CN101830715A - Preparation method of CaO refractory and crucible for titanium alloy smelting - Google Patents
Preparation method of CaO refractory and crucible for titanium alloy smelting Download PDFInfo
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- CN101830715A CN101830715A CN 201010167509 CN201010167509A CN101830715A CN 101830715 A CN101830715 A CN 101830715A CN 201010167509 CN201010167509 CN 201010167509 CN 201010167509 A CN201010167509 A CN 201010167509A CN 101830715 A CN101830715 A CN 101830715A
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Abstract
The invention relates to a preparation method of CaO refractory and a crucible for titanium alloy smelting with high hydrability resistance, belonging to the technical field of the preparation process of high-temperature refractory. In the preparation method, a raw material formula of the CaO refractory comprises 82-92mol percent of calcium oxide, 5-15mol percent of zirconium oxide and 1-5mol percent of titanium oxide; in addition, a binder polyvinyl butyral (PVB) is added with the weight accounting for 2-3 percent of the total weight of the oxides; then burdening, ball-milling and molding are carried out to prepare a platy sample or a crucible green body; then sintering is carried out at 1700-1780 DEG C; and finally the CaO refractory is prepared. The CaO refractory prepared by the method has the characteristics of good thermal stability and high hydrability resistance; and a hydrability test shows that the hydration rate of the refractory is lower than 0.2 percent and the volume density of the refractory is 3.37-3.59g/cm<3>.
Description
Technical field
The present invention relates to a kind of titanium or titanium alloy melting that is used for, and have high hydration resistance can the CaO refractory materials and the preparation method of crucible, belong to high-temperature refractory fabricating technology field.
Technical background
Along with the high quality of molten steel, relevant refractory materials is had higher requirement the particularly refractory materials requirement that can not pollute molten steel.The CaO refractory materials does not only pollute molten steel and can catch oxide inclusion in the molten steel, has the effect of purify hot metal, and aboundresources, cheap; The CaO refractory materials also has certain advantage aspect smelting titanium alloy in addition, but CaO aquation very easily in air, so its use is restricted.
Although the various constantly development to some extent of technology that prevent the CaO aquation, aquation is still inevitable.Some surface preparations can improve the hydration resistance of CaO refractory materials to a certain extent, but the not basic problem that solves the easy aquation of CaO material, and the film that forms on surface chance thermal capacitance is easily decomposed the use properties of restriction goods.Another kind method is to introduce salt or oxide-based additive, coats CaO crystal grain, forms the hydration resistance that improves the CaO refractory materials in conjunction with firm tissue simultaneously.Using very successful as refractory materials is the Compound C aZrO3 of CaO and ZrO2, CaZrO3 is the high and the most stable a kind of compound of CaO content in the CaO2-ZrO2 system, and stable performance aspect smelting titanium alloy is an ideal titanium alloy melting refractory materials.This research is exactly under the prerequisite of not destroying CaO character, adopts the method for introducing additive ZrO2, TiO2 to improve the hydration resistance and the sintering character of CaO refractory materials, obtains a kind of crucible refractory material of titanium alloy melting preferably.
Summary of the invention
The purpose of this invention is to provide a kind of titanium or titanium alloy melting that is used for, and have high hydration resistance can the CaO refractory materials and the preparation method of crucible.
The present invention is a kind of CaO refractory materials of titanium alloy melting and preparation method of crucible of being used for, and it is characterized in that having following process and step:
A. determine and the design composition of raw materials that the raw material composition and the molar percentage thereof of this refractory materials are as follows:
Calcium oxide 82～92%,
Zirconium white 5～15%,
Titanium oxide 1～5%;
Binding agent polyvinyl butyral acetal (PVB) adds 2～3% of above-mentioned oxide compound gross weight in addition;
Above-mentioned calcium oxide, zirconium white, titanium oxide are the micro mist of 1～10 μ m;
B. the base substrate for preparing CaO refractory materials or crucible: above-mentioned calcium oxide, zirconium white, titanium oxide fine powder are pressed above-mentioned proportioning raw materials weigh batching, and add small amount of binder polyvinyl butyral acetal (PVB), be put in then and carried out ball milling in the ball mill 30～50 minutes; Then compound is entered the moulding process schedule of operation; The moulding program has two kinds, promptly prepares the moulding program of CaO refractory materials or preparation CaO crucible, its respectively schedule of operation be: (1) is pressed into sheet in mould; (2) in mould, be pressed into vessels crucible;
C. above-mentioned molding blank is carried out sintering, 500～650 ℃ of following sintering 2～6 hours; Be rapidly heated to 1700～1780 ℃, sintering 3～5 hours cools to room temperature then with the furnace again, promptly obtains CaO refractory materials or CaO crucible.
CaO refractory materials or crucible that the inventive method makes have higher volume density, and its density is 3.37～3.59g/cm
3Have higher hydration resistance, the hydrating capacity test shows: the material weightening finish is less than 0.2% after 28 days aquations.
The CaO crucible when the smelting titanium alloy container, under vacuum environment and 1500～1800 ℃ of smelting temperatures, the crucible after molten alloy is finished, its surfaces externally and internally is intact, does not react with titanium alloy, has guaranteed the purity and the alloy property of titanium alloy.
Embodiment
Now specific embodiments of the invention are described in down
Embodiment 1: the preparation process in the present embodiment is as follows:
(1). batching: adopt analytical pure calcium oxide, zirconium white, titanium oxide fine powder to do raw material.Carry out weigh batching by following molar percentage, composition of raw materials is as follows: calcium oxide 90%, zirconium white 7%, titanium oxide 3%; 2～3% the binding agent polyvinyl butyral acetal (PVB) that adds above-mentioned oxidation material gross weight in addition.
(2). ball milling: above-mentioned batching is put into ball mill, carried out ball milling 40 minutes.
(3). moulding: above-mentioned compound behind ball milling is put into mould be pressed into base substrate, can be pressed into sheet or vessels crucible.
(4). sintering: above-mentioned molding blank 600 ℃ of following sintering 4～5 hours, is being rapidly heated to 1750 ℃, and sintering 4 hours is chilled to room temperature with stove then, can make CaO refractory materials or CaO crucible.
Embodiment 2
The preparation process of present embodiment and the foregoing description 1 is identical.Different is to adopt the proportioning raw materials difference.
The proportioning raw materials of present embodiment is as follows: calcium oxide 84%, zirconium white 14%, titanium oxide 2% add 2～3% binding agent polyvinyl butyral acetal (PVB) of above-mentioned oxidation material gross weight in addition.Finally make CaO refractory materials or CaO crucible.
Above-mentioned sample is analyzed through X-ray diffractometer (XRD), and gained XRD figure stave is bright: its phase composite is mainly CaO, CaZrO
3Deng.
The volume density of above-mentioned sample is measured, the sample of embodiment 1, and its volume density is 3.38g/cm
3The sample of embodiment 2, its volume density are 3.54g/cm
3
Above-mentioned sample is in the aquation test, and its test condition is: in the atmosphere, its temperature is 25～30 ℃, and humidity is 65～75%; After depositing 28 days, the weightening finish of sample is less than 0.2% (aquation rate).The sample of embodiment 1 is 0.16%, and the sample of embodiment 2 is 0.11%.
Claims (1)
1. one kind is used for the CaO refractory materials of titanium alloy melting and the preparation method of crucible, it is characterized in that having following process and step:
A. determine and the design composition of raw materials that the raw material composition and the molar percentage thereof of this refractory materials are as follows:
Calcium oxide 82～92%,
Zirconium white 5～15%,
Titanium oxide 1～5%;
Binding agent polyvinyl butyral acetal (PVB), extra in addition 2～3% of the above-mentioned oxide compound gross weight that adds;
Above-mentioned calcium oxide, zirconium white, titanium oxide are the micro mist of 1～10 μ m;
B. the base substrate for preparing CaO refractory materials or crucible; Above-mentioned calcium oxide, zirconium white, titanium oxide fine powder are pressed above-mentioned proportioning raw materials weigh batching, and add small amount of binder polyvinyl butyral acetal (PVB), ball milling is 30～50 minutes then; Compound is entered the moulding process schedule of operation; The moulding program has two kinds, promptly prepares the moulding program of CaO refractory materials or preparation CaO crucible, its respectively schedule of operation be: (1) is pressed into sheet in mould; (2) in mould, be pressed into vessels crucible;
C. above-mentioned molding blank is carried out sintering, 500～650 ℃ of following sintering 2～6 hours; Be rapidly heated to 1700～1780 ℃, sintering 3～5 hours cools to room temperature then with the furnace again, promptly obtains CaO refractory materials or CaO crucible.
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| CN 201010167509 CN101830715A (en) | 2010-05-06 | 2010-05-06 | Preparation method of CaO refractory and crucible for titanium alloy smelting |
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| CN 201010167509 CN101830715A (en) | 2010-05-06 | 2010-05-06 | Preparation method of CaO refractory and crucible for titanium alloy smelting |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503489A (en) * | 2011-11-09 | 2012-06-20 | 上海大学 | BaZrO3 refractory material for smelting titanium alloy and preparation method of crucibles |
| CN102965528A (en) * | 2012-11-30 | 2013-03-13 | 上海大学 | Process for vacuum induction melting of titaniferous hydrogen storage alloy by using CaZrO3 refractory material |
| CN102994785A (en) * | 2012-11-30 | 2013-03-27 | 上海大学 | Method for smelting hydrogen storage alloy containing titanium from BaZrO3 refractory material by vacuum induction |
| CN103172390A (en) * | 2011-12-22 | 2013-06-26 | 沈阳鑫劲粉体工程有限责任公司 | Method for producing hydration-resistant high-purity calcium oxide crucible |
| CN105541354A (en) * | 2015-12-23 | 2016-05-04 | 上海大学 | A CaO refractory material used for a hydration-resisting crucible and a preparing method of the crucible |
| CN105906356A (en) * | 2016-04-25 | 2016-08-31 | 中国工程物理研究院材料研究所 | Method for preparing high-purity hydration-resisting calcium oxide crucible |
| CN107056255A (en) * | 2017-01-18 | 2017-08-18 | 武汉科技大学 | A kind of calcium oxide filter and preparation method thereof |
| CN109053202A (en) * | 2018-10-09 | 2018-12-21 | 武汉科技大学 | A kind of calcium zirconate crucible and preparation method thereof |
| CN113443923A (en) * | 2020-03-24 | 2021-09-28 | 中国科学院金属研究所 | Preparation method of CaO crucible for vacuum induction melting of Ti alloy |
| CN114105614A (en) * | 2021-12-03 | 2022-03-01 | 上海交通大学 | Material for preparing fiber composite hydration-resistant calcium oxide crucible, crucible and preparation method |
| CN115583830A (en) * | 2022-10-24 | 2023-01-10 | 中国科学院金属研究所 | Method for preparing alkaline forming crucible of ultra-low-sulfur high-temperature alloy |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2678887A (en) * | 1951-12-10 | 1954-05-18 | Nat Lead Co | Hydration resistant calcium oxide refractories |
-
2010
- 2010-05-06 CN CN 201010167509 patent/CN101830715A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2678887A (en) * | 1951-12-10 | 1954-05-18 | Nat Lead Co | Hydration resistant calcium oxide refractories |
Non-Patent Citations (1)
| Title |
|---|
| 《硅酸盐学报》 20091231 高永辉等 CaZrO3耐火材料的制备及其与钛合金熔体的界面反应 2007-2011 1 第37卷, 第12期 2 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503489A (en) * | 2011-11-09 | 2012-06-20 | 上海大学 | BaZrO3 refractory material for smelting titanium alloy and preparation method of crucibles |
| CN103172390A (en) * | 2011-12-22 | 2013-06-26 | 沈阳鑫劲粉体工程有限责任公司 | Method for producing hydration-resistant high-purity calcium oxide crucible |
| CN102965528A (en) * | 2012-11-30 | 2013-03-13 | 上海大学 | Process for vacuum induction melting of titaniferous hydrogen storage alloy by using CaZrO3 refractory material |
| CN102994785A (en) * | 2012-11-30 | 2013-03-27 | 上海大学 | Method for smelting hydrogen storage alloy containing titanium from BaZrO3 refractory material by vacuum induction |
| CN102994785B (en) * | 2012-11-30 | 2015-05-27 | 上海大学 | Method for smelting hydrogen storage alloy containing titanium from BaZrO3 refractory material by vacuum induction |
| CN105541354A (en) * | 2015-12-23 | 2016-05-04 | 上海大学 | A CaO refractory material used for a hydration-resisting crucible and a preparing method of the crucible |
| CN105906356A (en) * | 2016-04-25 | 2016-08-31 | 中国工程物理研究院材料研究所 | Method for preparing high-purity hydration-resisting calcium oxide crucible |
| CN107056255A (en) * | 2017-01-18 | 2017-08-18 | 武汉科技大学 | A kind of calcium oxide filter and preparation method thereof |
| CN109053202A (en) * | 2018-10-09 | 2018-12-21 | 武汉科技大学 | A kind of calcium zirconate crucible and preparation method thereof |
| CN113443923A (en) * | 2020-03-24 | 2021-09-28 | 中国科学院金属研究所 | Preparation method of CaO crucible for vacuum induction melting of Ti alloy |
| CN114105614A (en) * | 2021-12-03 | 2022-03-01 | 上海交通大学 | Material for preparing fiber composite hydration-resistant calcium oxide crucible, crucible and preparation method |
| CN115583830A (en) * | 2022-10-24 | 2023-01-10 | 中国科学院金属研究所 | Method for preparing alkaline forming crucible of ultra-low-sulfur high-temperature alloy |
| CN115583830B (en) * | 2022-10-24 | 2023-11-10 | 中国科学院金属研究所 | Method for preparing alkaline molding crucible of ultralow-sulfur high-temperature alloy |
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Application publication date: 20100915 |