CN110372384A - A kind of preparation method of transparent stealth material - Google Patents

A kind of preparation method of transparent stealth material Download PDF

Info

Publication number
CN110372384A
CN110372384A CN201910696756.7A CN201910696756A CN110372384A CN 110372384 A CN110372384 A CN 110372384A CN 201910696756 A CN201910696756 A CN 201910696756A CN 110372384 A CN110372384 A CN 110372384A
Authority
CN
China
Prior art keywords
preparation
transparent
stealth material
powder
oxide
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.)
Pending
Application number
CN201910696756.7A
Other languages
Chinese (zh)
Inventor
曾和平
黄延伟
贺嘉杨
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.)
East China Normal University
Chongqing Institute of East China Normal University
Original Assignee
East China Normal University
Chongqing Institute of East China Normal University
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 East China Normal University, Chongqing Institute of East China Normal University filed Critical East China Normal University
Priority to CN201910696756.7A priority Critical patent/CN110372384A/en
Publication of CN110372384A publication Critical patent/CN110372384A/en
Priority to US16/892,581 priority patent/US11465911B2/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C04B35/50—Shaped 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
    • 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
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445—Fluoride containing anions, e.g. fluosilicate
    • 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
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/665—Local sintering, e.g. laser sintering
    • 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
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent 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)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of preparation methods of transparent stealth material comprising following steps: S1, lithium fluoride and metal oxide being added in zirconium dioxide, is milled to average grain diameter no more than 1 μm, obtains mixed-powder；S2, the mixed-powder is compacted, reaction-sintered is carried out under the irradiation of laser, obtain the transparent stealth material.The present invention is catalyzed sintered zirconia base transparent ceramic using laser, laser input energy is absorbed using the sintering activity of material itself, catalytic reaction process, synthetic sample is sintered in the case where swashing light-catalysed high-heat environment, not only sintered sample is fine and close, transmissivity is high, and preparation method is simple, time saving, material-saving, cleanliness without any pollution, and it also can large-scale industrial production.

Description

A kind of preparation method of transparent stealth material
Technical field
The invention belongs to laser processing technologys and transparent ceramic material development field, and in particular to a kind of laser catalysis sintering Transparent stealth material and method.
Background technique
Ceramic material inside it because, there are the stomata of light absorbing impurity and generation light scattering, being difficult glass-like thoroughly It is bright, but if selecting suitable high pure raw material, and crystalline ceramics can be obtained by process means removal stomata, as oxide is saturating Bright ceramics, the not only high-transmission rate with visible light or near infrared region, but also mechanical strength, hardness height, high temperature resistant, electrical isolation Property and chemical stabilization type are good.The purposes of crystalline ceramics is very extensive, can be used to manufacture high rigidity, resistance to height in mechanical industry Warm, corrosion-resistant part may be used as high temperature corrosion-resisting material instead of stainless steel etc., in defense military, thoroughly on chemical industry A kind of bright transparent stealth material well of ceramics advantage.LiAlON and MgAlON is developed in recent years than relatively rapid transparent pottery Porcelain, generally there are two types of methods for their preparation, first is that reaction sintering, i.e., pass through reaction-sintered after directly mixing reaction raw materials Corresponding crystalline ceramics is obtained, this method process is complex, the second phase is easy to produce, along with reaction process is also with volume Expansion leads to the problem of secondary blowhole, seriously affects the transparency of ceramics；Second is that two-step method, i.e., first synthesizing ceramic powder, then lead to Oversintering obtains crystalline ceramics, although this method improves the performance of ceramics to a certain extent, process is increasingly complex.This Two methods are directed to solid phase reaction process, since the market price of raw material AlN of use was held high, improve preparation cost.Cause It is very necessary that this develops novel transparent ceramic material and the cost-efficiently preparation method of development.Zirconium oxide crystalline ceramics is most Pipe has studied many years, but still lack in terms of the innovation of the performance of material and material technology exploitation one kind it is cheap, Efficiently, the preparation method of suitable large-scale industrial application and corresponding High-quality transparent ceramic.
Summary of the invention
It is an object of the invention to propose a kind of preparation method of transparent stealth material, in the presence of solving the prior art The above problem.
The present invention is achieved by the following technical solutions:
A kind of preparation method of transparent stealth material comprising following steps:
S1, lithium fluoride and metal oxide are added in zirconium dioxide, are milled to average grain diameter no more than 1 μm, obtain Mixed-powder；
S2, the mixed-powder is compacted, reaction-sintered is carried out under the irradiation of laser, obtain the transparent stealthy material Material.
Preferably, the partial size of the mixed-powder is 10nm~1 μm.
Preferably, the additional amount of the lithium fluoride is the 0~10% of total weight, the addition of the metal oxide Amount is no more than the 50% of all elements total mole number in molar ratio.
Preferably, the metal oxide includes yttrium oxide, lutetium oxide, ytterbium oxide, dysprosium oxide, niobium At least one of oxide, magnesium oxide and aluminum oxide.
Preferably, in the mechanical milling process, be using zirconia ball as abrading-ball, with dehydrated alcohol, acetone or go from Sub- water is medium, and rotational speed of ball-mill is not less than 400rpm, and Ball-milling Time is no less than 12h.
Preferably, further include the steps that for mixed-powder being granulated in step S2, specifically:
Binder solution is added in three times in the mixed-powder, 100~500 meshes are crossed after grinding, obtain pellet；
The pellet is compacted, arranges after gluing, grinds at 500 DEG C, it is spare.
Preferably, the pressure for being compacted use is 10MPa.
Preferably, the power of the laser is 50~1200W.
Realization principle of the invention are as follows:
Since raw material has catalytic activity appropriate, laser transfers energy to raw material, is catalyzed and is reacted by cascade reaction Process chemically reacts, thus sintered sample.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the present invention is catalyzed sintered zirconia base transparent ceramic using laser, is absorbed and is swashed using the sintering activity of material itself Light input energy, catalytic reaction process are sintered synthetic sample in the case where swashing light-catalysed high-heat environment, and not only sintered sample causes It is close, transmissivity is high, and preparation method is simple, time saving, material-saving, cleanliness without any pollution, also can large-scale industrial production；
2, the transparency of material of the invention is high, it is seen that light area transmissivity is ceramics in itself up to 80%, is had very Anticorrosive wear-resisting, the exhausted thermal property of good ceramic material.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention, Objects and advantages will become more apparent upon:
Fig. 1 is the preparation flow schematic diagram that laser catalysis of the invention is sintered transparent stealthy ceramic material；
Fig. 2 is the transparent stealthy ceramic material LiF/Yb that in the present invention prepared by embodiment 22Zr2O7X-ray diffractogram；
Fig. 3 is the transparent stealthy ceramic material Yb that in the present invention prepared by embodiment 32Zr2O7EDX energy spectrum analysis；
Fig. 4 is the transparent stealthy ceramic material LiF/Yb that in the present invention prepared by embodiment 42Zr2O7Type crystalline ceramics bulk sample Product.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
Embodiment 1
By raw material ZrO2Powder, mass fraction account for 5% LiF and Yb2O3Powder mixes, wherein Yb and Zr elemental mole ratios For 1:1, raw material is put into zirconia ball grinding jar and carries out ball milling, and using ethyl alcohol as ball milling medium, revolving speed 400rpm, Ball-milling Time 24 is small When, partial size is granulated mixture after ball milling between 500nm-1 μm to obtain microscopic particles size more after high-energy ball milling The product small, consistency is high, granulation process are as follows: using PVA organic plastic as binder solute, being with deionized water Solvent, the binder that configuration quality score is 8%, is divided to two to being added in uniformly mixed powder three times, carries out grinding 5 hours, Sieving, sieve mesh number is 500 mesh, and by the compacting after sieving, it is 10 hours viscous to carry out 500 DEG C of rows, to remove bubble removing, after natural cooling Regrinding is uniform.Powder after grinding is formed using hydraulic press, then the static pressure such as use are compacted at 100MPa, the retention time 3min, release are placed in copper crucible, select semiconductor laser, and optical maser wavelength 980nm, laser power 500W carry out laser Catalysis is sintered, sintering time 3min, obtains LiF/Yb after natural cooling2Zr2O7Type transparent ceramic material, the material is in visible light The transparency with higher within the scope of area 400-700nm.Fig. 1 is the schematic diagram of laser catalysis sintering transparent ceramics.
Embodiment 2
By raw material ZrO2Powder, mass fraction account for 0.5% LiF and Yb2O3Powder mixes, wherein Yb and Zr element mole Than for 1:1, raw material is put into zirconia ball grinding jar and carries out ball milling, using ethyl alcohol as ball milling medium, revolving speed 400rpm, Ball-milling Time 24 is small When, partial size is granulated mixture after ball milling between 500nm-1 μm to obtain microscopic particles size more after high-energy ball milling The product small, consistency is high, granulation process are as follows: using PVA organic plastic as binder solute, being with deionized water Solvent, the binder that configuration quality score is 8%, is divided to two to being added in uniformly mixed powder three times, carries out grinding 5 hours, Sieving, sieve mesh number is 500 mesh, and by the compacting after sieving, it is 12 hours viscous to carry out 500 DEG C of rows, to remove bubble removing, after natural cooling Regrinding is uniform.Powder after grinding is formed using hydraulic press, is compacted at 150MPa in static pressure such as uses, the retention time 5min, release are placed in copper crucible, select semiconductor laser, and optical maser wavelength 980nm, laser power 400W carry out laser Catalysis is sintered, sintering time 5min, obtains LiF/Yb after natural cooling2Zr2O7Type transparent ceramic material.The material is in visible light Transmissivity within the scope of area 400-700nm is up to 85%.Fig. 2 is laser catalysis sintering transparent ceramics LiF/Yb2Zr2O7X-ray Diffraction pattern, since LiF content is less, main diffraction peak Yb2Zr2O7Diffraction maximum.
Embodiment 3
By raw material nano ZrO2Powder and nanometer Yb2O3Powder mixing, wherein Yb and Zr elemental mole ratios are 1:1, and raw material is put Enter zirconia ball grinding jar and carries out ball milling, using acetone as ball milling medium, revolving speed 400rpm, Ball-milling Time 12 hours, through high-energy ball milling Partial size is between 50-200nm afterwards, is granulated that microscopic particles are smaller, consistency is high to obtain to mixture after ball milling Product, granulation process is as follows: using PVA organic plastic as binder solute, using deionized water as solvent, configuration quality The binder that score is 7%, is divided to two to being added in uniformly mixed powder three times, carries out grinding 3 hours, sieving, after sieving Compacting, carry out 500 DEG C of rows viscous 12 hours, to remove bubble removing, regrind after natural cooling uniform.Powder after grinding is adopted It is formed with hydraulic press 15MPa, retention time 3s, release is placed in copper crucible, selects semiconductor laser, optical maser wavelength 980nm, laser power 200W carry out laser catalysis and are sintered, sintering time 3min, obtain Yb after natural cooling2Zr2O7Type is transparent Ceramic material, the visible region transmissivity of material is up to 80%.Fig. 3 is laser catalysis sintering transparent ceramics Yb2Zr2O7EDX energy Spectrum analysis.
Embodiment 4
By raw material ZrO2Powder, mass fraction account for 9% LiF and Yb2O3Powder mixes, wherein Yb and Zr elemental mole ratios For 1:1, raw material is put into zirconia ball grinding jar and carries out ball milling, and using ethyl alcohol as ball milling medium, revolving speed 400rpm, Ball-milling Time 24 is small When, partial size is granulated mixture after ball milling between 500nm-1 μm to obtain microscopic particles size more after high-energy ball milling The product small, consistency is high, granulation process are as follows: using PVA organic plastic as binder solute, being with deionized water Solvent, the binder that configuration quality score is 8%, is divided to two to being added in uniformly mixed powder three times, carries out grinding 5 hours, Sieving, sieve mesh number is 500 mesh, and by the compacting after sieving, it is 12 hours viscous to carry out 500 DEG C of rows, to remove bubble removing, after natural cooling Regrinding is uniform.Powder after grinding is formed using hydraulic press, then the static pressure such as use are compacted at 300MPa, the retention time 10min, release are placed in copper crucible, select semiconductor laser, and optical maser wavelength 980nm, laser power 600W carry out laser Catalysis is sintered, sintering time 8min, obtains LiF/Yb after natural cooling2Zr2O7Type transparent ceramic material, the material is in visible light Transmissivity with higher within the scope of area 400-700nm can be used as function up to 80% or more in visual stealth technology Coating uses.Fig. 4 laser is catalyzed sintering transparent ceramics LiF/Yb2Zr2O7Type crystalline ceramics bulk sample.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring substantive content of the invention.

Claims (8)

1. a kind of preparation method of transparent stealth material, which comprises the steps of:
S1, lithium fluoride and metal oxide are added in zirconium dioxide, are milled to average grain diameter no more than 1 μm, are mixed Powder；
S2, the mixed-powder is compacted, reaction-sintered is carried out under the irradiation of laser, obtain the transparent stealth material.
2. the preparation method of transparent stealth material as described in claim 1, which is characterized in that the partial size of the mixed-powder is 10nm~1 μm.
3. the preparation method of transparent stealth material as described in claim 1, which is characterized in that the additional amount of the lithium fluoride is The 0~10% of total weight, the additional amount of the metal oxide are no more than the 50% of all elements total mole number in molar ratio.
4. the preparation method of transparent stealth material as claimed in claim 1 or 3, which is characterized in that the metal oxide packet Include at least one in yttrium oxide, lutetium oxide, ytterbium oxide, dysprosium oxide, niobium oxide, magnesium oxide and aluminum oxide Kind.
5. the preparation method of transparent stealth material as described in claim 1, which is characterized in that in the mechanical milling process, be with Zirconia ball is abrading-ball, and using dehydrated alcohol, acetone or deionized water as medium, rotational speed of ball-mill is not less than 400rpm, Ball-milling Time No less than 12h.
6. the preparation method of transparent stealth material as described in claim 1, which is characterized in that further include that will mix in step S2 The step of granulating powders, specifically:
Binder solution is added in three times in the mixed-powder, 100~500 meshes are crossed after grinding, obtain pellet；
The pellet is compacted, arranges after gluing, grinds at 500 DEG C, it is spare.
7. the preparation method of transparent stealth material as described in claim 1, which is characterized in that the pressure for being compacted use for 10MPa。
8. the preparation method of transparent stealth material as described in claim 1, which is characterized in that the power of the laser is 50~ 1200W。
CN201910696756.7A 2019-07-30 2019-07-30 A kind of preparation method of transparent stealth material Pending CN110372384A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201910696756.7A CN110372384A (en) 2019-07-30 2019-07-30 A kind of preparation method of transparent stealth material
US16/892,581 US11465911B2 (en) 2019-07-30 2020-06-04 Method for preparing ceramic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910696756.7A CN110372384A (en) 2019-07-30 2019-07-30 A kind of preparation method of transparent stealth material

Publications (1)

Publication Number Publication Date
CN110372384A true CN110372384A (en) 2019-10-25

Family

ID=68257158

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910696756.7A Pending CN110372384A (en) 2019-07-30 2019-07-30 A kind of preparation method of transparent stealth material

Country Status (1)

Country Link
CN (1) CN110372384A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4421671A (en) * 1982-06-18 1983-12-20 General Electric Company Rare-earth-doped yttria-gadolinia ceramic scintillators
CN103113106A (en) * 2013-01-25 2013-05-22 福建福晶科技股份有限公司 Preparation method of pyrochlore-type A2B2O7 transparent ceramics
CN103708839A (en) * 2012-10-03 2014-04-09 信越化学工业株式会社 Method of manufacturing transparent sesquioxide sintered body, and transparent sesquioxide sintered body manufactured by the method
CN105236980A (en) * 2015-11-19 2016-01-13 中国工程物理研究院化工材料研究所 ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic
CN109851377A (en) * 2019-03-18 2019-06-07 广东朗研科技有限公司 A kind of induced with laser high temperature solid state reaction generation A2B2O7The method of type heat barrier coat material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4421671A (en) * 1982-06-18 1983-12-20 General Electric Company Rare-earth-doped yttria-gadolinia ceramic scintillators
CN103708839A (en) * 2012-10-03 2014-04-09 信越化学工业株式会社 Method of manufacturing transparent sesquioxide sintered body, and transparent sesquioxide sintered body manufactured by the method
CN103113106A (en) * 2013-01-25 2013-05-22 福建福晶科技股份有限公司 Preparation method of pyrochlore-type A2B2O7 transparent ceramics
CN105236980A (en) * 2015-11-19 2016-01-13 中国工程物理研究院化工材料研究所 ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic
CN109851377A (en) * 2019-03-18 2019-06-07 广东朗研科技有限公司 A kind of induced with laser high temperature solid state reaction generation A2B2O7The method of type heat barrier coat material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
夏征农等主编: "《大辞海 第37卷 材料科学卷》", 31 December 2015, 上海辞书出版社 *

Similar Documents

Publication Publication Date Title
CN105130438B (en) A kind of method that boron carbide ceramics composite is prepared based on reaction-sintered
CN107117616A (en) A kind of method that utilization ternary MAX material prepares stratiform MXenes materials
KR101622569B1 (en) Nuclear fuel composite pellets and its fabrication method
CN104529457B (en) Pressureless sintering boron carbide ceramics preparation method based on coarse granule powder
CN103030396A (en) Boron carbide silicon carbide composite ceramic and preparation method thereof
CN109851377B (en) Laser-induced high-temperature solid-phase reaction for generating A2B2O7Method for forming thermal barrier coating material
CN102503538A (en) Continuously pore-forming silicon carbide ceramic material and preparation method for same
CN109592982A (en) A kind of boron carbide neutrons in nuclei absorbing material and preparation method
CN110204309A (en) One kind composite diphase material of cordierite-mullite containing zirconium and preparation method thereof
CN101570438B (en) Method for preparing superfine boron carbide powder
CN112142477A (en) Nano lignin-silicon nitride based ceramic and preparation method thereof
CN101894594B (en) Sub-stoichiometric UO2-xPreparation process of annular core block
CN110256092A (en) A kind of heat barrier coat material and preparation method thereof
CN104944432B (en) A kind of ultra-fine richness10B titanium diboride powders and preparation method thereof
CN108585848A (en) A kind of KSr2Nb5O15The preparation method of transparent ferroelectric ceramics
CN105185424A (en) Nuclear reactor core neutron absorbing material terbium titanate pellet and preparation method thereof
CN109592981B (en) Porous rare earth titanate heat insulation material and preparation method and application thereof
CN101789271A (en) Neutron absorption ball
US20220306543A1 (en) Method for preparing boron carbide material
CN110372384A (en) A kind of preparation method of transparent stealth material
CN114195486B (en) One-step method for preparing MgO-Nd 2 Zr 2 O 7 Method for forming multiphase ceramic inert fuel base material
CN102432295A (en) Ceramic substrate neutron absorption ball and preparation method thereof
CN115433007A (en) Solar spectrum wide-frequency absorption material and preparation method thereof
KR101574224B1 (en) oxide nuclear fuel pellet and the method for manufacturing thereof
CN103708419B (en) Method for preparing of high-activity LiH microspheres through wet 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