CN105948751A - Neodymium-doped strontium fluoride laser transparent ceramic and preparation method thereof - Google Patents

Neodymium-doped strontium fluoride laser transparent ceramic and preparation method thereof Download PDF

Info

Publication number
CN105948751A
CN105948751A CN201610250499.0A CN201610250499A CN105948751A CN 105948751 A CN105948751 A CN 105948751A CN 201610250499 A CN201610250499 A CN 201610250499A CN 105948751 A CN105948751 A CN 105948751A
Authority
CN
China
Prior art keywords
srf
transparent ceramic
neodymium
laser transparent
butyl 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
Application number
CN201610250499.0A
Other languages
Chinese (zh)
Other versions
CN105948751B (en
Inventor
宋京红
房亚华
梅炳初
朱春辉
张紫微
周志伟
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.)
Wuhan University of Technology WUT
Original Assignee
Wuhan University of Technology WUT
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 Wuhan University of Technology WUT filed Critical Wuhan University of Technology WUT
Priority to CN201610250499.0A priority Critical patent/CN105948751B/en
Publication of CN105948751A publication Critical patent/CN105948751A/en
Application granted granted Critical
Publication of CN105948751B publication Critical patent/CN105948751B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/553—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on fluorides
    • 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
    • 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
    • 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
    • C04B35/645—Pressure 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
    • C04B2235/02—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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • 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)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Luminescent Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a neodymium-doped strontium fluoride laser transparent ceramic. According to the invention, neodymium ions and a strontium fluoride matrix undergo a chemical reaction to form a displacement solid solution, and hot-pressing sintering, post-treatment and other operations are carried out so as to obtain the laser transparent ceramic with a density approximate to 99.8%. A preparation method for the laser transparent ceramic comprises the following steps: preparing Nd<3+>: SrF2 nanometer powder by using an azeotropic distillation process and then carrying out azeotropic distillation with n-butanol as an entrainer to maximally remove moisture in gel, wherein obtained powder is not prone to agglomeration, has uniform particle size distribution, and has a grain size of 15 to 30 nm; and preparing the laser transparent ceramic by using vacuum hot-pressing sintering technology with LiF as a sintering aid. The prepared laser transparent ceramic has maximum transmittance of 85.83% in visible and near-infrared wave bands and has strong absorption peaks at 576 nm, 735 nm and 796 nm. The preparation method is simple, suitable for large-scale production and low in cost; and the prepared laser transparent ceramic has good optical homogeneity.

Description

Neodymium doping strontium fluoride laser transparent ceramic and preparation method thereof
Technical field
The invention belongs to advanced light function crystalline ceramics research field, be specifically related to a kind of neodymium doping strontium fluoride laser transparent ceramic and Its preparation method.
Background technology
Since nineteen sixty Maiman develops first ruby solid state laser (list of references Maiman T H.Optical and Microwave-optical experiments in ruby.Phys.Rev.Lett., 1960,4 (11): 564-566), Solid State Laser technology is swift and violent Development.In all of solid laser material, the combination property of YAG crystal is optimum.There are some difficult yet with laser crystal With the shortcoming overcome, material supply section scholar is exploring novel solid laser material always.1964, Hatch (list of references Hatch S E,Parsons W F,Weagley R J.Hot pressed polycrystalline CaF2:Dy2+laser.Appl.Phys. Lett., 1964,5 (8): 153-154) with DyF3And CaF3Powder body is raw material, is ground into particle size 150um after melting in a vacuum Powder body, then use vacuum hot pressing sintering technique be prepared for Dy3+:CaF2Crystalline ceramics.Sample passes through annealing process, to eliminate Thermal stress, then makes Dy under the x-ray irradiation of 0.25Mev3+It is reduced into Dy2+.Under Liquid Nitrogen Cooling Condition, use xenon Lamp pumping Dy3+:CaF2Crystalline ceramics realizes laser output, and laser threshold is 24.6J (similar to monocrystalline), and this is in history first Individual solid ceramic laser instrument.
In the developing history of laser ceramics, oxide series laser pottery is always the object of most study, the most excellent laser Performance is also that the yttrium-aluminium-garnet (YAG) from oxide is upper to be produced.First block of oxide laser ceramics is American scholar Nd prepared by Greskovic3+: Y2O3-Th2O3(10%) pottery (sees document Greskovich C, Chernoch J P.Polycrystalline Ceramic Lasers [J] .Journal of Applied Physics, 1973,44 (10): 4599-4606.).Except Oxide laser ceramics, the also fluoride laser pottery of most study, Russia Basiev research group Yb3+Doping CaF2-SrF2Pottery (sees document Basiev T T, Doroshenko M E, Fedorov P P, et al.Efficient Laser Based on CaF2-SrF2-YbF3Nanoceramics[J].Optics Letters,2008,33(5):521-523.)。
The atom of rare earth element has abundant electron energy level, there is 4f track in electronic configuration, creates for multiple energy level transition Condition, is widely used in optical, electrical, magnetic field.Neodymium ion (Nd3+) have the most excellent relative to other rare earth ions Point: 1. can produce laser in nearly hundred kinds of different substrates, including crystal, glass, pottery, liquid.2. belong to four-level system, And there is the metastable energy level of a high-quantum efficiency.3., from visible near infrared region, there is a lot of bar absorption band, can ensure that Effective pumping.4. some absorption bands effectively can couple with the transmitting band of GaAs-GaAlAs laser instrument, therefore Nd3+It is well suited for In the photonics based on GaAs or device.Sr Yu Ca is same family element in the periodic table of elements, with SrF2 Nd is prepared for substrate3+: SrF2Laser ceramics is extremely important.
Summary of the invention
It is an object of the invention to provide a kind of neodymium doping strontium fluoride laser transparent ceramic and preparation method thereof, pottery prepared by the method Consistency high, transmitance high.
For achieving the above object, the technical solution used in the present invention is: a kind of neodymium doping strontium fluoride laser transparent ceramic, its feature It is that it is by Nd3+:SrF2Wet gel, n-butyl alcohol and sintering aid are prepared from, and use n-butyl alcohol to carry out azeotropic steaming as entrainer Evaporate and make Nd3+:SrF2Water in wet gel is removed, and temperature continues to be increased to the boiling point of n-butyl alcohol, by remaining entrainer n-butyl alcohol Steam, be dried, grind, obtain Nd3+:SrF2Nano-powder；Then with LiF as sintering aid, Nd3+:SrF2Nano-powder is adopted With vacuum heating-press sintering, obtain neodymium doping strontium fluoride laser transparent ceramic.
Described Nd3+:SrF2Wet gel is by comprising Sr (NO3)2·4H2O、Nd(NO3)3·6H2O and KF 2H2O is prepared from.
The preparation method of a kind of neodymium doping strontium fluoride laser transparent ceramic, it is characterised in that comprise the following steps:
1) Sr (NO is pressed3)2·4H2O、Nd(NO3)3·6H2O、KF·2H2The proportioning of O is 0.0398mol-0.1194mol:0.0020 Mol-0.0063mol:0.0520mol-0.175mol, chooses Sr (NO3)2·4H2O、Nd(NO3)3·6H2O and KF 2H2O；
By Sr (NO3)2·4H2O and Nd (NO3)3·6H2O magnetic stirring apparatus soluble in water is stirred being configured to cation mixing Liquid；By KF 2H2O magnetic stirring apparatus soluble in water is stirred being configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr2+And Nd3+Cationic solution in, after having titrated, use Magnetic stirrer, then stands products therefrom；
3) by step 2) products therefrom carries out ultrasonic waves for cleaning, is centrifugally separating to obtain Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 60%～70% of wet gel quality, by step 3) gained Nd3+:SrF2 Wet gel adds n-butyl alcohol, and is sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when being increased to the boiling point of n-butyl alcohol, refluxes at this temperature, the most whole azeotropic process Terminate, obtain colloid；
6) by step 5) colloid after distillation is placed in baking oven and is dried, and obtains the powder body loosened, then through grinding, the most available Nd3+:SrF2Nano-powder；
7) with LiF as sintering aid, weigh step 6) in Nd3+:SrF2Nano-powder loads in graphite jig, is placed on after compacting Vacuum hotpressing stove is sintered；
8) by step 7) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, obtains neodymium doping strontium fluoride laser transparent ceramic.
In such scheme, step 1) described in Sr in cation mixed liquor2+、Nd3+Molar concentration be 0.25～10mol/L. F in anion solutions-Molar concentration be 0.5～20mol/L.Doping Nd3+For 1%mol～10%mol.
In such scheme, step 2) in, rate of titration is 50～200ml/min, and the standing products therefrom time is 3～12h.
In such scheme, step 3) in after centrifuge carries out separating three times, there is lamination, gained white in gained wet gel Wet gel be pure SrF on upper strata2, red wet gel is Nd in lower floor3+:SrF2, the wet gel of white is removed, leaves redness Wet gel.
In such scheme, step 5) in the temperature of system when being increased to the boiling point 117 DEG C of n-butyl alcohol, reflux 30min at this temperature, In azeotropic process, can Continuous Observation azeotropic temperature and removing moisture volume, when suspension temperature rises to azeotropic system During boiling point, the moisture in gel is removed so that the form of azeotropic mixture is carried over, after in colloid, hydrone is substantially completely removed, and body The temperature of system continues to be increased to the boiling point of n-butyl alcohol, is steamed by remaining entrainer n-butyl alcohol, uses conventional drying mode by residual Remaining entrainer n-butyl alcohol removes.
In such scheme, step 5) in, azeotropic distillation method uses Organic Alcohol (n-butyl alcohol) to process front axle shell as entrainer Body, forms azeotropic mixture by the moisture of alcohol with precursor powder surface and makes moisture be removed, the most significantly weaken chemistry between granule The formation of key, the gathering between suppression granule, thus prevent the formation of hard aggregation in dry run.
In such scheme, step 7) in, it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, Weigh the Nd of 2g3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder Pour in the graphite jig that internal diameter is 16mm.
In such scheme, step 7) in, vacuum hotpressing stove is sintered for: be warming up to 400 DEG C-800 DEG C for the first time, insulation Time is 60 minutes, then is warming up to 620 DEG C-1000 DEG C, and temperature retention time is 30-40 minute, lowers the temperature as furnace cooling.
In such scheme, step 7) in vacuum hotpressing stove used be the KZG-113 type vacuum hotpressing stove that Shanghai occasion honor produces, its The key technical indexes is: rated temperature 2000 DEG C, maximum pressure 20T, vacuum is 6.67 × 10-3Under Pa, the maximum speed that heats up Rate is 50 DEG C/min, and calandria is graphite material.
In such scheme, step 8) in sample first polish on coarse sandpaper, the fineness of sand paper is more and more higher, it is ensured that the table of sample Face cut is more and more tiny, on sand paper while polishing, it should be noted that ensure that each position of sample is condition of equivalent thickness；When being polished to After certain thickness, using the aluminium oxide nano powder of different fineness to be polished on buffing machine, the fineness of aluminium oxide is first equally Big rear little, polishing 30 minutes every time.
First the present invention prepares Nd with azeotropic distillation method3+: SrF2Nano-powder, this method is made relative to the most conventional sedimentation method Standby powder dispersity is good, and crystal habit is good, even particle size distribution, and fluorescent emission intensity strengthens.Then use LiF as burning Knot auxiliary agent hot pressing and sintering technique prepares laser transparent ceramic, and gained sample optical homogeneity is good.
The present invention compared with prior art has the advantage that
1) present invention prepares nano-powder initially with azeotropic distillation method, carries out dehydrate with micro Nano material, and n-butyl alcohol replaces After the water of wet gel, it is possible not only to reduce the capillary force in dry run, stops the formation of hydrogen bond between granule in removing process, The butoxy of the esterified formation of particle surface simultaneously also can produce space steric effect, to a certain extent close between suppression micelle, All these effects can effectively eliminate the formation of gel particle chemical bond, stops intergranular hard aggregation in dry run.
2) use LiF as sintering aid, the transmitance of sintering activity and laser transparent ceramic can be significantly improved.Easily prepare The laser transparent ceramic of large scale, and shape is easily controlled.Ceramic material sintering process is simple, and manufacturing cycle is a couple of days, is suitable for Large-scale production, cost is relatively low.Owing to not limited by the effect of segregation, it is possible to achieve high-concentration dopant, optical homogeneity is good.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 gained neodymium doping strontium fluoride laser transparent ceramic.It can be seen that root According to Scherrer formula L=k λ/β cos θ, K is Scherrer constant, and its value is 0.89, and β is integration halfwidth degree, in the process calculated In, radian (rad) need to be converted into, θ is the angle of diffraction, and λ is X-ray wavelength, and its value is 0.154056nm, can obtain crystal grain chi Very little for 53.40nm, lattice paprmeter is 4.903nm.
Fig. 2 is the schematic diagram of the embodiment of the present invention 1 gained neodymium doping strontium fluoride laser transparent ceramic.It can be seen that thoroughly Cross sample it is clear that following word, a diameter of 16mm of sample, present the color that redness is the rare earth ion neodymium of doping.
Fig. 3 is the transmitance of the embodiment of the present invention 1 gained neodymium doping strontium fluoride laser transparent ceramic.It can be seen that swash The transmitance of light crystalline ceramics is higher, at the maximum transmission of visible ray, near infrared band more than 80%, 576nm, 735nm, Having stronger absworption peak at 796nm, optical homogeneity is good.
Fig. 4 is the absorption spectrum of the embodiment of the present invention 1 gained neodymium doping strontium fluoride laser transparent ceramic.It can be seen that Spectrum occurs in that the absworption peak being centrally located at 352nm, 521nm, 576nm, 735nm, 796nm and 865nm, and these are inhaled Receive peak and belong to the characteristic absorption peak of trivalent Nd ion, correspond respectively to Nd ion from ground state4I9/2To excited state4D1/2+4D3/2+4G5/2+2I11/2、4G7/2+4G9/2+2K13/2、4G5/2+2G7/2、4F7/2+4S3/2、4F5/2+2H9/2With4F3/2Transition.
Fig. 5 is the photoluminescence intensity of the embodiment of the present invention 1 gained neodymium doping strontium fluoride laser transparent ceramic.Can from figure Go out, the fluorescence spectrum excited under the wavelength of 796nm, spectrum have three launch band 850-950nm, 1000-1150nm, 1300-1400nm, correspond to respectively4F3/2→4I9/2,4F3/2→4I11/2,4F3/2→4I13/2Transition.
As can be seen from Figure 3: the optical homogeneity of pottery prepared by the present invention is good.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but the present invention not only office It is limited to the following examples.
Embodiment is with the Sr (NO of purity >=99.0%3)2·4H2O, purity >=99.9%Nd (NO3)3·6H2O purity >=99.0%KF ·2H2O, n-butyl alcohol is raw material, with LiF as sintering aid, uses vacuum hotpressing stove to be sintered.
Embodiment 1
A kind of neodymium strontium doping calcium fluoride laser ceramics, its preparation method comprises the steps:
1) 0.0796molSr (NO is weighed3)2·4H2O、0.0042molNd(NO3)3·6H2O is dissolved in 80ml water and stirring with magnetic force Mix device to be stirred being configured to cation mixed liquor；Weigh 0.175molKF 2H2O is dissolved in 100ml water entering with magnetic stirring apparatus Row stirring is configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr with 90ml/min speed2+And Nd3+Cationic solution in, After having titrated, by magnetic stirrer 30 minutes so that it is fully react, there is layering after standing 7 hours in products therefrom Phenomenon, (red wet gel is Nd in lower floor to sink to bottom3+:SrF2, it is i.e. required product, following example are identical)；
3) by step 2) products therefrom carry out ultrasonic waves for cleaning, with TG16-WS table model high speed centrifuge at 11000r/min bar Centrifugation under part (15min, 4 times) obtains Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 60% of wet gel quality, by step 3) gained Nd3+:SrF2Wet gel Middle addition n-butyl alcohol, and be sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in 250ml there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when rising to 92 DEG C, water-n-butyl alcohol azeotropic, the moisture in colloidal sol by n-butyl alcohol with azeotropic The form of thing is taken out of and is removed.When the temperature of system continues the boiling point 117 DEG C rising to n-butyl alcohol, the moisture of colloid is taken off completely Removing, backflow 30min is to steam unnecessary n-butyl alcohol at this temperature, and the most whole azeotropic process terminates；
6) by step 5) distillation after colloid be placed in air dry oven at 120 DEG C of dry 12h, obtain the powder body loosened, then Nd is i.e. can get through grinding3+:SrF2Nano-powder；
7) it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs about 2g's Nd3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder is poured internal diameter into and is In the graphite jig of 16mm；Use LiF to be sintered as sintering aid vacuum hotpressing stove, be warming up to 400 DEG C for the first time, Temperature retention time is 60 minutes, then is warming up to 620 DEG C, and temperature retention time is 40 minutes, lowers the temperature as furnace cooling.
8) by step 8) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, the most i.e. can get neodymium doping strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doping strontium fluoride laser transparent ceramic sample is polished on sand paper in various degree thick, thin successively, The fineness of sand paper is more and more higher, it is ensured that the surface scratch of sample is more and more tiny, after being polished to certain thickness, on buffing machine The aluminium oxide nano powder using different fineness is polished, and i.e. can get Nd3+:SrF2Laser transparent ceramic, records its consistency > 99.8%, transmitance > 85% (i.e. consistency is high, transmitance high), optic communication, medical treatment, lidar light detection and ranging and Up-conversion luminescence field has potential using value.
Embodiment 2
A kind of neodymium strontium doping calcium fluoride laser ceramics, its preparation method comprises the steps:
1) 0.0637molSr (NO is weighed3)2·4H2O、0.0033molNd(NO3)3·6H2O is dissolved in 80ml water and stirring with magnetic force Mix device to be stirred being configured to cation mixed liquor；Weigh 0.0764molKF 2H2O is dissolved in 100ml water and uses magnetic stirring apparatus It is stirred being configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr with 80ml/min speed2+And Nd3+Cationic solution in, After having titrated, by magnetic stirrer 30 minutes so that it is fully react, there is layering after standing 6 hours in products therefrom Phenomenon, sinks to bottom；
3) by step 2) products therefrom carry out ultrasonic waves for cleaning, with TG16-WS table model high speed centrifuge at 11000r/min bar Centrifugation under part (15min, 4 times) obtains Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 63% of wet gel quality, by step 3) gained Nd3+:SrF2Wet gel Middle addition n-butyl alcohol, and be sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in 250ml there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when rising to 92 DEG C, water-n-butyl alcohol azeotropic, the moisture in colloidal sol by n-butyl alcohol with azeotropic The form of thing is taken out of and is removed.When the temperature of system continues the boiling point 117 DEG C rising to n-butyl alcohol, the moisture of colloid is taken off completely Removing, backflow 30min is to steam unnecessary n-butyl alcohol at this temperature, and the most whole azeotropic process terminates；
6) by step 5) distillation after colloid be placed in air dry oven at 120 DEG C of dry 12h, obtain the powder body loosened, then Nd is i.e. can get through grinding3+:SrF2Nano-powder；
7) it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs about 2g's Nd3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder is poured internal diameter into and is In the graphite jig of 16mm；Using LiF is that sintering aid is sintered in vacuum hotpressing stove, is warming up to 500 DEG C for the first time, Temperature retention time is 60 minutes, then is warming up to 700 DEG C, and temperature retention time is 40 minutes, lowers the temperature as furnace cooling.
8) by step 6) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, the most i.e. can get neodymium doping strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doping strontium fluoride laser transparent ceramic sample is polished on sand paper in various degree thick, thin successively, The fineness of sand paper is more and more higher, it is ensured that the surface scratch of sample is more and more tiny, after being polished to certain thickness, on buffing machine The aluminium oxide nano powder using different fineness is polished, and i.e. can get Nd3+:SrF2Laser transparent ceramic, records its consistency > 99.8%, light transmittance > 85% (i.e. consistency is high, transmitance high), optic communication, medical treatment, lidar light detection and ranging and Up-conversion luminescence field has potential using value.
Embodiment 3
A kind of neodymium doping strontium fluoride laser transparent ceramic, its preparation method comprises the steps:
1) 0.0398molSr (NO is weighed3)2·4H2O、0.0020molNd(NO3)3·6H2O is dissolved in 80ml water and stirring with magnetic force Mix device to be stirred being configured to cation mixed liquor；Weigh 0.0520molKF 2H2O is dissolved in 100ml water and uses magnetic stirring apparatus It is stirred being configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr with 70ml/min speed2+、Nd3+Cationic solution in, After having titrated, by magnetic stirrer 30 minutes so that it is fully react, there is layering after standing 5 hours in products therefrom Phenomenon, sinks to bottom；
3) by step 2) products therefrom carry out ultrasonic waves for cleaning, with TG16-WS table model high speed centrifuge at 11000r/min bar Centrifugation under part (15min, 4 times) obtains Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 65% of wet gel quality, by step 3) gained Nd3+:SrF2Wet gel Middle addition n-butyl alcohol, and be sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in 250ml there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when rising to 92 DEG C, water-n-butyl alcohol azeotropic, the moisture in colloidal sol by n-butyl alcohol with azeotropic The form of thing is taken out of and is removed.When the temperature of system continues the boiling point 117 DEG C rising to n-butyl alcohol, the moisture of colloid is taken off completely Removing, backflow 30min is to steam unnecessary n-butyl alcohol at this temperature, and the most whole azeotropic process terminates；
6) by step 5) distillation after colloid be placed in air dry oven at 120 DEG C of dry 12h, obtain the powder body loosened, then Nd is i.e. can get through grinding3+:SrF2Nano-powder；
7) it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs about 2g's Nd3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder is poured internal diameter into and is In the graphite jig of 16mm；Using LiF is that sintering aid is sintered in vacuum hotpressing stove, is warming up to 600 DEG C for the first time, Temperature retention time is 60 minutes, then is warming up to 800 DEG C, and temperature retention time is 30 minutes, lowers the temperature as furnace cooling.
8) by step 7) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, the most i.e. can get neodymium doping strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doping strontium fluoride laser transparent ceramic sample is polished on sand paper in various degree thick, thin successively, The fineness of sand paper is more and more higher, it is ensured that the surface scratch of sample is more and more tiny, after being polished to certain thickness, on buffing machine The aluminium oxide nano powder using different fineness is polished, and i.e. can get Nd3+:SrF2Laser transparent ceramic, records its consistency > 99.7%, light transmittance > 80% (i.e. consistency is high, transmitance high), optic communication, medical treatment, lidar light detection and ranging and Up-conversion luminescence field has potential using value.
Embodiment 4
A kind of neodymium doping strontium fluoride laser transparent ceramic, its preparation method comprises the steps:
1) 0.1035molSr (NO is weighed3)2·4H2O、0.0054molNd(NO3)3·6H2O is dissolved in 80ml water and stirring with magnetic force Mix device to be stirred being configured to cation mixed liquor；Weigh 0.1242molKF 2H2O is dissolved in 100ml water and uses magnetic stirring apparatus It is stirred being configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr with 100ml/min speed2+、Nd3+Cationic solution in, After having titrated, by magnetic stirrer 30 minutes so that it is fully react, there is layering after standing 4 hours in products therefrom Phenomenon, sinks to bottom；
3) by step 2) products therefrom carry out ultrasonic waves for cleaning, with TG16-WS table model high speed centrifuge at 11000r/min bar Centrifugation under part (15min, 4 times) obtains Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 67% of wet gel quality, by step 3) gained Nd3+:SrF2Wet gel Middle addition n-butyl alcohol, and be sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in 250ml there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when rising to 92 DEG C, water-n-butyl alcohol azeotropic, the moisture in colloidal sol by n-butyl alcohol with azeotropic The form of thing is taken out of and is removed.When the temperature of system continues the boiling point 117 DEG C rising to n-butyl alcohol, the moisture of colloid is taken off completely Removing, backflow 30min is to steam unnecessary n-butyl alcohol at this temperature, and the most whole azeotropic process terminates；
6) by step 5) distillation after colloid be placed in air dry oven at 120 DEG C of dry 12h, obtain the powder body loosened, then Nd is i.e. can get through grinding3+:SrF2Nano-powder；
7) it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs about 2g's Nd3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder is poured internal diameter into and is In the graphite jig of 16mm；Using LiF is that sintering aid is sintered in vacuum hotpressing stove, is warming up to 700 DEG C for the first time, Temperature retention time is 60 minutes, then is warming up to 900 DEG C, and temperature retention time is 40 minutes, lowers the temperature as furnace cooling.
8) by step 7) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Neodymium doping strontium fluoride laser transparent ceramic is i.e. can get after twin polishing, example.
This enforcement gained neodymium doping strontium fluoride laser transparent ceramic sample is polished on sand paper in various degree thick, thin successively, sand The fineness of paper is more and more higher, it is ensured that the surface scratch of sample is more and more tiny, after being polished to certain thickness, adopts on buffing machine It is polished with the aluminium oxide nano powder of different fineness, i.e. can get Nd3+:SrF2Laser transparent ceramic, records its consistency > 99.7%, light transmittance > 75% (i.e. consistency is high, transmitance high), optic communication, medical treatment, lidar light detection and ranging and Up-conversion luminescence field has potential using value.
Embodiment 5
A kind of neodymium strontium doping calcium fluoride laser ceramics, its preparation method comprises the steps:
1) 0.1194molSr (NO is weighed3)2·4H2O、0.0063molNd(NO3)3·6H2O is dissolved in 80ml water and uses magnetic agitation Device is stirred being configured to cation mixed liquor；Weigh 0.1431molKF 2H2O is dissolved in 100ml water entering with magnetic stirring apparatus Row stirring is configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr with 110ml/min speed2+、Nd3+Cationic solution in, After having titrated, by magnetic stirrer 30 minutes so that it is fully react, there is layering after standing 3 hours in products therefrom Phenomenon, sinks to bottom；
3) by step 2) products therefrom carry out ultrasonic waves for cleaning, with TG16-WS table model high speed centrifuge at 11000r/min bar Centrifugation under part (15min, 4 times) obtains Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 70% of wet gel quality, by step 3) gained Nd3+:SrF2Wet gel Middle addition n-butyl alcohol, and be sufficiently mixed under strength mechanical agitation, mixed suspension is transferred in 250ml there-necked flask Carry out oil bath heating；
5) when step 4) temperature of system is when rising to 92 DEG C, water-n-butyl alcohol azeotropic, the moisture in colloidal sol by n-butyl alcohol with azeotropic The form of thing is taken out of and is removed.When the temperature of system continues the boiling point 117 DEG C rising to n-butyl alcohol, the moisture of colloid is taken off completely Removing, backflow 30min is to steam unnecessary n-butyl alcohol at this temperature, and the most whole azeotropic process terminates；
6) by step 5) distillation after colloid be placed in air dry oven at 120 DEG C of dry 12h, obtain the powder body loosened, then Nd is i.e. can get through grinding3+:SrF2Nano-powder；
7) it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs about 2g's Nd3+:SrF2Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, gained powder is poured internal diameter into and is In the graphite jig of 16mm；Use LiF to be sintered in vacuum hotpressing stove as sintering aid, be warming up to 800 for the first time DEG C, temperature retention time is 60 minutes, then is warming up to 1000 DEG C, and temperature retention time is 40 minutes, lowers the temperature as furnace cooling.
8) by step 7) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, the most i.e. can get neodymium doping strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doping strontium fluoride laser transparent ceramic sample is polished on sand paper in various degree thick, thin successively, The fineness of sand paper is more and more higher, it is ensured that the surface scratch of sample is more and more tiny, after being polished to certain thickness, on buffing machine The aluminium oxide nano powder using different fineness is polished, and i.e. can get Nd3+:SrF2Laser transparent ceramic, records its consistency > 99.65%, light transmittance > 75% (i.e. consistency is high, transmitance high), optic communication, medical treatment, lidar light detection and ranging and Up-conversion luminescence field has potential using value.

Claims (10)

1. a neodymium doping strontium fluoride laser transparent ceramic, it is characterised in that it is by Nd3+:SrF2Wet gel, n-butyl alcohol and sintering Auxiliary agent is prepared from, and uses n-butyl alcohol to carry out azeotropic distillation as entrainer and makes Nd3+:SrF2Water in wet gel is removed, temperature Continue to be increased to the boiling point of n-butyl alcohol, remaining entrainer n-butyl alcohol is steamed, be dried, grind, obtain Nd3+:SrF2Nano powder Body；Then with LiF as sintering aid, Nd3+:SrF2Nano-powder uses vacuum heating-press sintering, obtains neodymium doping strontium fluoride laser Crystalline ceramics.
A kind of neodymium doping strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that described Nd3+:SrF2 Wet gel is by comprising Sr (NO3)2·4H2O、Nd(NO3)3·6H2O and KF 2H2O is prepared from.
A kind of neodymium the most as claimed in claim 1 doping strontium fluoride laser transparent ceramic preparation method, it is characterised in that include with Lower step:
1) Sr (NO is pressed3)2·4H2O、Nd(NO3)3·6H2O、KF·2H2The proportioning of O is 0.0398mol-0.1194mol:0.0020 Mol-0.0063mol:0.0520mol-0.175mol, chooses Sr (NO3)2·4H2O、Nd(NO3)3·6H2O and KF 2H2O；
By Sr (NO3)2·4H2O and Nd (NO3)3·6H2O magnetic stirring apparatus soluble in water is stirred being configured to cation mixing Liquid；By KF 2H2O magnetic stirring apparatus soluble in water is stirred being configured to anion solutions；
2) will be dissolved with F-Anion solutions dropwise instill dissolved with Sr2+And Nd3+Cationic solution in, after having titrated, use Magnetic stirrer, then stands products therefrom；
3) by step 2) products therefrom carries out ultrasonic waves for cleaning, is centrifugally separating to obtain Nd3+:SrF2Wet gel；
4) it is Nd by the addition of n-butyl alcohol3+:SrF2The 60%～70% of wet gel quality, by step 3) gained Nd3+:SrF2 Wet gel adds n-butyl alcohol, and mixes under strength mechanical agitation, transfer to mixed suspension there-necked flask is carried out Oil bath is heated；
5) when step 4) temperature of system is when being increased to the boiling point of n-butyl alcohol, refluxes at this temperature, the most whole azeotropic process Terminate, obtain colloid；
6) by step 5) colloid after distillation is placed in baking oven and is dried, obtain the powder body loosened, then through grinding, obtain Nd3+:SrF2 Nano-powder；
7) with LiF as sintering aid, weigh step 6) in Nd3+:SrF2Nano-powder loads in graphite jig, is placed on after compacting Vacuum hotpressing stove is sintered；
8) by step 7) sample after sintering takes out, the most respectively with thick, fine sandpaper mill, then on precise grinding polisher Twin polishing, obtains neodymium doping strontium fluoride laser transparent ceramic.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 1) Sr in cation mixed liquor described in2+、Nd3+Molar concentration be 0.25～10mol/L.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 1) F in anion solutions described in-Molar concentration be 0.5～20mol/L.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 1) step 2 described in) in, rate of titration is 50～200ml/min, and the standing products therefrom time is 3～12h.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 1) step 3 described in) in after centrifuge carries out separating three times, there is lamination in gained wet gel, gained white wet solidifying Glue is pure SrF on upper strata2, red wet gel is Nd in lower floor3+:SrF2, the wet gel of white is removed, leaves the wet solidifying of redness Glue.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 1) step 5 described in) in the temperature of system when being increased to the boiling point 117 DEG C of n-butyl alcohol, reflux 30min at this temperature, In azeotropic process, can Continuous Observation azeotropic temperature and removing moisture volume, when suspension temperature rises to azeotropic system During boiling point, the moisture in gel is removed so that the form of azeotropic mixture is carried over, after in colloid, hydrone is substantially completely removed, and body The temperature of system continues to be increased to the boiling point of n-butyl alcohol, is steamed by remaining entrainer n-butyl alcohol, uses conventional drying mode by residual Remaining entrainer n-butyl alcohol removes.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 7), in, it is Nd by the addition of sintering aid LiF3+:SrF2The 0.5%～5% of nano-powder quality, weighs the Nd of 2g3+:SrF2 Nano-powder and sintering aid LiF wet mixing two hours in ethanol, in 80 DEG C of drying, it is 16mm's that gained powder pours internal diameter into In graphite jig.
The preparation method of a kind of neodymium the most according to claim 3 doping strontium fluoride laser transparent ceramic, it is characterised in that step Rapid 7) in, vacuum hotpressing stove is sintered for: being for the first time warming up to 400 DEG C-800 DEG C, temperature retention time is 60 minutes, then Being warming up to 620 DEG C-1000 DEG C, temperature retention time is 30-40 minute, lowers the temperature as furnace cooling.
CN201610250499.0A 2016-04-21 2016-04-21 Neodymium adulterates strontium fluoride laser transparent ceramic and preparation method thereof Expired - Fee Related CN105948751B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610250499.0A CN105948751B (en) 2016-04-21 2016-04-21 Neodymium adulterates strontium fluoride laser transparent ceramic and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610250499.0A CN105948751B (en) 2016-04-21 2016-04-21 Neodymium adulterates strontium fluoride laser transparent ceramic and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105948751A true CN105948751A (en) 2016-09-21
CN105948751B CN105948751B (en) 2018-11-13

Family

ID=56917826

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610250499.0A Expired - Fee Related CN105948751B (en) 2016-04-21 2016-04-21 Neodymium adulterates strontium fluoride laser transparent ceramic and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105948751B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109279895A (en) * 2018-10-12 2019-01-29 信阳师范学院 The method of fluorite mineral polycrystalline transparent ceramic is prepared under a kind of cryogenic conditions
CN111362699A (en) * 2020-05-07 2020-07-03 信阳师范学院 Preparation method of composite-structure strontium fluoride optical material
CN116553931A (en) * 2022-01-29 2023-08-08 广西科技大学 Preparation method for improving easy cracking of rare earth doped strontium fluoride transparent ceramic

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102126857A (en) * 2011-01-31 2011-07-20 武汉理工大学 Method for preparing transparent calcium fluoride ceramic
CN102674843A (en) * 2012-04-28 2012-09-19 武汉理工大学 Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof
US20120275479A1 (en) * 2010-05-18 2012-11-01 Lawrence Livermore National Security, Llc Method and System For Modulation Of Gain Suppression In High Average Power Laser Systems

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120275479A1 (en) * 2010-05-18 2012-11-01 Lawrence Livermore National Security, Llc Method and System For Modulation Of Gain Suppression In High Average Power Laser Systems
CN102126857A (en) * 2011-01-31 2011-07-20 武汉理工大学 Method for preparing transparent calcium fluoride ceramic
CN102674843A (en) * 2012-04-28 2012-09-19 武汉理工大学 Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
GANG LU ET AL.: "Fabrication and properties of highly transparent Nd-doped CaF2 ceramics", 《MATERIALS LETTERS》 *
T.T.BASIEV ET AL.: "First ceramic laser in the visible spectral range", 《OPTICAL MATERIALS EXPRESS》 *
T.T.BASIEV ET AL.: "SrF2:Nd3 laser fluoride ceramics", 《OPTICS LETTERS》 *
云利娜等: "共沸蒸馏脱水技术在纳米材料制备中的应用", 《河南化工》 *
智广林: "Er:CaF2激光陶瓷的制备与性能研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109279895A (en) * 2018-10-12 2019-01-29 信阳师范学院 The method of fluorite mineral polycrystalline transparent ceramic is prepared under a kind of cryogenic conditions
CN111362699A (en) * 2020-05-07 2020-07-03 信阳师范学院 Preparation method of composite-structure strontium fluoride optical material
CN116553931A (en) * 2022-01-29 2023-08-08 广西科技大学 Preparation method for improving easy cracking of rare earth doped strontium fluoride transparent ceramic

Also Published As

Publication number Publication date
CN105948751B (en) 2018-11-13

Similar Documents

Publication Publication Date Title
CN100360469C (en) Dual mixed yttrium aluminium garnet transparent ceramic material and it preparation process
CN100564310C (en) The yttrium aluminum garnet transparent ceramic material and the preparation method of codope
Chen et al. Lanthanide activator doped NaYb 1− x Gd x F 4 nanocrystals with tunable down-, up-conversion luminescence and paramagnetic properties
JP6911811B2 (en) Manufacturing method of transparent ceramics for Faraday rotator
CN102126857B (en) Method for preparing transparent calcium fluoride ceramic
Yu et al. Fabrication of Nd: YAG transparent ceramics using powders synthesized by citrate sol-gel method
CN105378542B (en) Magneto-optic memory technique and its manufacture method and magnetic-optic devices
CN108998030B (en) Composite material with energy transfer effect and preparation method and application thereof
CN101224974A (en) Yttrium-aluminium series small crystal transparent ceramic material and preparation method
CN105948751A (en) Neodymium-doped strontium fluoride laser transparent ceramic and preparation method thereof
CN104031647B (en) A kind of preparation method of round pie europium doping vanadic acid lanthanum red fluorescence powder
JP6821813B2 (en) Nitride light emitting material and light emitting device containing it
CN102515548B (en) Surface-plasma-enhanced optical wavelength converting glass ceramic adopting silver nanoparticles and preparation method thereof
WO2019169868A1 (en) Fluorescent ceramic and preparation method therefor
CN112299861B (en) AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic
JP2011099040A (en) METHOD OF PRODUCING beta SIALON PHOSPHOR
CN106536449A (en) Transparent metal fluoride ceramic
CN101898787A (en) Method for synthesizing submicron cerium oxide by using liquid cerium chloride as raw material
Yu et al. A strategy to prepare highly redispersible and strongly luminescent α-NaYF 4: Eu 3+ hybrid nanostructures with multi-channel excitation
Syu et al. Microemulsion‐Mediated Synthesis and Characterization of YBO 3: Ce 3+ Phosphors
CN104046356A (en) Preparation method of YAG:Ce&lt;3+&gt; yellow fluorescent powder with granularity of 13-15 microns
CN107686345A (en) A kind of preparation method of Ce doping YAG luminescent ceramics
Zhang et al. The effect of Y3+ doping upon Nd: S-FAP transparent ceramics for effective spectral performance improvement
CN103539359B (en) Rare-earth-doped fluoride micro-nano crystalline substance-fluorine phosphorous glass matrix material and preparation method thereof
CN102211942A (en) Preparation method of Er: YAG polycrystal transparent ceramic 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
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20181113

Termination date: 20190421