Preparation method of YVO4 transparent laser ceramic containing lanthanide rare soil and scandium

A technology of lanthanide rare earth and laser ceramics, which is applied in the field of material smelting to achieve the effects of short production cycle, simple raw material preparation, and easy control of the process flow

Inactive Publication Date: 2013-05-08
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

[0005] The well-known neodymium-doped yttrium vanadate (Nd:YVO 4 ) is currently under competitive pressure from Nd:YAG transparent ceramics. The ceramic sintering method makes the doping concentration of Nd:YAG greater than 6% atomic concentration, so that its absorption length can be compared with that of Nd:YVO 4 Comparable to the single crystal; Another defect is that the thermal conductivity of Nd:YAG ceramics is significantly higher than that of Nd:YVO 4 , limiting the Nd:YVO 4 To play its excellent role, in order to further improve the performance limitations of laser equipment and single crystal materials, the present invention proposes to prepare transparent Ln:Y(Sc)VO 4 Laser ceramics, replaced in YVO by Sc with similar properties to Y atoms 4 Part of the Y atoms in the structure is used to improve the thermal conductivity of the material, and the complex electronic structure of lanthanide rare earth ions is used to improve the laser emission performance, broaden the laser emission wavelength, and effectively increase the doping concentration of rare earth ions, greatly improving the material The performance and operability of the preparation reduce the complicated single crystal stretching preparation process. The survey of relevant literature and patent data shows that there are few technical solutions proposed by this patent in the world to prepare Ln:Y(Sc)VO 4 Report on transparent laser ceramic materials

Method used

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  • Preparation method of YVO4 transparent laser ceramic containing lanthanide rare soil and scandium

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Experimental program
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Effect test

Embodiment 1

[0020] Prepare yttrium oxide (Y 2 o 3 ) powder, scandium oxide (Sc 2 o 3 ) powder and vanadium oxide (V 2 o 5 ) powder, adding a total of 2% neodymium oxide (Nd 2 o 3 ) powder (mol percent), 2% thulium oxide (Tm 2 o 3 ) powder (molar percentage), the magnesium oxide (MgO) powder (molar percentage) of 0.01% of the total amount, 0.01% (mass percentage) of the total amount of high-purity TEOS, put into the polytetrafluoroethylene ball mill tank, add dehydrated alcohol And corundum ceramic balls, rotating speed 800rad / min, ball milling for 6 hours. Take it out and evaporate it to dryness with an evaporator, and grind it through a 200-mesh sieve. Use a 100MPa pressure shaft to pressurize in one direction, press it into a disc with a diameter of 10-20mm, and press it further in a cold isostatic pressing device with a pressure of 350MPa. Put into vacuum sintering furnace for pretreatment, vacuum degree 10 -3 Pa, the pretreatment temperature is 900 degrees, and the holding ...

Embodiment 2

[0022] Preparation of Y(Sc)VO by Wet Chemical Method 4 powder (wherein the content of scandium is 10% by molar ratio) and neodymium oxide (Nd 2 o 3 ) powder, sodium oxide (Na 2 O) a mixture of powders, wherein the content of neodymium oxide is 1% (molar percentage) of the total amount, ytterbium oxide (Yb2 o 3 ) content is 2% (mole percentage) of the total amount, sodium oxide (Na 2 O) powder content (molar percentage) is 0.005% of total amount, adds 0.01% (mass percentage) high-purity TEOS of total amount, puts into polytetrafluoroethylene ball mill jar, adds dehydrated alcohol and corundum ceramic ball, rotating speed 800rad / min, ball milling for 8 hours. Take it out and evaporate it to dryness with an evaporator, and grind it through a 200-mesh sieve. Use a 100MPa pressure shaft to pressurize in one direction, and further press in a cold isostatic pressing device with a pressure of 300MPa. Put into vacuum sintering furnace for pretreatment, vacuum degree 10 -3 Pa, t...

Embodiment 3

[0024] Yttrium oxide (Yttria) was prepared by wet chemical method 2 o 3 ) powder, scandium oxide (Sc 2 o 3 ) powder, lanthanum oxide (La 2 o 3 ) powder, europium oxide (Eu 2 o 3 ) powder, magnesium oxide (MgO) powder and vanadium oxide (V 2 o 5 ) powder mixture, in which yttrium oxide (Y 2 o 3 ) powder, scandium oxide (Sc 2 o 3 ) powder and vanadium oxide (V 2 o 5 ) in a molar ratio of 3:2:5, the content of lanthanum oxide is 2% (mol percent) of the total amount, the content of europium oxide is 4% (mol percent) of the total amount, and the content of magnesium oxide (MgO) (mol percent) is the total 0.005% of the total amount, and 0.015% (mass percentage) of the total amount of high-purity TEOS was put into an alumina ball mill jar, adding absolute ethanol and corundum ceramic balls, and ball milled for 12 hours at a speed of 1100 rad / min. Take it out and evaporate it to dryness with an evaporator, and grind it through a 200-mesh sieve. Use a 120MPa pressure axi...

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Abstract

The invention relates to a transparent laser ceramic material, in particular to a preparation method of YVO4 transparent laser ceramic containing lanthanide rare soil and scandium, belonging to the technical field of material metallurgy. The method comprises the following steps of: mixing the raw materials for burning yttrium vanadate laser material, lanthanide rare soil oxide and vanadium oxide powder according to the proportion, grinding, sieving by 200 meshes after drying processing, pressing into bisque; carrying out vacuum sintering to the bisque with the vacuum degree of less than 10<-3>Pa, temperature-rising speed of 1 to 10 DEG C for every minute, sintering temperature of 1500 to 2000 DEG C and insulating time of 4 to 80 hours; and sintering ingot blanks, cooling with a furnace, annealing, carrying out planar processing after being taken out, and obtaining the transparent laser ceramics after precisely polishing. The invention can improve the content of the rare soil element in the material and improve the heat conducting property, can prepare transparent ceramic with larger size, has shorter preparing period and lower cost, and better solves the problems that the doping concentration of single-crystal material is hard to be improved, the preparation with larger size is difficult and the like, thus leading the comprehensive performance of the material to be improved.

Description

technical field [0001] The invention relates to a transparent laser ceramic material, especially YVO containing lanthanide rare earth and scandium 4 The invention discloses a method for preparing transparent laser ceramics, which belongs to the technical field of material metallurgy. Background technique [0002] Laser transparent ceramic materials are important raw materials for a new generation of solid-state lasers, which have an important impact on the development of high-power and small-volume laser technologies. Related technologies can be applied to navigation, precision measurement, manufacturing, medical and health fields, etc. The technology of transparent laser ceramics was originally mastered by Japan, and representative patents include JP05-286761, JP05-286762, JP05-294722, JP05-294273, JP294722, etc., and then the United States, Germany, Britain, France, etc. followed up and developed corresponding In my country, the Shanghai Institute of Ceramics, Chinese Acad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/622C04B35/50C04B35/495
Inventor 冯晶肖冰陈敬超于杰李宁周荣
Owner KUNMING UNIV OF SCI & TECH
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