CN105837215A - Preparation method of neodymium-yttrium-doped strontium fluoride laser transparent ceramic - Google Patents
Preparation method of neodymium-yttrium-doped strontium fluoride laser transparent ceramic Download PDFInfo
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Abstract
The invention discloses a preparation method of a neodymium-yttrium-doped strontium fluoride laser transparent ceramic with high transparency and excellent mechanical properties. The preparation method comprises the following steps: processing 0.5at.%Nd<3+>,5at.%Y<3+>:SiF2 monocrystal into a standard rectangular-solid sample, putting the sample into a graphite mold, and separating the sample from the graphite mold with double-layer graphite paper; finally, putting the monocrystal-filled mold into a vacuum hot-pressing furnace, heating the sample according to the set technological parameters, and carrying out press forging in the fixed direction; when the sample reaches certain relative deformation, stopping pressurizing the sample, and shutting down the vacuum hot-pressing furnace procedure; and when the furnace temperature drops to room temperature, taking out the sample, sanding, and polishing to obtain the neodymium-yttrium-doped strontium fluoride laser ceramic. The method has the advantages of simple technique and lower cost, avoids the ceramic preparation process by the powder sintering technique, and can be used for preparing the polycrystal with comparable optical properties with the monocrystal and excellent mechanical properties.
Description
Technical field
The invention belongs to field of new, be specifically related to the preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic.
Background technology
It is big (-12ev) that rare-earth-doped fluoride crystal has energy gap, and transparency range is wide (125nm～10 μm), and refractive index is little
(～1.434, Vis～NIR), low (～the 390cm of phonon energy-1) etc. the incomparable advantage of oxide and become the most comprehensive
One of optical material that can be the most excellent.Simultaneously as the doping of rare earth ion so that its structure exists the electric charge of multi-form
Compensate, be easily formed broadness and smooth Absorption and emission spectra, be conducive to producing the shortest pulse laser, thus be widely used
In laser medium material.
Owing to strontium fluoride crystal belongs to fluorite type structure, Sr2+It is positioned at summit and the center of area position of cubic cell, forms face-centered cubic heap
Long-pending, F-Being filled in cubical body-centered, from the point of view of space lattice, it is by a set of Sr2+Face-centered cubic lattice and two set F-'s
Face-centered cubic lattice is interspersed to be formed.Sr in its structure2+It is filled only with the half in cube space, therefore in (111) veil direction
On there is electrostatic repulsion, cause crystal being parallel on (111) veil direction easily occur cleavage, thus the machine of these monocrystal materials
Tool poor-performing.
Optical property and the physical property of fluoride its excellence of crystalline ceramics are favored by many scientific research personnel, but, make at present
Standby fluoride crystalline ceramics is still based on traditional powder body forming and sintering method, and this method comprises preparation and two stages of sintering of powder body.
Lu Gang uses coprecipitation to prepare fluoride nano powder body, then has prepared transmitance through vacuum heating-press sintering and be up to 90%
Nd:CaF2Crystalline ceramics (sees document Lu G, Mei B C, Song J H, et al.Fabrication and properties of highly
transparent Nd-Doped CaF2Ceramics [J] .materials Letters, 2014,115:162-164.), but, at present this
Plant the fluoride pottery using traditional ceramics preparation technology to prepare all to fail to obtain the output of preferable laser, be primarily due to fluorination
Thing facile hydrolysis, can produce a kind of oxygen fluoride in pulverizing process and be adsorbed in the surface of nano-powder, and be difficult to eliminate, and becomes
For the dephasign in crystalline ceramics, destroy the optical homogeneity of pottery, thus affect laser output.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic, the method technique is simple,
And the crystalline ceramics not only excellent in optical properties of preparation, mechanical performance is also improved significantly.
For achieving the above object, the technical solution used in the present invention is: the preparation of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic
Method, it is characterised in that comprise the following steps:
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2Monocrystalline is (with Bridgman-Stockbarge method for growing, during the place of production is
Academy of science of state Shanghai silicate institute, for existing product) be processed into size be respectively 36 × 5 × 3mm, 6 × 6 × 4mm,
5 × 5 × 9mm standard cuboid sample；
2) by step 1) sample put in cylinder graphite jig, between sample and mould with double-layer graphite paper isolate, then will
Mould equipped with sample is put in vacuum hotpressing stove；
3) heat the sample to 900-1200 DEG C, be incubated 10-30min, then carry out forge hot process along fixed-direction, obtain sample
Product；
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forge hot is polished, polishing, obtain neodymium yttrium and mix
Miscellaneous strontium fluoride laser transparent ceramic.
0.5at.%Nd described in such scheme3+, 5at.%Y3+: SiF2Crystal raw material is with Bridgman-Stockbarge method for growing, and the place of production is China
Academy of science's Shanghai silicate institute.
In such scheme, step 3) in carry out forge hot along fixed-direction and be processed as: respectively along crystal growth direction or be perpendicular to crystalline substance
Bulk-growth direction is forged and pressed.
In such scheme, step 3) heat the sample to 1050 DEG C, it is incubated 10min.
In such scheme, step 3) in pressure be 0.4t-0.9t, forge time is 10-15min.
In such scheme, step 3) in vacuum be 9 × 10-3Below pa (vacuum in vacuum hotpressing stove).
The neodymium doped yttrium strontium fluoride laser transparent ceramic prepared according to such scheme is after sanding and polishing, and it is at visible ray, near-infrared
Wave band transmitance is about 86%；The strongest absworption peak and the pumping of wider absorption wide-band, beneficially laser is had at 796nm,
And its mechanical performance all obtains raising in various degree.
The present invention is with 0.5at.%Nd3+, 5at.%Y3+: SiF2Monocrystalline is raw material, has broken the biography by powder sintering preparation pottery
System technique, utilize heat forging technology to prepare crystalline ceramics, it is to avoid the adverse effect produced in powder body preparation process, the work related to
Skill is simple, and cost is relatively low, while maintaining the optical property that monocrystalline is excellent, improves its mechanical performance.
The invention have the benefit that
1) raw material of the present invention is monocrystalline, effectively prevent powder body manufacturing cycle long, and the impact pottery occurred in pulverizing process
The dephasign of porcelain optical property, it is possible to obtain the ceramic product of excellent optical property.
2) present invention uses heat forging technology to prepare crystalline ceramics, and the technique related to is simple, and efficiency is higher, and to a certain extent
Solve the problem that monocrystalline size is difficult to grow up.
3) mechanical performances such as the crystalline ceramics comprcssive strength that prepared by the present invention, bending strength, fracture toughness all have than monocrystalline and substantially carry
High.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 and 2 gained neodymium doped yttrium strontium fluoride laser transparent ceramic and the XRD figure of monocrystalline.
Fig. 2 is the shape appearance figure of the embodiment of the present invention 1 gained neodymium doped yttrium strontium fluoride laser transparent ceramic.
Fig. 3 is the transmitance figure of the embodiment of the present invention 1 gained neodymium doped yttrium strontium fluoride laser transparent ceramic.
Fig. 4 is the room temperature absorption spectrogram of the embodiment of the present invention 1 gained neodymium doped yttrium strontium fluoride laser transparent ceramic.
Detailed description of the invention
Embodiment 1
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2Monocrystalline is (with Bridgman-Stockbarge method for growing, during the place of production is
Academy of science of state Shanghai silicate institute, for existing product, shows mutually) it is processed into a size of 36 × 5 × 3mm standard cuboid
Sample (or claiming sample).
2) monocrystalline sample is put in cylinder graphite jig, isolate, to reduce sample with double-layer graphite paper between sample and mould
And the frictional force between graphite jig, then the mould that will be equipped with monocrystalline puts in vacuum hotpressing stove.
3) 9 × 10 are reached when vacuum-3During below pa, begin to warm up, during to 1050 DEG C, be incubated 20min, start along crystal raw
Length direction pressurizes, and pressure is 0.4-0.9t, during certain deformation to be achieved, stops pressurization, closes vacuum hotpressing stove program.
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forging is carried out two-sided polishing, polishing, obtains neodymium
Doped yttrium strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doped yttrium strontium fluoride laser ceramics records its consistency > 99.9%, light transmittance > 80%, the present embodiment institute
The XRD figure obtaining neodymium doped yttrium strontium fluoride laser ceramics is shown in Fig. 1, it can be seen that single crystal samples crystal face has two orientations,
After forging and pressing along the direction of growth, crystal face originally is destroyed, diffraction maximum corresponding to (111) weakens and even disappear, and (311) are corresponding
Diffraction maximum weakens and offsets, and (220), (400) and the diffraction maximum of (331) occurs simultaneously.Above-mentioned phenomenon all absolutely proves
Monocrystalline internal structure there occurs change clearly, and lattice parameter changes, and forge hot makes original crystal face be destroyed, and is formed
Defect sturcture.Fig. 2 is the shape appearance figure of the present embodiment products obtained therefrom, it is clear that the word below sample, Fig. 3 is
The transmitance figure of products obtained therefrom, maximum transmission reaches 86%, and Fig. 4 is the abosrption spectrogram of gained sample, and it is at 796nm
There are the strongest absworption peak and the pumping of wider Absorber Bandwidth, beneficially laser.Table 1 is mixed for the embodiment of the present invention 1 gained neodymium yttrium
The test result of the some mechanical performance of miscellaneous strontium fluoride laser ceramics.It can be seen that the mechanical performance of products obtained therefrom is all than monocrystalline
Improve.
Embodiment 2
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2It is long that monocrystalline is processed into a size of 36 × 5 × 3mm standard
Cube sample (or claiming sample).
2) monocrystalline sample is put in cylinder graphite jig, isolate, to reduce sample with double-layer graphite paper between sample and mould
And the frictional force between graphite jig, then the mould that will be equipped with monocrystalline puts in vacuum hotpressing stove.
3) 9 × 10 are reached when vacuum-3During below pa, begin to warm up, during to 1050 DEG C, be incubated 10min, start along being perpendicular to
Crystal growth direction pressurizes, and pressure is 0.4-0.9t, during certain deformation to be achieved, stops pressurization, closes vacuum hotpressing stove program.
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forging is carried out two-sided polishing, polishing, obtains
Neodymium doped yttrium strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doped yttrium strontium fluoride laser ceramics records its consistency > 99.9%, light transmittance > 80%, the present embodiment institute
The XRD figure obtaining neodymium doped yttrium strontium fluoride laser ceramics is shown in Fig. 1, it can be seen that after edge is perpendicular to direction of growth forging and stamping,
(111) corresponding diffraction maximum is wholly absent, and the diffraction maximum of (220) is higher, and the diffraction maximum of (311) correspondence weakens.Above-mentioned phenomenon
All having absolutely proved that monocrystalline internal structure there occurs change clearly, lattice parameter changes, and forge hot makes original crystal face quilt
Destroy, define defect sturcture, and along when being perpendicular to direction of growth forging and stamping, this defect can become apparent from.It is at 796nm
There are the strongest absworption peak and the pumping of wider Absorber Bandwidth, beneficially laser in place.
Embodiment 3
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2It is long that monocrystalline is processed into a size of 36 × 5 × 3mm standard
Cube sample (or claiming sample).
2) monocrystalline sample is put in cylinder graphite jig, isolate, to reduce sample with double-layer graphite paper between sample and mould
And the frictional force between graphite jig, then the mould that will be equipped with monocrystalline puts in vacuum hotpressing stove.
3) 9 × 10 are reached when vacuum-3During below pa, begin to warm up, during to 950 DEG C, be incubated 15min, start along being perpendicular to
Crystal growth direction pressurizes, and pressure is 0.4-0.9t, during certain deformation to be achieved, stops pressurization, closes vacuum hotpressing stove program.
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forging is carried out two-sided polishing, polishing, obtains
Neodymium doped yttrium strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doped yttrium strontium fluoride laser ceramics records its consistency > 99.9%, light transmittance > 80%, it is at 796nm
There are the strongest absworption peak and the pumping of wider Absorber Bandwidth, beneficially laser in place.
Embodiment 4
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2It is long that monocrystalline is processed into a size of 36 × 5 × 3mm standard
Cube sample.
2) monocrystalline sample is put in cylinder graphite jig, isolate, to reduce sample with double-layer graphite paper between sample and mould
And the frictional force between graphite jig, then the mould that will be equipped with monocrystalline puts in vacuum hotpressing stove.
3) 9 × 10 are reached when vacuum-3During below pa, begin to warm up, during to 950 DEG C, be incubated 10min, start along crystal raw
Length direction pressurizes, and pressure is 0.4-0.9t, during certain deformation to be achieved, stops pressurization, closes vacuum hotpressing stove program.
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forging is carried out two-sided polishing, polishing, obtains
Neodymium doped yttrium strontium fluoride laser transparent ceramic.
The present embodiment gained neodymium doped yttrium strontium fluoride laser ceramics records its consistency > 99.9%, light transmittance > 80%, it is at 796nm
There are the strongest absworption peak and the pumping of wider Absorber Bandwidth, beneficially laser in place.
Table 1 is the test result of the some mechanical performance of the embodiment of the present invention 1 gained neodymium doped yttrium strontium fluoride laser transparent ceramic.
Table 1
Embodiment 5
Essentially identical with the one in embodiment 1-4, difference is: step 1) in specimen size be 6 × 6 × 4mm or
5×5×9mm.The performance of gained neodymium doped yttrium strontium fluoride laser ceramics is consistent with corresponding embodiment.
Embodiment 6
Essentially identical with the one in embodiment 1-4, difference is: step 3) in begin to warm up, during to 1200 DEG C,
Insulation 30min.The performance of gained neodymium doped yttrium strontium fluoride laser ceramics is close with corresponding embodiment.
Claims (6)
1. the preparation method of a neodymium doped yttrium strontium fluoride laser transparent ceramic, it is characterised in that comprise the following steps:
1) by ready raw material 0.5at.%Nd3+, 5at.%Y3+: SiF2Monocrystalline is processed into sample；
2) by step 1) sample put in cylinder graphite jig, between sample and mould with double-layer graphite paper isolate, then will
Mould equipped with sample is put in vacuum hotpressing stove；
3) heat the sample to 900-1200 DEG C, be incubated 10-30min, then carry out forge hot process along fixed-direction, obtain sample
Product；
4) when furnace temperature is cooled to room temperature, take out sample, the sample after forge hot is polished, polishing, obtain neodymium yttrium and mix
Miscellaneous strontium fluoride laser transparent ceramic.
The preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that
Step 1) in the size of sample be respectively 36 × 5 × 3mm, 6 × 6 × 4mm, 5 × 5 × 9mm standard cuboid.
The preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that
Step 3) in carry out forge hot along fixed-direction and be processed as: respectively along crystal growth direction or be perpendicular to crystal growth direction forging and stamping.
The preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that
Step 3) heat the sample to 1050 DEG C, it is incubated 10min.
The preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that
Step 3) in pressure be 0.4t-0.9t, forge time is 10-15min.
The preparation method of a kind of neodymium doped yttrium strontium fluoride laser transparent ceramic the most according to claim 1, it is characterised in that
Step 3) in vacuum be 9 × 10-3Below pa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673658A (en) * | 2016-12-27 | 2017-05-17 | 武汉理工大学 | Praseodymium-doped strontium fluoride laser ceramics capable of facilitating red and orange light laser output, and preparation method of laser ceramics |
| 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 (1)
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| CN104009389A (en) * | 2014-06-06 | 2014-08-27 | 中国科学院物理研究所 | Application of femtosecond mode-locked laser and Nd, Y: srF2material in laser |
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2016
- 2016-04-22 CN CN201610255717.XA patent/CN105837215A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104009389A (en) * | 2014-06-06 | 2014-08-27 | 中国科学院物理研究所 | Application of femtosecond mode-locked laser and Nd, Y: srF2material in laser |
Non-Patent Citations (1)
| Title |
|---|
| WEIWEI LI ET AL.: "Nd3+, Y3+-codoped SrF2 laser ceramics", 《OPTICAL MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673658A (en) * | 2016-12-27 | 2017-05-17 | 武汉理工大学 | Praseodymium-doped strontium fluoride laser ceramics capable of facilitating red and orange light laser output, and preparation method of laser ceramics |
| 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 |
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