also contain a large amount of plutoniums and (mainly are 239Pu) with time actinium series nucleic (particularly neptunium, americium, curium, berkelium and californium), the safe handling of these higher chain products has become the whole world with disposal and has had challenging science and technology problem.
The eighties in 20th century, it is found that La 2O 3-ZrO 2The pyrochlore constitution material that the sosoloid of (La represents lanthanon) system forms has good ion (comprising positively charged ion, negatively charged ion and electronics) conductivity, is the solid electrolyte material of one type of promising high-temperature fuel cell.1987, the Uehara of Japan etc. systematically studied ZrO first 2-Gd 2O 3The high temperature solid state reaction of system utilizes ZrO 2And Gd 2O 3Powder raw material can synthesize the Gd of pyrochlore constitution in the mol ratio of broad and TR 2Zr 2O 7, " solid ion " (" Solid State Ionics ") magazine 23 phases of version in 1987 the 137th～143 page of ZrO by name 2-Gd 2O 3(" the Stability and antiphase domain structure of the pyrochlore solid solution in the ZrO of the stability of pyrrhite and antiphase domain structure in the system 2-Gd 2O 3System ") article announced this research.Yet,, adopt the Gd of the synthetic desirable stoicheiometry of high temperature solid state reaction under the normal pressure at present owing to receive the restriction of reaction kinetics 2Zr 2O 7Required optimum temps is 1550 ℃; The generated time that needs in most cases surpasses 48 hours even the longer time; This explains that it is a kind of difficult synthetic material, and Ewing R C is published in " earth and planetary science wall bulletin " (" Earth Planet.Sci.Lett ") magazine 229 phases of version in 2005,165～181 pages plutonium by name and time actinium series nucleic: safety is confined the article of (" Plutonium and " minor " actinides:safe sequestration ") and has been announced this report.
The gadolinium zirconium pyrrhite (Gd of anti-irradiation 2Zr 2O 7) be the desirable base material that solidifies the actinium series nucleic.Main application background is to two different aspects: (1) rare earth doped gadolinium zirconium pyrrhite is used for the exploitation of following high-temperature solid fuel battery as the ion conductive solid electrolyte material; The gadolinium zirconium pyrrhite of (2) doping group of the lanthanides and actinoid is used for high-level waste and solidifies actinium series nucleic and fission product element.
When B.P.Mandal etc. utilize the cured body of the synthesized solidified neodymium of high-temperature solid phase reaction method, nearly 120 hours of the time of whole compound experiment; When profits such as S.J.Patwe use the same method the cured body of synthesized solidified Ce, also used the identical time." alloy and compound journal (" Journal of Alloys and Compounds ") magazine was published 389 phase 243-246 pages or leaves of 437 phase 260-263 pages or leaves and version in 2005 in 2007, the Gd of common component by name 2-xNd xZr 2O 7The preparation and high temperature X-ray diffraction (" the Preparation and high temperature-XRD studies on a pyrochlore series with the general composition Gd of pyrrhite series 2-xNd xZr 2O 7") and Gd 2Zr 2-xCe xO 7Synthetic, the sign of some compound and lattice thermal expansion (" Synthesis, characterization and lattice thermal expansion of some compounds in the Gd in the pyrrhite system 2Zr 2-xCe xO 7System ") two pieces of articles announced this two experiments respectively.
At present, the solid state reaction compound method cost of pyrrhite is high, efficient is low, can't be near the actual needs of through engineering approaches.
Summary of the invention
In order to solve the problems of the technologies described above, the present invention provides a kind of efficient high, practical Gd 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery, its technical scheme is following:
A kind of Gd 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery may further comprise the steps:
1) batching
By molecular formula Gd 2-xA xZr 2-yB yO 7Stoichiometric ratio in (0≤x≤2,0≤y≤2) is got Gd 2O 3, ZrO 2, A 2O 3And BO 2In two kinds, three kinds or four kinds of powder stocks, wherein elements A and B are REE or actinoid, the calculation formula of the mass percent of elements A or B does
W = M k M P × 100 %
Wherein, M kFor x (or y) multiply by the relative atomic weight of elements A (or B), M pExpression pyrochlore constitution material Gd 2-xA xZr 2-yB yO 7Molecular weight;
If x=0 and y=0 then obtain Gd 2Zr 2O 7The prescription of pyrrhite matrix stupalith, Gd 2O 3With ZrO 2Desirable stoichiometric ratio be 1: 2;
The value of x confirms that said elements A is at Gd 2-xA xZr 2-yB yO 7The scope of the mass percent in (0≤x≤2,0≤y≤2);
If during x=0, then be the material Gd of pyrochlore constitution 2Zr 2-yB yO 7If x=2, then A 3+Complete displacement Gd of equal value 3+, become Gd 2Zr 2-yB yO 7If 0＜x＜2, then A 3+Part displacement Gd of equal value 3+, become Gd 2Zr 2-yB yO 7
The value of y confirms that said element B is at Gd 2-xA xZr 2-yB yO 7The scope of the mass percent in (0≤x≤2,0≤y≤2);
If during y=0, then be the material Gd of pyrochlore constitution 2-xA xZr 2O 7If y=2, then B 4+Complete displacement Zr of equal value 4+, become Gd 2-xA xB 2O 7If 0＜y＜2, then B 4+Part displacement Zr of equal value 4+, become Gd 2-xA xZr 2-yB yO 7
2) grind
With three kinds in the step 1) or two kinds of material powders according to the accurate weighing of the formulating of recipe of step 1) after, its mixture was ground 1～3 hour, obtain finely dispersed mixed powder, the size-grade distribution peak value after this mixed powder grinds is controlled at 1～5 μ m3) drying
With step 2) composite granule of gained makes drying treatment through infrared rays, vacuum or a conventional oven;
4) dry-pressing formed
Mixed powder is packed in the cylindrical steel mould, is green compact through press compression moulding under the pressure of 20～40MPa; The integrity of moulding is decided by by the length-to-diameter ratio of moulding sample, usually less than 1, otherwise when the demoulding, can cause sample to damage.
5) HTHP sintering
The green compact of processing are packed in the thin-walled canning tube of refractory metal or alloy or chemical inert material; In high-temperature high-pressure apparatus, carry out the HTHP solid state reaction; Its pressure range is 0.15～6GPa, and TR is 1200～1600 ℃, and the heat-insulation pressure keeping time is 15～30min; Release then, cooling, taking-up goods promptly make and solidify the compound with pyrochlore constitution.Used high-tension apparatus comprises any device and the equipment that can produce above temperature and pressure condition; When on dissimilar high-temperature high-pressure apparatuses, operating; Need according to relevant working specification operational outfit, and note heating, the time variable control of heat-insulation pressure keeping and cooling release.
Desirable stoichiometric ratio described in the step 1) is a mol ratio.
Step 2) grinding plant that uses in is the ball mill (in enormous quantities) of mortar (short run) or zirconia ceramics liner and mill ball.
Mould inner wall baste paraffin body in step 4), the paraffin of baking 1h removal sample surfaces under the high temperature more than 200 ℃ then.
The thickness of thin-walled described in the step 5) is 0.1～0.2mm.Said canning tube is metal molybdenum pipe, hexagonal boron nitride pipe.Used high-tension apparatus is six-plane piercer, belt type press, hot isostatic press and hot pressed sintering machine.
Beneficial effect of the present invention:
The present invention is a raw material with the multivariant oxide mixture in very wide pressure and scope, has realized having the Gd of pyrochlore constitution simultaneously 2-xA xZr 2-yB yO 7The dense sintering of the synthetic and pottery of (0≤x≤2,0≤y≤2) compound, required time is merely 15～30min, has shortened the preparation time of pyrrhite pottery greatly, and the time more used than conventional art shortens 100 times at least, has improved efficient, and is practical.
Description of drawings
Fig. 1 is the sem photograph of the embodiment of the invention 15 synthetic samples;
Fig. 2 is the sem photograph of the embodiment of the invention 16 synthetic samples;
Fig. 3 is the sem photograph of the embodiment of the invention 17 synthetic samples;
Fig. 4 is the sem photograph of the embodiment of the invention 18 synthetic samples;
Fig. 5 is the XRD figure of embodiment 19～29 synthetic samples.
Embodiment
Below in conjunction with the accompanying drawing embodiment method of the present invention is done explanation in further detail.
Embodiment of the invention 1-10: a kind of HTHP solid state reaction compound method of pyrrhite comprises batching, grinding, drying, dry-pressing formed and synthetic five steps of HTHP.
Said batching step is pressed stoichiometric equation Gd 2-xA xZr 2O 7Get Gd 2O 3, ZrO 2With trivalent element oxide compound A 2O 3Three kinds of raw materials, said trivalent element oxide compound adopts Nd 2O 3, then the calculation formula of the mass percent of Nd does
W 1 = M Nd M 0 = 144.24 x 144.24 x + 16 × 7 + ( 2 - x ) × 257.25 + 2 × 91.22 × 100 %
Wherein, 0＜x≤2, the value of x is confirmed the mass percent W of said trivalent element Nd 1Scope, its formulating of recipe is seen table 1.In the table, when at%Nd representes that Nd replaces Gd at the atomic percentage conc of Gd position.
Table 1 adds Nd 2O 3Formulating of recipe
Figure BSA00000694183000042
Can draw the mass percent W of said trivalent element Nd 1Scope be: 0＜W 1≤49.5%.
Said grinding steps grinds the mixture of above-mentioned three kinds of raw materials 1～8 hour, grinds 3 hours in the present embodiment, obtains finely dispersed mixed powder; This grinding steps grinds in the solvent absolute ethyl alcohol, removes by filter solvent then.
Said drying step is made drying treatment with composite granule through infrared rays.
Said dry-pressing formed step is green compact through punching block, under the pressure of 7.5MPa through press compression moulding with above-mentioned composite granule; Said compression moulding step can be suppressed into cylindrical green compact with above-mentioned composite granule, and its diameter is 8mm, highly for 6mm.
Said HTHP sintering step carries out HTHP solid state reaction sintering with said green compact in HTHP instrument (present embodiment employing six top surface); Wherein pressure range is 3～6GPa; TR is 1200～1600 ℃; The heat-insulation pressure keeping time is 15～30min, and release then, cooling, taking-up sample promptly make the compound with pyrochlore constitution of solidification simulation nucleic.HTHP instrument in this HTHP sintering step can adopt the six top surface device, and before the sintering, elder generation puts into six-plane piercer after green compact dry-pressing formed in the step 4 are fitted into sintering cavity.
Among the embodiment 1-10, the mass percent W of said trivalent element Nd 1Be provided with pressure, temperature and heat-insulation pressure keeping time processing parameter in the said HTHP synthesis step and see table 2.
The synthesis technologic parameter of table 2 embodiment 1-10
Figure BSA00000694183000043
Figure BSA00000694183000051
Embodiment of the invention 11-18: a kind of HTHP solid state reaction compound method of pyrrhite comprises batching, grinding, drying, dry-pressing formed and five steps of HTHP sintering.
In the present embodiment, press chemical formula Gd 2Zr 2-yB yO 7Get Gd 2O 3, ZrO 2With quadrivalent element oxide compound BO 2Prescription, wherein, said quadrivalent element oxide compound adopts CeO 2, the mass percent (W of Ce then 2) calculation formula do
W 2 = M Ce M 0 = 140.12 y 140.12 y + 16 × 7 + ( 2 - y ) × 91.22 + 2 × 257.25 × 100 %
Wherein, 0＜y≤2, the value of y is confirmed the mass percent W of said trivalent element Ce 2Scope, each formulating of recipe is seen like table 3.At%Ce representes that Ce replaces the atomic percentage conc of Zr position in the table.
Table 3 adds CeO 2Formulating of recipe
Figure BSA00000694183000053
Can draw the mass percent W of said quadrivalent element Ce 2Scope be: 0＜W 2≤39.65%.
Said grinding steps grinds the mixture of above-mentioned three kinds of raw materials 1～8 hour, grinds 1 hour in this instance, obtains finely dispersed composite granule; This grinding steps grinds in solvent comprises water ethanol, removes by filter solvent then.
Said drying step is made drying treatment with composite granule through vacuum unit.
Said dry-pressing formed step is green compact through punching block, under the pressure of 10MPa through press compression moulding with above-mentioned composite granule; Said compression moulding step can be suppressed into square with above-mentioned composite granule.
Said HTHP sintering step carries out HTHP solid state reaction sintering with said green compact in high-temperature high-pressure apparatus; Wherein pressure is 3～6GPa; Temperature is 1300～1600 ℃; The heat-insulation pressure keeping time is 5～20 minutes, and release then, cooling, taking-up green compact promptly make the compound with pyrochlore constitution of solidification simulation nucleic.HTHP instrument in this HTHP sintering step adopts six top surface, before the sintering, puts into six-plane piercer after earlier green compact dry-pressing formed in the step 4 to be fitted into sintering cavity.
Among the embodiment 11-18, the mass percent W of Ce 2Be provided with pressure, temperature and heat-insulation pressure keeping time processing parameter in the said HTHP sintering step and see table 4.Like Fig. 1-shown in Figure 4, be the sem photograph of embodiment 15-18 synthetic sample.
The synthesis technologic parameter of table 4 embodiment 11-18
Figure BSA00000694183000054
Figure BSA00000694183000061
Embodiment of the invention 19-29: a kind of HTHP solid state reaction compound method of pyrrhite comprises batching, grinding, drying, dry-pressing formed and five steps of HTHP sintering.
Said batching step is by molecular formula Gd 2-xA xZr 2-yB yO 7In the ratio of stoichiometric number get Gd 2O 3, ZrO 2, trivalent element oxide compound A 2O 3With quadrivalent element oxide compound BO 2Four kinds of raw materials, wherein said trivalent element oxide compound A 2O 3With quadrivalent element oxide compound BO 2Adopt Nd respectively 2O 3And CeO 2, the mass percent W of Nd then 3Mass percent W with Ce 4Be respectively
W 3 = M Nd M 0 = 144.24 x 257.25 ( 2 - x ) + 144.24 x + 91.22 ( 2 - y ) + 140.12 y + 16 × 7 × 100 %
W 4 = M Ce M 0 = 140.12 y 157.25 ( 2 - x ) + 144.24 x + 91.22 ( 2 - y ) + 140.12 y + 16 × 7 × 100 %
Wherein, 0≤x≤2,0≤y≤2, the value of x and y is confirmed the mass percent W of said trivalent element A 3Mass percent W with said quadrivalent element B 4Scope, the formulating of recipe of each embodiment is seen table 5.Fig. 5 is the XRD figure of embodiment 19～29 synthetic samples.
Table 5 adds Nd simultaneously 2O 3And CeO 2Formulating of recipe
Figure BSA00000694183000064
Can draw the mass percent W of said trivalent element Nd 3Scope be 0≤W 3≤42.38%, the mass percent W of said quadrivalent element Ce 4Scope be 0≤W 4≤41.17%.
Said grinding steps grinds the mixture of above-mentioned three kinds of raw materials 1～8 hour, grinds in the present embodiment to obtain finely dispersed composite granule in 8 hours; This grinding steps grinds in solvent acetone, removes by filter solvent then.
Said drying step is made drying treatment with composite granule through a conventional oven.
Said dry-pressing formed step is green compact through punching block, under the pressure of 20MPa through press compression moulding with above-mentioned composite granule; Said compression moulding step can be suppressed into the right cylinder green compact with above-mentioned composite granule.
Said HTHP synthesis step carries out HTHP solid state reaction sintering with said green compact in high-temperature high-pressure apparatus; Wherein pressure range is 0.15～0.35GPa; TR is 1300～1400 ℃; Heat-insulation pressure keeping time 20～30min, cools, takes out sample at release then, promptly makes the compound with pyrochlore constitution.High-temperature high-pressure apparatus in this HTHP synthesis step adopts the hot pressed sintering machine.Before the sintering, earlier green compact dry-pressing formed in the step 4 are fitted in the graphite grinding tool cavity, pressurize again and switch on heating.Concrete synthesis technologic parameter is seen table 6.
The synthesis technologic parameter of table 6 embodiment 19-29
Figure BSA00000694183000071
Fig. 1～4th, the method for the invention make the ESEM typical figure of product, and Fig. 5 is the X-ray diffraction typical case collection of illustrative plates that the method for the invention makes product.The product that above-mentioned all embodiment make all has same micro-structural feature.
The above; Be merely the preferable embodiment of the present invention; Protection scope of the present invention is not limited thereto; Any technician who is familiar with the present technique field is in the technical scope that the present invention discloses, and the simple change of the technical scheme that obtains or equivalence replacement all fall in protection scope of the present invention with may be obvious that.

Claims (7)

1. Gd 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that, may further comprise the steps:
1) batching
By molecular formula Gd 2-xA xZr 2-yB yO 7Stoichiometric ratio in (0≤x≤2,0≤y≤2) is got Gd 2O 3, ZrO 2, A 2O 3And BO 2In two kinds, three kinds or four kinds of powder stocks, wherein elements A and B are REE or actinoid, the calculation formula of the mass percent of elements A or B does
W = M k M P × 100 %
Wherein, M kFor x (or y) multiply by the relative atomic weight of elements A (or B), M pExpression pyrochlore constitution material Gd 2-xA xZr 2-yB yO 7Molecular weight;
If x=0 and y=0 then obtain Gd 2Zr 2O 7The prescription of pyrrhite matrix stupalith, Gd 2O 3With ZrO 2Desirable stoichiometric ratio be 1: 2;
The value of x confirms that said elements A is at Gd 2-xA xZr 2-yB yO 7The scope of the mass percent in (0≤x≤2,0≤y≤2);
If during x=0, then be the material Gd of pyrochlore constitution 2Zr 2-yB yO 7If x=2, then A 3+Complete displacement Gd of equal value 3+, become Gd 2Zr 2-yB yO 7If 0＜x＜2, then A 3+Part displacement Gd of equal value 3+, become Gd 2Zr 2-xB yO 7
The value of y confirms that said element B is at Gd 2-xA xZr 2-yB yO 7The scope of the mass percent in (0≤x≤2,0≤y≤2);
If during y=0, then be the material Gd of pyrochlore constitution 2-xA xZr 2O 7If y=2, then B 4+Complete displacement Zr of equal value 4+, become Gd 2-xA xB 2O 7If 0＜y＜2, then B 4+Part displacement Zr of equal value 4+, become Gd 2-xA xZr 2-yB yO 7
2) grind
With three kinds in the step 1) or two kinds of material powders according to the accurate weighing of the formulating of recipe of step 1) after, its mixture was ground 1～3 hour, obtain finely dispersed mixed powder, the size-grade distribution peak value after this mixed powder grinds is controlled at 1～5 μ m;
3) drying
With step 2) composite granule of gained makes drying treatment through infrared rays, vacuum or a conventional oven;
4) dry-pressing formed
Mixed powder is packed in the cylindrical steel mould, is green compact through press compression moulding under the pressure of 20～40MPa;
5) HTHP sintering
The green compact of processing are packed in the thin-walled canning tube of refractory metal or alloy or chemical inert material; In high-temperature high-pressure apparatus, carry out the HTHP solid state reaction; Its pressure range is 0.15～6GPa, and TR is 1200～1600 ℃, and the heat-insulation pressure keeping time is 15～30min; Release then, cooling, taking-up goods promptly make and solidify the compound with pyrochlore constitution.
2. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that desirable stoichiometric ratio described in the step 1) is a mol ratio.
3. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that step 2) in the grinding plant that uses be the ball mill of mortar or zirconia ceramics liner and mill ball.
4. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that, mould inner wall baste paraffin body in step 4), the paraffin of baking 1h removal sample surfaces under the high temperature more than 200 ℃ then.
5. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that the thickness of thin-walled described in the step 5) is 0.1～0.2mm.
6. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that canning tube described in the step 5) is metal molybdenum pipe, hexagonal boron nitride pipe.
7. Gd according to claim 1 2Zr 2O 7The HTHP fast synthesis method of pyrrhite base pottery is characterized in that used high-tension apparatus is six-plane piercer, belt type press, hot isostatic press and hot pressed sintering machine in the step 5).
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