Titanium-containing calcium hexaaluminate material and preparation method thereof

Abstract

A titanium-containing calcium hexaaluminate material and preparation method thereof is disclosed. The technical solution is: using 60˜80 wt % alumina micro powder, 5˜20 wt % calcium-containing micro powder, 10˜20 wt % titania micro powder and 1˜10 wt % manganese oxide micro powder as raw materials, blending the raw materials evenly in a planetary ball mill to obtain a blend, machine pressing the blend at 100˜200 MPa to obtain a green body, drying the green body at 110˜200° C. for 12˜36 h, and incubating the dried green body at 1500˜1800° C. for 1˜8 h to obtain the titanium-containing calcium hexaaluminate material. The present disclosure has low cost and simple process, and the prepared titanium-containing calcium hexaaluminate material has the characteristics of good chemical stability, high thermal shock resistance and strong melt resistance to titanium-aluminum alloy.

Claims

1. A method of preparing a titanium-containing calcium hexaaluminate material, comprising: blending 60-80 wt % alumina powder, 5-20 wt % calcium-containing powder, 10-20 wt % titania powder and 1-10 wt % manganese oxide powder in a planetary ball mill to obtain a blend; machine pressing the blend under 100-200 MPa to obtain a green body; drying the green body at 110-200° C. for 12-36 h; and incubating the dried green body at 1500-1800° C. for 1-8 h to obtain the titanium-containing calcium hexaaluminate material.

2. The method of claim 1, wherein a Al.sub.2O.sub.3 content of the alumina powder is 98 wt % or more, and a particle size D.sub.50 of the alumina powder is 1-8 μm.

3. The method of claim 1, wherein the calcium-containing powder is one or more of calcium hydroxide and calcium carbonate; and a particle size D.sub.50 of the calcium-containing powder is 1-10 μm.

4. The method of claim 1, wherein a TiO.sub.2 content of the titania powder is 90 wt % or more, and a particle size D.sub.50 of the titania powder is 1-10 μm.

5. The method of claim 1, wherein a MnO content of the manganese oxide powder is 90 wt % or more, and a particle size D.sub.50 of the manganese oxide powder 1-8 μm.

Description

DETAILED DESCRIPTION OF EMBODIMENTS

(1) The disclosure is further described below in combination with specific embodiments, not as a limitation to its scope of protection.

(2) To avoid duplication, the raw materials involved in the embodiments are uniformly described as follows and are not given unnecessary details in the particular embodiments.

(3) The Al.sub.2O.sub.3 content of the alumina micro powder was 98 wt % or more, and the particle size D.sub.50 of the alumina micro powder was 1˜8 μm.

(4) The particle size D.sub.50 of the calcium-containing containing micro powder was 1˜10 μm.

(5) The TiO.sub.2 content of the titanium oxide micro powder is 90 wt % or more, and the particle size D.sub.50 of the titanium oxide micro powder is 1˜10 μm.

(6) The MnO content of the manganese oxide micro powder is 90 wt % or more, and the particle size D.sub.50 of the manganese oxide micro powder is 1˜8 μm.

Embodiment 1

(7) A titanium-containing calcium hexaaluminate material and preparation method thereof. 60˜65 wt % alumina micro powder, 15˜20 wt % calcium-containing micro powder, 15˜20 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(8) The calcium-containing micro powder is calcium hydroxide.

(9) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 92 wt %.

Embodiment 2

(10) A titanium-containing calcium hexaaluminate material and preparation method thereof. 60˜65 wt % alumina micro powder, 15˜20 wt % calcium-containing micro powder, 15˜20 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(11) The calcium-containing micro powder is calcium carbonate.

(12) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 92 wt %.

Embodiment 3

(13) A titanium-containing calcium hexaaluminate material and preparation method thereof. 60˜65 wt % alumina micro powder, 15˜20 wt % calcium-containing micro powder, 15˜20 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(14) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(15) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 90 wt %.

Embodiment 4

(16) A titanium-containing calcium hexaaluminate material and preparation method thereof. 60˜65 wt % alumina micro powder, 15˜20 wt % calcium-containing micro powder, 15˜20 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(17) The calcium-containing micro powder is calcium hydroxide.

(18) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 90 wt %.

Embodiment 5

(19) A titanium-containing calcium hexaaluminate material and preparation method thereof. 65˜67 wt % alumina micro powder, 12˜17 wt % calcium-containing micro powder, 13˜18 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(20) The calcium-containing micro powder is calcium carbonate.

(21) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 93 wt %.

Embodiment 6

(22) A titanium-containing calcium hexaaluminate material and preparation method thereof. 65˜67 wt % alumina micro powder, 12˜17 wt % calcium-containing micro powder, 13˜18 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(23) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(24) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 93 wt %.

Embodiment 7

(25) A titanium-containing calcium hexaaluminate material and preparation method thereof. 65˜67 wt % alumina micro powder, 12˜17 wt % calcium-containing micro powder, 13˜18 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1650˜1800° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(26) The calcium-containing micro powder is calcium hydroxide.

(27) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 91 wt %.

Embodiment 8

(28) A titanium-containing calcium hexaaluminate material and preparation method thereof. 65˜70 wt % alumina micro powder, 12˜17 wt % calcium-containing micro powder, 13˜18 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(29) The calcium-containing micro powder is calcium carbonate.

(30) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 90 wt %.

Embodiment 9

(31) A titanium-containing calcium hexaaluminate material and preparation method thereof. 70˜75 wt % alumina micro powder, 8˜13 wt % calcium-containing micro powder, 12˜16 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(32) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(33) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 94 wt %.

Embodiment 10

(34) A titanium-containing calcium hexaaluminate material and preparation method thereof. 70˜75 wt % alumina micro powder, 8˜13 wt % calcium-containing micro powder, 12˜16 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(35) The calcium-containing micro powder is calcium hydroxide.

(36) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 94 wt %.

Embodiment 11

(37) A titanium-containing calcium hexaaluminate material and preparation method thereof. 70˜75 wt % alumina micro powder, 8˜13 wt % calcium-containing micro powder, 12˜16 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(38) The calcium-containing micro powder is calcium carbonate.

(39) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 91 wt %.

Embodiment 12

(40) A titanium-containing calcium hexaaluminate material and preparation method thereof. 70˜75 wt % alumina micro powder, 8˜13 wt % calcium-containing micro powder, 12˜16 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(41) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(42) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2).sub.6O.sub.19 phase content greater than 92 wt %.

Embodiment 13

(43) A titanium-containing calcium hexaaluminate material and preparation method thereof. 75˜80 wt % alumina micro powder, 5˜10 wt/calcium-containing micro powder, 10˜14 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(44) The calcium-containing micro powder is calcium hydroxide.

(45) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 95 wt %.

Embodiment 14

(46) A titanium-containing calcium hexaaluminate material and preparation method thereof. 75˜80 wt % alumina micro powder, 5˜10 wt/calcium-containing micro powder, 1˜14 wt % titania micro powder and 1˜6 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(47) The calcium-containing micro powder is calcium carbonate.

(48) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 95 wt %.

Embodiment 15

(49) A titanium-containing calcium hexaaluminate material and preparation method thereof. 75˜80 wt % alumina micro powder, 5˜10 wt/calcium-containing micro powder, 10˜14 wt % titania micro powder and 4˜10 wt/manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 100˜150 MPa to obtain a green body. The green body was dried at 150˜200° C. for 12˜24 h. The dried green body was incubated at 1500˜1650° C. for 4˜8 h to obtain the titanium-containing calcium hexaaluminate material.

(50) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(51) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2)O.sub.19 phase content greater than 92 wt %.

Embodiment 16

(52) A titanium-containing calcium hexaaluminate material and preparation method thereof. 75˜80 wt % alumina micro powder, 5˜10 wt/calcium-containing micro powder, 10˜14 wt % titania micro powder and 4˜10 wt % manganese oxide micro powder were used as raw materials. The raw materials were blended evenly in a planetary ball mill to obtain a blend. The blend was machine pressed at 150˜200 MPa to obtain a green body. The green body was dried at 110˜160° C. for 24˜36 h. The dried green body was incubated at 1650˜1800° C. for 1˜5 h to obtain the titanium-containing calcium hexaaluminate material.

(53) The calcium-containing micro powder is a mixture of calcium hydroxide and calcium carbonate.

(54) The titanium-containing calcium hexaaluminate material prepared in this embodiment was tested to have a Ca((Al.sub.0.84Ti.sub.0.16).sub.2).sub.6O.sub.19 phase content greater than 91 wt %.

(55) Compared with the prior art, the disclosure has the following beneficial effects.

(56) (1) The alumina micro powder, calcium micro powder, titania micro powder and manganese oxide micro powder are taken as raw materials, blended evenly, machine pressed into shape, dried and treated by high-temperature heat to obtain the titanium-containing calcium hexaaluminate material with simple process. The raw materials used in the disclosure have wide sources. In addition, compared with the electrofusion method, the energy consumption of the titanium-containing calcium hexaaluminate material prepared by the sintering method is lower. Therefore, the production cost is low.

(57) (2) The calcium-containing micro powder used in the disclosure decomposes during the heat treatment process to form high activity CaO powder, which can react rapidly with other micro powder raw materials. In addition, the introduced manganese oxide micro powder can replace aluminum ions and titanium ions by solution treatment. On the one hand, the reaction of raw materials is promoted to form Ca((Al.sub.0.84Ti.sub.0.16).sub.2).sub.6O.sub.19 titanium-containing calcium hexaaluminate phase; on the other hand, the lattice of titanium-containing calcium hexaaluminate phase is stabilized to prevent desolvation during cooling. Therefore, the TiO.sub.2 component in the titanium-containing calcium hexaaluminate material can stably exist in the titanium-containing calcium hexaaluminate phase during the cooling process, which is not easy to desolvent and has good chemical stability.

(58) (3) The TiO.sub.2 components in the present disclosure are all able to stably exist in the titanium-containing calcium hexaaluminate phase during the heating-cooling process, avoiding the occurrence of solution-desolvation phenomenon during the heating-cooling process. When the temperature change occurs, the material internal components and the structural changes are not large, which effectively reduces the probability of heat stress generation. Therefore, the titanium-containing calcium hexaaluminate material has good thermal shock resistance.

(59) (4) The product of the present disclosure has a low content of impurity phases, where the main material phase composition is Ca((Al.sub.0.84Ti.sub.0.16).sub.2).sub.6O.sub.19 phase. The material components are uniform with both TiO.sub.2 and Al.sub.2O.sub.3 components in the material phase. When it is in contact with the titanium-aluminum alloy melt, the interactions of Ti components and Al components in the alloy melt and the refractory material are inhibited simultaneously. Therefore, the erosion of the titanium aluminum alloy melt is better resisted. The product is an ideal raw material to prepare refractory materials for titanium-aluminum alloy melting.

(60) As examined, the content of Ca((Al.sub.0.84Ti.sub.0.16).sub.2).sub.6O.sub.19 phase in the titanium-containing calcium hexaaluminate material prepared in the present disclosure was more than 90 wt %.

(61) Therefore, the present disclosure has low cost and simple process, and the prepared titanium-containing calcium hexaaluminate material has the characteristics of good chemical stability, high thermal shock resistance and strong melt resistance to titanium-aluminum alloy, which is an ideal raw material for preparing refractory material for titanium-aluminum alloy melting.