CN106396664A - A magnesium-based lanthanum aluminate ceramic manufacturing method - Google Patents

A magnesium-based lanthanum aluminate ceramic manufacturing method Download PDF

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CN106396664A
CN106396664A CN201610612070.1A CN201610612070A CN106396664A CN 106396664 A CN106396664 A CN 106396664A CN 201610612070 A CN201610612070 A CN 201610612070A CN 106396664 A CN106396664 A CN 106396664A
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hot
ceramic
temperature
raw material
lanthanum aluminate
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鲁飞
刘树峰
孙良成
刘小鱼
白洋
王峰
李慧
成宇
陈蓓新
邢正茂
李德辉
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Baotou Rare Earth Research Institute
Santoku Corp
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Baotou Rare Earth Research Institute
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts

Abstract

The invention relates to a magnesium-based lanthanum aluminate ceramic manufacturing method. The method is characterized by including (1) a step of raw material matching, namely a step of matching magnesium oxide, alumina and lanthana which are adopted as raw materials according to a stoichiometric ratio of LaMgAl<11>O<19>, (2) a step of raw material mixing, namely a step of adding the matched raw materials into a ball mill tank, performing wet ball milling for 12-24 h, taking out, and drying slurry, and (3) a step of hot-pressing forming, namely a step of weighing a proper amount of the mixed powder into a mold, putting into a hot-pressing sintering furnace, and hot-pressing in vacuum to form a ceramic material, wherein the hot-pressing forming temperature is 1550-1700 DEG C, the forming pressure is 18-30 MPa and the temperature and the pressure are maintained for 0.5-2 h. The method is advantageous in that the manufactured ceramic is high in relative density, free of outer cracks, free of inner pores, good in thermal shock resistance and free of cracks after high-temperature cooling cycles, and resistance to fused salt corrosion is good so that a ceramic product in a high-temperature fused salt (fluorine salts and chlorine salts) system is free of obvious seepage and low in leaching rate.

Description

A kind of magnesio lanthanum aluminate process for preparing ceramic
Technical field
The present invention relates to a kind of magnesio lanthanum aluminate process for preparing ceramic, belong to Material Field.
Background technology
Magnesio lanthanum aluminate（LaMgAl11O19）Fusing point is high, and thermal conductivity is low, less than 2000 DEG C no phase transformations, structure and thermally-stabilised Property is good, is a kind of high temperature resistance refractory material of great application prospect.At present with regard to LaMgAl11O19Research focus primarily upon heat The aspects such as barrier coating, catalyst carrier and phosphor host.Chinese patent CN100551870C reports a kind of magnesio aluminum Sour lanthanum heat barrier coat material preparation method.The method prepares high-purity magnesio lanthanum aluminate ceramic material using two step solid sintering technologies, As thermal barrier coating target；Chinese patent CN103623818B proposes a kind of thin shell shaped noble metal catalyst and preparation method thereof, Inventive method adopts LaMgAl11O19Make lamellar composite carrier shell；Chinese patent CN103421507B gives a kind of magnesium nitride Base lanthanum aluminate fluorescent material and preparation method thereof.The method that the method adopts carbothermal reduction-nitridation, with LaMgAl11O19For raw material, In high-temperature ammonolysis atmosphere, reaction obtains nitrogenizing magnesio lanthanum aluminate fluorescent material.
LaMgAl at this stage11O19Ceramic material adopts conventional solid sintering process to prepare, due to LaMgAl mostly11O19Sintering Temperature drift, is difficult to densification sintering under conventional process conditions, finished product density is not high.Ceramic toughness is poor, uses During brittle fracture easily occurs, lead to it can not bear larger mechanical shock and thermal shock, thermal shock resistance is not high, greatly limit Make its extensive application.
Content of the invention
The purpose of the present invention is the problem existing for background technology, provides a kind of magnesio lanthanum aluminate process for preparing ceramic. The method adopts hot pressing and sintering technique to prepare LaMgAl11O19Pottery, realizes molding and sintering is synchronous carries out it is ensured that powder Granule is in close contact, and reduces sintering temperature, accelerates densification process；Manufactured ceramic relative density is high, outside flawless, interior Portion imporosity；Good thermal shock, occurs without crackle after high temperature cooling circulation.
The pottery resistance to fused salt corrosion excellent performance that the inventive method manufactures, in high-temperature molten salt（Villiaumite, villaumite）Under system, pottery Products appearance shape remains intact, do not have cracking, expand and top layer ceramic particle such as comes off at the phenomenon.
The method of the present invention comprises the following steps：
（1）Raw material and proportioning：Raw material is made with magnesium oxide, aluminium oxide, lanthana, by LaMgAl11O19Stoichiometric proportion dispensing；
（2）Raw material mixes：The material that proportioning is completed takes out after putting into wet ball grinding 12-24h in ball grinder, dries slurry；
（3）Hot-forming：Weigh appropriate mixed powder to load in mould, put into hot-pressed sintering furnace hot-forming under vacuum conditions Ceramic material, wherein：Hot-forming temperature is 1550-1700 DEG C, and briquetting pressure is 18-30MPa, heat-insulation pressure keeping 0.5-2 hour.
The temperature drying slurry described in step 2 is 60-200 DEG C.
The present invention, compared with background technology, has an advantageous effect in that：Manufactured ceramic relative density is high, outside nothing is split Stricture of vagina, internal imporosity；Good thermal shock, occurs without crackle after high temperature cooling circulation；Resistance to fused salt corrosion excellent performance, in high-temperature molten salt （Villiaumite, villaumite）Under system, there is not obvious seepage in ceramic, and dissolution rate is low.
Brief description
Fig. 1 is in embodiment 1, the X ray diffracting spectrum of the magnesio lanthanum aluminate ceramic material of preparation.
Specific embodiment
Embodiment 1：
A kind of magnesio lanthanum aluminate ceramic material manufacture method, specifically includes following steps：
（1）Raw material and proportioning：Raw material is made with magnesium oxide, aluminium oxide, lanthana, by LaMgAl11O19Stoichiometric proportion dispensing；
（2）Raw material mixes：The material that proportioning is completed is put in polyurethane ball-milling pot, with zirconia ball and dehydrated alcohol as grinding medium Matter wet ball grinding 12 h, dries slurry, 60 DEG C of drying temperature；
（3）Hot-forming：Weigh appropriate mixed powder to load in graphite jig, put into hot-pressed sintering furnace hot pressing under vacuum conditions Forming ceramic material, vacuum is higher than 1 × 10-2Pa, hot pressing temperature is 1550 DEG C, and briquetting pressure is 30MPa, and heat-insulation pressure keeping 2 is little When.
High-purity magnesio lanthanum aluminate pottery can be obtained through above-mentioned technique, X ray diffracting spectrum is shown in accompanying drawing 1.Ceramic phase is to close Degree 99.1%, good thermal shock, it is warming up to 1200 DEG C, cool to room temperature with the furnace, ceramic complete appearance, flawless and hidden split appearance. Corrode 24 h, 80 μm of fused salt penetration depth, magnesio aluminum in fused salt in 1050 DEG C of mixed rare earth fluoride molten-salt electrolysis plastidome The dissolution rate 200 μ g/g of sour lanthanum characteristic element Mg；After corroding 10 h in 1200 DEG C of calcium chloride molten salt systems, fused salt penetration depth 220 μm, the dissolution rate 700 μ g/g of magnesio lanthanum aluminate characteristic element Mg, the dissolution rate 690 μ g/g of La in fused salt.
Embodiment 2：
A kind of magnesio lanthanum aluminate ceramic material manufacture method, specifically includes following steps：
（1）Raw material and proportioning：Raw material is made with magnesium oxide, aluminium oxide, lanthana, by LaMgAl11O19Stoichiometric proportion dispensing；
（2）Raw material mixes：The material that proportioning is completed is put in polyurethane ball-milling pot, with zirconia ball and deionized water as grinding medium Matter wet ball grinding 18 h, dries slurry, 150 DEG C of drying temperature；
（3）Hot-forming：Weigh appropriate mixed powder to load in graphite jig, put into hot-pressed sintering furnace hot pressing under vacuum conditions Forming ceramic material, vacuum is higher than 1 × 10-2Pa, hot pressing temperature is 1600 DEG C, and briquetting pressure is 25MPa, heat-insulation pressure keeping 1.5 Hour.
The high-purity magnesio lanthanum aluminate pottery relative density 99.0% obtaining through above-mentioned technique, good thermal shock, it is warming up to 1200 DEG C, cool to room temperature with the furnace, ceramic complete appearance, flawless and hidden split appearance.In 1050 DEG C of mixed rare earth fluoride fused salt electricity Corrode 24 h, 85 μm of fused salt penetration depth, the dissolution rate 210 μ g/ of magnesio lanthanum aluminate characteristic element Mg in fused salt in solution plastidome g；After corroding 10 h in 1200 DEG C of calcium chloride molten salt systems, 205 μm of fused salt penetration depth, magnesio lanthanum aluminate characteristic element in fused salt The dissolution rate 670 μ g/g of the dissolution rate 690 μ g/g of plain Mg, La.
Embodiment 3：
A kind of magnesio lanthanum aluminate ceramic material manufacture method, specifically includes following steps：
（1）Raw material and proportioning：Raw material is made with magnesium oxide, aluminium oxide, lanthana, by LaMgAl11O19Stoichiometric proportion dispensing；
（2）Raw material mixes：The material that proportioning is completed is put in polyurethane ball-milling pot, with zirconia ball and deionized water as grinding medium Matter wet ball grinding 24 h, dries slurry, 200 DEG C of drying temperature；
（3）Hot-forming：Weigh appropriate mixed powder to load in graphite jig, put into hot-pressed sintering furnace hot pressing under vacuum conditions Forming ceramic material, vacuum is higher than 1 × 10-2Pa, hot pressing temperature is 1700 DEG C, and briquetting pressure is 18MPa, heat-insulation pressure keeping 0.5 Hour.
The high-purity magnesio lanthanum aluminate pottery relative density 98.8% obtaining through above-mentioned technique, good thermal shock, it is warming up to 1200 DEG C, cool to room temperature with the furnace, ceramic complete appearance, flawless and hidden split appearance.In 1050 DEG C of mixed rare earth fluoride fused salt electricity Corrode 24 h, 82 μm of fused salt penetration depth, the dissolution rate 200 μ g/ of magnesio lanthanum aluminate characteristic element Mg in fused salt in solution plastidome g；After corroding 10 h in 1200 DEG C of calcium chloride molten salt systems, 210 μm of fused salt penetration depth, magnesio lanthanum aluminate characteristic element in fused salt The dissolution rate 680 μ g/g of the dissolution rate 690 μ g/g of plain Mg, La.

Claims (2)

1. a kind of magnesio lanthanum aluminate process for preparing ceramic, is characterized in that：Comprise the following steps：
（1）Raw material and proportioning：Raw material is made with magnesium oxide, aluminium oxide, lanthana, by LaMgAl11O19Stoichiometric proportion dispensing；
（2）Raw material mixes：The material that proportioning is completed takes out after putting into wet ball grinding 12-24h in ball grinder, dries slurry；
（3）Hot-forming：Weigh appropriate mixed powder to load in mould, put into hot-pressed sintering furnace hot-forming under vacuum conditions Ceramic material, wherein：Hot-forming temperature is 1550-1700 DEG C, and briquetting pressure is 18-30MPa, heat-insulation pressure keeping 0.5-2 hour.
2. a kind of magnesio lanthanum aluminate process for preparing ceramic according to claim 1, is characterized in that：Dry described in step 2 The temperature of slurry is 60-200 DEG C.
CN201610612070.1A 2016-07-31 2016-07-31 A magnesium-based lanthanum aluminate ceramic manufacturing method Pending CN106396664A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848139A (en) * 2020-06-24 2020-10-30 北京理工大学 High-emissivity LaMgAl11O19Method for producing ceramic
WO2021120021A1 (en) * 2019-12-17 2021-06-24 深圳市大富科技股份有限公司 Ceramic material and preparation method therefor

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Publication number Priority date Publication date Assignee Title
CN1353676A (en) * 1999-03-29 2002-06-12 大森守 Method for preparing eutectic ceramics
CN101723658A (en) * 2009-12-23 2010-06-09 中国地质大学（北京） Low thermal-conductivity GdMgAl11O19 high temperature-resistant ceramic material and preparation method thereof
CN102584236A (en) * 2012-03-12 2012-07-18 中国地质大学（北京） Preparation method of PrMgAl11O19 high temperature resistant ceramic material
CN102826836A (en) * 2012-09-04 2012-12-19 中国地质大学（北京） LnMgAl11O19-Al2O3 complex phase wear resistant ceramic material used for down-the-hole hammer
CN106278264A (en) * 2016-07-31 2017-01-04 包头稀土研究院 A kind of high density chromic lanthanum ceramics heater manufacture method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN101723658A (en) * 2009-12-23 2010-06-09 中国地质大学（北京） Low thermal-conductivity GdMgAl11O19 high temperature-resistant ceramic material and preparation method thereof
CN102584236A (en) * 2012-03-12 2012-07-18 中国地质大学（北京） Preparation method of PrMgAl11O19 high temperature resistant ceramic material
CN102826836A (en) * 2012-09-04 2012-12-19 中国地质大学（北京） LnMgAl11O19-Al2O3 complex phase wear resistant ceramic material used for down-the-hole hammer
CN106278264A (en) * 2016-07-31 2017-01-04 包头稀土研究院 A kind of high density chromic lanthanum ceramics heater manufacture method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021120021A1 (en) * 2019-12-17 2021-06-24 深圳市大富科技股份有限公司 Ceramic material and preparation method therefor
CN111848139A (en) * 2020-06-24 2020-10-30 北京理工大学 High-emissivity LaMgAl11O19Method for producing ceramic

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