CN106800410A - A kind of yttria-base laser ceramics of Yb sensitizations and preparation method thereof - Google Patents

A kind of yttria-base laser ceramics of Yb sensitizations and preparation method thereof Download PDF

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CN106800410A
CN106800410A CN201710024864.0A CN201710024864A CN106800410A CN 106800410 A CN106800410 A CN 106800410A CN 201710024864 A CN201710024864 A CN 201710024864A CN 106800410 A CN106800410 A CN 106800410A
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nitrate
compound
oxide
acetic acid
yttria
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王焕平
田颖
杨清华
徐时清
雷若姗
邓德刚
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China Jiliang University
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Abstract

The yttria-base laser ceramics of Yb sensitizations disclosed by the invention, its crystal grain has core shell structure, and stratum nucleare is (Y, Yb, M)2O3Phase, shell are (Y, N)2O3Phase, wherein M are rare earth luminous ion, N is sintering aid.Preparation process is as follows：The compound of the compound of yttrium, the compound of ytterbium and M is mixed first, is calcined (Y, Yb, M)2O3Powder, then the compound of yttrium is mixed with the compound of N, calcine (Y, N)2O3Powder, then mixes above two powder；Or (Y, Yb, M) is directly added into after the compound of yttrium is mixed with the compound of N2O3Powder mixing, calcining；Mixed powder isostatic pressing, the vacuum-sintering that will be obtained, cool down after annealing.The present invention is using sintering character excellent (Y, N)2O3Thin layer is to (Y, Yb, M)2O3Mutually coated, distortion of lattice can be reduced on the basis of ceramic post sintering performance is improved, so as to obtain excellent laser activity.

Description

A kind of yttria-base laser ceramics of Yb sensitizations and preparation method thereof
Technical field
The present invention relates to a kind of yttria-base laser ceramics and preparation method thereof, especially the yttria-base laser of Yb sensitizations Ceramics and preparation method thereof, belong to materials science field.
Background technology
Yittrium oxide is cubic system crystal, with excellent light transmission, and with fusing point is high, chemistry and photochemistry is steady Qualitative good, thermal conductivity is high, optical transparence wide ranges (0.23~8.0 μm) the advantages of, particularly in region of ultra-red, with 80% Theoretical transmission above；Its phonon energy is low, easily realizes the doping vario-property of rare earth ion, can suppress without spoke to a certain extent Transition is penetrated, the probability of radiation transistion is improved, is as the important base of solid laser medium material so as to improve luminous quantum efficiency Material.
Y2O3Melt temperature be up to 2430 DEG C, a polycrystalline phase transformation for opposite hexagonal phase is also occurred that cube at 2280 DEG C, because This is difficult to grow Y using traditional czochralski method2O3Monocrystalline.Using traditional ceramics technique, can be far below Y2O3At a temperature of fusing point Crystalline ceramics is prepared, production cost, improve production efficiency is saved, it is often more important that ceramic preparation technology easily realizes active ions It is highly doped, can greatly improve laser output power so that refractory oxide be used as optical medium and laser medium It is possibly realized.The sintering temperature of yttrium oxide transparent ceramic is general more than 2000 DEG C, is prepared using vacuum-sintering and nano-powder After technology, sintering temperature drops to 1700 DEG C, lower than its melt temperature 700 DEG C.Ceramic material is polycrystal, its crystal boundary, stomata The scattering loss that can all increase light with the imperfection of lattice etc. causes the opacity of material, for Y2O3Base transparent ceramic Research discovery, La3+And Zr4+Doping can be effectively improved Y2O3The sintering character of base transparent ceramic, improves Y2O3The densification of base ceramics Degree, so as to improve its transmitance.
Rear-earth-doped Y2O3The laser activity of base transparent ceramic has been widely studied, and it is dense that such as Lu prepares doping It is the Nd of 1.5 at% to spend:Y2O3Crystalline ceramics, the LD with 807 nm is pumping source, under the pump power of 742 mW, is obtained The laser output of 160 mW.Akira first reported the Yb of diode pumping:Y2O3Femtosecond ceramic laser, is absorbing 2.6 W Draw power when, obtain the laser output of centre wavelength 1076.5 nm, the mW of mean power 420.Kong utilizes Yb:Y2O3Pottery Porcelain laser, realizes the laser output of the nm of wavelength 1078, the W of peak power 4.2.Further to improve Y2O3The burning of crystalline ceramics Knot performance and luminescent properties, the red seminars of Shanghai University Yang Qiu are with La2O3It is sintering aid, using low-temperature sintering method in nothing The good yttrium lanthanum oxide laser ceramic of the transparency is prepared under pressure reducing atmosphere, the La of addition is found2O3Effectively improve Y2O3Thoroughly The sintering character of bright ceramics, and with good laser spectrum performance.US military laboratory reports in Er first3+:Y2O3 2.71 μm of mid-infrared laser output is obtained in crystalline ceramics, at room temperature the mW of peak power output 380.
Although yttria-base laser ceramics has obtained extensive research report, from the point of view of current present Research both at home and abroad, When doping concentration of rare earth ion is relatively low, lasing efficiency is relatively low；Although in theory can be rare earth ion doped dense by increasing Degree come improving laser performance, but correlative study show laser ceramics with the raising of rear-earth-doped concentration occur scattering increase, The problems such as beam quality factor is reduced.Because the directionality of laser is extremely strong, any small refraction can all cause light to reflect and draw Play error and loss.Therefore, Y is being kept2O3On the premise of the good chemistry and photochemistry performance of base transparent ceramic, it is to avoid it goes out Now big distortion of lattice, reduction scattering loss, is Y while keeping good sintering character2O3Base laser ceramics more extensively should Key.
The content of the invention
Yttria-base laser ceramics it is an object of the invention to provide a kind of Yb sensitizations and preparation method thereof, makes yttria-base The crystal grain of laser ceramics has core shell structure, and stratum nucleare solid solution enters the rare earth ion of Yb sensitizations, and shell solid solution enters sintering aid, so that On the basis of distortion of lattice is reduced, beneficial to the sintering character and laser activity that improve yttria-base laser ceramics.
The yttria-base laser ceramics of Yb sensitizations of the invention, it is characterised in that the crystal grain of ceramics has core shell structure, core Layer is (Y1-x-yYbxMy)2O3Phase, shell are (Y1-zNz)2O3Phase, wherein 0.01≤x≤0.1,0.005≤y≤0.1, 0.05≤z≤0.2, M is one or two in rare earth luminous ion Tm, Ho, Dy, Er, Pr and Nd, and N is sintering aid One or more in La, Zr, Ti, Mn, Al, Ca, Zn and Mg, shell material is 0.01~0.2 with the mol ratio of stratum nucleare material: 1。
The preparation method of the yttria-base laser ceramics of Yb sensitizations of the present invention, there is following two schemes：
Scheme 1：
The method for preparing the yttria-base laser ceramics of Yb sensitizations, comprises the steps：
(1) compound of the compound of yttrium, the compound of ytterbium and M element is weighed by the amount of stratum nucleare material, and is put into deionized water In be well mixed, then with zirconia ball for mill be situated between, ball milling mixing 4~24 hours, dry after again 1250~1550 DEG C calcine 2~8 hours, obtain Yb and enter Y with M solid solutions2O3In (Y, Yb, M)2O3Phase powder；
(2) weigh the compound of yttrium and the compound of N element by the amount of shell material, and be put into deionized water and be well mixed, It is subsequently adding (Y, Yb, the M) of step (1) synthesis2O3Phase powder, ball milling mixing 4~24 hours, is then sprayed mixture Dry, remove deionized water；
(3) powder obtained after spray drying is put into mould, in the forming under the pressure of 10~40 MPa, is then warmed up to 1050~1250 DEG C are incubated 1~4 hour, are placed into after cooling in isostatic pressing machine, and isostatic pressed is carried out under 180~300 MPa；
(4) product after isostatic pressed is put in a vacuum furnace, 4~24 hours is incubated at 1550~1750 DEG C, exist again after cooling Annealed 2~8 hours in 900~1500 DEG C of air, obtain the yttria-base laser ceramics of Yb sensitizations.
In this programme, the compound of described yttrium is one or more in yittrium oxide, yttrium nitrate and acetic acid yttrium；Described The compound of ytterbium is one or more in ytterbium oxide, ytterbium nitrate and acetic acid ytterbium；The compound of described M element be thulium oxide, Thulium nitrate, acetic acid thulium, holimium oxide, holmium nitrate, acetic acid holmium, dysprosia, dysprosium nitrate, acetic acid dysprosium, erbium oxide, erbium nitrate, acetic acid erbium, One or two in praseodymium oxide, praseodymium nitrate, praseodymium acetate, neodymia, neodymium nitrate and acetic acid neodymium；The compound of described N element For lanthanum nitrate, lanthanum acetate, zirconium nitrate, acetic acid zirconium, butyl titanate, Titanium Nitrate, manganese nitrate, manganese acetate, aluminum nitrate, aluminum acetate, One or more in calcium nitrate, calcium acetate, zinc nitrate, zinc acetate, magnesium nitrate and magnesium acetate.
Scheme 2：
The method for preparing the yttria-base laser ceramics of Yb sensitizations, comprises the steps：
(1) compound of the compound of yttrium, the compound of ytterbium and M element is weighed by the amount of stratum nucleare material, and is put into deionized water In be well mixed, then with zirconia ball for mill be situated between, ball milling mixing 4~24 hours, dry after again 1250~1550 DEG C calcine 2~8 hours, obtain Yb and enter Y with M solid solutions2O3In (Y, Yb, M)2O3Phase powder；
(2) weigh the compound of yttrium and the compound of N element by the amount of shell material, and be put into deionized water and be well mixed, Then it is situated between by mill of zirconia ball, ball milling mixing 4~24 hours is calcined 1~4 hour at 1050~1250 DEG C again after drying, and is obtained Obtain N solid solutions and enter Y2O3In (Y, N)2O3Phase powder；
(3) powder that above-mentioned steps (1) are prepared with step (2) is mixed, is put into ball grinder, be mill with zirconia ball It is situated between, ball milling mixing 4~24 hours obtains mixed powder；
(4) it is compressing after above-mentioned mixed powder is dried, by the isostatic cool pressing of 180~300 MPa, then it is placed on vacuum drying oven In, 4~24 hours are incubated at 1550~1750 DEG C, annealed 2~8 hours in 900~1500 DEG C of air again after cooling, obtain To the yttria-base laser ceramics of Yb sensitizations.
In this programme, the compound of described yttrium is one or more in yittrium oxide, yttrium nitrate and acetic acid yttrium；Described The compound of ytterbium is one or more in ytterbium oxide, ytterbium nitrate and acetic acid ytterbium；The compound of described M element be thulium oxide, Thulium nitrate, acetic acid thulium, holimium oxide, holmium nitrate, acetic acid holmium, dysprosia, dysprosium nitrate, acetic acid dysprosium, erbium oxide, erbium nitrate, acetic acid erbium, One or two in praseodymium oxide, praseodymium nitrate, praseodymium acetate, neodymia, neodymium nitrate and acetic acid neodymium；The compound of described N element For lanthana, lanthanum nitrate, lanthanum acetate, zirconium oxide, zirconium nitrate, acetic acid zirconium, titanium oxide, butyl titanate, Titanium Nitrate, manganese oxide, Manganese nitrate, manganese acetate, aluminum oxide, aluminum nitrate, aluminum acetate, calcium oxide, calcium nitrate, calcium acetate, zinc oxide, zinc nitrate, zinc acetate, One or more in magnesia, magnesium nitrate and magnesium acetate.
The invention has the advantages that：The compound of the compound of yttrium, the compound of ytterbium and M first is carried out into ball milling to mix Close, then in 1250~1550 DEG C of calcinings, you can obtain Yb and enter Y with M solid solutions2O3In (Y, Yb, M)2O3Phase powder, because Yb is Sensitizer, M are rare earth luminous ions（One or two in Tm, Ho, Dy, Er, Pr and Nd）, the structure has good luminous Performance；Then the compound of yttrium and the compound of N are coated on (Y, Yb, M)2O3Around phase powder, or by the compound of yttrium (Y, N) is obtained with the compound ball milling mixing of N and by 1050~1250 DEG C of calcinings2O3After powder, then with (Y, Yb, M)2O3Phase Powder mixes, because N is sintering aid ion（One or more in La, Zr, Ti, Mn, Al, Ca, Zn, Mg）, therefore (Y, N)2O3 Mutually there is good sintering activity；(Y,Yb,M)2O3The synthesis temperature of powder is 1250~1550 DEG C, (Y, N)2O3The conjunction of powder It it is 1050~1250 DEG C into temperature, due to the difference of synthesis temperature so that (Y, N)2O3Diameter of particle is than (Y, Yb, M)2O3Powder Body particle diameter is tiny much, when both powders are mixed, by both ratio of control, can obtain it is tiny (Y, N)2O3Powder is enclosed in thick (Y, Yb, M)2O3Circumgranular structure, shaping with sintering after can obtain stratum nucleare for (Y, Yb,M)2O3Phase, shell are (Y, N)2O3The yttria-base ceramics of phase.With (Y, Yb, M)2O3It is stratum nucleare, (Y, N)2O3It is the knot of shell Structure, realize sensitized ions/light emitting ionic and sintering aid ion separates doping, thereby reduces distortion of lattice, improves The laser activity of ceramics, simultaneously because (Y, the N) of sintering aid doping2O3Mutually there is good sintering character, ceramics are effectively improved Consistency and light transmission, so that yttria-base of the invention ceramics have good laser activity.The present invention prepares work Skill is simply controllable.
Specific embodiment
With reference to example, the invention will be further described.
Embodiment 1：(Y0.84Yb0.08Tm0.04Ho0.04)2O3-0.01(Y0.95La0.05)2O3（X=0.08, y=0.08, z= 0.05, M=Tm, Ho, N=La）
The yttrium nitrate of 0.84 mol, the ytterbium nitrate of 0.08 mol, the thulium nitrate of 0.04 mol, the holmium nitrate of 0.04 mol is weighed to put Enter in deionized water and be well mixed, be then situated between by mill of zirconia ball, ball milling mixing 4 hours is calcined at 1550 DEG C again after drying 2 hours, obtain (Y, Yb, Tm, Ho)2O3Phase powder.The yttrium nitrate of 0.0095 mol, the lanthanum nitrate of 0.0005 mol is weighed to be put into It is well mixed in deionized water, is subsequently adding (Y, Yb, Tm, the Ho) of above-mentioned synthesis2O3Phase powder, ball milling mixing 4 hours, then Mixture is spray-dried, deionized water is removed.The powder obtained after spray drying is put into mould, 10 MPa's Forming under the pressure, is then warmed up to 1050 DEG C and is incubated 4 hours, is placed into after cooling in isostatic pressing machine, is carried out under 300 MPa Isostatic pressed；Product after isostatic pressed is put in a vacuum furnace, 4 hours is incubated at 1750 DEG C, again in 1500 DEG C of sky after cooling Annealed 2 hours in gas, that is, obtain the yttria-base laser ceramics of Yb sensitizations of the invention.
Embodiment 2：(Y0.985Yb0.01Dy0.005)2O3-0.2(Y0.88La0.09Zr0.03)2O3（X=0.01, y=0.005, z= 0.12, M=Dy, N=La, Zr）
Weigh yittrium oxide, the yttrium nitrate of 0.085 mol, the ytterbium nitrate of 0.01 mol, the acetic acid dysprosium of 0.005 mol of 0.45 mol It is put into deionized water and is well mixed, is then situated between by mill of zirconia ball, ball milling mixing 24 hours, again at 1250 DEG C after drying Calcining 8 hours, obtains (Y, Yb, Dy)2O3Phase powder.Weigh yttrium nitrate, the lanthanum nitrate of 0.018 mol, 0.006 of 0.176 mol The zirconium nitrate of mol is well mixed in being put into deionized water, is then situated between by mill of zirconia ball, ball milling mixing 24 hours, after drying Calcined 1 hour at 1050 DEG C again, obtained (Y, La, Zr)2O3Phase powder.By (Y, Yb, the Dy) of above-mentioned preparation2O3Phase powder with (Y,La,Zr)2O3Phase powder is mixed, and is put into ball grinder, is situated between by mill of zirconia ball, and ball milling mixing 24 hours is mixed Close powder；Will above-mentioned mixed powder dry after it is compressing, by the isostatic cool pressing of 180 MPa, then put in a vacuum furnace, 1550 DEG C are incubated 24 hours, are annealed 8 hours in 900 DEG C of air again after cooling, that is, obtain the oxygen of Yb sensitizations of the invention Change yttrium base laser ceramics.
Embodiment 3：(Y0.8Yb0.1Er0.1)2O3-0.1(Y0.8La0.1Ti0.05Al0.05)2O3（X=0.1, y=0.1, z=0.2, M= Er, N=La, Ti, Al）
Weigh the yittrium oxide of 0.25 mol, the yttrium nitrate of 0.15 mol, the acetic acid yttrium of 0.15 mol, the ytterbium nitrate of 0.1 mol, The acetic acid erbium of 0.1 mol is well mixed in being put into deionized water, is then situated between by mill of zirconia ball, and ball milling mixing 12 hours is done Calcined 6 hours at 1500 DEG C again after dry, obtained (Y, Yb, Er)2O3Phase powder.Weigh yttrium nitrate, 0.04 mol of 0.04 mol Acetic acid yttrium, the lanthanum acetate of 0.01 mol, the butyl titanate of 0.005mol, the aluminum nitrate of 0.005mol be put into deionized water It is well mixed, it is subsequently adding (Y, Yb, the Er) of above-mentioned synthesis2O3Phase powder, ball milling mixing 12 hours, is then carried out mixture Spray drying, removes deionized water.The powder obtained after spray drying is put into mould, in the forming under the pressure of 20 MPa, Then 1250 DEG C are warmed up to and are incubated 2 hours, placed into after cooling in isostatic pressing machine, isostatic pressed is carried out under 200 MPa；Will etc. Product after static pressure is put in a vacuum furnace, and 8 hours are incubated at 1650 DEG C, and annealing 5 is small in 1200 DEG C of air again after cooling When, that is, obtain the yttria-base laser ceramics of Yb sensitizations of the invention.
Embodiment 4：(Y0.87Yb0.05Pr0.08)2O3-0.1(Y0.9Zr0.04Mn0.03Ca0.03)2O3（X=0.05, y=0.08, z= 0.1, M=Pr, N=Zr, Mn, Ca）
Weigh yittrium oxide, 0.1 mol yttrium nitrates, 0.17 mol acetic acid yttriums, acetic acid ytterbium, 0.08 of 0.05 mol of 0.3 mol The praseodymium acetate of mol is well mixed in being put into deionized water, is then situated between by mill of zirconia ball, ball milling mixing 10 hours, after drying Calcined 7 hours at 1450 DEG C again, obtained (Y, Yb, Pr)2O3Phase powder.Weigh acetic acid yttrium, the vinegar of 0.004 mol of 0.09 mol Sour zirconium, the manganese acetate of 0.003 mol, the calcium acetate of 0.003 mol are well mixed in being put into deionized water, then with zirconia ball For mill is situated between, ball milling mixing 12 hours is calcined 2 hours at 1150 DEG C again after drying, and is obtained (Y, Zr, Mn, Ca)2O3Phase powder.Will (Y, Yb, the Pr) of above-mentioned preparation2O3Phase powder and (Y, Zr, Mn, Ca)2O3Phase powder is mixed, and is put into ball grinder, with oxygen Change zirconium ball for mill is situated between, ball milling mixing 8 hours obtains mixed powder；It is compressing after above-mentioned mixed powder is dried, by 250 The isostatic cool pressing of MPa, then puts in a vacuum furnace, 12 hours is incubated at 1600 DEG C, after cooling again in 1300 DEG C of air Annealing 3 hours, that is, obtain the yttria-base laser ceramics of Yb sensitizations of the invention.
Embodiment 5：(Y0.88Yb0.08Nd0.04)2O3-0.15(Y0.88La0.1Zn0.01Mg0.01)2O3（X=0.08, y=0.04, z= 0.12, M=Nd, N=La, Zn, Mg）
Weigh during the yttrium nitrate of 0.88 mol, the acetic acid ytterbium of 0.08 mol, the acetic acid neodymium of 0.04 mol are put into deionized water and mix Uniformly, then it is situated between by mill of zirconia ball, ball milling mixing 24 hours is calcined 7 hours at 1350 DEG C again after drying, obtain (Y, Yb,Nd)2O3Phase powder.Weigh the yttrium nitrate of 0.132 mol, the lanthanum nitrate of 0.015 mol, the zinc acetate of 0.0015 mol, The magnesium acetate of 0.0015 mol is well mixed in being put into deionized water, is subsequently adding (Y, Yb, the Nd) of above-mentioned synthesis2O3Phase powder, , then be spray-dried for mixture by ball milling mixing 6 hours, removes deionized water.The powder obtained after spray drying is put Enter in mould, in the forming under the pressure of 15 MPa, be then warmed up to 1100 DEG C and be incubated 3 hours, isostatic pressing machine is placed into after cooling In, isostatic pressed is carried out under 200 MPa；Product after isostatic pressed is put in a vacuum furnace, 20 hours are incubated at 1550 DEG C, it is cold But annealed 3 hours in 1450 DEG C of air again after, that is, obtain the yttria-base laser ceramics of Yb sensitizations of the invention.

Claims (10)

1. the yttria-base laser ceramics that a kind of Yb is sensitized, it is characterised in that the crystal grain of ceramics has core shell structure, and stratum nucleare is (Y1-x-yYbxMy)2O3Phase, shell are (Y1-zNz)2O3Phase, wherein 0.01≤x≤0.1,0.005≤y≤0.1,0.05 ≤ z≤0.2, M is one or two in rare earth luminous ion Tm, Ho, Dy, Er, Pr and Nd, N be sintering aid La, Zr, One or more in Ti, Mn, Al, Ca, Zn and Mg, shell material is 0.01~0.2 with the mol ratio of stratum nucleare material:1.
2. the method for preparing the yttria-base laser ceramics that the Yb described in claim 1 is sensitized, it is characterised in that including following steps Suddenly：
(1) compound of the compound of yttrium, the compound of ytterbium and M element is weighed by the amount of stratum nucleare material, and is put into deionized water In be well mixed, then with zirconia ball for mill be situated between, ball milling mixing 4~24 hours, dry after again 1250~1550 DEG C calcine 2~8 hours, obtain Yb and enter Y with M solid solutions2O3In (Y, Yb, M)2O3Phase powder；
(2) weigh the compound of yttrium and the compound of N element by the amount of shell material, and be put into deionized water and be well mixed, It is subsequently adding (Y, Yb, the M) of step (1) synthesis2O3Phase powder, ball milling mixing 4~24 hours, is then sprayed mixture Dry, remove deionized water；
(3) powder obtained after spray drying is put into mould, in the forming under the pressure of 10~40 MPa, is then warmed up to 1050~1250 DEG C are incubated 1~4 hour, are placed into after cooling in isostatic pressing machine, and isostatic pressed is carried out under 180~300 MPa；
(4) product after isostatic pressed is put in a vacuum furnace, 4~24 hours is incubated at 1550~1750 DEG C, exist again after cooling Annealed 2~8 hours in 900~1500 DEG C of air, obtain the yttria-base laser ceramics of Yb sensitizations.
3. it is according to claim 2 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that it is described The compound of yttrium is one or more in yittrium oxide, yttrium nitrate and acetic acid yttrium.
4. it is according to claim 2 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that it is described The compound of ytterbium is one or more in ytterbium oxide, ytterbium nitrate and acetic acid ytterbium.
5. it is according to claim 2 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that described M The compound of element be thulium oxide, thulium nitrate, acetic acid thulium, holimium oxide, holmium nitrate, acetic acid holmium, dysprosia, dysprosium nitrate, acetic acid dysprosium, One kind or two in erbium oxide, erbium nitrate, acetic acid erbium, praseodymium oxide, praseodymium nitrate, praseodymium acetate, neodymia, neodymium nitrate and acetic acid neodymium Kind.
6. it is according to claim 2 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that described N The compound of element is lanthanum nitrate, lanthanum acetate, zirconium nitrate, acetic acid zirconium, butyl titanate, Titanium Nitrate, manganese nitrate, manganese acetate, nitre One or more in sour aluminium, aluminum acetate, calcium nitrate, calcium acetate, zinc nitrate, zinc acetate, magnesium nitrate and magnesium acetate.
7. the method for preparing the yttria-base laser ceramics that the Yb described in claim 1 is sensitized, it is characterised in that including following steps Suddenly：
(1) compound of the compound of yttrium, the compound of ytterbium and M element is weighed by the amount of stratum nucleare material, and is put into deionized water In be well mixed, then with zirconia ball for mill be situated between, ball milling mixing 4~24 hours, dry after again 1250~1550 DEG C calcine 2~8 hours, obtain Yb and enter Y with M solid solutions2O3In (Y, Yb, M)2O3Phase powder；
(2) weigh the compound of yttrium and the compound of N element by the amount of shell material, and be put into deionized water and be well mixed, Then it is situated between by mill of zirconia ball, ball milling mixing 4~24 hours is calcined 1~4 hour at 1050~1250 DEG C again after drying, and is obtained Obtain N solid solutions and enter Y2O3In (Y, N)2O3Phase powder；
(3) powder that above-mentioned steps (1) are prepared with step (2) is mixed, is put into ball grinder, be mill with zirconia ball It is situated between, ball milling mixing 4~24 hours obtains mixed powder；
(4) it is compressing after above-mentioned mixed powder is dried, by the isostatic cool pressing of 180~300 MPa, then it is placed on vacuum drying oven In, 4~24 hours are incubated at 1550~1750 DEG C, annealed 2~8 hours in 900~1500 DEG C of air again after cooling, obtain To the yttria-base laser ceramics of Yb sensitizations.
8. it is according to claim 7 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that it is described The compound of yttrium is one or more in yittrium oxide, yttrium nitrate and acetic acid yttrium；The compound of described ytterbium is ytterbium oxide, nitric acid One or more in ytterbium and acetic acid ytterbium.
9. it is according to claim 7 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that described M The compound of element be thulium oxide, thulium nitrate, acetic acid thulium, holimium oxide, holmium nitrate, acetic acid holmium, dysprosia, dysprosium nitrate, acetic acid dysprosium, One kind or two in erbium oxide, erbium nitrate, acetic acid erbium, praseodymium oxide, praseodymium nitrate, praseodymium acetate, neodymia, neodymium nitrate and acetic acid neodymium Kind.
10. it is according to claim 7 prepare Yb sensitization yttria-base laser ceramics method, it is characterised in that it is described The compound of N element is lanthana, lanthanum nitrate, lanthanum acetate, zirconium oxide, zirconium nitrate, acetic acid zirconium, titanium oxide, butyl titanate, nitre Sour titanium, manganese oxide, manganese nitrate, manganese acetate, aluminum oxide, aluminum nitrate, aluminum acetate, calcium oxide, calcium nitrate, calcium acetate, zinc oxide, nitre One or more in sour zinc, zinc acetate, magnesia, magnesium nitrate and magnesium acetate.
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