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Yb-doped strontium fluorophosphate microcrystal/Yb-doped fluorophosphate glass composite material and preparation method thereof

A technology of ytterbium fluorophosphate and phosphate glass, which is applied in the field of ultrafast laser materials, can solve problems such as difficult control of microcrystalline morphology, and achieve the effects of reducing solid-state reactions, good controllability, and avoiding corrosion

Active Publication Date: 2015-05-13
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because of the CaF 2 The formation of the crystallite is re-precipitated during the cooling process, so the morphology of the crystallite is difficult to control

Method used

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  • Yb-doped strontium fluorophosphate microcrystal/Yb-doped fluorophosphate glass composite material and preparation method thereof
  • Yb-doped strontium fluorophosphate microcrystal/Yb-doped fluorophosphate glass composite material and preparation method thereof
  • Yb-doped strontium fluorophosphate microcrystal/Yb-doped fluorophosphate glass composite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0032] In this embodiment, the ytterbium-doped strontium fluorophosphate crystallite and the ytterbium-doped fluorophosphate glass composite material are formed by uniformly dispersing the ytterbium-doped strontium fluorophosphate crystallite containing 5 mol% ytterbium in the ytterbium-doped fluorophosphate glass body containing 2 mol% ytterbium , the weight ratio of the ytterbium-doped strontium fluorophosphate microcrystal is 10%, the size of the ytterbium-doped strontium fluorophosphate microcrystal is 10-20 microns, and the transmittance of the composite material in the visible light band is greater than 80%.

[0033] Embodiment The preparation method of ytterbium-doped strontium fluorophosphate microcrystal and ytterbium-doped fluorophosphate glass composite material comprises the following steps:

[0034] (1) 10MgF in molar ratio 2 -20CaF 2 -20SrF 2 -6BaF 2 -4NaF-38AlF 3 -2YbF 3 Melting at 900°C to obtain fluoride glass; by mass ratio 50NaPO 3 -50Al(PO 3 ) 3 Mel...

Embodiment 2～4

[0044] This group of examples investigates the sintering process and preparation method of ytterbium-doped strontium fluorophosphate microcrystals and ytterbium-doped fluorophosphate glass micro-nano composite materials. The results of the examples show that the hot pressing temperature is 550°C to 650°C, the hot pressing head pressure is 20MPa to 50MPa, the hot isostatic pressing temperature is 500°C to 600°C, and the hot isostatic pressing pressure is in the range of 100MPa to 200MPa. The materials are all transparent, and the XRD diffraction pattern of the composite sample shows an obvious glass diffraction envelope and the crystal diffraction peak of S-FAP.

Embodiment 2

[0046] (1) 10MgF in molar ratio 2 -20CaF 2 -20SrF 2 -6BaF 2 -4NaF-38AlF 3 -2YbF 3 Melting at 900°C to obtain fluoride glass; by mass ratio 50NaPO 3 -50Al(PO 3 ) 3 Melted at 900°C to obtain phosphate glass. The fluoride glass clinker and the phosphate glass clinker with a weight ratio of 85:15 were stirred and mixed at 900° C. to obtain a fluorophosphate glass with a refractive index nd of 1.430. Glass raw materials are all analytically pure, of which AlF 3 Take NH 4 AlF 4 introduce. Pulverizing the above fluorophosphate glass to obtain fluorophosphate glass powder;

[0047] (2) Measure Sr(NO 3 ) 2 and Yb(NO 3 ) 3 solution, the Sr(NO 3 ) 2 , Yb(NO 3 ) 3 The solution was uniformly mixed under magnetic stirring, and distilled water was added to the mixed solution to the Sr in the mixed solution 2+ The concentration is 0.5mol / L, and at the same time, the mixed solution is heated to 100°C in a water bath to obtain a mother salt solution. Weigh excess NH 4 HF ...

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Abstract

The invention relates to a Yb-doped strontium fluorophosphate microcrystal / Yb-doped fluorophosphate glass composite material and a preparation method thereof. The composite material is prepared by uniformly dispersing Yb-doped strontium fluorophosphate microcrystals comprising 5mol% of Yb in a Yb-doped fluorophosphate glass system comprising 2mol% of Yb, wherein a weight percent of the Yb-doped strontium fluorophosphate microcrystals is 10-50%, and a size of the Yb-doped strontium fluorophosphate microcrystals is 10-20 microns. According to the invention, heat treatment for the mixed powder is carried out at a low temperature, and therefore a solid phase reaction between a glass phase and a microcrystal phase during the heat treatment process is reduced, corrosion of the glass to the microcrystals during a sintering process is prevented, inherent forms of the doped microcrystals are kept, and controllability is good. The transmittance, in the visible light band, of the composite material is greater than 80%.

Description

technical field [0001] The invention relates to an ultrafast laser material, in particular to an ytterbium-doped strontium fluorophosphate microcrystalline-doped ytterbium fluorophosphate glass composite material and a preparation method thereof Background technique [0002] Ultrafast laser has four characteristics: ultrashort pulse, high peak power, high repetition rate and wide spectrum. Wide range of applications. At present, the working media for producing ultrafast lasers are mainly: Nd: phosphate glass, Yb: S-FAP single crystal, Yb: YAG ceramics and Yb: CaF 2 single crystal etc. Among them, Nd phosphate glass can be prepared in large size, but its thermal performance is poor, and it cannot work at high repetition frequency; Yb:S-FAP has excellent thermal performance and emission interface, but due to the influence of segregation coefficient, it has high optical quality and uniform doping The large-scale preparation of heterogeneous Yb:S-FAP single crystals is a diff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C10/16C03C3/32
Inventor 范金太张龙姜雄伟袁新强姜本学毛小建
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI