LV11172B - Method for production of modified ceramic condenser materials based on titanium oxides - Google Patents

Abstract

Invention concerns method for production of modified titanium dioxide ceramic material, including production of inorganic substances, the synthesis of which is carried under the impact of oxygen or air plasma, used in production of dielectric ceramic condensers.More dense and harder ceramic material is to be obtained in ecologically pure synthesis carried out in reactor under the impact of low temperature plasma. Oxide powders, including titanium, aluminium, silicon, scandium, and magnesium oxide powders are treated with low temperature oxygen or air plasma. This is followed by vapour condensation. Powder of delicate (50-100 nm) fuzzy particles that clamps in dense material with 1.5-1.8% microporosity , pore size (1.8-2)x10<3> nm and microhardness (925-930)x10<3> kg/m<2> at 1,170-1,220 K is obtained when temperature of plasma is 5,200-5,800 K , temperature of gases used in the hardening is 2,400-3,600K, relation between aggregate and consumed plasma gas is 0.12-0.2, relation between gases used in hardening and plasma gas is 0.6-1.2.

Description

The present invention relates to a process for the preparation of a modified ceramic material of titanium dioxide, including the extraction of inorganic substances by synthesis of oxygen or air plasma for use in the manufacture of dielectric ceramic capacitors.

Modified Ti0 ₂ is one of the best compounds, technically and economically, for the production of capacitor materials / 1 /. The high demands on the dielectric properties of capacitor materials (e.g., 10 "dielectric losses) can only be met by obtaining very dense ceramics. Extremely high ceramic and mechanical properties should be the material when making large-format or complex configuration products. Thin film capacitor dielectric characteristics can be improved if a high-frequency generator magnetroniskā as a target could be used instead of a ceramic mosaic (Latv.pat. No. P-92-14, Int Cl ⁵ Ξ01 Β 3A2, 1994.J) (TIQ ₂ 80,4- 88.2 wt%, MgO 0.1-0.3 wt%, Al ₂ U ^ 5.8-16.7 wt%, SiO ₂ 1.1-9.3 wt%) / 2 / , but a monolithic '0.2 m drive.

The most common method of obtaining dielectric ceramic material is ceramic based on mechanical mixing, continuous milling and sintering (USSR aut.

No. 1271850. Int. Cl ⁵ 35/46, Ξ01 B 3/12, 1986) / 3 /. The disadvantage of this sophisticated technique is the prolonged grinding and mixing operations, during which the product is contaminated by the milling bodies. This leads to the formation of pores and inclusions on the surface of the ceramic, resulting in microporous density (> 6%), thermal expansion coefficient (<85 degrees) and electrical properties (dielectric loss A 10 ^).

Increasing the mechanical strength of the material (800-920 g / mm) and reducing the microporousness (4-6.3%) can be achieved by modifying titanium dioxide ceramics by chemical deposition (US Pat. No. 5049528, Int. 01 ^ 004 B 35/02 , 1991) / 4 /. The main disadvantage of this method is the large amounts of waste water containing toxic substances. Ti0 ₂ ceramics, which are modified by chemical deposition difficult sasmalcināma.cādi train, powder particles of not less than 500 to 5000 nm.

The finer powders (particle size 20-4Ό0 na) and without toxic waste water enter the oasis phase by flame hydrolysis one nl-./J (2333 aut. Fr. 1 '/ 51720 Irt.

0 ^? 5/46,

1992), 5, · The specific surface area of the obtained powder is 250-300 thousand, the disadvantage of this method is air pollution in the air and it also makes the process more expensive in many stages of the process.

to obtain a fine grind, the titanium dioxide ceramic is ground in water with a vinyl acetate dispersant, dried and crushed with copolymer vim.yl acetate-malea.acid di semen (2S2.S aut. app. Ir.15234-65. | -

Int. Ol ² 004 · 2 55/46, 1939) / 6 /. In the absence of this method, the product contains a further 0.2-1.0 wt.% Of the dispersant, 15.1-29, in the form of a liquid phase which determines relatively porous <microporous rp / \ mechanically resistant (micro-hardness 530 s). / mm ^1-) ceramic iejūsan _ļ either a low thermal expansion coefficient (k 36.10 jrad ^z '~). Closest to the technical solution, what is proposed is titanium dioxide modification by chemical deposition to reduce process, duration and energy consumption, feedstock mixing and material synthesis by injection of feedstock solutions in a reactor under pressure (2S23 aut. Tr. 1753562. Int. 01 ^ 55/45, 1992, prototype) / 7, · For this purpose, the solution is mixed in molar: 3a0l2 = (3-15): 1 by spraying at a pressure of 1.2-5,

Tk 3n: 3aCl ₀ + TiO _{4 4} (4.5-6.0): 1. Blown ao, ^.

low chlorine ions and calcined in monolithic products at sintering temperatures of 1170-1220 T. The disadvantage of this method is the large amounts of waste water containing toxic substances. 7i0 _? ceramic, modified by chemical deposition, is hard to grind ^! Ian. ~ tzecnoa like this:

atm over solution of null sue s of f i 1 tr e, i zp and v erc. an nn;

.v minor - <ξ: 00-5000 nm.

Ceramic obtained by prototype technology is quite porous, (micrororality 4-6%, pore size (4-3) .10 ^ nm and relatively low hardness, micro-hardness (630-920) .10 ^ kg, m * ^- /.

The object of the present invention is to provide an ecologically pure synthesis process which obtains a powertrain active particle powder, which densely sinter the monolithic ceramic parts in a sintering process, producing high density and micro hardness products.

In order to blow denser and harder ceramics, we offer an ecologically clean synthesis process in a low-temperature plasma reactor.

BAD ORIGINAL

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For dispersing active oxide powders in dispersed dispersions, their homogeneous mixtures are carried. complex compounds, coarse dispersed powders of titanium, aluminum, silicon, sneeze, mapnium compounds with a particle size (20-130) .13 µm are treated with oxygen or generate low temperature plasma with subsequent vapor condensation. 2im purpose raw material powder with towing _e āz5. - Oxygen or vapor is supplied to the low temperature plasma beam by high frequency discharge at temperature. and 5203-5303. the bundle undergoes decomposition and evaporation of the raw materials, as well as the vapor mixing of the components, which gives the blown sheaf? u.psto the vigor. Next, the low-temperature plasma with oxide vapors at temperatures of 2400-5300 22 is fed into a quenching oxygen or cold bag. The rapid cooling of the bundle determines the formation of a highly dispersed powder of oxide, mixtures or compounds. The introduced spherical particles are 100 nm in size. The particle size is determined by the particle concentration in the bundle (ratio of mass to plasma yeast consumption), the ratio of annealing to the plasma forming nase, the temperature of the beam in the area of the quenching phase.

the ratio of the consumption of _Q- plasma to plasma-forming _Q is 0.123.2 and that of quenching to plasma-forming isase is 0.3-1.2. the reported ratios and the beams temperature (2400-3600 k) in the quenching gas injection zone were determined experimentally by studying the dependence of specific surface and particle sizes on undetermined parameters.

Synthesized modified, sr KjO, Al ₂ 0 ^ 0 ^ _o 3c and Si0 _o oxides of titanium dioxide compacts disks of 0.01 to 0.10 m in diameter at a pressure of 500-1500 K / cm "and fired at a temperature of 1170 to 1220 k. Table 1 shows the composition and physical properties of the blown and prototype material of the proposed technology.

Example.

2.7 nas., 3 2. _3, 4, ^ mas.% 11-0-, ->?

it.3 Sc-, 0- and 30 riOp ovoids with a trawling barrier oadod low-temperature plasma o with high frequency discharge (af power density 11 W / cn ^- ) with a resolution of 5300 bundle 22 <decomposition of raw materials, evaporation, component vapor mixing. The following is a description of the low temperature plasma temp of ousmus from:

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The synthesized powder is pressed into disks at 0.1 m at 5o0 kg / cm and calcined at 1170 E for 1 h. endurance.

The following examples were executed with an analogous, technology-only change in component ratios, plasma to quench temperature, mass to plasma gas ratio, quench to plasma ratio. If the ratio of the mass of powder to the gas constituting the plasma increases above 0.2, the particle size increases and the activity of the powder decreases. As this ratio drops below 0.12, the particle size decreases, but also the process productivity decreases and the power consumption increases. The quenching-to-plasma gas ratio decreases - below 0.6 - inefficient because low quenching gas consumption does not significantly reduce bundle temperature and does not improve particle growth conditions. Increasing the quenching / plasma forming gas ratio above 1.2 does not significantly reduce the particle size, so further increasing the ratio is not useful. High cooling speeds prevent the formation of composite connections. If the quenching gas is supplied to the crucible with a temperature above 3600E, the particle size will increase because the powder will not evaporate completely due to the short contact time of the particles with the beam. Lowering the quenching gas temperature below 2400 E has little effect on particle size and powder composition as oxide condensation and particle growth occur at much higher temperatures.

Compared to the prototype, the proposed process, while maintaining a high T1O2 content (78.9-81.4 wt%), low ceramic firing temperature (1170-1220 E), allows synthesis of 3-15 finer, fluffy particle powders that sinter during the firing process. 2 to 3 times denser in ceramics with a 5% increase in microhardness. The multiplied properties of the ceramic greatly increase the material's service life: it is possible to produce large parts and reduce dielectric losses.

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1. Obtaining Transparent Thin Films of Oxides and Metaloxynitrides by High-Frequency Lightning Evaporation / A.Gorin, V.Kilasovs, A.Martinovs, etc. // Electrical Engineering, 1991 · - N.6pp. 3-12.

2. Latv.R. pat. Int. Cl ^ ΗΘ1Β 3/12. Dielectric Thin Film Material / I.Aboltiņa, R.Ramata, J.Kļaviņš, etc. Accepted 04.03.94.

3- I27135O. USSR autopl. Int. Ol ⁵ CO4B 35/46, HOIB 3/12. Production of Segmented Ceramic Capacitor Shaft / E.Mamčic, I.Bertošs, V.Larčeva, V.Kotļar. Iesn. 12/30/84. IT. 3832228 / 29-55 »Publ. 11/21/86. Bil. IT. 43.

4. 5049528. U.S. Pat. Int. Cl ^ C04B 35/02. Method for Preparation of Captive Composition by Polymer Solution / W.Moffatt. Publ. 9/17/91. Bil.S. 1130.— N. 3.

5. 1761720. USSR aut.apl. Int. 01 ^ C04B 35/46. Ceramic material / J.Mazurkevich, l.Zozulu, I.Kobasa, etc. Iesn. 6/15/89.

N. 4705427/55. Publ. i5.O9.92. Bil. IT. 34.

6. 1628466 USSR aut.apl. Int. Cl ^ C04B 35/46. Powdered Ceramic · as a Fabricated Material Surface Reflection Technique for the Production of Monolithic Capacitors /. Iesn. 13-02.89. Publ. 15.10.92.

Bil. N. 38.

7. 1768562. USSR aut.apl. Int. 01 ^ 004B 35 46 .._ Magnetic._head. method of obtaining titanium and barium oxide material of plates / T.Limar, J.Kagan, L.Shepelenko et al. Iesn. 7/19/90.

IT. 4852818/26. Publ. 15.10.92. Bil. IT. 38. Prototype.

Claims (1)

Formula of the Invention The process for the production of modified titanium dioxide ceramic material / monolithic capacitors / process, which simultaneously mixes the reactor in the reactor and synthesizes the material with subsequent sintering to a sintering temperature, is characterized by the fact that the oxide mixing and condensation.