CN108751991A - A kind of laser sintered preparation Tb:Lu2O3The method of ceramics - Google Patents

A kind of laser sintered preparation Tb:Lu2O3The method of ceramics Download PDF

Info

Publication number
CN108751991A
CN108751991A CN201810939210.5A CN201810939210A CN108751991A CN 108751991 A CN108751991 A CN 108751991A CN 201810939210 A CN201810939210 A CN 201810939210A CN 108751991 A CN108751991 A CN 108751991A
Authority
CN
China
Prior art keywords
ceramics
ion
laser
powder
plain embryo
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
Application number
CN201810939210.5A
Other languages
Chinese (zh)
Other versions
CN108751991B (en
Inventor
张乐
侯晨
蒋志刚
陈浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xuzhou Huayan Special Ceramic Co., Ltd.
Original Assignee
Xuzhou Jiangsu Normal University Laser Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Xuzhou Jiangsu Normal University Laser Technology Co Ltd filed Critical Xuzhou Jiangsu Normal University Laser Technology Co Ltd
Priority to CN201810939210.5A priority Critical patent/CN108751991B/en
Publication of CN108751991A publication Critical patent/CN108751991A/en
Application granted granted Critical
Publication of CN108751991B publication Critical patent/CN108751991B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/665Local sintering, e.g. laser sintering
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/78Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786Micrometer sized grains, i.e. from 1 to 100 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646Optical properties
    • C04B2235/9653Translucent or transparent ceramics other than alumina

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Luminescent Compositions (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of laser sintered preparation Tb:Lu2O3The method of ceramics, specifically:According to chemical structural formula (Lu1‑ xTbx)2O3The stoichiometric ratio of middle each element weighs reaction raw materials powder respectively, and citric acid and ethylene glycol are added in the raw material mixed and stirs evenly to obtain presoma;Then precursor powder is heated, is ground, sublevel section calcining;Adhesive polyethylene alcoholic solution is added in powder after firing and disc-shaped is prepared into using dry-pressing formed method, obtains plain embryo piece;Plain embryo piece is placed on a Lu2O3On gasket, two-sided sintering is carried out to it with laser;It is finally ground polishing treatment, obtains Tb:Lu2O3Ceramics.Method provided by the invention can effectively inhibit Tb3+Ion is to Tb4+Ion transit improves Tb inside ceramics3+The content of ion, it can be achieved that the green emission of high intensity, preparation process is simple under the excitation of 323nm ultraviolet lights, energy conservation and environmental protection, for ceramics sample relative density obtained up to 99.9%, transmitance is high, and compactness is good.

Description

A kind of laser sintered preparation Tb:Lu2O3The method of ceramics
Technical field
The invention belongs to ceramic materials preparation technology fields, and in particular to a kind of laser sintered preparation Tb:Lu2O3Ceramics Method.
Background technology
Luteium oxide (Lu2O3) under visible light and infrared light high transmittance being all had, emission cross section is big, and phonon energy is low, Density is high, while having good mechanical performance and hot property.Therefore, luteium oxide is a kind of outstanding laser medium material and sudden strain of a muscle Bright body material, has broad application prospects.Lu2O3With cubic crystal structure, optical isotropy, refractive index independent of By nanometer crystal technique and high temperature sintering technique crystalline ceramics can be made in powder by directionality.Meanwhile Lu2O3Crystalline ceramics can be with Realize more conveniently variety classes, various concentration rare earth ion doping, to possess extensive optical application.
In rare earth ion, Tb3+The ionic radius and Lu of ion3+The ionic radius of ion is close, therefore, Tb3+Ion is mixed Enter Lu2O3The distortion of lattice generated after lattice it is smaller, it can be achieved that higher concentration doping.Under the excitation of ultraviolet light, Tb3+Ion It can occur5D4Energy level to7F5The transition of energy level, so as to provide green light, therefore, Tb for the synthesis of white light:Lu2O3Crystalline ceramics exists White light LEDs field is widely used.In addition, Tb:Lu2O3The thermal conductivity of crystalline ceramics is high, is conducive to distributing for heat, is waiting Gas ions field of flat panel displays is also with a wide range of applications.
Vacuum-sintering is widely used in Tb as a kind of sintering processing effectively facilitating densification:Lu2O3Crystalline ceramics It prepares.During vacuum-sintering, ceramics are internal to will produce a large amount of Lacking oxygen, needs to anneal by prolonged high temperature air (1450 DEG C × 10h) make up Lacking oxygen.But during air anneal, inevitable that a large amount of Tb3+Ion With O2Reaction generates Tb4+Ion, and Tb4+Ion does not shine, Tb3+The reduction of ion concentration will result directly in Tb:Lu2O3Ceramics hair The decline of optical property.In addition, in traditional vacuum sintering technique, for the densification process of Effective Regulation ceramics, MgO, The sintering aids such as TEOS are essential.But the introducing of sintering aid will cause electricity price uneven.In sintering process, charge Compensating action can lead to Tb3+Ion is to Tb4+Ion transit, to influence the luminous mass of ceramics.Therefore, using vacuum-sintering It is difficult to Tb in sintering process3+To Tb4+Transformation effectively controlled.And traditional vacuum-sintering needs higher burning Junction temperature (1600~1800 DEG C) and longer soaking time (8~20h), this also causes sintered ceramic crystalline grain size universal Larger (10~30 μm), mechanical performance is bad, it is difficult to meet the needs of Vehicles Collected from Market is to its mechanical property.
Invention content
The object of the present invention is to provide a kind of laser sintered preparation Tb:Lu2O3The method of ceramics, can effectively inhibit Tb3+ Ion is to Tb4+Ion transit, and sintering temperature is low, the time is short.
To achieve the above object, the technical solution adopted by the present invention is as follows:A kind of laser sintered preparation Tb:Lu2O3Ceramics Method includes the following steps:
(1) according to chemical structural formula (Lu1-xTbx)2O3The stoichiometric ratio of middle each element is weighed respectively containing lutetium ion Lu3+ Compound and contain terbium ion Tb3+Compound powder as reaction raw materials, wherein x is Tb3+Adulterate Lu3+Moles the hundred of position Score, 0.001≤x≤0.02;
(2) citric acid and ethylene glycol solution are added in the material powder mixed, and stirs evenly, it is molten to obtain presoma Liquid, wherein the molar ratio of metal ion and citric acid is 0.2~0.5, and citric acid and quality of glycol ratio are 1~2;
(3) precursor solution is heat-treated under the conditions of 70~80 DEG C, removes extra moisture, is cooled to room temperature, Grinding, obtains precursor powder;Then 5~7h of precalcining under the conditions of the precursor powder after grinding being placed in 500~800 DEG C, Extra organic matter is removed, then 1~3h is calcined under the conditions of the precursor powder after precalcining is placed in 800~1200 DEG C;
(4) adhesive polyethylene alcoholic solution is added in powder after firing to be plasticized, is suppressed using dry pressing At disc-shaped, plain embryo piece is obtained, wherein poly-vinyl alcohol solution addition is the 1.0~7.0% of tabletting powder quality;
(5) plain embryo piece is placed on a Lu2O3On gasket, sintering is carried out at the same time to plain embryo piece two sides with laser, is obtained Ceramic element embryo;
(6) the plain embryo of sintered ceramics is ground and is polished to 1~3mm, obtain Tb:Lu2O3Crystalline ceramics.
Preferably, described to contain lutetium ion Lu in step (1)3+Compound be luteium oxide or lutecium nitrate, it is described to contain terbium Ion Tb3+Compound be terbium nitrate, terbium chloride, it is a kind of in terbium oxide.
Preferably, in step (4), a concentration of 0.05~0.2g/ml of the poly-vinyl alcohol solution.
Preferably, in step (4), the degree of polymerization of the polyvinyl alcohol is 1600~1900.
Preferably, in step (4), pressing pressure is 800~1200Mpa, a diameter of 2.0~6.0mm of plain embryo piece, thickness For 0.5~3.0mm.
Preferably, in step (5), laser output power density is 3.2~3.4W/mm2, 4.9~5.5mm of beam diameter.
Preferably, in step (5), laser scanning speed is 2~12mm/s.
Compared with prior art, the present invention has the advantages that:
1. during laser sintered, the internal generation that will not have Lacking oxygen of ceramics, therefore sintered sample be not necessarily into Row air anneal, therefore can effectively inhibit Tb3+Ion is to Tb4+Ion transit;And laser sintering technology is used, due to not It needs to introduce any sintering aid, therefore can avoid the internal electricity price energy imbalance of ceramics, to inhibit charge compensation to act on The Tb brought4+The generation of ion improves Tb inside ceramics3+The content of ion, under the excitation of 323nm ultraviolet lights, it can be achieved that The green emission of high intensity.
2. method provided by the invention prepares Tb:Lu2O3Sintering time needed for crystalline ceramics is short, and laser sintered process only needs 3 ~15min, energy conservation and environmental protection are easy to produce in batches;And the ceramic crystalline grain size of laser sintered preparation is small (1~5 μm), mechanical performance Preferably, meet demand of the Vehicles Collected from Market to crystalline ceramics mechanical property.
3. Tb prepared by method provided by the invention:Lu2O3The relative density of crystalline ceramics sample has very well up to 99.9% Compactness, transmitance is high, and laser output may be implemented.
Description of the drawings
Fig. 1 is Tb prepared by the embodiment of the present invention 2:Lu2O3The XRD diagram of crystalline ceramics.
Specific implementation mode
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Unless otherwise indicated, raw material used in following embodiment is commercial product, and the purity of material powder is all higher than In 99.9%.
Embodiment 1:(Lu0.999Tb0.001)2O3Crystalline ceramics
According to (Lu0.999Tb0.001)2O3The stoichiometric ratio of middle each element weighs Lu respectively2O3And Tb4O7Powder is as anti- Answer raw material;
Citric acid is diluted to a concentration of 0.05g/ml with distilled water, citric acid and second two are added in the raw material mixed (molar ratio of metal ion and citric acid is 0.2 to alcoholic solution, and citric acid and quality of glycol ratio are 1), and to stir evenly, and are obtained Precursor solution;
Precursor solution is heated to 70 DEG C of heat preservations for 24 hours, to remove extra moisture, is cooled to room temperature, then place it in It is ground in mortar, obtains precursor powder;Then by the precursor powder after grinding at 500 DEG C precalcining 5h, to go The calcining 1h at 800 DEG C is placed in Muffle furnace except extra organic matter, then by the precursor powder after precalcining.
Adhesive polyethylene alcohol (degree of polymerization is 1600~1900) solution of 0.05g/ml is added in powder after firing It is plasticized, and dry pressing is used to be compressed into a diameter of 2.0mm, thickness as the disk of 0.5mm, pressure 80Mpa is obtained To plain embryo piece.
The good plain embryo piece of dry-pressing is placed on a Lu2O3On gasket, with laser with the laser beam pair of a diameter of 4.9mm It is sintered, and the power of laser is with 0.01W/mm2Linear power rise to 3.2W/mm2, and kept at maximum power 70s, sweep speed 2mm/s, complete laser sintered time are 5min.During this, plain embryo piece two sides is sintered simultaneously.Most Afterwards, ceramic plain embryo is ground and is polished to 1mm, obtain Tb:Lu2O3Crystalline ceramics.
Ceramics sample manufactured in the present embodiment is Lu2O3Phase, without other dephasigns, ceramic purity is higher.Ceramic crystalline grain size 3.2 μm, optical transmittance is 81.0% at 400nm, and optical quality is good, may be implemented in the case where carrying out 323nm light excitations The green light of 550nm exports.
Embodiment 2:(Lu0.995Tb0.005)2O3Crystalline ceramics
According to (Lu0.995Tb0.005)2O3The stoichiometric ratio of middle each element weighs Lu (NO respectively3)3·6H2O and Tb (NO3)3·5H2O powders are as reaction raw materials;
Citric acid is diluted to a concentration of 0.1g/ml with distilled water, citric acid and second two are added in the raw material mixed (molar ratio of metal ion and citric acid is 0.3 to alcoholic solution, and citric acid and quality of glycol ratio are 1.5), and to stir evenly, and are obtained To precursor solution;
Precursor solution is heated to 75 DEG C of heat preservations for 24 hours, to remove extra moisture, is cooled to room temperature, then place it in It is ground in mortar, obtains precursor powder;Then by the precursor powder after grinding at 700 DEG C precalcining 5h, to go The calcining 2h at 1000 DEG C is placed in Muffle furnace except extra organic matter, then by the precursor powder after precalcining.
Be added in powder after firing adhesive polyethylene alcohol (degree of polymerization be 1600~1900) solution of 0.1g/ml into Row plasticizing, and dry pressing is used to be compressed into a diameter of 4.0mm, thickness as the disk of 1.5mm, pressure 120Mpa is obtained To plain embryo piece.
The good plain embryo piece of dry-pressing is placed on a Lu2O3On gasket, with laser with the laser beam pair of a diameter of 5.2mm It is sintered, and the power of laser is with 0.02W/mm2Linear power rise to 3.3W/mm2, and kept at maximum power 85s, sweep speed 10mm/s, complete laser sintered time are 7min.During this, plain embryo piece two sides is sintered simultaneously. Finally, ceramic plain embryo is ground and is polished to 2mm, obtain Tb:Lu2O3Crystalline ceramics.
Fig. 1 is the XRD diagram of ceramics sample, it can be seen that sample Lu2O3Phase, without other dephasigns, ceramic purity is higher.Pottery 2 μm of porcelain crystallite dimension, optical transmittance are 80.7% at 400nm, and optical quality is good, can in the case where carrying out 323nm light excitations To realize the green light output of 550nm.
Embodiment 3:(Lu0.98Tb0.02)2O3Crystalline ceramics
According to (Lu0.98Tb0.02)2O3The stoichiometric ratio of middle each element weighs Lu (NO respectively3)3·6H2O and TbCl3· 6H2O powders are as reaction raw materials;
Citric acid is diluted to a concentration of 0.2g/ml with distilled water, citric acid and second two are added in the raw material mixed (molar ratio of metal ion and citric acid is 0.5 to alcoholic solution, and citric acid and quality of glycol ratio are 2), and to stir evenly, and are obtained Precursor solution;
Precursor solution is heated to 80 DEG C of heat preservations for 24 hours, to remove extra moisture, is cooled to room temperature, then place it in It is ground in mortar, obtains precursor powder;Then by the precursor powder after grinding at 800 DEG C precalcining 7h, to go The calcining 3h at 1200 DEG C is placed in Muffle furnace except extra organic matter, then by the precursor powder after precalcining.
Be added in powder after firing adhesive polyethylene alcohol (degree of polymerization be 1600~1900) solution of 0.2g/ml into Row plasticizing, and dry pressing is used to be compressed into a diameter of 6.0mm, thickness as the disk of 3.0mm, pressure 150Mpa is obtained To plain embryo piece.
The good plain embryo piece of dry-pressing is placed on a Lu2O3On gasket, with laser with the laser beam pair of a diameter of 5.5mm It is sintered, and the power of laser is with 0.03W/mm2Linear power rise to 3.4W/mm2, and kept at maximum power 100s, sweep speed 12mm/s, complete laser sintered time are 8min.During this, plain embryo piece two sides is sintered simultaneously. Finally, ceramic plain embryo is ground and is polished to 3mm, obtain Tb:Lu2O3Crystalline ceramics.
Ceramics sample manufactured in the present embodiment is Lu2O3Phase, without other dephasigns, ceramic purity is higher.Ceramic crystalline grain size 2.8 μm, optical transmittance is 80.6% at 400nm, and optical quality is good, may be implemented in the case where carrying out 323nm light excitations The green light of 550nm exports.

Claims (7)

1. a kind of laser sintered preparation Tb:Lu2O3The method of ceramics, which is characterized in that include the following steps
(1) according to chemical structural formula (Lu1-xTbx)2O3The stoichiometric ratio of middle each element is weighed respectively containing lutetium ion Lu3+Change It closes object and contains terbium ion Tb3+Compound powder as reaction raw materials, wherein x is Tb3+Adulterate Lu3+The mole percent of position, 0.001≤x≤0.02;
(2) citric acid and ethylene glycol solution are added in the material powder mixed, and stirs evenly, obtains precursor solution, Wherein, the molar ratio of metal ion and citric acid is 0.2~0.5, and citric acid and quality of glycol ratio are 1~2;
(3) precursor solution is heat-treated under the conditions of 70~80 DEG C, removes extra moisture, is cooled to room temperature, ground, Obtain precursor powder;Then 5~7h of precalcining under the conditions of the precursor powder after grinding being placed in 500~800 DEG C, removal are more Remaining organic matter, then calcine 1~3h under the conditions of the precursor powder after precalcining is placed in 800~1200 DEG C;
(4) adhesive polyethylene alcoholic solution is added in powder after firing to be plasticized, is compressed into justifying using dry pressing Sheet obtains plain embryo piece, and wherein poly-vinyl alcohol solution addition is the 1.0~7.0% of tabletting powder quality;
(5) plain embryo piece is placed on a Lu2O3On gasket, sintering is carried out at the same time to plain embryo piece two sides with laser, obtains ceramics Plain embryo;
(6) the plain embryo of sintered ceramics is ground and is polished to 1~3mm, obtain Tb:Lu2O3Crystalline ceramics.
2. laser sintered preparation Tb according to claim 1:Lu2O3The method of ceramics, which is characterized in that in step (1), It is described to contain lutetium ion Lu3+Compound be luteium oxide or lutecium nitrate, it is described to contain terbium ion Tb3+Compound be terbium nitrate, It is a kind of in terbium chloride, terbium oxide.
3. laser sintered preparation Tb according to claim 1 or 2:Lu2O3The method of ceramics, which is characterized in that step (4) In, a concentration of 0.05~0.2g/ml of the poly-vinyl alcohol solution.
4. laser sintered preparation Tb according to claim 1 or 2:Lu2O3The method of ceramics, which is characterized in that step (4) In, the degree of polymerization of the polyvinyl alcohol is 1600~1900.
5. laser sintered preparation Tb according to claim 1 or 2:Lu2O3The method of ceramics, which is characterized in that step (4) In, pressing pressure is 800~1200Mpa, and a diameter of 2.0~6.0mm of plain embryo piece, thickness is 0.5~3.0mm.
6. laser sintered preparation Tb according to claim 1 or 2:Lu2O3The method of ceramics, which is characterized in that step (5) In, laser output power density is 3.2~3.4W/mm2, 4.9~5.5mm of beam diameter.
7. laser sintered preparation Tb according to claim 1 or 2:Lu2O3The method of ceramics, which is characterized in that step (5) In, laser scanning speed is 2~12mm/s.
CN201810939210.5A 2018-08-17 2018-08-17 Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic Active CN108751991B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810939210.5A CN108751991B (en) 2018-08-17 2018-08-17 Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810939210.5A CN108751991B (en) 2018-08-17 2018-08-17 Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic

Publications (2)

Publication Number Publication Date
CN108751991A true CN108751991A (en) 2018-11-06
CN108751991B CN108751991B (en) 2020-03-13

Family

ID=63967181

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810939210.5A Active CN108751991B (en) 2018-08-17 2018-08-17 Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic

Country Status (1)

Country Link
CN (1) CN108751991B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256074A (en) * 2019-07-16 2019-09-20 上海应用技术大学 A kind of yttrium stablizes terbium oxide powder, magneto-optic crystalline ceramics and preparation method thereof
CN111233471A (en) * 2020-01-29 2020-06-05 桂林理工大学 Square tungsten bronze structure Mo3Nb2O14Method for producing materials and use thereof
CN112209710A (en) * 2020-10-17 2021-01-12 江苏师范大学 Method for preparing Ce: YAG fluorescent ceramic by laser sintering
WO2022189655A1 (en) * 2021-03-12 2022-09-15 Technische Universität Darmstadt Method and device for producing ceramics and ceramic product

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760157A (en) * 2005-06-28 2006-04-19 中国科学院上海硅酸盐研究所 A kind of preparation method of lutecia based transparent ceramics
CN102093054A (en) * 2010-12-01 2011-06-15 中国科学院上海光学精密机械研究所 Faraday magnetic rotation transparent ceramic and preparation method thereof
US20110150735A1 (en) * 2006-11-01 2011-06-23 Lawrence Livermore National Security, Llc. Fabrication of Transparent Ceramics Using Nanoparticles Synthesized Via Flame Spray Pyrolysis
CN104529449A (en) * 2014-12-18 2015-04-22 徐州市江苏师范大学激光科技有限公司 Method for preparing yttrium oxide-based transparent ceramic employing two-step sintering method
CN104557012A (en) * 2014-12-18 2015-04-29 徐州市江苏师范大学激光科技有限公司 Preparation method of Pr:LuAG ceramic scintillator

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760157A (en) * 2005-06-28 2006-04-19 中国科学院上海硅酸盐研究所 A kind of preparation method of lutecia based transparent ceramics
US20110150735A1 (en) * 2006-11-01 2011-06-23 Lawrence Livermore National Security, Llc. Fabrication of Transparent Ceramics Using Nanoparticles Synthesized Via Flame Spray Pyrolysis
CN102093054A (en) * 2010-12-01 2011-06-15 中国科学院上海光学精密机械研究所 Faraday magnetic rotation transparent ceramic and preparation method thereof
CN104529449A (en) * 2014-12-18 2015-04-22 徐州市江苏师范大学激光科技有限公司 Method for preparing yttrium oxide-based transparent ceramic employing two-step sintering method
CN104557012A (en) * 2014-12-18 2015-04-29 徐州市江苏师范大学激光科技有限公司 Preparation method of Pr:LuAG ceramic scintillator

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DAGMARA KULESZA ET AL.: "Lu2O3:Tb,Hf storage phosphor", 《RADIATION MEASUREMENTS》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256074A (en) * 2019-07-16 2019-09-20 上海应用技术大学 A kind of yttrium stablizes terbium oxide powder, magneto-optic crystalline ceramics and preparation method thereof
CN111233471A (en) * 2020-01-29 2020-06-05 桂林理工大学 Square tungsten bronze structure Mo3Nb2O14Method for producing materials and use thereof
CN112209710A (en) * 2020-10-17 2021-01-12 江苏师范大学 Method for preparing Ce: YAG fluorescent ceramic by laser sintering
WO2022189655A1 (en) * 2021-03-12 2022-09-15 Technische Universität Darmstadt Method and device for producing ceramics and ceramic product

Also Published As

Publication number Publication date
CN108751991B (en) 2020-03-13

Similar Documents

Publication Publication Date Title
CN108751991A (en) A kind of laser sintered preparation Tb:Lu2O3The method of ceramics
CN104557013B (en) Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics
CN103265954A (en) Potassium-sodium niobate based oxide up-conversion luminescent material and preparation method thereof
CN113213928B (en) Fluorescent ceramic, preparation method and application thereof
CN101265082A (en) Method for preparing transparent magnesium-aluminum spinel ceramic
JPH0225864B2 (en)
CN102515752A (en) Transparent ceramic material and preparation method thereof
CN111925202B (en) Yttrium aluminum garnet powder without sintering aid, yttrium aluminum garnet ceramic, and preparation method and application thereof
CN113149652B (en) High-light-transmittance transparent ceramic prepared based on cold sintering technology and preparation method thereof
CN102815941B (en) Rare-earth-ion-doped lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof
Lin et al. Emission color-tunable and optical temperature sensing properties of Er3+/La3+ co-doped (K0. 5Na0. 5) NbO3 optoelectronic transparent ceramic
CN101985399B (en) Method for preparing Re:YAG polycrystalline transparent ceramics by slip casting and reaction-sintering
CN101148357A (en) Method for preparing Yb3+ mixed lanthanum yttrium oxide upconversion luminous transparent laser ceramic
CN110357624B (en) High-dielectric-constant glass frit modified strontium zirconate doped potassium-sodium niobate lead-free transparent ceramic material and preparation method thereof
CN103232237A (en) Preparation method of normal-pressure-sintered transparent zirconium oxide ceramic material
CN102815945B (en) Lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof
CN108046794B (en) Method for preparing yttrium titanate transparent ceramic by using coprecipitation method synthetic powder
KR100891952B1 (en) Oxide-based target for transparent conductive film and method for manufacturing the same, and oxide-based transparent conductive film
CN111393166B (en) High-thermal-stability fluorescent ceramic for white light LED/LD and preparation method thereof
CN115557787B (en) Sesquioxide transparent ceramic and preparation method thereof
CN100358834C (en) High light output quick attenuation flash ceramic and its preparing method
CN106588014A (en) Luminescence enhanced Tm<3+>-doped Lu2O3-based transparent ceramic and preparation method thereof
CN113754436B (en) Preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic
CN103073295B (en) Preparation method of Er3+ and Tm3+ co-doped yttrium lanthanum oxide scintillating material transparent ceramic material
CN113045310B (en) Method for preparing lanthanum gadolinium zirconate transparent ceramic by AM gel casting process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20200214

Address after: 221441 Shenghui logistics park, Shijian village, Gaoliu Town, Xinyi City, Xuzhou City, Jiangsu Province

Applicant after: Xuzhou Huayan Special Ceramic Co., Ltd.

Address before: 221000 57 Heping Road, No. 4, west campus, Yunlong campus, Jiangsu Normal University, Xuzhou, Jiangsu.

Applicant before: XUZHOU JIANGSU NORMAL UNIVERSITY LASER TECHNOLOGY CO., LTD.

GR01 Patent grant