Ceramic material and method of its production

 

(57) Abstract:

Usage: as contrast agents in radiology, as well as to obtain phosphors, the active medium of the laser pigments. The inventive material includes at least one oxide of element M2O3selected from the group of oxides of trivalent elements, where M is Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Bi, In, Rh, Sb, Ga 50-55, Ta2O5or Ta2O5and Nb2O5the rest is up to 100%. A mixture of oxides of the corresponding trivalent elements homogenized, annealed at a temperature of 1000 to 1300oC, this step raises the temperature at the 50oC with a dwell time at each increase for 8 - 10 hours, before each temperature increase spend homogenization of the mixture. 2 S. p. f-crystals, 1 table.

The invention relates to inorganic chemistry, in particular ceramic material and method of its production, suitable for use in radiology and can be used as a radiopaque substances for the diagnosis of larynx, trachea, bronchi, abdominal neoplasms, digestive tract, urinary and biliary tract, as well as to obtain phosphors, the active medium of the laser, pigments and the.To. Szymanowski N. L. A radiopaque contrast agent, M. Medicine, 1980, S. 217). However, its disadvantage is the low energy absorption coefficient of x-rays in the energy interval used in x-rays and, hence, low contrast. In addition, because of the dark color it is hardly seen on the mucous membrane.

The closest in technical essence to the proposed material is a composition of the inorganic filler containing various combinations of, for example, oxides of La2O3, SrO, Gd2O3, Y2O3Ta2O5(U.S. patent N 4714721, C 04 B 35/01, 1987). The filler particles may be present in the material in the form of, for example, the calcined product or mixture of initial components. This filler can be used as a radiopaque substance. The ratio of the initial components in a known filler next weight. Gd2O31 - 31,0; SrO 7 32,0; La2O30 18; the sum of the oxides Gd2O3+ SrO + La2O324,0 40,0. Here the proportion Gd2O3and/or La2O3and/or SrO may partially be substituted with up to 5 weight. for example, at least one of the oxides of Y2O3or Ta2O5.

Insufficient the material in the energy range 15 - 150 Kev.

Also known is a method of obtaining compounds MTaO4where M is a rare earth element (Compounds of rare earth elements. Zirconate, garraty, niobates, tantalate, antimonate. M. Nauka, 1985, S. 87-89). According to the method of initial oxides pressed and annealed at a temperature of 1250oC for 70 h or 1500oC for 48 hours And annealing the pressed samples is carried out in 2 to 3 stages with intermediate homogenization every 10 to 20 h annealing.

The disadvantage of this method is the production of a material in the form of tablets, resulting in the impossibility of applying it to the tissues of the body.

The technical result of the invention is the increase of the coefficient of x-ray absorption (a) of ceramic material in the energy range 15 to 150 Kev, which increases its contrast or luminescence intensity.

To achieve provided by the invention technical result of the proposed ceramic material containing at least one oxide of M2O3selected from the group of oxides of trivalent elements, where M Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Bi, In, Rh, Sb, Ga, and Ta2O5or Ta2O5and Nb<5or Ta2O5and Nb2O5- the rest is up to 100,

which corresponds to the empirical formula

M1xTaa1xO4x (1)

or

M1x(Ta1-yNby)1+/-xO4+/-x< / BR>
where 0x0,1

0y0,1

and the method thereof, which consists in obtaining a ceramic-based material of the oxide of the element M2O3selected from the group of oxides of trivalent elements, where M Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Bi, In, Rh, Sb, Ga, and Ta2O3or Ta2O5and Nb2O5and includes homogenization of the mixture of the respective oxides of trivalent elements, the annealing mixture, cooling to room temperature, and the material has the following ratio of components, mol.

M2O350 55

Ta2O5or Ta2O5and Nb2O5- the rest is up to 100

the annealing is conducted at a temperature of 1000 to 1300oC, this step raises the temperature of annealing at 50oC and maintained at each step the temperature rise 8 10 h, at the same time before each increase of annealing temperature hold intermediate homogenization of the mixture.

At the present time of patent and technical literature is not the SUB>2O5in the claimed relationship, and how to obtain it.

The proposed method consists in the following. The initial mixture consisting of at least one oxide of trivalent element selected from the group Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Bi, In, Rh, Sb, Ga and tantalum oxide or tantalum oxide and niobium oxide, taken in the following ratio of components, mol.

M2O350 55

Ta2O5or Ta2O5and Nb2O5- the rest is up to 100

thoroughly homogenized in a ball mill, moistening the mixture with ethyl alcohol, then placed in Lundby crucible or crucible of the noble metal and annealed in air at a temperature of 1000 to 1300oC at this step raises the temperature at the 50oC and maintained at each step the temperature rise 8 10 h, and prior to each subsequent temperature increase spend intermediate homogenization of the mixture. After annealing the samples are removed from the furnace and arbitrarily cooled to room temperature. The completeness of the final product control rentgenofazovym (XRD) and chemical (HA) tests. The output is 100%, the absorption Coefficient of x-ray radiation in the energy range 15 to 150 Kev and the tube 60 kV. Use aluminum filter phantom thickness of 22 mm, the Value of a (101)/10where 10the intensity incident on the target radiation 1 the intensity of radiation transmitted through the target. The measurements were conducted at shestipolosnoy apparatus. The average particle size determined photosedimentation analysis instrument company "Fritsch".

The method is illustrated by the following examples,

Example 1. Take 5,00 g Ce2O3and 6,09 g Ta2O5thoroughly homogenized in a ball mill with 2 ml of ethanol for 30 minutes the Mixture is placed in alongby the crucible and put into the oven. Annealed in air at a temperature of 1000oC for 9 h, and then the crucible is removed from the furnace and cooled in air to room temperature. Then the mixture is again homogenized in a ball mill for 30 min with the addition of 2 ml of ethanol, placed in a crucible, then put into the oven, raise the oven temperature by 50oC up to a temperature of 1300oC, which is the final temperature of annealing. According to the HA receives the material composition, mol% Ce2O3- 52, Ta2O548. According to the XRD structure of monoclinic material. The absorption coefficient in the energy range 15 to 150 Kev a 0,29 0,46; average particle size of 19 μm. Output the material composition (mol%): Pr2O352, Ta2O548. The structure is monoclinic. The absorption coefficient a 0,29 0,46, the average particle size of 18 microns.

Examples 3 59 presented in the table. Conditions obtain as in example 1.

Examples 17 to 48 (see table). show property boundary compositions obtained as in example 1.

Examples 49 to 52 (see table). show properties of the material containing combinations of oxides M2O3. Conditions obtain as in example 1.

To prove the materiality of the requested interval the contents of the components in the composition of the material and conditions you receive the following examples.

Example 60. Take 3.00 g La2O3and 9,49 g Ta2O3and treated as in example 1. Get the material composition, mol% of La2O330, Ta2O370. However, this material has an absorption coefficient of 0.20 to 0.23, i.e., less contrast than proposed. In addition, it decomposes in water at the temperature of the human body. The structure is a mixture of hexagonal, monoclinic and orthorhombic structures.

Example 61. Take 6,00 g Y2O3and Ta2O5and processed as in example 1. Receive material mole Y2O3- 70; Ta2

Example 62. Take 5,00 g Ce2O3and Ta2O5and processed as in example 1, but starting temperature annealing 900oC. Receive material Ce2O352; Ta2O548 mol but the absorption coefficient a of 0.20 to 0.25. Therefore, the material is less contrast than obtained by the proposed method.

Example 63. Take 5,00 g Ce2O3and 6,09 g Ta2O5and treated as in example 1, but the final temperature annealing 1400oC. Receive material mole Ce2O352; Ta2O5- 48 with properties as in example 1. However, it is a waste of energy.

Example 64. Take 5,00 g Ce2O3and 6,09 g Ta2O5and treated as in example 1. But stepwise temperature increase lead through 100oC. Receive material, mol Ce2O352; Ta2O548. The coefficient a of 0.20 to 0.25. Therefore, it is less contrast than obtained by the proposed method.

Example 65. Take 5,00 g Ce2O3and 6,09 g Ta2O5and clicks; a2O548. The coefficient a of 0.20 to 0.25. Therefore, it is less contrast than obtained by the proposed method.

Example 66. Take 5,00 g Ce2O3and 6,09 g Ta2O5and treated as in example 1, but the final annealing is carried out for 15 hours Receive material mole Ce2O352; Ta2O5- 48 with properties as in example 1, but it is a waste of energy.

Example 67. Take 5,00 g Ce2O3and 6,09 g Ta2O5and treated as in example 1, but after annealing at 1000oC does not perform homogenization of the mixture. Receive material, mol Ce2O352; Ta2O548. The coefficient a of 0.20 to 0.25. Therefore, it is less contrast than obtained by the proposed method.

Other examples are given in the table.

1. Ceramic material on the basis of at least one oxide of element M2O3selected from the group of oxides of trivalent elements, where M Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Ri, In, Rh, Sb, Ga and Ta2O5or Ta2O5and Nb2O5, characterized in that the composition of the material has the following ratio of components, mol.

M2O350 55

Ta2O5or Ta is ve at least one oxide of element M2O3selected from the group of oxides of trivalent elements, where M Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, La, Bi, In, Rh, Sb, Ga and Ta2O5or Ta2O5and Nb2O5including homogenization of the mixture of the respective oxides of trivalent elements, the annealing mixture, cooling to room temperature, characterized in that the composition of the material has the following ratio of components, mol.

M2O350 55

Ta2O5or Ta2O5and Nb2O5- The rest is up to 100%

the annealing is conducted at a temperature of 1000 to 1300oWith speed raise the annealing temperature 50oC and maintained at each step the temperature rise 8 10 h, and before each increase of annealing temperature hold intermediate homogenization of the mixture.

 

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