CN103408304A - Preparation method of kularite ceramic solidifying body - Google Patents
Preparation method of kularite ceramic solidifying body Download PDFInfo
- Publication number
- CN103408304A CN103408304A CN2013103205140A CN201310320514A CN103408304A CN 103408304 A CN103408304 A CN 103408304A CN 2013103205140 A CN2013103205140 A CN 2013103205140A CN 201310320514 A CN201310320514 A CN 201310320514A CN 103408304 A CN103408304 A CN 103408304A
- Authority
- CN
- China
- Prior art keywords
- monazite
- preparation
- cerium
- raw material
- polyvinyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a preparation method of a kularite ceramic solidifying body. The preparation method is characterized in that Ce2(C2O4)3.10H2O, An2 (C2O4)3.10H2O/oxide of An (An=Gd, Pr and Eu) and NH4H2PO4 are taken as raw materials; the high-quality kularite ceramic solidifying body is prepared according to formulation designing and the steps such as fine grinding, drying, granulating, forming, adhesive removing and vacuum hot-pressing sintering at a lower temperature. The kularite ceramic solidifying body prepared according to the preparation method is high in heat stability, mechanical stability, chemical stability and anti-radiation stability, is applicable to the safe solidification treatment of high-level waste, particularly applicable to the safe solidification treatment of high-level minor actinides waste which is high in radioactivity and toxicity, and long in half life period, and also applicable to the engineering application of high-level waste ceramic solidification treatment needing remote operation.
Description
Technical field
The invention belongs to solidification of radwaste and process, relate to a kind of preparation method of cerium monazite of ceramic solidification body.Cerium monazite of ceramic solidification body prepared by the inventive method is specially adapted to the ceramic solidification of time actinium series high-level waste and processes.
Background technology
Along with the development of human society, the demand of the energy is increased day by day, yet the fossil energies such as coal, oil are just day by day exhausted, the mankind have to find safety, effectively, clean substitute energy, to realize the Sustainable development of human society.Just under this megatrend, nuclear energy has obtained development and popularization energetically, but develop nuclear energy when to the mankind, bringing great economic benefit and social benefit, also produced a large amount of radwastes, human survival and physical environment have been formed to huge threat, seriously restricted the development of nuclear energy, especially high-level radwaste (abbreviation high-level waste), its radioactive level is high, and toxicity is large, corrodibility is strong, the heat release amount is large, and long half time is processed with the disposal difficulty quite large, if allow it enter physical environment, will cause great harm.How to process safely and effectively and to dispose high-level waste, having become day by day urgent important topic and task that nuclear power development faces.
At present, both at home and abroad the processing of high-level waste is all tended at first the high-level waste of high-level waste or process aftertreatment is cured to processing (vitrification and ceramic solidification) with disposal, then the high-level waste cured body is carried out to dark geological disposal, by high-level waste and environment for human survival and physical environment isolation, reduce to greatest extent the harm of nuclear radiation to Human and nature circle.
The vitrification Technology is comparative maturity, and has realized a small amount of through engineering approaches application, but because its curing medium material is glassy phase, glassy phase belongs to the steady phase of unsettled Jie, therefore, glass solidified body will reach the safe geological disposal more than 10000 years, and its long-term safety is alarming.
With glass solidified body, compare, of ceramic solidification body (comprises artificial rock cured body, be the titanate ceramics cured body) geological stability, chemical stability, thermostability and anti-radiation performance, all much better than glass solidified body, therefore, ceramic solidification is the especially desirable dielectric material of actinium series high-level waste of solidification treatment high-level waste.The actinium series nucleic has long half time, bio-toxicity high, its safely and effectively treatment and disposal become the outer problem of relatively paying close attention to of Present Domestic.
With artificial rock, solidify and compare, abroad to cerium monazite (CePO
4) research of ceramic solidification is less, the domestic report that there is not yet.In prior art, research work mainly concentrates on liquid phase method (comprising chemical precipitation method and sol-gel method) and solid phase method prepares cerium monazite and of ceramic solidification body thereof.Liquid phase method technique is more loaded down with trivial details, and technology controlling and process requires high, be unfavorable for the through engineering approaches application of actinium series high-level waste solidification treatment, and solid phase method technique is simple, is convenient to control.At present, the research of cerium monazite solidification simulation time actinium series nucleic [gadolinium (Gd), praseodymium (Pr), europium (Eu)] and vacuum heating-press sintering simulation time actinium series nucleic (gadolinium, praseodymium, europium) cerium monazite of ceramic solidification body there is not yet report.
Summary of the invention
Purpose of the present invention is intended to overcome deficiency of the prior art, and a kind of preparation method of cerium monazite of ceramic solidification body is provided, and particularly provides a kind of vacuum heating-press sintering to prepare cerium monazite (CePO
4) method of ceramic solidification of radwaste body.The present invention is directed to the safe solidification treatment of Minor actinides [neptunium (Np), americium (Am), curium (Cm)], consider the security of work, use the lanthanon [praseodymium (Pr), europium (Eu), gadolinium (Gd)] approached the most with Minor actinides [neptunium (Np), americium (Am), curium (Cm)] character to simulate Minor actinides, praseodymium (Pr), europium (Eu), gadolinium (Gd) are simulated respectively neptunium (Np), americium (Am), curium (Cm); With Ce
2(C
2O
4)
310H
2O, An
2(C
2O
4)
310H
2The oxide compound of O/An (An=Gd, Pr, Eu), NH
4H
2PO
4Deng being raw material, by formulating of recipe and solid phase reaction process, adopt simple and practical vacuum hot pressing sintering technique, the cerium monazite of ceramic solidification body for preparing high purity, high-compactness at lower temperature, obtain high-performance time actinium series nucleic cerium monazite of ceramic solidification body, the through engineering approaches application of processing time actinium series nucleic high-level waste for the solitary ground mass ceramic solidification of cerium lays the foundation.
Content of the present invention is: a kind of preparation method of cerium monazite of ceramic solidification body is characterized in that comprising the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O is 37.28～75.89%, NH
4H
2PO
4Be 23.68～24.1%, Gd
2(C
2O
4)
310H
2O is that 0.01～39.04% composition and mass percent example are got each raw material;
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water (can be the common domestic waters such as distilled water, deionized water or tap water) is 1: 1.5～3.5: 1.0～2.0 mass ratio, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 3～6 hours, again material was dried 2～5 hours at the temperature of 50～90 ℃, obtain the powder of oven dry; Described raw material total mass is and obtains raw material Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4And Gd
2(C
2O
4)
310H
2The quality summation of O.
C, granulation: the polyvinyl alcohol colloidal sol that adds powder quality 5～8 % of oven dry in the powder of drying, mixing granulation, again successively with after 16～20 orders, 200～250 purpose sieve screenings, 16～20 purpose minus mesh and 200～250 mesh sieve material loadings are the granulation material made, and this granulation material can meet the requirement of next step moulding to material performance well;
The mass percent concentration of described polyvinyl alcohol (being called for short PVA) colloidal sol is 10～15%;
D, moulding and binder removal: the granulation material is packed in steel die, in the upper pressure compression moulding with 10～40MPa of hydropress (equipment can be the DF-4 type hydraulic machine that Tianjin Gangdong Technology Development Co., Ltd. produces), then the pressure of using 100～250MPa, through cold isostatic press moulding (equipment can be the LDT100/320-300 type cold isostatic press that aircraft industry river western motor-driven device factory produces), makes molding blank; Again by molding blank thermal treatment 120～300 minutes at the temperature of 700～800 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace (equipment can be the ZT-40-20Y type vacuum sintering funace that Shanghai Chen Hua Electric Furnace Corp Ltd. produces) under the condition of 1050～1200 ℃ of temperature, pressure 20～40MPa sintering 30～240 minutes, namely make (high-quality) cerium monazite of ceramic solidification body.
In content of the present invention: described step a batching can replace with: press Ce
2(C
2O
4)
310H
2O is 46.83～75.85%, NH
4H
2PO
4Be 24.11～29.74%, Gd
2O
3Be that 0.04～23.43% composition and mass percent example are got each raw material.
In content of the present invention: described step a batching can also replace with: press Ce
2(C
2O
4)
310H
2O is 37.92～75.89%, NH
4H
2PO
4Be 24.08～24.1%, Pr
2(C
2O
4)
310H
2O is that 0.01～38% composition and mass percent example are got each raw material.
In content of the present invention: described step a batching can also replace with: press Ce
2(C
2O
4)
310H
2O is 47.50～75.85%, NH
4H
2PO
4Be 24.11～30.17%, Pr
6O
11Be that 0.04～22.33% composition and mass percent example are got each raw material.
In content of the present invention: described step a batching can also replace with: press Ce
2(C
2O
4)
310H
2O is 37.48～75.89%, NH
4H
2PO
4Be 23.81～24.1%, Eu
2(C
2O
4)
310H
2O is that 0.01～38.71% composition and mass percent example are got each raw material.
In content of the present invention: described step a batching can also replace with: press Ce
2(C
2O
4)
310H
2O is 47.15～75.85%, NH
4H
2PO
4Be 24.11～29.95%, Eu
2O
3Be that 0.04～22.9% composition and mass percent example are got each raw material.
In content of the present invention: mass percent concentration described in step c is that the preparation method of 10～15% polyvinyl alcohol (being called for short PVA) colloidal sol is: composition and mass percent example by polyvinyl alcohol 10～15%, glycerine 6～8%, dehydrated alcohol 2～4%, distilled water 75～80% are got each raw material; Distilled water is poured in container, (can in thermostat water bath) be heated to 90～95 ℃, then in the process constantly stirred, (slowly gradually) add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 5～10 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 10～15% polyvinyl alcohol (being called for short PVA) colloidal sol.
It is that 1700～2500(molecular weight ranges is 74800～11000 that described polyvinyl alcohol (be called for short PVA) is chosen the polymerization degree) polyvinyl alcohol be raw material, concrete model can be PVA1799, PVA2099, PVA2299 and PVA2499, and there are Sichuan vinylon plant, Taiwan Changchun Petrochemical Co., Ltd., Yantai spark the earth chemical industry company limited etc. in products production producer.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) monazite [Monazite, (Ce, La ...) PO
4] have excellent chemical stability, mechanical stability, thermostability and anti-radiation performance, be one of the most stable mineral of nature, be to solidify the desirable mineral of actinium series high-level waste; Authigenic Rare Earth Mineral-Monazite usually comprises the radioactive decay product of a large amount of U, Th and uranium thorium, thereby monazite solid solution actinium series well nucleic; Therefore, the monazite of ceramic solidification body is the desirable curing medium material solidified from the actinide elements of separating high-level waste;
(2) adopt the present invention, with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4Deng being raw material, praseodymium (Pr), gadolinium (Gd), europium (Eu) are simulated respectively time actinium series radionuclide neptunium (Np), curium (Cm), americium (Am), employing graphite is that the vacuum sintering funace of heating element is hot-press sintering equipment, adopt solid phase reaction process to prepare the monazite of ceramic solidification body, the simple process practicality, be conducive to the engineering application, can prepare high performance cerium monazite of ceramic solidification body;
(3) adopt the present invention, during vacuum heating-press sintering, due to the effect of vacuum, be conducive to the gas purging of base substrate inside, improve the density of sintered compact.Pressure energy during sintering reduces sintering temperature, shortens sintering time, improves the density of sintered compact; The graphite of take is the vacuum sintering funace of heating element, can make time actinium series nucleic be in lower valency, is conducive to the lattice solid solution of cerium monazite to inferior actinium series nucleic; Under temperature, pressure acting in conjunction, synthesis of high purity cerium monazite at a lower temperature, and realize that simultaneously the cerium monazite is to simulating solid solution and the densification sintering thereof of time actinium series radionuclide (Gd, Pr, Eu); Adopt vacuum hot pressing sintering technique to prepare cerium monazite of ceramic solidification body, be conducive to prevent the pollution to environment of harmful or radioactive gas;
(4) technique of the present invention is succinctly practical, can under lesser temps (1050-1200 ℃), prepare high-compactness, highly purified cerium monazite of ceramic solidification body; Under hot pressing function, inferior actinium series nucleic enters cerium monazite (CePO
4) occupy Ce in lattice
3+Position, form stable An
x Ce
1-
x PO
4(An: inferior actinium series nucleic,
xFor variable) cerium monazite of ceramic solidification body; In the sintering process of high-performance cerium monazite of ceramic solidification body, realize simultaneously the synthetic of high purity cerium monazite and to the solid solution of inferior actinium series nucleic; The engineering application that Technology of the present invention is particularly suitable for needing the high-level waste ceramic solidification of telemanipulation to process;
(5) adopt the present invention, the cerium monazite of ceramic solidification body of making has good thermostability, mechanical stability, chemical stability and anti-irradiation stability, be mainly used in the safe solidification treatment of high-level waste, be particularly suitable for that radioactivity is strong, toxicity is large, the safe solidification treatment of the inferior actinium series high-level waste of long half time; By this technique, obtaining the leaching yield of density high (relative theory density reaches 98%-99%), actinium series nucleic of cured body, low (in 90 ℃, the aqueous solution of pH=5-9, soak, the normalization method leaching yield of 42 days reaches 10
-4-10
-6Gm
-2D
-1);
(6) the present invention adopts simple and practical vacuum hot pressing sintering technique, the cerium monazite of ceramic solidification body for preparing at a lower temperature high purity, high-compactness, the through engineering approaches application of processing time actinium series high-level waste for the ceramic solidification of cerium monazite lays the foundation, preparation technology is simple, easily operation, practical.
Embodiment
Embodiment given below intends so that the invention will be further described; but can not be interpreted as it is limiting the scope of the invention; the person skilled in art to some nonessential improvement and adjustment that the present invention makes, still belongs to protection scope of the present invention according to the content of the invention described above.
Embodiment 1:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Gd
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.06wt.%(weight percentage), NH
4H
2PO
424.02wt.%, Gd
2(C
2O
4)
310H
2O 7.92wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution gadolinium.
Embodiment 2:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Pr
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.30wt.%(weight percentage), NH
4H
2PO
424.10wt.%, Pr
2(C
2O
4)
310H
2O 7.61wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution praseodymium.
Embodiment 3:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Eu
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.14wt.%(weight percentage), NH
4H
2PO
424.04wt.%, Eu
2(C
2O
4)
310H
2O 7.82wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution europium.
Embodiment 4:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Gd
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 60.29wt.%(weight percentage), NH
4H
2PO
423.93wt.%, Gd
2(C
2O
4)
310H
2O 15.78wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution gadolinium.
Embodiment 5:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Pr
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 60.70wt.%(weight percentage), NH
4H
2PO
424.09wt.%, Pr
2(C
2O
4)
310H
2O 15.21wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution praseodymium.
Embodiment 6:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Eu
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 60.42wt.%(weight percentage), NH
4H
2PO
423.98wt.%, Eu
2(C
2O
4)
310H
2O 15.60wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 3.0: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution europium.
Embodiment 7:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Gd
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.06wt.%(weight percentage), NH
4H
2PO
424.02wt.%, Gd
2(C
2O
4)
310H
2O 7.92wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1150 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution gadolinium.
Embodiment 8:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Pr
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.30wt.%(weight percentage), NH
4H
2PO
424.10wt.%, Pr
2(C
2O
4)
310H
2O 7.61wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 2(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1150 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution praseodymium.
Embodiment 9:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Eu
2(C
2O
4)
310H
2O is raw material, fills a prescription to be: Ce
2(C
2O
4)
310H
2O 68.14wt.%(weight percentage), NH
4H
2PO
424.04wt.%, Eu
2(C
2O
4)
310H
2O 7.82wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1150 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution europium.
Embodiment 10:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Eu
2O
3For raw material, filling a prescription is: Ce
2(C
2O
4)
310H
2O 71.08wt.%(weight percentage), NH
4H
2PO
425.08wt.%, Eu
2O
33.84wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1150 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution europium.
Embodiment 11:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Pr
6O
11For raw material, filling a prescription is: Ce
2(C
2O
4)
310H
2O 66.03wt.%(weight percentage), NH
4H
2PO
426.21wt.%, Pr
6O
117.76wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1150 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution praseodymium.
Embodiment 12:
A kind of preparation method of cerium monazite of ceramic solidification body is with Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4, Gd
2O
3For raw material, filling a prescription is: Ce
2(C
2O
4)
310H
2O 65.7wt.%(weight percentage), NH
4H
2PO
426.08wt.%, Gd
2O
38.22wt.%; The various raw materials of weighing, select material: ball: dehydrated alcohol is or/and water is 1: 2.5: the 1.5(mass ratio), adopt planetary mills ball milling 4h, dry, add 6% polyvinyl alcohol (PVA) colloidal sol (concentration of PVA is 12%), batch mixing, screening, granulation.Powder after granulation is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure cold isostatic compaction of 200MPa on hydropress; Molding blank was 700 ℃ of thermal treatments 300 minutes; Base substrate after thermal treatment in vacuum sintering funace under 1100 ℃, 30MPa sintering 120 minutes, obtain the cerium monazite of ceramic solidification body of solid solution gadolinium.
Embodiment 13:
A kind of preparation method of cerium monazite of ceramic solidification body, comprise the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O is 66.5%, NH
4H
2PO
4Be 24.0%, Gd
2(C
2O
4)
310H
2O is that 9.5% composition and mass percent example are got each raw material;
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water is the mass ratio of 1: 2.5: 1.5, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 4.5 hours, again material was dried 3.5 hours at the temperature of 70 ℃, obtain the powder of oven dry;
C, granulation: polyvinyl alcohol (PVA) colloidal sol that adds powder quality 6.5 % of oven dry in the powder of drying, mixing granulation, again successively with after 18 orders, 220 purpose sieve screenings, 18 purpose minus mesh and 220 mesh sieve material loadings are the granulation material made, and this granulation material can meet the requirement of next step moulding to material performance well;
The mass percent concentration of described polyvinyl alcohol (being called for short PVA) colloidal sol is 12.5%;
D, moulding and binder removal: the granulation material is packed in steel die, in the upper pressure compression moulding with 25MPa of hydropress (equipment can be the DF-4 type hydraulic machine that Tianjin Gangdong Technology Development Co., Ltd. produces), then the pressure of using 175MPa, through cold isostatic press moulding (equipment can be the LDT100/320-300 type cold isostatic press that aircraft industry river western motor-driven device factory produces), makes molding blank; Again by molding blank thermal treatment 210 minutes at the temperature of 750 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace (equipment can be the ZT-40-20Y type vacuum sintering funace that Shanghai Chen Hua Electric Furnace Corp Ltd. produces) under the condition of 1120 ℃ of temperature, pressure 30MPa sintering 130 minutes, namely make (high-quality) cerium monazite of ceramic solidification body.
Embodiment 14:
A kind of preparation method of cerium monazite of ceramic solidification body, comprise the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O 56.42%, NH
4H
2PO
423.89%, Gd
2(C
2O
4)
310H
2The composition of O 19.69% and mass percent example are got each raw material;
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water is the mass ratio of 1: 1.5: 1.0, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 3 hours, again material was dried 5 hours at the temperature of 50 ℃, obtain the powder of oven dry;
C, granulation: polyvinyl alcohol (PVA) colloidal sol that adds the powder quality 5% of oven dry in the powder of drying, mixing granulation, again successively with after 16 orders, 200 purpose sieve screenings, 16 purpose minus mesh and 200 mesh sieve material loadings are the granulation material made, and this granulation material can meet the requirement of next step moulding to material performance well;
The mass percent concentration of described polyvinyl alcohol (being called for short PVA) colloidal sol is 10%;
D, moulding and binder removal: the granulation material is packed in steel die, with the pressure compression moulding of 10MPa, then use the pressure of 100MPa through the cold isostatic press moulding on hydropress, make molding blank; Again by molding blank thermal treatment 300 minutes at the temperature of 700 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace under the condition of 1050 ℃ of temperature, pressure 40MPa sintering 30 minutes, namely make (high-quality) cerium monazite of ceramic solidification body.
Embodiment 15:
A kind of preparation method of cerium monazite of ceramic solidification body, comprise the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O 75.82%, NH
4H
2PO
424.10%, Gd
2(C
2O
4)
310H
2The composition of O 0.08% and mass percent example are got each raw material;
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water is the mass ratio of 1: 3.5: 2.0, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 6 hours, again material was dried 2 hours at the temperature of 90 ℃, obtain the powder of oven dry;
C, granulation: polyvinyl alcohol (PVA) colloidal sol that adds powder quality 8 % of oven dry in the powder of drying, mixing granulation, again successively with after 20 orders, 250 purpose sieve screenings, 20 purpose minus mesh and 250 mesh sieve material loadings are the granulation material made, and this granulation material can meet the requirement of next step moulding to material performance well;
The mass percent concentration of described polyvinyl alcohol (being called for short PVA) colloidal sol is 15%;
D, moulding and binder removal: the granulation material is packed in steel die, with the pressure compression moulding of 40MPa, then use the pressure of 250MPa through the cold isostatic press moulding on hydropress, make molding blank; Again by molding blank thermal treatment 120 minutes at the temperature of 800 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace under the condition of 1200 ℃ of temperature, pressure 20MPa sintering 240 minutes, namely make (high-quality) cerium monazite of ceramic solidification body.
Embodiment 16-22:
A kind of preparation method of cerium monazite of ceramic solidification body, comprise the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O is 37.28～75.89%, NH
4H
2PO
4Be 23.68～24.10%, Gd
2(C
2O
4)
310H
2O is that 0.01～39.04% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water is 1: 1.5～3.5: 1.0～2.0 mass ratio, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 3～6 hours, again material was dried 2～5 hours at the temperature of 50～90 ℃, obtain the powder of oven dry;
In each embodiment, the concrete quality of each component sees the following form than consumption:
Annotate: described raw material total mass is that step a obtains raw material Ce
2(C
2O
4)
310H
2O, NH
4H
2PO
4And Gd
2(C
2O
4)
310H
2The quality summation of O.
C, granulation: polyvinyl alcohol (PVA) colloidal sol that adds powder quality 5～8 % of oven dry in the powder of drying, mixing granulation, again successively with after 16～20 orders, 200～250 purpose sieve screenings, 16～20 purpose minus mesh and 200～250 mesh sieve material loadings are the granulation material made, and this granulation material can meet the requirement of next step moulding to material performance well;
The mass percent concentration of described polyvinyl alcohol (being called for short PVA) colloidal sol is 10～15%;
D, moulding and binder removal: the granulation material is packed in steel die, in the upper pressure compression moulding with 10～40MPa of hydropress (equipment can be the DF-4 type hydraulic machine that Tianjin Gangdong Technology Development Co., Ltd. produces), then the pressure of using 100～250MPa, through cold isostatic press moulding (equipment can be the LDT100/320-300 type cold isostatic press that aircraft industry river western motor-driven device factory produces), makes molding blank; Again by molding blank thermal treatment 120～300 minutes at the temperature of 700～800 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace (equipment can be the ZT-40-20Y type vacuum sintering funace that Shanghai Chen Hua Electric Furnace Corp Ltd. produces) under the condition of 1050～1200 ℃ of temperature, pressure 20～40MPa sintering 30～240 minutes, namely make (high-quality) cerium monazite of ceramic solidification body.
Embodiment 23-29:
A kind of preparation method of cerium monazite of ceramic solidification body, described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 46.83～75.85%, NH
4H
2PO
4Be 24.11～29.74%, Gd
2O
3Be that 0.04～23.43% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
Arbitrary in the other the same as in Example 1 3-22, omit.
Embodiment 30-36:
A kind of preparation method of cerium monazite of ceramic solidification body, described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 37.92～75.89%, NH
4H
2PO
4Be 24.08～24.1%, Pr
2(C
2O
4)
310H
2O is that 0.01～38% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
Arbitrary in the other the same as in Example 1 3-22, omit.
Embodiment 37-43:
A kind of preparation method of cerium monazite of ceramic solidification body, described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 47.50～75.85%, NH
4H
2PO
4Be 24.11～30.17%, Pr
6O
11Be that 0.04～22.33% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
Arbitrary in the other the same as in Example 1 3-22, omit.
Embodiment 44-50:
A kind of preparation method of cerium monazite of ceramic solidification body, described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 37.48～75.89%, NH
4H
2PO
4Be 23.81～24.1%, Eu
2(C
2O
4)
310H
2O is that 0.01～38.71% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material is shown in
Arbitrary in the other the same as in Example 1 3-22, omit.
Embodiment 51-57:
A kind of preparation method of cerium monazite of ceramic solidification body, described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 47.15～75.85%, NH
4H
2PO
4Be 24.11～29.95%, Eu
2O
3Be that 0.04～22.9% composition and mass percent example are got each raw material;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
Arbitrary in the other the same as in Example 1 3-22, omit.
Embodiment 58:
The preparation method of above-mentioned cerium monazite of ceramic solidification body, the preparation method of polyvinyl alcohol described in step c (being called for short PVA) colloidal sol can be: composition and mass percent example by polyvinyl alcohol 12.5%, glycerine 7%, dehydrated alcohol 3%, distilled water 77.5% are got each raw material; Distilled water is poured in container, (can in thermostat water bath) be heated to 90～95 ℃, then in the process constantly stirred, (slowly gradually) add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 8 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 12.5% polyvinyl alcohol (being called for short PVA) colloidal sol.
Embodiment 59:
The preparation method of above-mentioned cerium monazite of ceramic solidification body, the preparation method of polyvinyl alcohol described in step c (being called for short PVA) colloidal sol can also be: composition and mass percent example by polyvinyl alcohol 10%, glycerine 6%, dehydrated alcohol 4%, distilled water 80% are got each raw material; Distilled water is poured in container, (can in thermostat water bath) be heated to 90～95 ℃, then in the process constantly stirred, (slowly gradually) add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 5 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 10% polyvinyl alcohol (being called for short PVA) colloidal sol.
Embodiment 60:
The preparation method of above-mentioned cerium monazite of ceramic solidification body, the preparation method of polyvinyl alcohol described in step c (being called for short PVA) colloidal sol can also be: composition and mass percent example by polyvinyl alcohol 15%, glycerine 8%, dehydrated alcohol 2%, distilled water 75% are got each raw material; Distilled water is poured in container, (can in thermostat water bath) be heated to 90～95 ℃, then in the process constantly stirred, (slowly gradually) add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 10 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 15% polyvinyl alcohol (being called for short PVA) colloidal sol.
Embodiment 61-67:
In the preparation method of above-mentioned cerium monazite of ceramic solidification body, the preparation method of polyvinyl alcohol described in step c (being called for short PVA) colloidal sol can also be: composition and mass percent example by polyvinyl alcohol 10～15%, glycerine 6～8%, dehydrated alcohol 2～4%, distilled water 75～80% are got each raw material; Distilled water is poured in container, (can in thermostat water bath) be heated to 90～95 ℃, then in the process constantly stirred, (slowly gradually) add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 5～10 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 10～15% polyvinyl alcohol (being called for short PVA) colloidal sol;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
In the mass percent concentration of the polyvinyl alcohol that each embodiment makes (be called for short PVA) colloidal sol and table, the mass percent use numerical quantity of polyvinyl alcohol is corresponding identical; Arbitrary in the other the same as in Example 5 8-60, omit.
In above-described embodiment: described polyvinyl alcohol (be called for short PVA) is preferably and chooses the polymerization degree is that 1700～2500(molecular weight ranges is 74800～11000) polyvinyl alcohol be raw material, concrete model can be PVA1799, PVA2099, PVA2299 and PVA2499, and there are Sichuan vinylon plant, Taiwan Changchun Petrochemical Co., Ltd., Yantai spark the earth chemical industry company limited etc. in products production producer.
In above-described embodiment: hydropress described in steps d can be that DF-4 type hydraulic machine, described cold isostatic press that Tianjin Gangdong Technology Development Co., Ltd. produces can be the LDT100/320-300 type cold isostatic presses that aircraft industry river western motor-driven device factory produces, and vacuum sintering funace described in step e can be the ZT-40-20Y type vacuum sintering funace that Shanghai Chen Hua Electric Furnace Corp Ltd. produces.
In above-described embodiment: each raw material adopted is commercially available prod.
In above-described embodiment: in the percentage adopted, do not indicate especially, be quality (weight) percentage (weight percentage); Described quality (weight) can be all gram or kilogram.
In above-described embodiment: the processing parameter in each step (temperature, time, pressure, concentration etc.) and each amounts of components numerical value etc. are scope, and any point is all applicable.
In content of the present invention and above-described embodiment, the not concrete technology contents of narrating is with existing technology.
The invention is not restricted to above-described embodiment, content of the present invention is described all can implement and have described good result.
Claims (8)
1. the preparation method of a cerium monazite of ceramic solidification body, is characterized in that comprising the following steps:
A, batching: press Ce
2(C
2O
4)
310H
2O is 37.28～75.89%, NH
4H
2PO
4Be 23.68～24.10%, Gd
2(C
2O
4)
310H
2O is that 0.01～39.04% composition and mass percent example are got each raw material;
B, fine grinding are dried: by the raw material total mass: ball: dehydrated alcohol is or/and water is 1: 1.5～3.5: 1.0～2.0 mass ratio, by raw material, ball and dehydrated alcohol or/and water dropped in the planetary mills ball milling ball milling 3～6 hours, again material was dried 2～5 hours at the temperature of 50～90 ℃, obtain the powder of oven dry;
C, granulation: the polyvinyl alcohol colloidal sol that adds powder quality 5～8 % of oven dry in the powder of drying, mixing granulation, successively with after 16～20 orders, 200～250 purpose sieve screenings, 16～20 purpose minus mesh and 200～250 mesh sieve material loadings are the granulation material made again;
The mass percent concentration of described polyvinyl alcohol colloidal sol is 10～15%;
D, moulding and binder removal: the granulation material is packed in steel die, with the pressure compression moulding of 10～40MPa, then use the pressure of 100～250MPa through the cold isostatic press moulding on hydropress, make molding blank; Again by molding blank thermal treatment 120～300 minutes at the temperature of 700～800 ℃, make the base substrate after thermal treatment;
E, vacuum heating-press sintering: by the base substrate after thermal treatment in vacuum sintering funace under the condition of 1050～1200 ℃ of temperature, pressure 20～40MPa sintering 30～240 minutes, namely make cerium monazite of ceramic solidification body.
2. by the preparation method of the described cerium monazite of claim 1 of ceramic solidification body, it is characterized in that: described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 46.83～75.85%, NH
4H
2PO
4Be 24.11～29.74%, Gd
2O
3Be that 0.04～23.43% composition and mass percent example are got each raw material.
3. by the preparation method of the described cerium monazite of claim 1 of ceramic solidification body, it is characterized in that: described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 37.92～75.89%, NH
4H
2PO
4Be 24.08～24.1%, Pr
2(C
2O
4)
310H
2O is that 0.01～38% composition and mass percent example are got each raw material.
4. by the preparation method of the described cerium monazite of claim 1 of ceramic solidification body, it is characterized in that: described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 47.50～75.85%, NH
4H
2PO
4Be 24.11～30.17%, Pr
6O
11Be that 0.04～22.33% composition and mass percent example are got each raw material.
5. by the preparation method of the described cerium monazite of claim 1 of ceramic solidification body, it is characterized in that: described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 37.48～75.89%, NH
4H
2PO
4Be 23.81～24.1%, Eu
2(C
2O
4)
310H
2O is that 0.01～38.71% composition and mass percent example are got each raw material.
6. by the preparation method of the described cerium monazite of claim 1 of ceramic solidification body, it is characterized in that: described step a batching replaces with: press Ce
2(C
2O
4)
310H
2O is 47.15～75.85%, NH
4H
2PO
4Be 24.11～29.95%, Eu
2O
3Be that 0.04～22.9% composition and mass percent example are got each raw material.
7. by the preparation method of claim 1,2,3,4,5 or 6 described cerium monazite of ceramic solidification bodies, it is characterized in that: mass percent concentration described in step c is that the preparation method of 10～15% polyvinyl alcohol colloidal sol is: composition and mass percent example by polyvinyl alcohol 10～15%, glycerine 6～8%, dehydrated alcohol 2～4%, distilled water 75～80% are got each raw material; Distilled water is poured in container, be heated to 90～95 ℃, then in the process constantly stirred, add polyvinyl alcohol, after polyvinyl alcohol dissolves, add glycerine, mix and add again dehydrated alcohol after 5～10 minutes, last at the temperature of 90～95 ℃, stirred 3 hours, namely make mass percent concentration and be 10～15% polyvinyl alcohol colloidal sol.
8. by the preparation method of the described cerium monazite of claim 7 of ceramic solidification body, it is characterized in that: it is 1700～2500 polyvinyl alcohol that described polyvinyl alcohol is chosen the polymerization degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310320514.0A CN103408304B (en) | 2013-07-29 | 2013-07-29 | Preparation method of kularite ceramic solidifying body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310320514.0A CN103408304B (en) | 2013-07-29 | 2013-07-29 | Preparation method of kularite ceramic solidifying body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103408304A true CN103408304A (en) | 2013-11-27 |
| CN103408304B CN103408304B (en) | 2014-08-13 |
Family
ID=49601363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310320514.0A Expired - Fee Related CN103408304B (en) | 2013-07-29 | 2013-07-29 | Preparation method of kularite ceramic solidifying body |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103408304B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844190A (en) * | 2015-04-08 | 2015-08-19 | 西南科技大学 | Method for preparing fluorapatite ceramic solidified body |
| CN105004681A (en) * | 2015-06-08 | 2015-10-28 | 西南科技大学 | Chemical stability evaluating method of fluorapatite ceramic solidification body |
| CN105777101A (en) * | 2016-03-31 | 2016-07-20 | 西南科技大学 | Zirconium sodium phosphate-monazite glass ceramic solidified body and preparation method thereof |
| CN109761624A (en) * | 2019-03-06 | 2019-05-17 | 娄底市安地亚斯电子陶瓷有限公司 | A kind of ceramic prilling method and its application |
| CN116655355A (en) * | 2023-07-31 | 2023-08-29 | 成都大学 | Preparation method of alkali pyrolusite ceramic solidified body for solidifying cesium |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4314909A (en) * | 1980-06-30 | 1982-02-09 | Corning Glass Works | Highly refractory glass-ceramics suitable for incorporating radioactive wastes |
| CN102568636A (en) * | 2012-02-21 | 2012-07-11 | 浙江大学 | CaTiZr (calcium, titanium and zirconium)-phase glass ceramic waste forms and preparation method thereof |
-
2013
- 2013-07-29 CN CN201310320514.0A patent/CN103408304B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4314909A (en) * | 1980-06-30 | 1982-02-09 | Corning Glass Works | Highly refractory glass-ceramics suitable for incorporating radioactive wastes |
| CN102568636A (en) * | 2012-02-21 | 2012-07-11 | 浙江大学 | CaTiZr (calcium, titanium and zirconium)-phase glass ceramic waste forms and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| X.DESCHANELS等: "Plutonium incorporation in phosphate and titanate ceramics for minor actinide containment", 《JOURNAL OF NUCLEAR MATERIALS》 * |
| 车春霞等: "放射性废物固化处理的研究及应用现状", 《材料导报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844190A (en) * | 2015-04-08 | 2015-08-19 | 西南科技大学 | Method for preparing fluorapatite ceramic solidified body |
| CN105004681A (en) * | 2015-06-08 | 2015-10-28 | 西南科技大学 | Chemical stability evaluating method of fluorapatite ceramic solidification body |
| CN105004681B (en) * | 2015-06-08 | 2018-06-08 | 西南科技大学 | A kind of chemical stability evaluation method of fluor-apatite ceramic solidification body |
| CN105777101A (en) * | 2016-03-31 | 2016-07-20 | 西南科技大学 | Zirconium sodium phosphate-monazite glass ceramic solidified body and preparation method thereof |
| CN105777101B (en) * | 2016-03-31 | 2018-07-20 | 西南科技大学 | A kind of sodium zirconium phosphate-monazite glass ceramics firming body and preparation method thereof |
| CN109761624A (en) * | 2019-03-06 | 2019-05-17 | 娄底市安地亚斯电子陶瓷有限公司 | A kind of ceramic prilling method and its application |
| CN116655355A (en) * | 2023-07-31 | 2023-08-29 | 成都大学 | Preparation method of alkali pyrolusite ceramic solidified body for solidifying cesium |
| CN116655355B (en) * | 2023-07-31 | 2023-10-10 | 成都大学 | Preparation method of alkali pyrolusite ceramic solidified body for solidifying cesium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103408304B (en) | 2014-08-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102930915B (en) | A kind of preparation method of solidification of radwaste body | |
| CN103408304B (en) | Preparation method of kularite ceramic solidifying body | |
| CN104844190B (en) | A kind of preparation method of fluor-apatite ceramic solidification body | |
| CN102584018B (en) | A kind of method of preparing high-radioactivity effluent glass-ceramic solidified body in microwave process | |
| CN102779561B (en) | Method for solidifying actinium series nuclide by pyrochlore type rare earth zirconate | |
| CN111533557A (en) | Pyrochlore type high-entropy oxide solidified body and preparation method thereof | |
| CN100364017C (en) | Method for preparing high radioactive waste curing treatment base material | |
| CN111039674B (en) | Gadolinium zirconate ceramic for solidifying TRPO simulation waste and preparation method thereof | |
| CN106045495B (en) | A kind of porous fluor-apatite ceramic preparation of Adsorption of Radioactive nucleic | |
| CN104401982A (en) | Nuclear graphite material preparation method | |
| CN111302784B (en) | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body | |
| CN105777101B (en) | A kind of sodium zirconium phosphate-monazite glass ceramics firming body and preparation method thereof | |
| CN102208223B (en) | Preparation method for strontium-cesium co-solidified body | |
| CN112466503A (en) | Preparation method of glass ceramic body for solidifying Cs-containing soil | |
| CN101894594B (en) | Sub-stoichiometric UO2-xPreparation process of annular core block | |
| CN110734283A (en) | Preparation method of novel phosphate composite ceramic solidified material | |
| CN107500775B (en) | Preparation method of SiC-based complex phase ceramic solidified body for radioactive graphite solidification treatment | |
| CN102730756A (en) | Preparation method for pyrochlore type rare-earth zirconate | |
| CN113121220A (en) | Method for treating radioactive waste liquid by phosphate minerals | |
| CN105004681A (en) | Chemical stability evaluating method of fluorapatite ceramic solidification body | |
| CN106847360A (en) | A kind of method that utilization granite solidifies radwaste | |
| CN109824355B (en) | Treatment method of radioactive waste organic solvent tributyl phosphate pyrolysis furnace ash | |
| CN103992095B (en) | The SHS process of zirconolite-rich type prosthetic graft and densifying method | |
| CN110606664B (en) | Method for preparing pyrochlore phase borosilicate glass ceramic cured substrate by one-step method | |
| CN114195486B (en) | One-step method for preparing MgO-Nd 2 Zr 2 O 7 Method for forming multiphase ceramic inert fuel base material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140813 Termination date: 20190729 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |