CN108314323A - A kind of glass ceramic composite material preparation method containing pyrochlore - Google Patents
A kind of glass ceramic composite material preparation method containing pyrochlore Download PDFInfo
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- CN108314323A CN108314323A CN201810263203.8A CN201810263203A CN108314323A CN 108314323 A CN108314323 A CN 108314323A CN 201810263203 A CN201810263203 A CN 201810263203A CN 108314323 A CN108314323 A CN 108314323A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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Abstract
The glass ceramic composite material preparation method containing pyrochlore that the present invention relates to a kind of, and in particular to a kind of precursor powder is prefabricated+and sintering reaction prepares and contains Ln2Ti2O7The method of pyrochlore borosilicate glass ceramic composite.This method prepares high-purity nm Ln with collosol and gel (sol gel) method first2Ti2O7Then precursor powder is uniformly mixed with the glass raw material after melt water quenching by design proportion, after being pressed into block blank, at 1100~1200 DEG C keep the temperature 1~12h can be made different quality than contain Ln2Ti2O7Pyrochlore borosilicate glass ceramic composite.Sample prepared by the present invention has many advantages, such as that phase purity is high, pyrochlore phase and glass baseplate compatibility are good, two-phase proportion is adjustable.
Description
Technical field
A kind of glass ceramic composite material preparation method containing pyrochlore, and in particular to a kind of precursor powder is prefabricated+it burns
Prepared by knot reaction contains Ln2Ti2O7The method of the borosilicate glass ceramic composite of pyrochlore.
Background technology
With the promotion of reactor burnup, the extension of refulling cycle and use MOX (Mixed Oxide Fuel) fuel
Deng, in the spentnuclear fuel post-processing flow of uranium plutonium codecontamination, the high activity liquid waste of generation (High-Level Liquid Waste,
HLLW) irradiation intensity and alpha activity level constantly enhance.According to statistics, though the HLLW that spentnuclear fuel per ton is generated only account for it is useless
The 3% of object total volume but contains in spentnuclear fuel 95% or more radioactivity.Therefore, the long-term safety processing of HLLW is disposed
As the key points and difficulties of countries in the world Abfallwirtschaft, while it being also one of the key factor for restricting world nuclear industry development.
In recent years, the glass solidification of HLLW because the inclusion quantity to actinium series nucleic low (≤0.4wt.%), long-time stability it is poor
The problems such as (easy split-phase and the water-soluble yellow phase of generation), limit the development of HLLW glass solidifications；The ceramic solidification of HLLW have than
The stronger resistance to alpha irradiation of glass, anti-leaching ability and thermal stability are, it can be achieved that larger actinium series nucleic inclusion quantity and effectively avoid glass
The split-phase and yellow phase problem that glass solidification generates.But the production technology of ceramics is complicated, synthesis condition harshness (high temperature and pressure), technique behaviour
Make discontinuously, the engineering to limit HLLW ceramic solidifications is promoted.
Glass ceramics is manufactured a kind of ceramic complex phase material being combined with glass by melting, molding and heat treatment
Material.Radionuclide is fixed in crystallization ceramic phase in glass ceramics firming body or with " isomorph " substitution or disperse
It is distributed in inertia glass matrix.Compared with glass solidification, glass ceramics has higher mechanical strength, preferably heat-resisting and change
Learn stability.Compared with ceramic solidification, the preparation process of glass ceramics is simple, can form ceramic phase at a lower temperature.In addition,
Actinium series nucleic will obtain the double shield of glass and ceramics and more effectively be isolated with biosphere.Therefore, glass ceramics has become
Cure the new candidate base materials of HLLW.
Currently, the glass-ceramic curing substrate for HLLW has developed many candidate materials.Wherein, zirconolite
CaZrTi2O7Glass ceramics constrains it to the inclusion quantity of actinium series nucleic and further applies less；Ca4-xRE6+x(PO4)6O2Glass
Under lower alpha irradiation metamict easily occurs for ceramic phase in ceramics；Monazite LnPO4LnPO in glass ceramics4Thermal conductivity
It is low that ceramic phase crackle will certainly be promoted to generate, actinium series nucleic is accelerated to leach.Therefore, the ceramic phase in existing glass ceramics firming body
It is poor to be primarily present irradiation, chemistry and thermal stability, the deficiencies such as low to actinium series nucleic solid solubility.
Titanium-based pyrochlore (A=Ln or An) because having excellent Radiation hardness and chemical stability, it is praised
To be the curing substrate of Excitation Bands prime ideal.Australia Zhang in 2013 etc. takes the lead in having prepared titanium-based pyrochlore-borosilicic acid
Salt glass ceramics curing system, they are successfully synthesized by rational composition design on borosilicate glass matrix
(Ca1.25U0.75)Ti2O7、(Ca0.75Gd0.35Hf0.1U0.4Pu0.4)Ti2O7Titanium-based pyrochlore.But in the glass-ceramic preparation process
In, in addition to titanium-based pyrochlore, also Ca3Al6Si2O16、USiO4It is generated etc. unstable crystalline phase, this will certainly reduce glass ceramics
Stability limits the further development of the glass ceramics curing substrate.
Invention content
The glass ceramic composite material preparation method containing pyrochlore that the present invention provides a kind of, glass prepared by this method
Glass-ceramic composite has many advantages, such as that phase purity is high, pyrochlore-glass two-phase good compatibility, two-phase proportion is adjustable.
What the present invention was achieved through the following technical solutions：
A kind of glass ceramic composite material preparation method containing pyrochlore, processing step are as follows：
Step 1：Sol-gel methods prepare Ln2Ti2O7Pyrochlore presoma
According to Ln2Ti2O7Ln lanthanum nitrates (Ln=Sm, Eu, Gd, Er, Lu) corresponding to the calculating of the atomic ratio measuring of Ti in molecular formula
With the dosage of butyl titanate, a certain amount of deionized water, ethyl alcohol/nitric acid is used in combination to dissolve lanthanum nitrate and butyl titanate respectively,
It stirs 3~5h and obtains two kinds of clear solutions；It takes and matches two kinds of solution and mixed at room temperature, and add network into mixed solution
Gel is made in mixture citric acid and polyethylene glycol-20000, adjusts the pH to 5.0 of gel with ammonium hydroxide later；
Gel is atomised in 350~400 DEG C of corundum crucible using compressed air as atomizing medium, later moves to crucible
4h is kept the temperature at 900 DEG C pyrochlore precursor powder is made in high temperature furnace.
Step 2：Fusion method prepares glass presoma
SiO in mass ratio2∶Al2O3∶H3BO3∶Na2CO3=(64~67): (8.5~10): (5~6): (18.5~20) claim
Measure glass raw material；Water quenching after being melted at 1400 DEG C after raw material grinding uniformly；Glass after water quenching is regrind into powder.
Step 3：Sintering process prepares Ln2Ti2O7Pyrochlore-borosilicate glass ceramic composite
Take pyrochlore precursor powder and the glass powder (30~90) in mass ratio after water quenching in step 2 in step 1:
(70~10), which are ground, to be mixed, and is pressed into block blank at 8~10MPa later；Preforming block blank is put into high temperature
It is sintered in stove, sintering temperature is 1100~1200 DEG C, 1~12h of sintering time；It cools to room temperature with the furnace, obtains Ln2Ti2O7
Pyrochlore-borosilicate glass composite material.
A kind of glass ceramic composite material preparation method containing pyrochlore, it is characterised in that：Obtained in step 1 is
High-purity, nanometer Ln2Ti2O7Pyrochlore powder.
A kind of glass ceramic composite material preparation method containing pyrochlore, it is characterised in that：Glass obtained in step 2
Glass ingredient is uniform, and thermal stability is high, is not easy crystallization.
A kind of glass ceramic composite material preparation method containing pyrochlore, it is characterised in that：Glass ceramics in step 3
Composite material, Ln2Ti2O7Pyrochlore is unique crystalline phase in glass matrix, and no other dephasigns generate, and phase purity is high.
, it is characterised in that：Glass ceramic composite material in step 3, Ln2Ti2O7Pyrochlore is distributed on glass matrix
Uniformly, crystallite dimension is controllable；Two intersection interfaces are clearly non-microcracked, and compatibility is good.
A kind of glass ceramic composite material preparation method containing pyrochlore, which is characterized in that the glass ceramics in step 3
Composite material, pyrochlore/glass two-phase mass ratio can arbitrarily regulate and control to obtain the glass ceramics sample of different ratio.
Beneficial effects of the present invention：
The advantages of present invention is compared with existing Excitation Bands element glass ceramic solidification base material is：
(1) HLLW glass solidifications has been selected to be engineered containing of the borosilicate glass system of application as pyrochlore phase
Body has thermal stability, the better advantage of water resistance；
(2) solidification main phase of the titanium-based pyrochlore as actinium series nucleic is used, Radiation hardness and chemical stability are more preferable；
(3) the titanium-based pyrochlore for using sol-gel (sol-gel) method to prepare, has the advantages that high-purity；
(4) glass ceramic composite material prepared by the present invention can guarantee that pyrochlore is uniquely the presence of ceramics on glass matrix
Phase, phase purity is high, and no other water-soluble, stability difference dephasigns generate；
(5) glass ceramic composite material prepared by the present invention, pyrochlore-glass two-phase good compatibility, interface is without fine fisssure
Line generates；
(6) glass ceramic composite material prepared by the present invention, two-phase proportion can be carried out according to the actinium series radionuclide content of containing
Arbitrary proportion is adjusted, high to actinium series nucleic type and content adaptability.
Description of the drawings
Further the present invention will be described with reference to the accompanying drawings and examples.
Fig. 1 is 900 DEG C of Sm dealt in embodiment 12Ti2O7The X-ray diffractogram of pure pyrochlore precursor powder
Spectrum.
Fig. 2 is to contain Sm in embodiment 12Ti2O7The X-ray diffractogram of the borosilicate glass ceramic composite of pyrochlore
Spectrum.
Fig. 3 is to contain Gd in embodiment 22Ti2O7The X-ray diffractogram of the borosilicate glass ceramic composite of pyrochlore
Spectrum.
Fig. 4 is different ratio Er in embodiment 32Ti2O7The X-ray of pyrochlore-borosilicate glass ceramic composite is spread out
Penetrate collection of illustrative plates.
Fig. 5 is to contain Er in embodiment 4 under the conditions of different disposal2Ti2O7The borosilicate glass ceramic composite of pyrochlore
X ray diffracting spectrum.
Fig. 6 is to contain Sm in embodiment 12Ti2O7The SEM of the borosilicate glass ceramic composite of pyrochlore schemes.
Specific implementation mode
It is the part specific implementation example of the present invention below.But institute's protection domain of the present invention is without being limited thereto.
Embodiment 1：As shown in Figure 1, Figure 2, Figure 6 shows, the borosilicate glass ceramic composite of the pyrochlore containing Sm2Ti2O7
Preparation method, steps are as follows：
Step 1：Sol-gel methods prepare the preparation of Sm2Ti2O7 pyrochlores
To prepare in terms of 3g pyrochlores Sm2Ti2O7, weigh Sm (NO3) 36H2O of 5.2434g, with 30ml deionized waters into
Row dissolving；The butyl titanate for weighing 4.0157g is dissolved with ethyl alcohol and nitric acid, and respectively stirring is to being mixed after transparent；To mixed
It closes addition citric acid, polyethylene glycol-20000 in solution and gel is made, ammonium hydroxide is used in combination to adjust the pH to 5.0 of gel.
Gel is atomized into 350 DEG C of corundum crucible with compressed air, then moves to crucible in high temperature furnace at 900 DEG C
Pyrochlore powder is made in lower calcining 4h.
Step 2：Fusion method prepares glass presoma
Glass raw material is weighed with mass ratio SiO2: Al2O3: H3BO3: Na2CO3=65.75: 9.3: 5.64: 19.31；It will
Water quenching after being melted at 1400 DEG C after raw material grinding uniformly；Glass after water quenching is regrind into powder.
Step 3：Sintering process prepares Sm2Ti2O7 pyrochlores-borosilicate glass ceramic composite
Pyrochlore precursor powder in step 1 is taken to be carried out with the glass powder in mass ratio 50: 50 after water quenching in step 2
Grinding is mixed, and is pressed into block blank at 10MPa later；Preforming block blank is put into high temperature furnace and is sintered, is burnt
Junction temperature is 1200 DEG C, sintering time 6h；It cools to room temperature with the furnace, obtains the borosilicate of the Sm2Ti2O7 pyrochlores containing 50wt.%
Silicate glass ceramic composite.
Embodiment 2：As shown in figure 3, the preparation side of the borosilicate glass ceramic composite of the pyrochlore containing Gd2Ti2O7
Method, steps are as follows：
Step 1：Sol-gel methods prepare the preparation of Gd2Ti2O7 pyrochlores
To prepare in terms of 5g pyrochlores Gd2Ti2O7, weigh Gd (NO3) 36H2O of 8.6492g, with 30ml deionized waters into
Row dissolving；The butyl titanate for weighing 6.5181g is dissolved with ethyl alcohol and nitric acid, and respectively stirring is to being mixed after transparent；To mixed
It closes addition citric acid (8g/100ml), polyethylene glycol-20000 (5g/100ml) in solution and gel is made, be used in combination ammonium hydroxide to adjust solidifying
The pH to 5.0 of glue.
Gel is atomized into 350 DEG C of corundum crucible with compressed air, then moves to crucible in high temperature furnace at 900 DEG C
Pyrochlore powder is made in lower calcining 4h.
Step 2：Heat treating process prepares glass presoma
Glass raw material is weighed with mass ratio SiO2: Al2O3: H3BO3: Na2CO3=66: 9: 5.6: 19.4, raw material is ground
Water quenching after being melted at 1400 DEG C after uniformly；Glass after water quenching is regrind into powder.
Step 3：Sintering process prepares Gd2Ti2O7 pyrochlores-borosilicate glass ceramic composite
Pyrochlore precursor powder in step 1 is taken to be carried out with the glass powder in mass ratio 50: 50 after water quenching in step 2
Grinding is mixed, and is pressed into block blank at 8MPa later；Preforming block blank is put into high temperature furnace and is sintered, is sintered
Temperature is 1200 DEG C, sintering time 6h；It cools to room temperature with the furnace, obtains the borosilicate glass ceramics of the pyrochlore containing Gd2Ti2O7
Composite material.
Embodiment 3：As shown in figure 4, Er2Ti2O7 pyrochlores-borosilicate glass ceramic composite of different ratio
Preparation method, steps are as follows：
Step 1：Sol-gel methods prepare the preparation of Er2Ti2O7 pyrochlores
To prepare in terms of 5g pyrochlores Er2Ti2O7, weigh Er (NO3) 36H2O of 8.5063g, with 30ml deionized waters into
Row dissolving；The butyl titanate for weighing 6.2764g is dissolved with ethyl alcohol and nitric acid, and respectively stirring is to being mixed after transparent；To mixed
It closes addition citric acid (8g/100ml), polyethylene glycol-20000 (5g/100ml) in solution and gel is made, be used in combination ammonium hydroxide to adjust solidifying
The pH to 5.0 of glue.
Gel is atomized into 400 DEG C of corundum crucible with compressed air, then moves to crucible in high temperature furnace at 900 DEG C
Pyrochlore powder is made in lower calcining 4h.
Step 2：Fusion method prepares glass presoma
Glass raw material is weighed with mass ratio SiO2: Al2O3: H3BO3: Na2CO3=65: 10: 6: 19, raw material is ground equal
Water quenching after being melted at 1400 DEG C after even；Glass after water quenching is regrind into powder.
Step 3：Sintering process prepares Er2Ti2O7 pyrochlores-borosilicate glass ceramic composite of different ratio
Take glass powder in step 1 in pyrochlore precursor powder and step 2 after water quenching by quality (30~90)/
(70~10), which are ground, to be mixed, and is pressed into block blank at 8MPa later；Preforming block blank is put into high temperature furnace
It is sintered, sintering temperature is 1200 DEG C, sintering time 6h；Cool to room temperature with the furnace, the Er2Ti2O7 for obtaining different ratio is burnt
Green stone-borosilicate glass ceramic composite.
Embodiment 4：As shown in figure 5, the borosilicate glass ceramics of the pyrochlore containing Er2Ti2O7 are multiple under the conditions of different disposal
The preparation method of condensation material, steps are as follows：
Step 1：Sol-gel methods prepare the preparation of Er2Ti2O7 pyrochlores
To prepare in terms of 5g pyrochlores Er2Ti2O7, weigh Er (NO3) 36H2O of 8.5063g, with 30ml deionized waters into
Row dissolving；The butyl titanate for weighing 6.2764g is dissolved with ethyl alcohol and nitric acid, and respectively stirring is to being mixed after transparent；To mixed
It closes addition citric acid (8g/100ml), polyethylene glycol-20000 (5g/100ml) in solution and gel is made, be used in combination ammonium hydroxide to adjust solidifying
The pH to 5.0 of glue.
Gel is atomized into 400 DEG C of corundum crucible with compressed air, then moves to crucible in high temperature furnace at 900 DEG C
Pyrochlore powder is made in lower calcining 4h.
Step 2：Fusion method prepares glass presoma
Glass raw material is weighed with mass ratio SiO2: Al2O3: H3BO3: Na2CO3=65: 10: 6: 19, raw material is ground equal
Water quenching after being melted at 1400 DEG C after even；Glass after water quenching is regrind into powder.
Step 3：Sintering process prepares Er2Ti2O7 pyrochlores-borosilicate glass ceramic composite of different ratio
Pyrochlore precursor powder in step 1 is taken to be ground by quality 50/50 with the glass powder after water quenching in step 2
Mill is mixed, and is pressed into block blank at 8MPa later；Preforming block blank is put into high temperature furnace and is sintered, sintering temperature
Degree is respectively 1100 DEG C, 1150 DEG C, 1200 DEG C, and sintering time is respectively 1h, 6h, 12h；It cools to room temperature with the furnace, obtains difference
Er2Ti2O7 pyrochlores-borosilicate glass ceramic composite with when different disposal condition.
It should be noted that the above citing is only several specific embodiments of the present invention, the present invention be not limited only to
Upper embodiment can also have other deformations.Those skilled in the art directly exports from the disclosure of invention or draws indirectly
All deformations of Shen, are considered protection scope of the present invention.
Claims (6)
1. a kind of glass ceramic composite material preparation method containing pyrochlore, which is characterized in that comprise the steps of：
Step 1：Sol-gel methods prepare Ln2Ti2O7Pyrochlore presoma
According to Ln2Ti2O7Ln calculates the dosage of corresponding lanthanum nitrate and butyl titanate, Ln=to the atomic ratio measuring of Ti in molecular formula
Sm, Eu, Gd, Er, Lu are used in combination a certain amount of deionized water, ethyl alcohol/nitric acid to dissolve lanthanum nitrate and butyl titanate, stirring 3 respectively
~5h obtains two kinds of clear solutions；It takes and matches two kinds of solution and mixed at room temperature, and add complexing agent into mixed solution
Gel is made in citric acid and polyethylene glycol-20000, adjusts the pH to 5.0 of gel with ammonium hydroxide later；
Gel is atomised in 350~400 DEG C of corundum crucible using compressed air as atomizing medium, crucible is moved into high temperature later
4h is kept the temperature at 900 DEG C pyrochlore precursor powder is made in stove；
Step 2：Fusion method prepares glass presoma
SiO in mass ratio2∶Al2O3∶H3BO3∶Na2CO3=(64~67): (8.5~10): (5~6): (18.5~20) weigh glass
Glass raw material；Water quenching after being melted at 1400 DEG C after raw material grinding uniformly；Glass after water quenching is regrind into powder；
Step 3：Prepared by sintering process contains Ln2Ti2O7The borosilicate glass ceramic composite of pyrochlore
Take pyrochlore precursor powder and glass powder obtained (30~90) in mass ratio in step 2 in step 1: (70~
10) it is ground and is mixed, be pressed into block blank at 8~10MPa later；By preforming block blank be put into high temperature furnace into
Row sintering, sintering temperature are 1100~1200 DEG C, 1~12h of sintering time；It cools to room temperature with the furnace, obtains containing Ln2Ti2O7It burns green
The borosilicate glass composite material of stone.
2. a kind of glass ceramic composite material preparation method containing pyrochlore according to claim 1, it is characterised in that：Step
That obtained in rapid one is high-purity, nanometer Ln2Ti2O7Pyrochlore powder.
3. a kind of glass ceramic composite material preparation method containing pyrochlore according to claim 1, it is characterised in that：Step
Obtained in rapid two is the uniform glass of ingredient.
4. a kind of glass ceramic composite material preparation method containing pyrochlore according to claim 1, it is characterised in that：Step
Glass ceramic composite material in rapid three, Ln2Ti2O7Pyrochlore is unique crystalline phase in glass matrix.
5. a kind of glass ceramic composite material preparation method containing pyrochlore according to claim 1, it is characterised in that：Step
Glass ceramic composite material in rapid three, Ln2Ti2O7Pyrochlore is evenly distributed on glass matrix, and crystallite dimension is controllable；Two-phase
Interface is clearly non-microcracked.
6. a kind of glass ceramic composite material preparation method containing pyrochlore according to claim 1, which is characterized in that step
Glass ceramic composite material in rapid three, pyrochlore/glass two-phase mass ratio are controllable to obtain the glass ceramics of different ratio
Sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761500A (en) * | 2019-03-06 | 2019-05-17 | 西南科技大学 | A kind of preparation method of the borosilicate glass ceramic solidification body containing uranpyrochlore |
| CN115448599A (en) * | 2022-09-27 | 2022-12-09 | 山东国瓷功能材料股份有限公司 | Glass ceramic with opalescent effect and preparation method thereof |
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| CN103664192A (en) * | 2012-09-24 | 2014-03-26 | 西南科技大学 | Preparation method of pure-phase pyrochlore structure Ce2Zr2O7 |
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| CN103664192A (en) * | 2012-09-24 | 2014-03-26 | 西南科技大学 | Preparation method of pure-phase pyrochlore structure Ce2Zr2O7 |
Non-Patent Citations (2)
| Title |
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| LINGGEN KONG,ET AL: "A new method for production of glass-Ln2Ti2O7 pyrochlore (Ln=Gd, Tb, Er, Yb)", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761500A (en) * | 2019-03-06 | 2019-05-17 | 西南科技大学 | A kind of preparation method of the borosilicate glass ceramic solidification body containing uranpyrochlore |
| CN115448599A (en) * | 2022-09-27 | 2022-12-09 | 山东国瓷功能材料股份有限公司 | Glass ceramic with opalescent effect and preparation method thereof |
| CN115448599B (en) * | 2022-09-27 | 2023-10-31 | 山东国瓷功能材料股份有限公司 | Glass ceramic with opalescence effect and preparation method thereof |
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