CN110204332A - A kind of method of low-temperature fast-curing nucleic under electric field-assisted - Google Patents
A kind of method of low-temperature fast-curing nucleic under electric field-assisted Download PDFInfo
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Abstract
The present invention relates to a kind of method of low-temperature fast-curing nucleic under electric field-assisted, in particular to a kind of low-temperature fast-curing method for realizing nucleic using the method for electric field-assisted in 600 DEG C of temperatures above ranges belongs to nuke rubbish post-processing field.Oxide containing nucleic is mixed by ball milling first and is freeze-dried to obtain mixed powder by the present invention, then passes through compression molding；Critical electric field is applied to sample in 600 DEG C of temperatures above ranges, solid phase reaction quickly occurs under electric field action and generates target compound for compound.This method has synthesis temperature low, time short advantage, is effectively reduced energy consumption and has saved the time of reaction, provides very convenient and fast approach for the quickly synthesis in low temperature of prosthetic graft, the rapid curing of nucleic.
Description
Technical field
The present invention relates to a kind of method of low-temperature fast-curing nucleic under electric field-assisted, in particular to it is a kind of 600 DEG C with
Upper temperature range realizes the low-temperature fast-curing method of nucleic using the method for electric field-assisted, belongs to nuke rubbish post-processing field.
Background technique
With the continuous development of core correlative study, nuclear technology has reached its maturity, and is widely used in military, people's production
Etc., processing problem that is following then being nuke rubbish, the nuke rubbish that cannot be normally used for production still has centainly
Radioactivity, if handle it is unreasonable if can seriously affect ecological environment and human health.At present for nuclear waste disposal
There are two types of thinkings, the first is by using separation-transmuting, i.e. P-T method, and core is will be long-lived in utilization nuclear transmutation reaction
Life, high radioactivity nucleic are converted into the nucleic of middle short life, low-activity；Be for second height is put after nuke rubbish solidifies
It buries geology depths.P-T method requires technical level, hardware device, operating technology relatively high, it is difficult to walk out that laboratory is practical to answer
With, and solidify and bury then relatively maturation, equipment requirement is lower, therefore is solidified into a kind of mainstream selection of processing nuke rubbish.
Solidification usually there is several methods that, glass solidification, cement solidification, bitumen solidification, prosthetic graft solidification etc., prosthetic graft curing method
Low with leaching rate, the advantages that chemical stability is high and waste package capacity is big, obtains greatly concern.
Current prosthetic graft is usually all (1200 DEG C or more) sintering synthesis of (2-6h) high temperature for a long time under axial
, this sintering processing sintering temperature is high, sintering time is long, the high requirements on the equipment, therefore aggregate velocity is slow and at high cost.With
Pyrochlore-type prosthetic graft solidified body puts in the research that nuke rubbish is handled height, directly participates in reacting using nucleic oxide
Mineral crystal is generated, rather than part replaces solid solution, nucleic inclusion quantity can greatly improve, with SrCO3、CeO2、TiO2Exist for raw material
1450 DEG C, high temperature solid state reaction, which occurs, for heat preservation 5h can get the SrCeTi of pyrochlore constitution2O7Prosthetic graft solidified body.
In conclusion traditional prosthetic graft curing method needs calcination temperature high, the time is long, and energy consumption compared with
Greatly.
Summary of the invention
The purpose of the present invention is to solve above-mentioned technical problem, low-temperature fast-curing nucleic under a kind of electric field-assisted is provided
Method.This method realizes the quick of prosthetic graft in 600 DEG C of temperatures above ranges by applying certain electric field and current density
Synthesis efficiently solves the problems, such as that conventional artificial's synthetic method calcination temperature is high, the time is long.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of method of low-temperature fast-curing nucleic under electric field-assisted: it is uniform that nuke rubbish and adsorbent are mixed to get ingredient
Mixing gains, gains will be mixed by prototyping method and be prepared into the effigurate sample of tool, then by sample liter
Temperature applies the electric field of critical intensity to 600 DEG C or more at this temperature, keeps electric field until current spikes increase, to be achieved to set
Constant current is simultaneously stablized a period of time, and mixing material is made to quickly form solidified body.
The critical electric field is to apply the electric field strength that fast reaction can occur at a certain temperature；
Critical electric field effect under, to sample apply setting electric current be not less than critical current density electric current, it is described not
Less than the electric current of critical current density are as follows: the minimum electrical current density that fast reaction occurs is equal to experiment multiplied by the cross-sectional area of sample
Applied in current value；
The low-temperature fast-curing nucleic method, the nuke rubbish include La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy,
The solid phase of the elements such as Ho, Er, Tm, Yb, Lu, Sc, Ac, Th, Pa, U, Np, Pu, Am, Cm, Bk, Cf, Es, Fm, Md, Md, No or Lr
Compound.
The low-temperature fast-curing method, applied electric field are steady electric field or alternating electric field；
The low-temperature fast-curing method, the critical electric field strength E are as follows: 10V/cm≤E≤1500V/cm；
The low-temperature fast-curing method, the critical current density j are as follows: 5mA/mm2≤j≤700mA/mm2；
The low-temperature fast-curing method, the retention time t are as follows: 0≤t≤60min.
The low-temperature fast-curing method, it is described to mix a certain proportion of one or more at being grouped into of gains
Nucleic oxide and adsorbent, adsorbent include but is not limited to zirconium oxide, titanium oxide etc.；
The mixed method includes but is not limited to the methods of ball-milling method, coprecipitation；
The low-temperature fast-curing method, the sample are including but not limited to be molded obtained by different prototyping methods
The manufacturing process such as forming, injection molding；
The low-temperature fast-curing method, there are many modes for the providing method of the electric field, including but not limited to exchange
Power supply, DC power supply etc.；
Beneficial effect
The invention proposes a kind of nucleic methods low-temperature fast-curing under electric field-assisted, efficiently solve conventional curing core
The problems of plain method, can by solidification temperature it is minimum be down to 600 degrees Celsius it is (conventional curing to need 1450 DEG C of heat preservations 5 small
When), curing time is most short to be down to 1s, and does not need external to apply pressure.In this invention, electric energy input is converted into sample
Interior energy, sample actual temperature is much higher than ambient temperature, and the defects of sample concentration can be improved in electric field, makes solidification rate significantly
Increase, therefore low-temperature fast-curing can be realized.
Detailed description of the invention
Fig. 1 is gadolinium oxide according to the present invention, neodymia and zirconium oxide (ratio 1:4:5) 600 under electric field-assisted
Pyrochlore X-ray diffraction (XRD) map that DEG C fast reaction generates；
Fig. 2 is gadolinium oxide according to the present invention, neodymia and zirconium oxide (ratio 4:1:5) 800 under electric field-assisted
Pyrochlore X-ray diffraction (XRD) map that DEG C fast reaction generates；
Fig. 3 is gadolinium oxide according to the present invention, neodymia and zirconium oxide (ratio 3:2:5) 1000 under electric field-assisted
Pyrochlore X-ray diffraction (XRD) map that DEG C fast reaction generates；
Fig. 4 is gadolinium oxide according to the present invention, neodymia and zirconium oxide (ratio 2:3:5) 1100 under electric field-assisted
Pyrochlore X-ray diffraction (XRD) map that DEG C fast reaction generates；
Fig. 5 is gadolinium oxide according to the present invention, neodymia and zirconium oxide (ratio 1:4:5) 800 under electric field-assisted
Pyrochlore X-ray diffraction (XRD) map and 1300 DEG C of conventional sintering sample X-ray diffraction (XRD) figures that DEG C fast reaction generates
Spectrum.
Specific embodiment
The invention will be further described with embodiment with reference to the accompanying drawing.
Embodiment 1:
A kind of method of low-temperature fast-curing nucleic under electric field-assisted, the specific steps are as follows:
A) prepared by sample:
Gadolinium oxide, neodymia and Zirconium oxide powder (molar ratio 1:4:5) is uniform by ball milling mixing, then it is molded into
Type.
B) synthesis in solid state:
The sample prepared is put into sintering furnace, 1000V electricity is applied to sample by external dc power supply at 600 DEG C
It presses (electric field strength E=1500V/cm), electric current is made to reach 0.6A (current density j=100mA/mm2), and 5s is kept, gadolinium oxide,
It is a phase that neodymia and zirconium oxide are dissolved under electric field action, is generated as (the Gd of pyrochlore constitution0.2Nd0.8)2Zr2O7, in low temperature
Lower realization rapid curing nucleic, and form stable pyrochlore constitution ceramics.
Embodiment 2:
A) prepared by sample:
Gadolinium oxide, neodymia and Zirconium oxide powder (molar ratio 4:1:5) is uniform by ball milling mixing, then it is molded into
Type.
B) solid phase reaction:
The sample prepared is put into sintering furnace, 400V electricity is applied to sample by external dc power supply at 800 DEG C
It presses (electric field strength E=500V/cm), electric current is made to reach 0.30A (current density j=50mA/mm2), and 10s is kept, gadolinium oxide,
It is a phase that neodymia and zirconium oxide are dissolved under electric field action, is generated as (the Gd of pyrochlore constitution0.8Nd0.2)2Zr2O7。
Embodiment 3:
A) prepared by sample:
Gadolinium oxide, neodymia and Zirconium oxide powder (molar ratio 3:2:5) is uniform by ball milling mixing, then it is molded into
Type.
B) solid phase reaction:
The sample prepared is put into sintering furnace, by adding AC power source (frequency 100Hz) to sample outside at 1000 DEG C
Product apply 80V voltage (electric field strength E=100V/cm), and electric current is made to reach 1.20A (current density j=200mA/mm2), and protect
1s is held, it is a phase that gadolinium oxide, neodymia and zirconium oxide are dissolved under electric field action, is generated as pyrochlore constitution
(Gd0.6Nd0.4)2Zr2O7。
Embodiment 4:
A) prepared by sample:
Gadolinium oxide, neodymia and Zirconium oxide powder (molar ratio 2:3:5) is uniform by ball milling mixing, then it is molded into
Type.
B) solid phase reaction:
The sample prepared is put into sintering furnace, 60V electricity is applied to sample by external dc power supply at 1100 DEG C
It presses (electric field strength E=75V/cm), electric current is made to reach 0.30A (current density j=50mA/mm2), and 5s is kept, gadolinium oxide, oxygen
It is a phase that change neodymium and zirconium oxide are dissolved under electric field action, is generated as (the Gd of pyrochlore constitution0.4Nd0.6)2Zr2O7。
Embodiment 5:
A) prepared by sample:
Gadolinium oxide, neodymia and Zirconium oxide powder (molar ratio 1:4:5) is uniform by ball milling mixing, then it is molded into
Type.
B) solid phase reaction:
The sample prepared is put into sintering furnace, 1. sample is applied by external dc power supply to sample at 800 DEG C
200V voltage (electric field strength E=250V/cm) makes electric current reach 0.30A (current density j=50mA/mm2), and 3s is kept, oxygen
Changing gadolinium, neodymia and zirconium oxide to be dissolved under electric field action is a phase, is generated as (the Gd of pyrochlore constitution0.2Nd0.8)2Zr2O7；
2. conventional sintering keeps 2h under 1500 degree to sample.
Above-described specific descriptions have carried out further specifically the purpose of invention, technical scheme and beneficial effects
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Fig. 1,2,3,4 and 5 respectively correspond the xrd figure of example 1-5, and through the invention and electric field-assisted solidification can contract significantly
Short curing time can carry out solidification nucleic under conditions of being far below conventional curing temperature, form stable pyrochlore constitution.
Above-described specific descriptions have carried out further specifically the purpose of invention, technical scheme and beneficial effects
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (8)
1. a kind of method of low-temperature fast-curing nucleic under electric field-assisted, it is characterised in that: mix nuke rubbish and adsorbent
Gains are uniformly mixed to ingredient, sample is made after molding, sample is then warming up to 600 DEG C or more, is applied at this temperature
Add the electric field of critical intensity, keep electric field until current spikes increase, setting electric current to be achieved is simultaneously stablized a period of time, makes to mix
Material quickly forms solidified body.
Under critical electric field effect, the electric current of critical current density is not less than to the setting electric current that sample applies, it is described to be not less than
The electric current of critical current density are as follows: the minimum electrical current density of fast reaction occurs be equal to multiplied by the cross-sectional area of sample to be applied
Current value.
2. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: the electricity
Field is steady electric field or alternating electric field.
3. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: described to face
The intensity E of the electric field of boundary's intensity are as follows: 10V/cm≤E≤1500V/cm.
4. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: described to face
Boundary current density j are as follows: 5mA/mm2≤j≤700mA/mm2。
5. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: described one
The section time is no more than 60 minutes.
6. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: described mixed
Close gains at being grouped into one or more nucleic oxides and adsorbent；The adsorbent includes zirconium oxide or oxidation
Titanium.
7. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: described mixed
Conjunction method includes ball-milling method or coprecipitation；The sample is obtained by different prototyping methods, and the prototyping method includes molding
Forming or injection molding.
8. the method for low-temperature fast-curing nucleic under a kind of electric field-assisted as described in claim 1, it is characterised in that: the core
Waste material include La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, Ac, Th, Pa, U, Np, Pu, Am, Cm,
The solid-phase compound of Bk, Cf, Es, Fm, Md, Md, No or Lr element.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563467A (en) * | 2019-10-14 | 2019-12-13 | 北京理工大学 | Preparation method of graphite interface on surface of low-temperature SiC fiber |
| CN112358295A (en) * | 2020-10-19 | 2021-02-12 | 中国工程物理研究院材料研究所 | Gadolinium zirconate-based nuclear waste solidified body and preparation method thereof |
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