CN104961454A - Transparent hafnium titanic acid lutecium ceramic material and preparing method thereof - Google Patents
Transparent hafnium titanic acid lutecium ceramic material and preparing method thereof Download PDFInfo
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Abstract
The invention relates to a transparent hafnium titanic acid lutecium ceramic material and a preparing method thereof. The chemical composition of the transparent hafnium titanic acid lutecium ceramic material is Lu2Ti2-xHfxO7, wherein 0<x<2, and preferably, 0.6<=x<2. The transparent hafnium titanic acid lutecium ceramic material is high in density, high in transmittance and capable of meeting the application requirements of fields of windows, laser media, high-refractive-index camera lens, scintillant matrixes and the like, and grain is small.
Description
Technical field
The present invention relates to a kind of transparent ceramic material, specifically hafnium metatitanic acid lutetium transparent ceramic material and preparation method thereof, belongs to technical field of ceramic material.
Background technology
Crystalline ceramics has the characteristics such as high temperature resistant, anticorrosive, high insulation, high strength, has the favorable optical performance not available for traditional ceramics simultaneously, has a wide range of applications in fields such as window, light display system and optoelectronic equipments.
Compared with the monocrystalline prepared with high-temperature melting method, crystalline ceramics generally adopts powder densification technology, have preparation temperature relatively low, can high density Uniform Doped ion, can the advantage such as structure composite, suitable batch production.The material of crystalline ceramics technology of preparing to some dystectic materials and some application of special occasions especially has realistic meaning.
Since reported first translucent alumina ceramics in 1962 [U.S.P.3026210], transparent ceramic material all obtains very large development in kind, technology of preparing and application.Prepare Al at present
2o
3, MgAl
2o
4[A.Krell, J.Klimke, T.Hutzler, J.Eur.Ceram.Soc., 2009,29 (2): 275-281] etc. utilize translucidus can crystalline ceramics, YAG:Nd [A.Ikesue, T.Kinoshita, K.Yoshida, J.Am.Ceram.Soc., 1995,78 (4): 1033-1037], (Y, Gd)
2o
3: Eu [U.S.P.4421671] etc. has crystalline ceramics and the PLZT [G.H.Haertling of luminescent properties, C.E.Land, J.Am.Ceram.Soc., 1971,54 (1): 1-10], PZT-PT [U.S.P.6746618] etc. have the crystalline ceramics of control optical property.
Containing rare earth ion hafnium/titanate (RE
2hf
2o
7/ RE
2ti
2o
7) there is defect fluorite structure (spacer Fm3m (225)) or burning rate stone structure (spacer Fd3m (227)), all belong to isometric system, there is the good characteristics such as high-melting-point, lower thermal conductivity, high ray absorption capacity simultaneously, in window, laser medium, high refractive index camera lens, scintillator etc., have good application prospect.At present, have been reported containing rare earth ion hafnium/titanate crystalline ceramics, comprising: La
2hf
2o
7[Y.Ji, D.Jiang, T.Fen, J.Shi, Mater.Res.Bull.2005,40 (3): 553-559.], Y
2hf
2o
7[X.Q.Zou, G.H.Zhou, H.L.Yi, Y.Yang, S.W.Wang, J.Inorg.Mater.2011,26:929-932], LaGdHf
2o
7[H.Yi, X.Zou, Y.Yang, G.Zhou, S.Wang, J.Am.Ceram.Soc., 2011,94:4120-4122], La
xy
2-xhf
2o
7[CN102557625 A], Y
2ti
2o
7and Yb
2ti
2o
7[CN 101343173 B] etc.But the sintering processing that preparation method generally adopts nitrogen atmosphere or vacuum is with no pressure, hot pressing or HIP sintering etc. are conventional, preparation temperature is relatively high, and the cycle is long.
Summary of the invention
For prior art Problems existing, the object of the present invention is to provide and a kind of there is novel transparent stupalith that density is high, crystal grain is little and preparation method thereof, for crystalline ceramics field increases a kind of product innovation, to meet the fields such as window, laser medium, high refractive index camera lens, scintillator to the performance requriements of transparent ceramic material.
At this, on the one hand, the invention provides a kind of hafnium metatitanic acid lutetium transparent ceramic material, the chemical constitution of described hafnium metatitanic acid lutetium transparent ceramic material is Lu
2ti
2-xhf
xo
7, wherein 0<x<2, preferably 0.6≤x<2.
Preferably, described hafnium metatitanic acid lutetium transparent ceramic material is single defective type fluorite phase.
Preferably, described hafnium metatitanic acid lutetium transparent ceramic material is more than 65% when thickness is 1mm to the straight line transmittance of infrared band.
Preferably, the density of described hafnium metatitanic acid lutetium transparent ceramic material is 99.4 ~ 100%, and average grain size is 400nm ~ 2 μm.
Hafnium metatitanic acid lutetium transparent ceramic material density of the present invention is high, crystal grain is little, transmitance is high, can meet the application requiring in the fields such as window, laser medium, high refractive index camera lens, scintillator matrix.
On the other hand, the present invention also provides the preparation method of above-mentioned hafnium metatitanic acid lutetium transparent ceramic material, comprising:
With Lu
2o
3, TiO
2, HfO
2powder is raw material, stoichiometrically proportioning, ball mill mixing, sieve, obtain raw material mixed powder; And
Gained mixed powder is carried out discharge plasma sintering.
The present invention adopts high-purity nm raw material to obtain in conjunction with discharge plasma sintering to have the hafnium metatitanic acid lutetium crystalline ceramics that crystal boundary is clean, crystal grain is little, density is high, and technological process is simple, the cycle is short, energy consumption is low, and Reactive Synthesis once completes with sintering; Phase composite and microstructure controlled, have the advantages that high-strength height is saturating.
Preferably, in described discharge plasma sintering, from room temperature to a certain temperature being less than sintering temperature, pre-add first pressure; From this certain temperature to sintering temperature, apply the second pressure, wherein the first pressure is less than the second pressure.
Preferably, the process system of described discharge plasma sintering is: from room temperature to 1100 DEG C, and precharge pressure is 10MPa ~ 50MPa; From 1100 DEG C to sintering temperature, pressure is 100 ~ 150MPa.
Preferably, be 10 ~ 100 DEG C/min from 1100 DEG C to the temperature rise rate of sintering temperature, sintering temperature is 1400 ~ 1550 DEG C, is incubated 5 ~ 60 minutes at a sintering temperature.
Preferably, the process system of described discharge plasma sintering is:
Heating and cooling system: from room temperature to 600 DEG C, temperature rise rate is 200 DEG C/min; From 600 DEG C to 1100 DEG C, temperature rise rate is 100 DEG C/min; 1100 DEG C of insulations 5 minutes; From 1100 DEG C to sintering temperature, temperature rise rate is 10 ~ 100 DEG C/min; After insulation terminates, pulsed current is set to 0, cools with furnace temperature;
Pressure regime: from room temperature to 1100 DEG C, precharge pressure is 10MPa ~ 50MPa; From 1100 DEG C to sintering temperature, pressure was increased to 100MPa and remains to insulation and terminates in 1 minute; Temperature-fall period, pressure unloaded in 1 minute.
Preferably, after being also included in described discharge plasma sintering, in 650 ~ 1100 DEG C of insulations annealing operation of 3 ~ 10 hours in air or oxygen atmosphere.
Compared with prior art, hafnium metatitanic acid lutetium transparent ceramic material of the present invention not only high, the high effective atomic number of density, and also specific refractory power is high, can meet the application requiring in the fields such as window, laser medium, high refractive index camera lens, scintillator matrix.The present invention adopts discharge plasma sintering mode, and sintering temperature is relatively low, the cycle is short, energy consumption is little, environmental friendliness, and technique is simple, easy handling, controllability are good, is conducive to microtexture and Properties Control.
Accompanying drawing explanation
Fig. 1 is discharge plasma sintering system figure;
Fig. 2 is the X-ray diffractogram of hafnium metatitanic acid lutetium transparent ceramic material in embodiment 1,2 and 3;
Fig. 3 is the transmittance curve in embodiment 1,2 and 3 after the polishing of hafnium metatitanic acid lutetium transparent ceramic material;
Fig. 4 is the micro-structure diagram of hafnium metatitanic acid lutetium transparent ceramic material in embodiment 1,2 and 3;
Fig. 5 is the transmittance curve in embodiment Isosorbide-5-Nitrae and 5 after the polishing of hafnium metatitanic acid lutetium transparent ceramic material;
Fig. 6 is the transmittance curve of hafnium metatitanic acid lutetium stupalith in reference examples 2.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
One aspect of the present invention provides a kind of hafnium metatitanic acid lutetium transparent ceramic material, and its chemical constitution is Lu
2ti
2-xhf
xo
7, wherein 0<x<2, is preferably 0.6≤x<2.
Hafnium metatitanic acid lutetium transparent ceramic material of the present invention is transparent material, particularly has higher straight line transmittance at infrared band, such as, is more than 65% when thickness is 1mm to the straight line transmittance of infrared band.
Hafnium metatitanic acid lutetium transparent ceramic material of the present invention is single defective type fluorite phase, belongs to isometric system.
Hafnium metatitanic acid lutetium transparent ceramic material density of the present invention is high, crystal grain is little.Its density can be 99.4 ~ 100% (see table 1), and average grain size can be 400nm ~ 2 μm (see Fig. 4).
Hafnium metatitanic acid lutetium transparent ceramic material provided by the invention has good application prospect in fields such as window, laser medium, high refractive index camera lens, scintillators.
Hafnium metatitanic acid lutetium transparent ceramic material of the present invention can be prepared by discharge plasma sintering.Such as, with commercial high-purity nm oxide powder for raw material, after mechanical ball milling mixes, adopt discharge plasma sintering, obtain hafnium metatitanic acid lutetium crystalline ceramics.Like this, utilize raw material reaction to carry out with sintering, preparation technology is simple, the cycle is short, without the need to adding sintering aid, can prepare the hafnium metatitanic acid lutetium crystalline ceramics that density is high, crystal grain is little simultaneously.
Key problem in technology of the present invention is that by high purity nanometer powders (such as commercial) be raw material, design composition and ratio, optimization sintering process parameter, control Monte Carlo method, to obtain that density is high, transmitance is high and the transparent ceramic material that crystal grain is little.Technique is simple, reaction with sinter carry out simultaneously, the cycle is short, energy consumption is low, microstructure is controlled.First designing composition and ratio, then mechanical batch mixing, last discharge plasma sintering and annealing, mainly through controlling sintering process parameter, comprising sintering temperature, pressure, temperature rise rate, soaking time etc.
As raw material, high-purity nm Lu can be used
2o
3, TiO
2, HfO
2nano-powder, it can be commercial, also can prepare voluntarily.The purity of each raw material is preferably more than 99.9%.The proportioning of each raw material is according to Lu
2ti
2-xhf
xo
7in stoichiometric ratio.Ball milling method can be adopted to carry out batch mixing, such as, can adopt wet ball grinding or dry ball milling.After ball milling, preferred mistake 200 mesh sieve, obtains the raw material mixed powder with appropriate particle size with this.
In the present invention, discharge plasma sintering can be carried out to the raw material mixed powder obtained.In sintering process, be preferably the pressurization of employing two step.That is, from room temperature to a certain temperature being less than sintering temperature, pre-add first pressure; From this certain temperature to sintering temperature, apply the second pressure, be wherein preferably the first pressure and be less than the second pressure.In one example, from room temperature to 1100 DEG C, precharge pressure is 10MPa ~ 50MPa; From 1100 DEG C to sintering temperature, pressure is 100 ~ 150MPa.In sintering schedule, utilize two step pressuring methods, can be easy to realize the crystalline ceramics preparation that density is high, crystal grain is little at short notice.Sintering temperature can be 1400 ~ 1550 DEG C, can be incubated 5 ~ 60 minutes at a sintering temperature.In addition, can be 10 ~ 100 DEG C/min from 1100 DEG C to the temperature rise rate of sintering temperature.
In sintering process, temperature rise rate also can periodically change.In one example, the temperature rise rate before 1100 DEG C is 100 DEG C/min, from 1100 DEG C to the temperature rise rate of sintering temperature be 10 ~ 100 DEG C/min.In addition, before 1100 DEG C, temperature rise rate also can periodically change, and such as, from room temperature to 600 DEG C, temperature rise rate is 200 DEG C/min; From 600 DEG C to 1100 DEG C, temperature rise rate is 100 DEG C/min.
After having sintered, can also anneal.Annealing can be carried out under containing the atmosphere of oxygen, such as air or oxygen atmosphere.Annealing can be carried out at 650 ~ 1100 DEG C.Annealing time can be 3 ~ 10 hours.
Below, exemplarily, the step of preparation method of the present invention is described.
A. the design of material powder and mixing
Adopt commercial high-purity nm Lu
2o
3, TiO
2, HfO
2nano-powder is raw material.According to Ti/Hf different mol ratio design proportioning, the mol ratio of three presses chemical formula, Lu
2ti
2-xhf
xo
7, wherein 0<x<2, preferably 0.6≤x<2; Carry out material powder to weigh.Add dehydrated alcohol and be made into slurry, utilize mechanical ball grinding machine to carry out batch mixing.Ball milling speed is 150-300 rev/min, and Ball-milling Time is 6-24 hour, dry 6-24 hour at 60-80 DEG C, and sieve 200 orders, obtains raw material mixed powder.
B. plasma discharging rapid reaction sintering
Gained powder is loaded graphite grinding tool, is then placed in discharging plasma sintering equipment, vacuumizes and sinter.In preparation process, need strict Controlling Technology parameter, comprise sintering temperature, pressure size and pressuring method, heat-up rate, soaking time etc.Concrete sintering schedule as shown in Figure 1.Heating and cooling system: from room temperature to 600 DEG C, temperature rise rate (V
f) be 200 DEG C/min; From 600 DEG C to 1100 DEG C, temperature rise rate is 100 DEG C/min; At 1100 DEG C of insulation 5min; From 1100 DEG C to sintering temperature, temperature rise rate is 10-100 DEG C/min; After insulation terminates, pulsed current is set to 0, cools with furnace temperature.Pressure regime: from room temperature to 1100 DEG C, precharge pressure (P
pre) be 10MPa-50MPa; From 1100 DEG C to sintering temperature, pressure is increased to 100MPa and remains to insulation and terminates in 1min; Temperature-fall period, pressure unloads in 1min.Usually, sintering temperature is 1400-1550 DEG C, and soaking time scope is 5-60min.Described sintering temperature and temperature rise rate are regulated automatically by program setting setting pulse size of current.
C. annealing operation
Sample after sintering is incubated 3-10 hour in 650-1100 DEG C in air or oxygen atmosphere.
Owing to adopting discharge plasma sintering, reaction is carried out with sintering simultaneously, and utilize two step pressuring methods in sintering schedule, can be easy to realize the crystalline ceramics preparation that density is high, crystal grain is little at short notice, have good application prospect in fields such as window, laser medium, high refractive index camera lens, scintillators.Preparation method provided by the invention have technique simple, without the need to sintering aid, the advantage such as preparation cycle is short, energy consumption is low, controllability is good, easy handling.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1:
Adopt commercial raw material Lu
2o
3(99.99%), TiO
2(99.9%), HfO
2(99.9%).Three kinds of raw materials are weighed according to mol ratio Lu:Ti:Hf=1:0.5:0.5 and puts into ball grinder with dehydrated alcohol and high-purity zirconia ball for medium ball milling 8h, 60 DEG C of dry 24h, cross 200 mesh sieves and obtain mixing raw materials.Then mixed raw material is put in graphite grinding tool, is then placed in discharging plasma sintering equipment and sinters.Sintering process system is specific as follows: in room temperature to 1100 DEG C, precharge pressure P
prefor 10MPa; From 1100 DEG C to 1450 DEG C, pressure is 100MPa, temperature rise rate V
fbe 10 DEG C/min; Soaking time is 45min.Anneal the sample after sintering at 1050 DEG C 6h, is then polished to 1mm, obtains Lu
2ti
1hf
1o
7crystalline ceramics.
Embodiment 2:
The process of basic repetition embodiment 1.Difference is that the mol ratio of three kinds of raw materials is Lu:Ti:Hf=1:0.7:0.3, prepares Lu
2ti
1.4Hf
0。6o
7crystalline ceramics.
Embodiment 3:
The process of basic repetition embodiment 1.Difference is that the mol ratio of three kinds of raw materials is Lu:Ti:Hf=1:0.1:0.9, prepares Lu
2ti
0.2Hf
1。8o
7crystalline ceramics.
Fig. 2 is the X ray diffracting spectrum of the hafnium metatitanic acid lutetium transparent ceramic material that embodiment 1-3 obtains, and as seen from the figure, along with the increase of Hf content, structure is single defective type fluorite phase;
Fig. 3 is the transmittance curve of the hafnium metatitanic acid lutetium transparent ceramic material that embodiment 1-3 obtains.The obtained thick sample of 1mm is all transparent, particularly has higher straight line transmittance at infrared band;
Fig. 4 is the micro-structure diagram of the hafnium metatitanic acid lutetium transparent ceramic material that embodiment 1-3 obtains.The crystal grain of made sample is all smaller.
Embodiment 4:
Adopt commercial raw material Lu
2o
3(99.99%), TiO
2(99.9%), HfO
2(99.9%).Three kinds of raw materials are weighed according to mol ratio Lu:Ti:Hf=1:0.5:0.5 and puts into ball grinder with dehydrated alcohol and high-purity zirconia ball for medium ball milling 16h, 80 DEG C of dry 12h, cross 200 mesh sieves and obtain mixing raw materials.Then mixed raw material is put in graphite grinding tool, is then placed in discharging plasma sintering equipment and sinters.Sintering process system is specific as follows: in room temperature to 1100 DEG C, precharge pressure P
prefor 50MPa; From 1100 DEG C to 1450 DEG C, pressure is 100MPa, temperature rise rate V
fbe 10 DEG C/min; Soaking time is 45min.Anneal the sample after sintering at 1050 DEG C 6h, is then polished to 1mm, obtains Lu
2ti
1hf
1o
7crystalline ceramics.Obtain Lu
2ti
1hf
1o
7crystalline ceramics.
Embodiment 5:
Adopt commercial raw material Lu
2o
3(99.99%), TiO
2(99.9%), HfO
2(99.9%).Three kinds of raw materials are weighed according to mol ratio Lu:Ti:Hf=1:0.5:0.5 and puts into ball grinder with dehydrated alcohol and high-purity zirconia ball for medium ball milling 24h, 80 DEG C of dry 12h, cross 200 mesh sieves and obtain mixing raw materials.Then mixed raw material is put in graphite grinding tool, is then placed in discharging plasma sintering equipment and sinters.Sintering process system is specific as follows: in room temperature to 1100 DEG C, and precharge pressure is 10MPa; From 1100 DEG C to 1450 DEG C, pressure is 100MPa, temperature rise rate V
fbe 100 DEG C/min; Soaking time is 45min.Anneal the sample after sintering at 1050 DEG C 6h, is then polished to 1mm, obtains Lu
2ti
1hf
1o
7crystalline ceramics.
Fig. 5 is the transmittance curve of the hafnium metatitanic acid lutetium transparent ceramic material that embodiment 1,4 and 5 obtains.The obtained thick sample of 1mm is all transparent, particularly has higher straight line transmittance at infrared band.Illustrate under the sintering schedule of two step pressurizations, regulate precharge pressure little on transmitance impact; Regulate sintering temperature to have a certain impact to transmitance, but infrared transmittivity is all more than 65%.
Comparative examples 1
The process of basic repetition embodiment 1.Difference is that sintering schedule adopts conventional Fast Sintering system: from room temperature to 600 DEG C, temperature rise rate is 200 DEG C/min; From 600 DEG C to sintering temperature 1450 DEG C, temperature rise rate is 100 DEG C/min; Pressure remains on 100MPa always.Gained Lu
2ti
1hf
1o
7pottery is opaque.
Comparative examples 2
The process of basic repetition embodiment 1.Difference is that sintering schedule adopts sintering schedule at a slow speed: from room temperature to 600 DEG C, temperature rise rate is 200 DEG C/min; From 600 DEG C to sintering temperature 1450 DEG C, temperature rise rate is 10 DEG C/min; Pressure remains on 100MPa always.Gained Lu
2ti
1hf
1o
7pottery is translucent.Transmittance curve is shown in Fig. 5.
Embodiment 1-5 listed by table 1, the relative density values in reference examples 1-2.Relative density adopts Archimedes's drainage to measure;
Table 1 embodiment 1-5, the relative density values of hafnium metatitanic acid lutetium stupalith in reference examples 1-2
| Relative density (%) | |
| Embodiment 1 | 99.42 |
| Embodiment 2 | 99.99 |
| Embodiment 3 | 99.81 |
| Embodiment 4 | 99.53 |
| Embodiment 5 | 99.67 |
| Reference examples 1 | 98.35 |
| Reference examples 2 | 99.36 |
As from the foregoing, when pressure being remained on always a certain value when not adopting two step pressuring methods, transparent hafnium metatitanic acid lutetium pottery cannot be obtained.In addition, the present invention utilizes two step pressuring methods in sintering schedule, can be easy to realize the high crystalline ceramics preparation of density at short notice.
In sum, the preparation method of a kind of hafnium metatitanic acid lutetium crystalline ceramics provided by the invention, owing to adopting discharge plasma sintering, reaction is carried out with sintering simultaneously, and utilize two step pressuring methods in sintering schedule, can be easy to realize the crystalline ceramics preparation that density is high, crystal grain is little at short notice, have good application prospect in fields such as window, laser medium, high refractive index camera lens, scintillators.
Claims (10)
1. a hafnium metatitanic acid lutetium transparent ceramic material, is characterized in that, the chemical constitution of described hafnium metatitanic acid lutetium transparent ceramic material is Lu
2ti
2-xhf
xo
7, wherein 0<x<2, be preferably 0.6≤
x<2.
2. hafnium metatitanic acid lutetium transparent ceramic material according to claim 1, is characterized in that, described hafnium metatitanic acid lutetium transparent ceramic material is single defective type fluorite phase.
3. hafnium metatitanic acid lutetium transparent ceramic material according to claim 1 and 2, is characterized in that, described hafnium metatitanic acid lutetium transparent ceramic material is more than 65% when thickness is 1mm to the straight line transmittance of infrared band.
4. hafnium metatitanic acid lutetium transparent ceramic material according to any one of claim 1 to 3, is characterized in that, the density of described hafnium metatitanic acid lutetium transparent ceramic material is 99.4 ~ 100%, and average grain size is 400nm ~ 2 μm.
5. a preparation method for the hafnium metatitanic acid lutetium transparent ceramic material according to any one of Claims 1-4, is characterized in that, comprising:
With Lu
2o
3, TiO
2, HfO
2powder is raw material, stoichiometrically proportioning, ball mill mixing, sieve, obtain raw material mixed powder; And
Gained mixed powder is carried out discharge plasma sintering.
6. preparation method according to claim 5, is characterized in that, in described discharge plasma sintering, from room temperature to a certain temperature being less than sintering temperature, and pre-add first pressure; From this certain temperature to sintering temperature, apply the second pressure, wherein the first pressure is less than the second pressure.
7. the preparation method according to claim 5 or 6, is characterized in that, the process system of described discharge plasma sintering is: from room temperature to 1100 DEG C, and precharge pressure is 10 MPa ~ 50 MPa; From 1100 DEG C to sintering temperature, pressure is 100 ~ 150MPa.
8. the preparation method according to any one of claim 5 to 7, is characterized in that, be 10 ~ 100 DEG C/min from 1100 DEG C to the temperature rise rate of sintering temperature, sintering temperature is 1400 ~ 1550 DEG C, is incubated 5 ~ 60 minutes at a sintering temperature.
9. the preparation method according to any one of claim 5 to 8, is characterized in that, the process system of described discharge plasma sintering is:
Heating and cooling system: from room temperature to 600 DEG C, temperature rise rate is 200 DEG C/min; From 600 DEG C to 1100 DEG C, temperature rise rate is 100 DEG C/min; 1100 DEG C of insulations 5 minutes; From 1100 DEG C to sintering temperature, temperature rise rate is 10 ~ 100 DEG C/min; After insulation terminates, pulsed current is set to 0, cools with furnace temperature;
Pressure regime: from room temperature to 1100 DEG C, precharge pressure is 10 MPa ~ 50 MPa; From 1100 DEG C to sintering temperature, pressure was increased to 100 MPa and remains to insulation and terminates in 1 minute; Temperature-fall period, pressure unloaded in 1 minute.
10. the preparation method according to any one of claim 5 to 9, is characterized in that, after being also included in described discharge plasma sintering, in 650 ~ 1100 DEG C of insulations annealing operation of 3 ~ 10 hours in air or oxygen atmosphere.
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| CN115677341A (en) * | 2021-07-28 | 2023-02-03 | 中国科学院上海硅酸盐研究所 | Bismuth-layered ferroelectric ceramic with high transparency and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677341A (en) * | 2021-07-28 | 2023-02-03 | 中国科学院上海硅酸盐研究所 | Bismuth-layered ferroelectric ceramic with high transparency and preparation method thereof |
| CN114349502A (en) * | 2022-03-21 | 2022-04-15 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
| CN114349502B (en) * | 2022-03-21 | 2022-06-03 | 中国人民解放军国防科技大学 | Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof |
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