CN110342927A - It is medical90Y-ZrO2Ceramic microsphere and preparation method thereof - Google Patents

It is medical90Y-ZrO2Ceramic microsphere and preparation method thereof Download PDF

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CN110342927A
CN110342927A CN201910599552.1A CN201910599552A CN110342927A CN 110342927 A CN110342927 A CN 110342927A CN 201910599552 A CN201910599552 A CN 201910599552A CN 110342927 A CN110342927 A CN 110342927A
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zro
ceramic microsphere
preparation
converted
drop
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田伟
秦芝
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Institute of Modern Physics of CAS
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K51/00—Preparations containing radioactive substances for use in therapy or testing in vivo
    • A61K51/02—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by the carrier, i.e. characterised by the agent or material covalently linked or complexing the radioactive nucleus
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K51/00—Preparations containing radioactive substances for use in therapy or testing in vivo
    • A61K51/12—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by a special physical form, e.g. emulsion, microcapsules, liposomes, characterized by a special physical form, e.g. emulsions, dispersions, microcapsules
    • A61K51/1241—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by a special physical form, e.g. emulsion, microcapsules, liposomes, characterized by a special physical form, e.g. emulsions, dispersions, microcapsules particles, powders, lyophilizates, adsorbates, e.g. polymers or resins for adsorption or ion-exchange resins
    • A61K51/1244—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by a special physical form, e.g. emulsion, microcapsules, liposomes, characterized by a special physical form, e.g. emulsions, dispersions, microcapsules particles, powders, lyophilizates, adsorbates, e.g. polymers or resins for adsorption or ion-exchange resins microparticles or nanoparticles, e.g. polymeric nanoparticles
    • A61K51/1251—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by a special physical form, e.g. emulsion, microcapsules, liposomes, characterized by a special physical form, e.g. emulsions, dispersions, microcapsules particles, powders, lyophilizates, adsorbates, e.g. polymers or resins for adsorption or ion-exchange resins microparticles or nanoparticles, e.g. polymeric nanoparticles micro- or nanospheres, micro- or nanobeads, micro- or nanocapsules
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a kind of generated by isotope conversion reaction it is medical90Y‑ZrO2Microballoon and preparation method thereof.This is medical90Y‑ZrO2Ceramic microsphere is first will by sol-gal process89Y and Zr are converted into simultaneously89Y and Zr are mixed uniformly89Y‑ZrO2Oxide gel sphere, gel ball obtain dry through over cleaning, drying process89Y‑ZrO2Oxide gel microballoon, microballoon are sintered into obtain under non-reducing atmosphere89Y‑ZrO2Ceramic microsphere；89Y‑ZrO2Ceramic microsphere passes through89Y(n,γ)90Y nuclear reaction, will89Y‑ZrO2It is converted into radioactive89Y‑ZrO2Ceramic bead.It is disclosed by the invention90Y‑ZrO2Microballoon specific radioactivity is high, and good biocompatibility, size tunable can be used for the treatment of tumour.

Description

It is medical90Y-ZrO2Ceramic microsphere and preparation method thereof
Technical field
The invention belongs to medical radioactive drug fields, and in particular to a kind of medical90Y-ZrO2Ceramic microsphere and its preparation Method.
Background technique
With the raising of human living standard, the disease incidence of tumour is also higher and higher.It is main for the treatment of tumour at present There are operation directly excision, chemotherapy and radiation therapy.Among these, radiation therapy can pass through external exposure and interior photograph again Two kinds of approach are penetrated to treat tumour.External exposure is usually to use Co-60 radioactive source, proton precessional magnetometer or heavy ion avcceleration It realizes, this method is maximum the disadvantage is that the injury of ray normal tissue is bigger.And interior irradiation is incited somebody to action by limited means Radionuclide is implanted into the patient, and is then treated by the effects of ionizing radiation of the particle of its transmitting to tumour.It is ideal Local internal radiotherapy nucleic, should have the characteristics that radiate high-energy pure beta ray, short-half-life, can be firmly combined with carrier. Yttrium-90Y is pure beta emitter, and having radiation high-energy pure beta ray, (highest energy 2.26MeV, average energy are 0.94MeV), half-life short (64.5h), short (mean range is 2.5mm, maximum to penetration range in tissue in biological tissue of human body Range is 10.3mm), 87% energy can be discharged in 8d, effective radioactivity sustainable 7.5 half-life period the advantages that, yttrium-90Y It is considered as the nucleic of radiation treatment in the irreplaceable part of the field of nuclear medicine, is especially proliferated faster malignant tumour such as Liver cancer and colorectal cancer Liver m etastases.In order to realize yttrium-90Y the field of nuclear medicine application, usually by pure beta emitter Yttrium-90Y is supported on certain carrier granular, then will contain yttrium-90The carrier granular of Y is injected into tumour by certain way Then position passes through yttrium-90Oncotherapy is realized in the interior irradiation of Y nucleic.
Up to the present, it has been carried out yttrium-90Y is supported on glass microsphere, in carbosphere, is respectively formed90Y glass microsphere With90Y carbosphere (Li Maoliang；Li Yi combustion；The patents such as Qian Jihui, the patent No.: CN201610655286.6).However, at home really It is few about load90Y's90Y-ZrO2The report of ceramic microsphere.
Summary of the invention
In view of the defects existing in the prior art, the purpose of the present invention is to provide a kind of simple process, size tunable, biologies Good medical of compatibility90Y-ZrO2Ceramic microsphere and preparation method thereof.
In order to reach the goals above, the invention adopts the following technical scheme:
It is a kind of medical90Y-ZrO2Ceramic microsphere is prepared by the method comprising the following steps:
1) will89Y and Zr are converted into oxide gel sphere；
2) gel ball cleaned, dried, obtain dry hydrous oxide gel ball；
3) the hydrous oxide gel ball is calcined under certain atmosphere, obtain single-phase, yttrium (89Y) uniformly Doping89Y-ZrO2Ceramic microsphere；
It 4) will be described89Y-ZrO2Ceramic microsphere passes through89Y(n,γ)90Y nuclear reaction, is converted into it90Y-ZrO2Ceramics are micro- Ball.
It will in above method step 1)89Y and Zr is converted into the specific of oxide gel sphere the preparation method is as follows: will include Have89The mixed solution of Y and Zr is mixed with gelling agent solution according to certain the mass ratio of the material example, and mixed solution passes through vibration excitor It is separated into drop with certain excited frequency, drop is heated by certain mode, the Zr in heating process in drop4+And Y3 +It hydrolyzes rapidly, hydrolysis promotes drop to be quickly converted to cured oxide gel sphere.
Wherein, described to include89The mixed solution of Y and Zr, Zr concentration range are 0.3mol/L to 2.5mol/L,89Y is dense Degree range is 0.01mol/L to 0.25mol/L.
The gelling agent solution be four ammonium of hexa-methylene (HMTA) and urea (Urea) mixed solution, wherein HMTA with The substance withdrawl syndrome of urea can be 1mol/L to 3.2mol/L, and the substance withdrawl syndrome proportional region of urea and HMTA can be with It is 0.2 to 1.0.The concrete configuration method of the gelling agent solution is as follows: weighing four ammonium of hexa-methylene (HMTA) of certain mass With urea (Urea) solid, deionized water dissolving is added.
Include89When the mixed solution of Y and Zr is mixed with gelling agent solution, the mass ratio of the material example model of the HMTA and Zr Enclose is 0.3 to 1.5.
The excited frequency range of the vibration excitor is 1-105Hz。
Include89The mixed solution of Y and Zr and the hybrid mode of gelling agent solution can mix for cooling in advance, can also be with For the instant on-line mixing of no cooling.
In the above method heating method of drop can be microwave heating (specific: microwave frequency can be 12.433GHz, Input power can be 50dBm), or traditional organic media heating, such as silicone oil heating.
The gel ball is mainly by Zr (OH)4、89Y(OH)3, HMTA, urea, Lauxite etc. is at being grouped as.
In above method step (2), the mode of the cleaning depends on the heating method of dropping liquid in step (1).If step Suddenly gel reaction is promoted using microwave heating in (1), step is directly cleaned with ammonia spirit in (2), then clear with deionized water It washes.If promoting gel reaction using organic media heating in step (1), first needed in step (2) with carbon tetrachloride or three Vinyl chloride cleaning, removes the silicone oil of gel ball surface, is then cleaned respectively with ammonia spirit again and deionized water is cleaned.
In above method step (2), the condition of the drying are as follows: drying temperature can be 25 DEG C to 100 DEG C, drying time It is longer than 2 hours.Specific condition is such as: be dried at room temperature for 24 hours, then at 60 DEG C it is 12 hours dry.
In above method step (3), the calcining carries out in non-reducing atmosphere, such as air, Ar gas, N2Gas etc.；Institute State the condition of calcining are as follows: with the heating rate of 1 DEG C/min to 30 DEG C/min, be heated to 800 DEG C to 1700 DEG C and keep the temperature；When heat preservation Between be longer than 2 hours.Specific condition is such as: being heated to 500 DEG C in air atmosphere with 3 DEG C/min and is kept for 4 hours, then with 10 DEG C/min is heated to 1350 DEG C, and kept for 5 hours.
Ceramic microsphere obtained in above method step (3) is mainly89Y Uniform Doped is in ZrO2It is single in crystal structure Phase oxide.
In above method step (4), the specific method is as follows for the nuclear reaction: will be obtained in step (3)89Y-ZrO2Pottery Porcelain microballoon is put into container, will89Y-ZrO2In ceramic microsphere89Y passes through nuclear reaction89Y (n, γ)90Y is converted into90Y, irradiation After 0.5h to 20h, accordingly89Y-ZrO2Ceramic microsphere is converted into90Y-ZrO2Ceramic microsphere.
The container is the material not activated under the conditions of neutron irradiation, such as: quartz glass.
Neutron required for the nuclear reaction occurs can (such as neutron flux be higher than 5*10 from reactor13n/cm2's Nuclear reactor), spallation target can also be derived from.
Ceramic microsphere obtained in step (4) is90Y Uniform Doped is in ZrO2In structure with single phase structure90Y- ZrO2Ceramic microsphere.
Obtained in step (4)90Y-ZrO2Ceramic microsphere partial size can be 20-1000 μm.
It is prepared by the present invention90Y-ZrO2In ceramic microsphere90The release rate of Y nucleic is low, the radioactivity suitable for local tumor Treatment.
It is also another object of the present invention to provide a kind of medicaments for being applicable in local tumor radiation treatment.
The active constituent of the medicament is prepared by the present invention90Y-ZrO2Ceramic microsphere.
Described90Y-ZrO2Ceramic microsphere can be infused in the radiation treatment for local tumor by certain way It is mapped to tumor locus, such as liver neoplasm.
Due to zirconium dioxide (ZrO2) have unique resistance to rupture, chemical stability, biocompatibility, at For a kind of indispensable medical material；And yttrium can form single congruent melting phase with zirconium dioxide, can be further improved two The chemical stability and resistance to rupture of zirconium oxide.Therefore the yttrium-pure β emitted90Y nucleic is supported on shape in zirconium dioxide microballoon At90Y-ZrO2Microballoon, and be applied to the treatment of clinically tumour, especially by the liver malignancy of unresectable, Have great importance.
Compared with the prior art, the present invention has the following advantages:
(1) present invention preparation90Y-ZrO2The method of ceramic microsphere is simple, and introducing impurity is few, and product purity is high；
(2)90Y-ZrO2Ceramic microsphere chemical stability in human body is good, good biocompatibility；
(3)90Y-ZrO2In90Y nucleic by lattice replace in a manner of and ZrO2Single-phase is formed,90Y slip is low.
(4)90Y-ZrO2Ceramic microsphere production cost is low, easy to promote and utilize.
Detailed description of the invention
Fig. 1 be 1 step 2 of embodiment obtain include89The photo in kind of the oxide gel sphere of Y and Zr；
Fig. 2 is what embodiment 1 was prepared89Y-ZrO2The XRD spectrum of ceramic microsphere；
Fig. 3 is what embodiment 1 was prepared89Y-ZrO2The SEM photograph of ceramic microsphere.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto, all of the invention Any modifications, equivalent replacements, and improvements etc. done within spirit and principle, should all be included in the protection scope of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
It is prepared by embodiment 1, immediately-sol-gel method for being combined without cooling mixing with Microwave-assisted firing90Y-ZrO2 Ceramic microsphere
The following steps are included:
(1) by the mixed solution of zirconyl nitrate and yttrium nitrate (89Zr concentration is 1.60mol/L, and Y concentration is 0.16mol/L, H+/Ce4+=0.4) and gelling agent HMUR solution (HMTA concentration be 3.18mol/L, urea concentration 3.18mol/L) respectively with The flow velocity of 1.98mL/min and 1.00mL/min is transported in T-type raw material liquid mixer, is carried out in 0.15mm capillary abundant Mixing, mixed feed liquid (HMTA/Zr=1.0) pass through vibration excitor exciting (excited frequency 10Hz), are dispersed into mixing drop.Liquid Drop forms gel ball, microwave frequency 12.433GHz, input power 50dBm across microwave heating system.
(2) gel ball is collected in the ammonia spirit of 0.5mol/L, and stands 0.5 hour；Then the ammonia of 0.5mol/L is used Aqueous solution to gel ball clean 5 times, 30 minutes every time, until cleaning solution conductivity is less than 760 μ S/cm；And then deionization is used Water cleaning 6 times, 30 minutes every time, until cleaning solution is less than 20 μ S/cm.
(3) bead in step (2) is dried at room temperature for drying 12 hours at 24 hours, 60 DEG C, then in Ar gas 500 DEG C are heated to 3 DEG C/min under atmosphere and is kept for 4 hours, are then heated to 1350 DEG C with 10 DEG C/min, and kept for 5 hours, Then the ceramics that diameter is about 50 μm can be obtained to room temperature in Temperature fall89Y-ZrO2Bead.
(4) ceramic bead that step (3) obtains is fitted into quartz glass tube and is placed in neutron flux higher than 5*1013n/cm2 Nuclear reactor in irradiate, in ceramic bead89Y will pass through nuclear reaction89Y (n, γ)90Y is converted into90Y, accordingly89Y-ZrO2 It is converted into90Y-ZrO2.It obtains90Y-ZrO2Bead specific radioactivity is greater than 300GBq/g Y.
Embodiment 2, traditional sol-gel method preparation90Y-ZrO2Ceramic microsphere
The following steps are included:
(1) by the mixed solution of zirconyl nitrate and yttrium nitrate (89Zr concentration is 1.60mol/L, and Y concentration is 0.16mol/L, H+/Ce4+=0.4) it is cooled down respectively with gelling agent HMUR solution (HMTA concentration is 3.18mol/L, urea concentration 3.18mol/L) To 0-5 DEG C, then under cooled conditions to be mixed respectively with molar ratio HMTA/Zr=0.8, mixed solution passes through Vibration excitor exciting is dispersed into drop, and drop instills in 90 DEG C of silicone oil and keeps 30min, and drop is occurred molten by the silicone oil heating of heat Glue gel reacts and is formed by curing gel ball.
(2) gel ball first passes around carbon tetrachloride and carries out cleaning four times, at least 30 minutes every time, removes gel ball surface Silicone oil.And then, gelled pill with the ammonia spirit of 0.5mol/L carry out cleaning 5 times, 30 minutes every time, until cleaning solution conductance Rate is less than 760 μ S/cm；Then 6 times are cleaned with deionized water, 30 minutes every time, until cleaning solution is less than 20 μ S/cm.
(3) bead in step (2) is 12 hours dry at 60 DEG C, then with 3 DEG C/min heating under air atmosphere It to 500 DEG C and is kept for 4 hours, 1350 DEG C, and holding 5 hours is then heated to 10 DEG C/min, then Temperature fall to room temperature, The ceramics that diameter is about 50 μm can be obtained89Y-ZrO2Bead.
(4) ceramic bead that step (3) obtains is fitted into quartz glass tube and is placed in neutron flux higher than 5*1013n/cm2 Nuclear reactor in irradiate, in ceramic bead89Y will pass through nuclear reaction89Y (n, γ)90Y is converted into90Y, accordingly89Y-ZrO2 It is converted into90Y-ZrO2.It obtains90Y-ZrO2Bead specific radioactivity is greater than 300GBq/g Y.

Claims (9)

1. a kind of90Y-ZrO2The preparation method of ceramic microsphere, includes the following steps:
1) will89Y and Zr cotransformation is oxide gel sphere；
2) gel ball cleaned, dried, obtain dry hydrous oxide gel ball；
3) the hydrous oxide gel ball is calcined, obtain single-phase,89Y Uniform Doped89Y-ZrO2Ceramics are micro- Ball；
It 4) will be described89Y-ZrO2Ceramic microsphere passes through89Y(n,γ)90Y nuclear reaction, is converted into it90Y-ZrO2Ceramic microsphere.
2. preparation method according to claim 1, it is characterised in that: will in the step 1)89Y and Zr are converted into oxide Gel ball it is specific the preparation method is as follows: will include89The mixed solution of Y and Zr is mixed with gelling agent solution, mixed molten Liquid is separated into drop by vibration excitor, and drop is heated, the Zr in heating process in drop4+And Y3+It hydrolyzes, makes the liquid Drop is converted into oxide gel sphere.
3. preparation method according to claim 2, it is characterised in that: described to include89In the mixed solution of Y and Zr, Zr Concentration range is 0.3mol/L to 2.5mol/L,89Y concentration range is 0.01mol/L to 0.25mol/L；
The gelling agent solution is the mixed solution of hexa-methylene four ammoniums and urea, wherein the object of hexa-methylene four ammoniums and urea The amount concentration of matter is 1mol/L to 3.2mol/L, the substance withdrawl syndrome proportional region of four ammonium of urea and hexa-methylene be 0.2 to 1.0；
It is described to include89In the mixed solution of Y and Zr and the mixed liquor of gelling agent solution, the object of hexa-methylene four ammoniums and Zr The amount proportional region of matter is 0.3 to 1.5；
The excited frequency range of the vibration excitor is 1-105Hz；
Include89The mixed solution of Y and Zr and the hybrid mode of gelling agent solution are that cooling mix in advance, or for without it is cooling immediately On-line mixing；
The heating method of the drop is that microwave heating or organic media heat.
4. preparation method according to claim 3, it is characterised in that: according to microwave heating drop in the step (1), It is directly cleaned with ammonia spirit in the step (2), is then cleaned with deionized water；According to organic Jie in the step (1) Matter heats, and first needs to be cleaned with carbon tetrachloride or trichloro ethylene in the step (2), removes organic Jie of gel ball surface Then matter is successively cleaned again with ammonia spirit and deionized water is cleaned, the organic media is silicone oil.
5. preparation method described in any one of -4 according to claim 1, it is characterised in that: in the step (3), the calcining It is carried out in non-reducing atmosphere；The condition of the calcining are as follows: with the heating rate of 1 DEG C/min to 30 DEG C/min, be heated to 800 DEG C to 1700 DEG C and keep the temperature.
6. preparation method described in any one of -4 according to claim 1, it is characterised in that: in the step (4), the core is anti- The method answered is as follows: will be obtained in step (3)89Y-ZrO2Ceramic microsphere passes through nuclear reaction89Y (n, γ)90Y is converted into90Y, spoke After 0.5h to 20h, accordingly89Y-ZrO2Ceramic microsphere is converted into90Y-ZrO2Ceramic microsphere；Required for the nuclear reaction occurs Neutron source in reactor or derive from spallation target.
7. any one of claim 1-6 the method is prepared90Y-ZrO2Ceramic microsphere.
8. according to claim 890Y-ZrO2Ceramic microsphere, it is characterised in that: described90Y-ZrO2Ceramic microsphere partial size is 20-1000μm。
9. described in claim 8 or 990Y-ZrO2Ceramic microsphere is in the medicament that preparation is used for local tumor radiation treatment Using.
CN201910599552.1A 2019-07-04 2019-07-04 It is medical90Y-ZrO2Ceramic microsphere and preparation method thereof Pending CN110342927A (en)

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李飒 等: "溶胶凝胶法制备二氧化锆微球", 《第十三届全国核化学与放射化学学术研讨会论文摘要集》 *
王斯妮等: "钇-90 微球的特性、放射栓塞的操作技术及安全防护—钇-90 微球放射栓塞系列回顾（一）", 《介入放射学杂质》 *

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Application publication date: 20191018