CN109761500A - A kind of preparation method of the borosilicate glass ceramic solidification body containing uranpyrochlore - Google Patents
A kind of preparation method of the borosilicate glass ceramic solidification body containing uranpyrochlore Download PDFInfo
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Abstract
The present invention relates to Radwastes treatment technical fields, and in particular to a kind of preparation method of the borosilicate glass ceramic solidification body containing uranpyrochlore, the preparation method use SiO2、Al2O3、Na2CO3、B2O3、CaF2、CaO、U3O8And TiO2For raw material, by wet mixing drying respectively and pre-sinterings, step melting, sintering and quenching the obtained borosilicate glass ceramic solidification body of method, the preparation method can regulate and control the crystallization rate of uranpyrochlore in glass, reduce nucleic and remains in composition in glass phase, nucleic U can not only be improved in the inclusion quantity of ceramic phase, and inclusion quantity of the nucleic U in entire solidified body can be improved, the obtained borosilicate glass ceramic solidification body containing uranpyrochlore has the advantages that crystal grain distribution is uniform, dense structure's degree is high, intensity is good.
Description
Technical field
The present invention relates to Radwastes treatment technical fields, and in particular to a kind of borosilicate glass containing uranpyrochlore
The preparation method of ceramic solidification body.
Background technique
In the process that the spentnuclear fuel of uranium plutonium codecontamination post-processes, high activity liquid waste (High-Level can be generated
Radioactive Wastes, HLWs), HLWs radioactivity is strong, toxicity is big, heat generation rate is high, if HLWs is banished into environment, it will
Greatly harm is generated to environment.
Have in the prior art by HLLW (high-level waste) glass solidification or by the approach of HLLW ceramic solidification to handling
HLLW, but HLLW glass solidification is because of the inclusion quantity to actinium series nucleic low (≤0.4wt.%) and poor (easy point of long-time stability
Phase and the water-soluble yellow phase of generation) the problems such as, so that development is mass produced in HLLW glass solidification；The ceramic solidification ratio HLLW of HLLW
Glass solidification has stronger resistance to alpha irradiation, anti-leaching ability and thermal stability, and HLLW ceramic solidification can realize biggish Excitation Bands
Plain inclusion quantity and the split-phase for effectively avoiding glass solidification from generating and Huang Xiang Wenti, however the production technology of HLLW ceramic solidification is multiple
Miscellaneous, synthesis condition harshness (high temperature and pressure), technological operation is discontinuous, so that the large-scale production for limiting HLLW ceramic solidification is answered
With.
In recent years, the glass ceramics solidified body of HLWs gradually by it has been proposed that, ideal solidification effect are as follows: hot
Actinium series nucleic (An) can preferentially select to be solid-solubilized in stable ceramic phase, and low nucleic of putting then mainly is assigned in remaining fission product etc.
There are in glass medium.Currently, having delivered in periodical " atomic energy science and technology ", " preparation process is to uranpyrochlore base glass ceramics
The influence of solidified body structure and performance " text, prepared by melting-heat treating process that this article discloses using pre-sintering in conjunction with ball milling
HLWs glass ceramics solidified body, although melting-heat treating process of this pre-sintering in conjunction with ball milling can be reduced nucleic U and remain in
Composition in glass phase, while composition of the nucleic U in ceramic phase is improved, but this method still has following problems: ceramics
Ratio mutually in entire solidified body is limited, and no person will affect the intensity of solidified body, and which limits ceramic phases to the packet of nucleic U
Capacity, so that solidified body cannot handle high-level waste to large extent.Therefore, it is necessary to further improve the glass ceramics of HLWs
Production technology, to promote the production application of HLWs glass ceramics.
Summary of the invention
For the prior art, there are above-mentioned technical problems, and it is an object of the invention to provide a kind of borosilicates containing uranpyrochlore
The preparation method of glass ceramics solidified body, the preparation method can improve nucleic not only and can improve nucleic U in the inclusion quantity of ceramic phase,
And inclusion quantity of the nucleic U in entire solidified body can be improved, the obtained borosilicate glass ceramic solidification containing uranpyrochlore
Body has the advantages that crystal grain distribution is uniform, dense structure's degree is high, intensity is good.
To achieve the above object, the present invention the following technical schemes are provided:
A kind of preparation method of borosilicate glass ceramic solidification body containing uranpyrochlore is provided, comprising the following steps:
Step 1: weighing the component of following weight percent:
Step 2: pretreated glass ceramic raw material
By SiO2、Al2O3、Na2CO3、B2O3、CaF2With six kinds of component wet mixing drying of CaO, it is mixed to obtain uniformly mixed first
Object is closed, by U3O8And TiO2Two kinds of component wet mixings drying, obtains the second uniformly mixed mixture, will first mixture with
Second mixture is respectively under an argon atmosphere with 650~750 DEG C of 1~3h of sintering, then by sintered first mixture
Ball milling is distinguished with the second mixture, and the first mixture after ball milling is the first glass ceramics raw material, the second mixture after ball milling
For the second glass ceramics raw material；
Step 3: fusion method prepares female glass
The first glass ceramics raw material is first packed into crucible, then 1~2h of melting at 1500~1550 DEG C, then by second
Glass ceramics raw material is added in the second glass ceramics raw material in melting, continues 2~3h of melting hours at 1500~1550 DEG C,
Then the glass ceramics raw material of the melting is poured into graphite jig, obtains female glass by the glass ceramics raw material melted；
Step 4: borosilicate glass ceramic solidification body of the heat treatment preparation containing uranpyrochlore
The resulting female glass of step 3 is formed into ceramic nucleus, so with 700~800 DEG C of 1~5h of heat treatment in air atmosphere
Continue ceramics nucleus described in 1~5h of heat treatment at 1100~1200 DEG C afterwards, after heat treatment, by 30~40s of ceramic nucleus quenching,
Then ceramic nucleus is solidified at normal temperature, the borosilicate glass ceramic solidification body containing uranpyrochlore is made.
Wherein, in the step 2, Ball-milling Time is 3~4h.
Wherein, in the step 3, the crucible is corundum crucible.
Wherein, in the step 4, ceramic nucleus is placed in -20~-10 DEG C of room temperature and carries out quenching.
Beneficial effects of the present invention:
(1) present invention reduces the composition of the glass matrix in solidified body, is conducive to the composition for improving ceramic matrix, this hair
Bright preparation method can be reduced solid solution capacity of the nucleic U in glass phase and improve nucleic U in the solid solution capacity of ceramic phase, work as ceramic base
When body increases, then inclusion quantity of the nucleic U in entire solidified body can be improved；The resulting glass ceramics solidified body of the present invention is burnt with uranium
Green stone be principal crystalline phase, raw material weight percentage of the invention can guarantee uranpyrochlore crystallization rate so that containing uranpyrochlore
Borosilicate glass ceramic solidification body institutional framework is fine and close, the porosity is low, ceramic phase is evenly distributed, glass/ceramic two-phase is compatible
Property is good.
(2) when pretreated glass ceramic raw material of the present invention, glass matrix raw material and the difference wet mixing of ceramic matrix raw material are dried
Dry, sintering and ball-milling treatment, resulting first glass ceramics raw material and the second glass ceramics raw material can be respectively sufficiently mixed；
And due to calcium uranium oxide CaUO4There is competition generting machanism between uranpyrochlore, separate pretreated feedstock, makes pottery being formed
Tri- kinds of Element generation calcium uranium oxide CaUO of Ca, O, U are avoided before porcelain phase4, thus the forming core for the pyrochlore being conducive in ceramic phase
With grow up, and then be conducive to the nucleus forming of female glass ceramics phase；And each raw material can be activated preferably after ball milling, be similarly served to favor
The formation of pyrochlore in female glass.
(3) present invention prepares female glass using fusion method, since the ingredient of the second glass ceramics raw material is to include nucleic U's
U3O8With the nucleating agent TiO of pyrochlore2, the first glass ceramics of elder generation's melting raw material of the present invention, then again by the second glass ceramics raw material
It is melted with the second glass ceramics raw material, the first glass ceramics raw material of molten condition can be made to coat the second glass not melted thoroughly
Glass ceramic raw material, so that solid solution capacity and degree of enrichment of the nucleic U in pyrochlore are improved, and TiO2Make again after nucleic U is wrapped by
Pyrochlore nucleation, improves the stable degree that pyrochlore contains nucleic U, and then improve solid solution capacity of the nucleic U in ceramic phase,
Avoid the problem that glass ceramics solidified body intolerant to alpha irradiation.
(4) present invention using sintering process obtain glass ceramics solidified body, the sintering process spontaneously formed in air atmosphere with
Uranpyrochlore is that the glass ceramics of principal crystalline phase solidifies, and ceramic phase is more uniformly spread in glass ceramics solidified body obtained, group
Knit that structure is more fine and close, the solid U amount in ceramic phase can also compare favourably with sintering process, improve the glass ceramics solidification of HLWs
The quality of body is conducive to the solidified body large-scale production and application of HLWs glass ceramics, while the channel of processing has been mentioned for radioactive waste.
(5) present invention is by the of short duration quenching of ceramic nucleus after high-temperature heat treatment, and cooling becomes rigid to ceramic nucleating surface immediately
Property, and stress is not present still in soft state inside ceramic nucleus, and in subsequent cooling, ceramic nucleus internal cooling speed
Slow down, improves the toughness inside ceramics, and the rigidity reinforced of ceramic surface, the intensity of ceramics is improved, so that in glass base
In the case that body is reduced, glass ceramics solidified body remains to maintain intensity to a certain extent.
(6) the borosilicate glass ceramic solidification body containing uranpyrochlore of the invention is big to the inclusion quantity of nucleic U, structure knits knot
Structure is fine and close, the porosity is low, ceramic phase is evenly distributed, glass/ceramic two-phase compatibility is good, is suitable for large-scale production and application；This
The preparation method of borosilicate glass ceramic solidification body of the invention containing uranpyrochlore, simple production process is easily operated, is suitable for
Large-scale promotion application.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 1；
Fig. 2 is the SEM image of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 1；
Fig. 3 is the XRD spectrum of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 2；
Fig. 4 is the SEM image of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 2；
Fig. 5 is the XRD spectrum of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 3；
Fig. 6 is the SEM image of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 3；
Fig. 7 is Al, Si, Ca, Ti, U in the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 2
The distribution map of element.
Specific embodiment
Below in conjunction with specific embodiments and drawings, the present invention is described in detail.
Embodiment 1.
The preparation method of a kind of borosilicate glass ceramic solidification body containing uranpyrochlore of the present embodiment, Step 1: claiming
Take the component of following weight percent: SiO220.5%, Al2O34%, Na2CO39%, B2O34%, CaF217.5%, CaO4%,
U3O825.5%, TiO215%；
Step 2: pretreated glass ceramic raw material
By SiO2、Al2O3、Na2CO3、B2O3、CaF2With six kinds of component wet mixing drying of CaO, it is mixed to obtain uniformly mixed first
Object is closed, by U3O8And TiO2Two kinds of component wet mixings drying, obtains the second uniformly mixed mixture, will first mixture with
Then second mixture mixes sintered first mixture and second respectively under an argon atmosphere with 650 DEG C of sintering 1h
It closes object and distinguishes ball milling 3h, the first mixture after ball milling is the first glass ceramics raw material, and the second mixture after ball milling is second
Glass ceramics raw material；
Step 3: fusion method prepares female glass
The first glass ceramics raw material is first packed into crucible, then the melting 1h at 1500 DEG C, then by the second glass ceramics
Raw material is added in the second glass ceramics raw material in melting, continues melting 2 hours, the glass ceramics melted at 1500 DEG C
Then the glass ceramics raw material of the melting is poured into graphite jig, obtains female glass by raw material；
Step 4: borosilicate glass ceramic solidification body of the heat treatment preparation containing uranpyrochlore
The resulting female glass of step 3 is located into 1h, formation ceramics nucleus, then at 1100 DEG C in air atmosphere with 700 DEG C of heat
Under continue be heat-treated 1h described in ceramics nucleus, after heat treatment, by ceramic nucleus quenching 30s, then at normal temperature by ceramic nucleus
The borosilicate glass ceramic solidification body containing uranpyrochlore is made in solidification.
In the present embodiment, in the step 3, the crucible is corundum crucible.
In the present embodiment, in the step 4, ceramic nucleus is placed in -20~-10 room temperature and carries out quenching.
Performance test:
From XRD spectrum shown in FIG. 1 as it can be seen that the borosilicate glass ceramics obtained by embodiment 1 containing uranpyrochlore are solid
Change body and forms the glass ceramics solidified body using uranpyrochlore as principal crystalline phase.
From SEM image shown in Fig. 2 as it can be seen that the borosilicate glass ceramics obtained by embodiment 1 containing uranpyrochlore are solid
Change body mainly to grow in glass with white, square, and distribution is more uniform, it is good with glass compatibility.Solidify body tissue to cause
Close, no obvious stomata generates.
Embodiment 2.
The preparation method of a kind of borosilicate glass ceramic solidification body containing uranpyrochlore of the present embodiment, Step 1: claiming
Take the component of following weight percent: SiO220%, Al2O32%, Na2CO38%, B2O33%, CaF217%, CaO3%,
U3O830%, TiO216%；
Step 2: pretreated glass ceramic raw material
By SiO2、Al2O3、Na2CO3、B2O3、CaF2With six kinds of component wet mixing drying of CaO, it is mixed to obtain uniformly mixed first
Object is closed, by U3O8And TiO2Two kinds of component wet mixings drying, obtains the second uniformly mixed mixture, will first mixture with
Then second mixture mixes sintered first mixture and second respectively under an argon atmosphere with 750 DEG C of sintering 3h
It closes object and distinguishes ball milling 4h, the first mixture after ball milling is the first glass ceramics raw material, and the second mixture after ball milling is second
Glass ceramics raw material；
Step 3: fusion method prepares female glass
The first glass ceramics raw material is first packed into crucible, then the melting 2h at 1550 DEG C, then by the second glass ceramics
Raw material is added in the second glass ceramics raw material in melting, continues melting 3h hours at 1550 DEG C, the glass pottery melted
Then the glass ceramics raw material of the melting is poured into graphite jig, obtains female glass by porcelain raw material；
Step 4: borosilicate glass ceramic solidification body of the heat treatment preparation containing uranpyrochlore
The resulting female glass of step 3 is formed into ceramic nucleus, then 1200 with 800 DEG C of heat treatment 5h in air atmosphere
Continue to be heat-treated ceramics nucleus described in 5h at DEG C, after heat treatment, by ceramic nucleus quenching 40s, then by ceramic nucleus in room temperature
The borosilicate glass ceramic solidification body containing uranpyrochlore is made in lower solidification.
In the present embodiment, in the step 3, the crucible is corundum crucible.
In the present embodiment, in the step 4, ceramic nucleus is placed in -20~-10 room temperature and carries out quenching.
Performance test:
From XRD spectrum shown in Fig. 3 as it can be seen that the borosilicate glass ceramics obtained by embodiment 2 containing uranpyrochlore are solid
Change the glass ceramics sample that body is principal crystalline phase.
Fig. 4 is the SEM image of the borosilicate glass ceramic solidification body containing uranpyrochlore obtained by embodiment 2, and Fig. 2 is
The SEM image of borosilicate glass ceramic solidification body obtained by embodiment 1 containing uranpyrochlore, Fig. 4 are compared with Fig. 2, with
The crystallization rate of the increase of uranium oxide content, uranpyrochlore is also increased.
From fig.7, it can be seen that the main preservation of U is in uranpyrochlore phase, the U remained in glass is few.
It is tested by the EDS to glass in obtained glass ceramics solidified body and ceramic each element, obtains table 1.
Table 1 is the EDS data of glass and ceramic each element in glass ceramics solidified body obtained by example 2
It is tested by the EDS to glass in obtained glass ceramics solidified body and ceramic each element, table 1 is obtained, from table 1
It is found that solid solution capacity of the U in pyrochlore is larger, 0.73f.u unit can reach, form (Ca1.05Na0.20U0.73)
(Ti1.48Al0.58) the pyrochlore phase of O7+x, it is almost identical as the design molecular formula of precipitated phase Ca1.25U0.75Ti2O7, and
Remaining U is then seldom in glass phase, has well solved the deficiency that a large amount of U are easily included in glass phase.
Embodiment 3.
The preparation method of a kind of borosilicate glass ceramic solidification body containing uranpyrochlore of the present embodiment, Step 1: claiming
Take the component of following weight percent: SiO223.5%, Al2O32.1%, Na2CO38.1%, B2O33.1%, CaF220%,
CaO3.1%, U3O820.1%, TiO220%；
Step 2: pretreated glass ceramic raw material
By SiO2、Al2O3、Na2CO3、B2O3、CaF2With six kinds of component wet mixing drying of CaO, it is mixed to obtain uniformly mixed first
Object is closed, by U3O8And TiO2Two kinds of component wet mixings drying, obtains the second uniformly mixed mixture, will first mixture with
Then second mixture mixes sintered first mixture and second respectively under an argon atmosphere with 700 DEG C of sintering 2h
It closes object and distinguishes ball milling 3.5h, the first mixture after ball milling is the first glass ceramics raw material, and the second mixture after ball milling is the
Two glass ceramics raw materials；
Step 3: fusion method prepares female glass
The first glass ceramics raw material is first packed into crucible, then the melting 1.5h at 1520 DEG C, then the second glass is made pottery
Porcelain raw material is added in the second glass ceramics raw material in melting, continues the glass melted melting 2.5h hours at 1520 DEG C
Then the glass ceramics raw material of the melting is poured into graphite jig, obtains female glass by glass ceramic raw material；
Step 4: borosilicate glass ceramic solidification body of the heat treatment preparation containing uranpyrochlore
The resulting female glass of step 3 is located into 3h, formation ceramics nucleus, then at 1150 DEG C in air atmosphere with 750 DEG C of heat
Under continue be heat-treated 2h described in ceramics nucleus, after heat treatment, by ceramic nucleus quenching 35s, then at normal temperature by ceramic nucleus
The borosilicate glass ceramic solidification body containing uranpyrochlore is made in solidification.
In the present embodiment, in the step 3, the crucible is corundum crucible.
In the present embodiment, in the step 4, ceramic nucleus is placed in -20~-10 room temperature and carries out quenching.
Performance test:
From XRD spectrum shown in fig. 5 as it can be seen that the borosilicate glass ceramics obtained by embodiment 3 containing uranpyrochlore are solid
Change body and forms the glass ceramics solidified body using uranpyrochlore as principal crystalline phase.
From SEM image shown in fig. 6 as it can be seen that the borosilicate glass ceramics obtained by embodiment 3 containing uranpyrochlore are solid
Change body mainly to grow in glass with white, square, and distribution is more uniform, it is good with glass compatibility.Solidify body tissue to cause
Close, no obvious stomata generates.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered
Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (4)
1. a kind of preparation method of borosilicate glass ceramic solidification body containing uranpyrochlore described in claim 1, feature
It is: the following steps are included:
Step 1: weighing the component of following weight percent:
Step 2: pretreated glass ceramic raw material
By SiO2、Al2O3、Na2CO3、B2O3、CaF2With six kinds of component wet mixing drying of CaO, the first uniformly mixed mixture is obtained,
By U3O8And TiO2Two kinds of component wet mixings drying, obtains the second uniformly mixed mixture, by first mixture and described the
Two mixtures are respectively under an argon atmosphere with 650~750 DEG C of 1~3h of sintering, then by sintered first mixture and second
Mixture distinguishes ball milling, and the first mixture after ball milling is the first glass ceramics raw material, and the second mixture after ball milling is second
Glass ceramics raw material；
Step 3: fusion method prepares female glass
The first glass ceramics raw material is first packed into crucible, then 1~2h of melting at 1500~1550 DEG C, then by the second glass
Ceramic raw material is added in the second glass ceramics raw material in melting, continues 2~3h of melting hours at 1500~1550 DEG C, obtains
Then the glass ceramics raw material of the melting is poured into graphite jig, obtains female glass by the glass ceramics raw material of melting；
Step 4: borosilicate glass ceramic solidification body of the heat treatment preparation containing uranpyrochlore
The resulting female glass of step 3 is formed ceramic nucleus, then existed in air atmosphere with 700~800 DEG C of 1~5h of heat treatment
Continue ceramics nucleus described in 1~5h of heat treatment at 1100~1200 DEG C, after heat treatment, by 30~40s of ceramic nucleus quenching, then
Ceramic nucleus is solidified at normal temperature, the borosilicate glass ceramic solidification body containing uranpyrochlore is made.
2. a kind of preparation method of borosilicate glass ceramic solidification body containing uranpyrochlore according to claim 1,
Be characterized in: in the step 2, Ball-milling Time is 3~4h.
3. a kind of preparation method of borosilicate glass ceramic solidification body containing uranpyrochlore according to claim 1,
Be characterized in: in the step 3, the crucible is corundum crucible.
4. a kind of preparation method of borosilicate glass ceramic solidification body containing uranpyrochlore according to claim 1,
It is characterized in: in the step 4, ceramic nucleus is placed in -20~-10 DEG C of room temperature and carries out quenching.
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| CN110590161A (en) * | 2019-10-10 | 2019-12-20 | 西南科技大学 | Adding V2O5Method for improving solubility of molybdenum oxide in glass ceramic solidified body |
| CN113912297A (en) * | 2021-08-02 | 2022-01-11 | 北京科技大学 | Pyrochlore-based glass ceramic for curing radioactive waste and preparation method thereof |
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