RO132655B1 - Borophosphate glass with magneto-optical properties and process for producing the same - Google Patents

Description

RO 132655 Β1

The present invention relates to boro-phosphate bottles with magneto-optical properties and to a process for obtaining them.

Patent application G / ass for Faraday rotary element '/ US 3971723 A refers to a boro-silicate glass, used as an element of a Faraday rotator, consisting mainly of (% molar): 10 ... 30 Tb ₂ O ₃ , 10 ... 30 AI ₂ O ₃ and 30 ... 80 SiO ₂ + B ₂ O ₃ , provided that SiO ₂ > 15 and B ₂ O ₃ > 10, plus optional components 0 ... 5 ZrO ₂ , 0 ... 1 Sb ₂ O ₃ , 0 ... 1 As ₂ O ₃ , and 0 ... 2 AIF ₃ . The glass has a high constant green and low light absorption in regions with visible wavelengths and infrared.

Patent application Faraday rotation g / asses / US 3935020 A, relates to borosilicate bottles for Faraday rotators which have a high constant Verdet and low susceptibility and are obtained by introducing a high amount of rare earth oxides into a basic borate glass . The bottles can be melted widely under standard conditions. The bottles have the following composition, in gravimetric percentages: 0 ... 12 SiO ₂ , 10 ... 42 B ₂ O ₃ , 0 ... 1 alkaline-earth oxides, 25 ... 57 an oxide of rare earths, 8. ..24 alkaline oxides, 1 ... 7 ZrO ₂ , 0 ... 7 WO ₃ , 0 ... 2 AI ₂ O ₃ and 0 ... 0.5 refining agent, where the alkaline-earth oxide is selected between CaO, BaO, ZnO, and combinations thereof, the rare earth oxide is Tb ₄ O ₇ or the combination of Tb ₄ O ₇ and La ₂ O ₃ , Tb ₄ O ₇ being present in an amount of 20 ... 45 gravimetric percentages, and the alkali metal oxide is selected from the group consisting of Na ₂ O, K ₂ O and combinations thereof.

Patent document CN 1342617A Faraday-rotation phosphorate g / ass with low non-linearrefractivity refers to a phosphate glass for Faraday rotator with a low nonlinear refractoriness and high Tb ³⁺ content containing 17 ... 26% Tb ₂ O ₃ , 70 ... 80% P ₂ O ₅ , 0 ... 6% AI ₂ O ₃ , 0 ... 6% B ₂ O ₃ , 0 ... 6% SiO ₂ , 0 ... 6% Na ₂ O plus K ₂ O, 0 ... 6% BaO, 0.1 ... 0.8% Sb ₂ O ₃ , or 0.1 ... 0.8% As ₂ O ₃ , or 0.1 ... 0.8% Sb ₂ O ₃ plus As ₂ O ₃ . The advantages are high Verdet constant, low nonlinear refractive index, high transparency in the visible or near infrared region and fairly good stability.

U.S. Pat. No. 2,0200,41750 Rare earth element-doped, Bi-Sb-AI-Si g / ass and its use in optics / amplifiers discloses a glass doped with rare earth elements, from the Bi ₂ O ₃ -Sb ₂ O _{3 system} -AI ₂ O ₃ -SiO ₂ , containing 1 ... 50% molar of Bi ₂ O ₃ , which is easier to incorporate than fluorine. The glass can be manufactured using the standard technique of melting the mixture of raw materials. The composition of the glass is: 1 ... 60% molar Sb ₂ O ₃ ; 0 ... 60% molar Bi ₂ O ₃ ; 0 ... 20% molar AI ₂ O ₃ ; 20 ... 90% molar SiO ₂ ; and 0 ... 4% molar Er ₂ O ₃ .

Patent application Preparation method ofbismuth-containing paramagnetic Faraday optics / rotation g / ass, CN 102627404 Describe the method of preparation of a vitreous Faraday paramagnetic rotator. The preparation method involves the uniform mixing of Er ₂ O ₃ , Bi ₂ O ₃ , B ₂ O ₃ , AI ₂ O ₃ , SiO ₂ , Sb ₂ O ₃ and ZrO ₂ to obtain the batch, melting at 1200 ... 1400 ° C , for 3 h, pouring the melt into a graphite mold, annealing at 550 ° C for 3 h and cooling to room temperature to obtain the Faraday rotator. The field of glass formation is extended and the melting temperature is reduced. The composition is in molar% 5 ... 35 Er ₂ O ₃ , 10 ... 38 Bi ₂ O ₃ , 5 ... 40 B ₂ O ₃ , 15 ... 45 AI ₂ O ₃ , 0 ... 5 SiO ₂ , 0 ... 1 Sb ₂ O ₃ and 0 ... 1 ZrO ₂ .

Patent application Paramagnetic Faraday rotator g / ass and preparation method thereof / CN 103708726 A discloses a bottle for Faraday paramagnetic rotator composition: 20 ... 25% molar SiC, 35 ... 42% molar Tb ₂ O ₃ , 18. ..20% molar AI ₂ O ₃ , 16 ... 21% molar B ₂ O ₃ , 1 ... 5% molar P ₂ O ₅ and the method of its preparation. The method of preparation comprises the following steps: uniform mixing of tetraaterbium heptaoxide, boric acid, aluminum oxide, ammonium diacid phosphate, antimony oxide, and silicon carbide to obtain the mixture of raw materials, and then melting it at high temperature. in the air, and finally pouring the glass melt into the stainless steel mold, and careful annealing so as to obtain the glass

RO 132655 Β1 paramagnetic for the Faraday rotator. The preparation method has the advantage that by the oxidation-reduction characteristics of the mixture of raw materials, the low valence of rare earth ions in glass is ensured, the platinum crucible provides corrosion protection, 3 and prevents the embedding of platinum ions in glass. The optical quality of the paramagnetic glass for the Faraday rotator is improved and the production technology is improved and simplified. The paramagnetic glass for the Faraday rotator thus prepared, has a high content in rare earths, low valence, high Green constant, high transmission in the visible field, 7 simple and industrially applicable preparation technology.

The technical problem solved by the invention consists in obtaining boron-phosphate bottles which have improved mechanical, thermal and chemical resistance as well as high quality magneto-optical properties. 11

Silicate glasses with magneto-optical properties melt at high temperatures and have lower magneto-optical properties than those of phosphate glasses. Phosphate bottles with 13 magneto-optical properties melt at lower temperatures but have low chemical and mechanical resistance. 15

Doped boron-phosphate bottles eliminate the above disadvantages in that they contain glass-forming oxides: 5 ... 20% boron oxide - B ₂ O ₃ and 14 ... 75% molar phosphorus oxide 17 - P ₂ O ₅ , as well as glass network modifiers: lithium oxide - Li ₂ O, in a proportion of 2 ... 15%, chemical, thermal and mechanical stabilizers: aluminum oxide - AI ₂ O ₃ , 2 ... 20% and zinc oxide - 19

ZnO 2 ... 20%, together with oxides that induce the magneto-optical properties, in percentages of 3 ... 75%, of the following oxides, introduced alone or in pairs: of transition metals: cobalt oxide 21 CoO, oxide of iron FeO, Fe ₂ O ₃ , Fe ₃ O ₄ , vanadium oxide V ₂ O ₃ , zirconium oxide, ZrO ₂ , niobium oxide, Nb ₂ O ₃ , molybdenum oxide, MoO ₂ , tungsten oxide, WO ₃ , of post-23 transition metals: tin oxide, Sn ₂ O ₃ , antimony oxide, Sb ₂ O ₃ , lead oxide PbO, bismuth oxide, Bi ₂ O ₃ , of rare earths: Tb ₂ O ₃ , Dy ₂ O ₃ , CeO ₂ , Eu ₂ O ₃ , Pr ₂ O ₃ , Nd ₂ O ₃ , Sm ₂ O ₃ , Gd ₂ O ₃ , 25

Ho ₂ O ₃ , Er ₂ O ₃ , Tm ₂ O ₃ , Yb ₂ O ₃ molar percentages and by the process of obtaining this new type of bottle, by the method of wet preparation of the mixture of raw materials, followed27 by pre-melting, melting, refining, conditioning, casting, annealing, shaping of the obtained glass.

The operations of the process for the preparation of the wet mixture of raw materials 29 used to obtain boron-static bottles according to the invention are as follows:

- gravimetric and volumetric dosing of raw materials, 31

- introduction of the raw materials in the homogenization vessel in the predetermined order;

- cold homogenization of raw materials in a niche with a mechanical homogenizer;

- partial drying mixture of raw materials, with partial removal of water (in quartz crucibles provided with electric stirrer with flexible shaft, on the electric hob) with continuous mixing, up to temperatures of 12O ... 15O ° C;

- pouring the mixture, when it is still fluid, into the melting crucible.37

The pre-melting step is performed between 150 ° C and 700 ... 900 ° C, with slow temperature rise, to remove gases from the mixture of raw materials and resulting from 39 chemical reactions without losing the mixture of raw materials.

The melting step, at temperatures of 950 ... 1300 ° C comprises the following 41 technological operations:

- melting the mixture of raw materials;

- refining the melt;

- homogenization of the melt, 45

- melt conditioning;

- lowering the temperature to the casting temperature.47

RO 132655 Β1

The shaping of the glass is performed by pouring the conditioned glass melt into pure spectral graphite molds, preheated in the annealing furnace, at the annealing temperature, specific to each glass composition. The molds contain parallelepiped nests with dimensions of 50 x 50 x 10 mm, in which the melt is poured.

The annealing is performed in electric furnaces for dental technique, provided with kanthal resistors (SiC wire), and the processing of samples for determining the physico-chemical properties is performed by cutting with a diamond disk, with a diameter of 100 mm. Samples cut to the required dimensions are subjected to sanding and polishing (polishing) operations.

Boron-phosphate bottles containing lithium oxide, aluminum oxide and zinc oxide, as well as doping oxides of transitional, post-transitional elements and rare earths have the advantages of lower melting temperatures and higher magneto-optical properties than glass. silicate with magneto-optical properties, and compared to phosphate bottles has the advantages of better chemical stability and mechanical properties, under conditions of similar or higher magneto-optical properties. The novelty of the invention consists in the fact that new glass materials with magneto-optical uses have been obtained, combining the properties of phosphate bottles with the advantages and novelty of the introduction of B ₂ O ₃ and ZnO. As the applications of phosphate bottles are diminished due to the reduced chemical stability, by adding trivalent ions, as a substitute for alkaline ions, the chemical and mechanical resistance has been improved. Stabilization of phosphate bottles was performed with B ₂ O ₃ combined with ZnO and / or PbO. Dopers, oxides of transitional, post-transitional metals and rare earths, ensure the high magneto-optical properties of these bottles, which have the advantages of combining these properties with high chemical and mechanical stability.

Volume boron-phosphate bottles, containing lithium oxide, aluminum oxide and zinc oxide, doped with one or pairs of transition and post-transition metal oxides, or with one or pairs of rare earth oxides, have the following improved characteristics : i) High homogeneity, in the whole volume of the bottle; ii) Lack of defects such as inclusions or stones; iii) Small number of gaseous inclusions and their very small size; iv) Lack of defects such as striations, threads, veins; v) Lack of stresses due to thermal gradients; vi) High visibility optical transmission (depending on use and near UV or near IR), over 80% in all useful areas; vii) high chemical, mechanical and thermal resistance; viii) Magneto-optical effect, rotating the plane of polarized light, comparable to the world level.

Presentation of the figures:

- fig. 1, technological flow according to the process proposed in the invention, comprising the main technological operations;

- fig. 2, pre-melting-melting-refining-homogenizing-conditioning program according to the invention, comprising temperatures, duration, mixing regime, for BPM2 glass;

- fig. 3, annealing program for doped BPM2 glass according to the process proposed in the invention, comprising the temperatures and durations of the stages of the annealing process of the cast glass plate;

- fig. 4, the optical transmission of one of the doped boro-phosphate bottles according to the invention, the glass code BPM2;

The following is at least one embodiment of the invention:

Example 1

The molar and gravimetric oxide composition for example 1 is that of table 1, for glass code BPM2, doped with Bi and Pb ions.

RO 132655 Β1

Molar and gravimetric oxide composition for boro-phosphate 1 doped glass code BPM2 Table 1 3

Glass Oxide B ₂ O ₃ p ₂ or ₅ Read ₂ O AI ₂ O ₃ ZnO Bi ₂ O ₃ PbO Total BPM2 % molar 20 50 10 9 5 3 3 100 BPM2 % gravimetric 11.43 58.27 2.45 7.53 3.34 11.48 5.50 100

The raw materials used are of analytical purity: lithium carbonate, Li ₂ CO ₃ , aluminum oxide, AI ₂ O ₃ , zinc oxide ZnO, phosphoric acid, H ₃ PO ₄ , lead oxide, PbO, bismuth oxide, 11 Bi ₂ O ₃ .

The technological flow for the process for obtaining the doped boro-static glass according to the invention is that shown in fig. 1.

The composition of the mixture of raw materials to obtain 100 g of boro-phosphate glass doped with code BPM2 is that of Table 2.

Composition of raw materials for 100g glass, for doped boro-phosphate glass code BPM219

Table 2

Glass Raw material B ₂ O ₃ h ₃ po ₄ Read ₂ CO ₃ AI ₂ O ₃ ZnO Bi ₂ O ₃ PbO BPM2 g 8.57 75.43 5.24 5.65 2.51 8.61 4.12

The raw materials used to introduce the oxides from Tables 1 and 2 into the 25-glass melt are:

- phosphoric acid, H ₃ PO ₄ pa, for the introduction of phosphorus oxide;

- lithium carbonate, Li ₂ CO ₃ , pa, for the introduction of lithium oxide;

- aluminum oxide, AI ₂ O ₃ , of purity pa, for the introduction of aluminum oxide; 29 - zinc oxide, ZnO, pa, for the introduction of zinc oxide;

- bismuth oxide III, Bi ₂ O ₃ , pa, for the introduction of bismuth oxide;

- lead oxide II, litter, PbO, p.a., for the introduction of lead oxide.

For the calculation of the composition of the mixture of raw materials, the percentage of volatilization of phosphorus oxide of 25% and lithium oxide of 15% shall be taken into account.

The dosing of the raw materials is carried out using the technical balance with an accuracy of 35 ± 1 g, for the main raw materials and the analytical balance with an accuracy of ± 10 ' ⁵ g in the case of dopants.37

Graded pipettes to the nearest ± 0,1 mL are used to measure phosphoric acid.

The technological operations in the process of preparing the mixture of wet raw materials 39, used to obtain BPM2 bottles, are the following: gravimetric and volumetric dosing of raw materials; introduction of raw materials into the homogenization vessel in the predetermined order; cold homogenization of raw materials, in a niche, with mechanical homogenizer, for 15 min; partial drying mixture of raw materials, with partial removal 43 of water (in quartz crucibles provided with electric stirrer with flexible shaft, on the electric hob) with continuous mixing, up to a temperature of 150 ° C; pouring the mixture, when it is still fluid, into the melting crucible of alumina.

RO 132655 Β1

The important chemical reactions that take place during the preparation of the mixture of raw materials are:

3Li ₂ CO ₃ + 2H ₃ PO ₄ - 2Li ₃ PO ₄ + 3H ₂ O + CO ₂ (1)

AND ₂ O ₃ + 2H ₃ PO ₄ - 2AI (PO) ₄ ) + 3H ₂ O (2)

3ZnO + 2H ₃ PO ₄ - Zn ₃ (PO ₄ ) ₂ + 3H ₂ O (3)

This process of wetly obtaining the mixture of raw materials to obtain the BPM2 bottle offers the advantages of a good homogenization of the raw materials in the preparation phase of the raw material mixture and also ensures the initiation of phosphate formation in the homogenization phase of the raw materials and metaphosphates in the pre-melting heat treatment phase. This process leads to shorter melting, refining and conditioning processes and helps to achieve high optical and magnetic homogeneity for the phosphate bottles made.

Preliminary heat treatment, pre-melting - thermal conditioning of the mixture of raw materials is performed in an electric furnace with silite bars (SiC), the mixture of raw materials being already introduced in the alumina crucible in which the melting takes place. The characteristics of the oven are: maximum working temperature: 1400 ° C; heating elements: forced bars; working enclosure dimensions: 400 x 300 x 200 mm; automatic temperature control in the oven. The heat treatment program for BPM2 glass is shown, together with the melting program, in FIG. 2 and table 3.

Melting takes place in the melting furnace equipped with superkanthal heating elements (MoSi ₂ ), with the following characteristics: maximum working temperature: 1600 ° C; heating elements: superkanthal elements; working enclosure dimensions: 280 x 150 x 150 mm; automatic temperature control in the oven. The melting program of the BPM2 glass is shown, together with the preliminary heat treatment program, in fig. 2 and table 3.

The melting stage comprises the following technological operations: melting the mixture of raw materials; melt refining; melt homogenization; melt conditioning; lowering the temperature to the casting temperature.

Pre-melting - melting - mechanical homogenization program for BPM2 glass

Table 3

Time [h] Temperature [° C] Stirring speed [rpm] 0 20 0.5 70 1 120 1.5 170 2 two hundred 2.25 two hundred 2.5 220 2.75 240 5 260 3.25 260 3.5 280

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Table 3 (continued)

Time [h] Temperature [° C] Stirring speed [rpm] 3.75 295 4 310 4.25 310 4.5 310 4.75 310 5 310 5.25 330 5.5 350 5.75 375 6 400 6.5 450 7 525 7.5 600 8 700 9 1000 10 1250 10.5 1250 two hundred 11 1250 two hundred 12 1250 two hundred 12.5 1200 150 13 1200 150 13.5 1200 -

For the homogenization of the glass melt, a mechanically actuated agitator is used, provided with a high purity sintered alumina stirring body, over 99%. The homogenization programs are established according to the viscosity of the melt, in this example the rotation speeds being of 200 and 150 rot / min.

The molding of BPM2 glass is performed by pouring the conditioned glass melt into pure spectral graphite molds, preheated in the annealing furnace, at the annealing temperature, specific to each glass composition, in this example, for BPM2 glass, being 500 ° C. The molds contain parallelepiped nests with dimensions of 50 x 50 x 10 mm, in which the melt is poured. The pouring is carried out quickly, in the part of the mold close to the pouring direction, until the appearance of the more viscous glass at the bottom of the crucible, when the pouring stops and the crucible is reintroduced in the oven, where it cools with it, with speeds of about 200 ° C / h.

The annealing operation aims to eliminate the stresses due to the thermal gradients that appeared during the processes of casting and cooling the molded glass. The annealing is carried out in an electric oven equipped with kanthal resistors (SiC wire), with the following characteristics: maximum working temperature: 1300 ° C; heating elements: resistors made of kanthal wire; enclosure dimensions: 300 x 250 x 150 mm; automatic temperature control in the oven.

RO 132655 Β1

The annealing program made for the BPM2 glass, according to the data on the characteristic temperatures and its coefficient of thermal expansion, is presented in fig. 3.

The processing of samples for the determination of physico-chemical properties is performed by cutting with a diamond disk, with a diameter of 100 mm, to the dimensions imposed by the methods of physico-chemical analysis and possible subsequent uses.

Samples cut to the required dimensions are subjected to sanding and polishing (polishing) operations. They are made on grinding machines, on felt-covered metal discs, using as grinding agent silicon carbide suspensions of three increasingly fine-grained granules, 250, 400 and 600 mesh and finally with the help of cerium oxide, of at least 800 mesh granulation, used as polishing agents.

The optical transmission for the BPM2 glass is shown in fig. 4.

Example 2

The procedure is similar to that of Example 1, with the following differences:

The composition of the boro-phosphate bottle of Example 2, doped with dysprosium oxide, Dy ₂ O ₃ and terbium oxide, Tb ₂ O ₃ is as shown in Table 4.

Molar and gravimetric oxide composition for boro-phosphate glass doped with code BPM6

Table 4

Glass Oxide B ₂ O ₃ p ₂ or ₅ Read ₂ O AI ₂ O ₃ ZnO Ι- ^ Υ2θ3 Tb ₂ O ₃ Total BPM6 % molar 20 50 10 9 5 3 3 100 BPM6 % gravimetric 11.29 57.57 2.42 7.44 3.30 9.08 0.90 100

The raw materials for the introduction of dysprosium and terbium oxides are dysprosium oxide, Dy ₂ O ₃ and terbium oxide, Tb ₂ O ₃ of analytical purity. Pre-melting programs are performed with an intermediate bearing at 300 ° C. The melting temperature is increased by 50 ° C to 1300 ° C. The speed of the refractory stirrer is higher, 250 and 200 rpm, respectively, and it is positioned closer to the bottom of the crucible. For BPM6 glass, the conditioning-homogenization melting program is the one presented in table 5.

Pre-melting - melting - mechanical homogenization program for BPM6 glass

Table 5

Time [h] Temperature [° C] Stirring speed [rpm] 0 20 0.5 70 1 120 1.5 170 2 1220

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Table 5 (continued)

Time [h] Temperature [° C] Stirring speed [rpm] 2.25 240 2.5 260 2.75 280 3 300 3.25 300 3.5 300 3.75 300 4 300 4.25 320 4.5 340 4.75 360 5 380 5.25 400 5.5 425 5.75 450 6 475 6.5 550 7 700 7.5 850 8 1000 9 1300 9.5 1300 240 10 1300 240 11 1300 240 11.5 1200 two hundred 12 1200 two hundred

The annealing program for BPM6 glass is similar to that for BPM2 glass in Example 1, but the annealing temperature is 480 ° C.

Example 3

The procedure is similar to that of Example 1, with the following differences:

The composition of the boro-phosphate glass in Example 3, doped with lead oxide PbO and bismuth oxide, Bi ₂ O ₃ is that shown in Table 6.

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Molar and gravimetric oxide composition for doped boron-phosphate glass code BPM8

Table 6

Glass Oxide B ₂ O ₃ p ₂ or ₅ Read ₂ O AI ₂ O ₃ ZnO Bi ₂ O ₃ PbO Total BPM8 % molar 5 14 2 2 2 15 60 100 BPM8 % gravimetric 100

Pre-melting programs are performed at lower speeds and intermediate bearings for temperatures of 175 ° C and 275 ° C. The melting temperature is lowered by 250 ° C to 1000 ° C. The speed of the refractory stirrer is 175 and 125 rpm and it is positioned above the bottom of the crucible. For BPM8 glass, the melting - conditioning - homogenization program is the one presented in table 7.

Pre-melting - melting - mechanical homogenization program for BPM8 glass

Table 7

Time [h] Temperature [° C] Stirring speed [rpm] 0 20 0.5 70 1 120 1.5 175 2 1751 2.25 175 2.5 175 2.75 two hundred 3 220 3.25 240 3.5 260 3.75 275 4 275 4.25 275 4.5 275 4.75 275 5 275 5.25 300 5.5 325 5.75 350

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Table 7 (continued)

Time [h] Temperature [° C] Stirring speed [rpm] 6 375 6.5 425 7 500 7.5 600 8 700 9 1000 10 1000 175 10.5 1000 175 11 1000 175 12 975 125 12.5 950 125 13 950 125 13.5 950 125 14 950 -

The annealing program for BPM8 glass is similar to that in Example 1, but the annealing temperature is 400 ° C.

Indication of how the invention is likely to be applied industrially. The invention can be applied industrially to obtain bottles for Faraday rotators or high quality magneto-optical sensors, as well as to any applications requiring materials with magneto-optical properties, the product according to the invention being obtained with low energy consumption and price, as well as mechanical strength, improved thermal and chemical compared to classic phosphate bottles.

Claims (2)

RO 132655 Β1 demand 1. Boron-phosphate bottles containing lithium oxide, aluminum oxide and zinc oxide, doped with rare earths, transitional and post-transitional metals, characterized in that they consist of a mixture of 5 ... 20% B ₂ O ₃ and 14 ... 75% P ₂ O ₅ , as well as glass modifiers 2 ... 15% Li ₂ O, chemical, thermal and mechanical stabilizers 2 ... 20% AI ₂ O ₃ and 2 ... 20% ZnO, 3 ... 75% oxides of transition metals: CoO, FeO, Fe ₂ O ₃ , Fe ₃ O ₄ , V ₂ O ₃ , ZrO ₂ , Nb ₂ O ₃ , MoO ₂ , WO ₃ , oxides of transition metals: Sn ₂ O ₃ , Sb ₂ O ₃ , PbO, Bi ₂ O ₃ , and rare earth oxidesTb ₂ O ₃ , Dy ₂ O ₃ , CeO ₂ , Eu ₂ O ₃ , Pr ₂ O ₃ , Nd ₂ O ₃ , Sm ₂ O ₃ , Gd ₂ O ₃ , Ho ₂ O ₃ , Er ₂ O ₃ , Tm ₂ O ₃ and Yb ₂ O ₃ , molar percentages. Process for obtaining boron-phosphate bottles according to Claim 1, characterized in that it has the following steps: wet preparation of the mixture of raw materials, gravimetric and volumetric dosing of the raw materials, introduction of the raw materials into the homogenization vessel in the order cold, homogenization of the raw materials, by mechanical homogenization, partial drying with partial removal of water under stirring and with continuous mixing, up to temperatures of 12O ... 15O ° C, pouring the mixture when it is still fluid, into the melting crucible , melting at temperatures between 150 ... 900 ° C with slow controlled temperature rise, melting, at temperatures of 950 ... 1300 ° C, melting the mixture of raw materials, refining the melt, homogenizing the melt, conditioning the melt, and then shaping glass by pouring the conditioned glass melt into pure spectral graphite molds, preheated in the annealing furnace, at the annealing temperature, d cutting with a diamond disk, grinding and polishing with silicon carbide of 250, 400 and 600 mesh and finally with the help of cerium oxide suspensions, with a minimum granulation of 800 mesh.