CN105384437B - A kind of preparation method of zircite product - Google Patents

A kind of preparation method of zircite product Download PDF

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CN105384437B
CN105384437B CN201510791392.2A CN201510791392A CN105384437B CN 105384437 B CN105384437 B CN 105384437B CN 201510791392 A CN201510791392 A CN 201510791392A CN 105384437 B CN105384437 B CN 105384437B
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closed container
product
gas
temperature
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CN105384437A (en
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唐玉宝
唐鹏
唐嵘
韦波宇
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YONGZHOU LINGLINGYUANDA NEW MATERIALS CO., LTD.
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Yongzhou Linglingyuanda New Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped 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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62645Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6265Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62645Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6268Thermal treatment of powders or mixtures thereof other than sintering characterised by the applied pressure or type of atmosphere, e.g. in vacuum, hydrogen or a specific oxygen pressure
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62685Treating the starting powders individually or as mixtures characterised by the order of addition of constituents or additives

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention relates to a kind of preparation method of zircite product, belong to technical field of polymer materials.The present invention is first by electric-melting zirconia particle, the material mixings such as hematite powder are placed in a closed container, and the mixed gas of containment vessel volume 1/2 is passed through to it, then the magnesium ribbon lighted is placed in closed container, and add after lime powder stirring, acetylene then is slowly introducing to it, after gas is passed through end, insulation, then it is naturally cooled to room temperature;The mixture that room temperature will be cooled in closed container takes out, and ball clays into power, then by its with after PDA glue mixings, drying.Beneficial effects of the present invention:Zircite product thermal coefficient of expansion produced by the present invention reduces 5~7% so that product will not produce peeling because of coefficient of thermal expansion height using process, squeeze off crowded broken phenomenon, it is ensured that the quality of product.

Description

A kind of preparation method of zircite product
Technical field
The present invention relates to a kind of preparation method of zircite product, belong to technical field of polymer materials.
Background technology
Zirconium oxide high specific surface area, with very high fusing point, high-purity compact zircite product has temperature in use high, resistance to Melt liquid erosion, antiscour, it is not easy precipitation, good chemical stability, is a kind of widely used high-performance refractory Product.ZrO2Fusing point is up to 2690 DEG C, is a kind of high grade refractory, high with fire resistance, and chemical stability is good, in oxygen Stable particular advantages under change, reduction and vacuum state.
For a long time, the oxidation for 2000 DEG C or higher of vitreous silica smelting furnace and superhard alloy intermediate frequency furnace Zirconium product, generally using 4.4~4.7wt% of stabilizer CaO content complete stable ZrO2To produce.Produce in this way Zircite product has the disadvantage that:Coefficient of thermal expansion is big, and thermal coefficient of expansion is high, with partially stabilized ZrO2Compare, thermal coefficient of expansion Almost partially stabilized ZrO2Twice, the complete stable ZrO at 1500 DEG C2Thermal coefficient of expansion is 11 × 10-6/ DEG C or higher.This Planting product is used for vitreous silica smelting furnace, often because coefficient of thermal expansion is excessive, and thermal shock resistance is poor and is squeezed off crowded broken or flake-off piece, Severe contamination vitreous silica, so as to cause product rejection.ZrO2Fusing point is very high, and (such as 1800 DEG C) are difficult to burn at a lower temperature Knot.
The content of the invention
Present invention mainly solves technical problem:For using calcium oxide as stabilizer, the zirconium oxide system being made under high temperature Product coefficient of thermal expansion is big, and thermal coefficient of expansion is high, causes its thermal shock resistance difference and is squeezed off crowded broken or flake-off piece, and is aoxidized under low temperature The problem of zirconium is difficult sintering again is mainly put there is provided a kind of preparation method of zircite product, the present invention by thermit reaction Go out substantial amounts of heat, while being passed through for acetylene can also improve temperature there is provided a kind of hot environment while the magnesia generated, nitridation The thermal coefficient of expansion when materials such as magnesium and the lime powder of addition solve the problems, such as that calcium oxide is used alone as stabilizer. Zircite product thermal coefficient of expansion produced by the present invention reduces 5~7% so that product will not be because of coefficient of thermal expansion in the process of use It is high and produce and peel off, squeeze off crowded broken phenomenon, it is ensured that the quality of product.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention:
(1)Count by weight, choose the electric-melting zirconia particle that 70~80 parts of particle diameters are 0.5~1mm, 17~25 parts red Iron ore powder, 1~2 part of aluminium powder, 2~3 parts of potassium chlorate mixing are placed in a closed container, and be passed through containment vessel volume to it The volume ratio of oxygen and nitrogen is 1 in 1/2 mixed gas, the mixed gas:9~1:10;
(2)Gas to be mixed is passed through after end, and the magnesium ribbon lighted is placed in closed container, makes the mixing in closed container Thing is reacted after 1~2h, when the temperature in closed container reaches 900~1000 DEG C, then adds electric-melting zirconia particle matter to it The lime powder of amount 25%, stirring is well mixed it, and it is 100~200r/min to control mixing speed, and mixing time is 25 ~30min;
(3)Then acetylene gas is passed through into closed container, is passed through once to it every 3~5min, 5~7 is passed through altogether It is secondary, and control to be passed through speed for 20~30mL/s, the temperature in closed container is improved to 1200~1300 DEG C, treat that gas is passed through After end, 1~2h is incubated, then it is naturally cooled to room temperature;
(4)The mixture that room temperature will be cooled in closed container takes out, and is placed in ball mill ball milling into 100~120 purposes Powder, then carried out after its PDA glue mixing with powder quality 1~2%, being placed in the baking oven that temperature is 70~80 DEG C Dry 30~45min, you can obtain a kind of zircite product.
The density of the zircite product of above-mentioned preparation is 4~4.5g/cm3, normal temperature is resistance to be pressed on 250~370MPa, and fusing point exists 2700~3000 DEG C.
The application of the present invention:Zircite product obtained above is used to make zirconium oxide abrasive material or oxygen is made Change zirconium coating material, applied to high performance turbine aero-engine.The grinding-material being made using the zircite product has hard Degree is big, small wear rate, service life length, can be greatly reduced the pollution of grinding raw material, and as coating material can with high temperature resistant, Temperature is up to 2700~3000 DEG C.
The beneficial effects of the invention are as follows:
(1)Zircite product thermal coefficient of expansion reduces 5~7% so that product will not be because of coefficient of thermal expansion in the process of use It is high and produce and peel off, squeeze off crowded broken phenomenon, it is ensured that the quality of product.
(2)Preparation process is simple, and cost is low.
Embodiment
Count by weight first, choose the electric-melting zirconia particle that 70~80 parts of particle diameters are 0.5~1mm, 17~25 parts Hematite powder, 1~2 part of aluminium powder, 2~3 parts of potassium chlorate mixing are placed in a closed container, and be passed through closed container body to it The mixed gas of product 1/2, the volume ratio of oxygen and nitrogen is 1 wherein in mixed gas:9~1:10;Gas to be mixed is passed through knot Shu Hou, the magnesium ribbon lighted is placed in closed container, the mixture in closed container is reacted after 1~2h, is treated in closed container Temperature when reaching 900~1000 DEG C, then add to it lime powder of electric-melting zirconia granular mass 25%, stirring makes it Well mixed, it is 100~200r/min to control mixing speed, and mixing time is 25~30min;Then it is passed through into closed container Acetylene gas, is passed through once every 3~5min to it, is passed through altogether 5~7 times, and controls to be passed through speed for 20~30mL/s, makes Temperature in closed container is improved to 1200~1300 DEG C, after gas is passed through end, is incubated 1~2h, then make its natural cooling To room temperature;The mixture that room temperature will be cooled in closed container takes out, and is placed in ball mill ball milling into 100~120 mesh powders, Again by after its PDA glue mixing with powder quality 1~2%, it is placed in the baking oven that temperature is 70~80 DEG C and is dried 30~45min, you can obtain a kind of zircite product.The density of zircite product is 4~4.5g/cm3, normal temperature is resistance to be pressed on 250 ~370MPa, fusing point is at 2700~3000 DEG C.
Example 1
Count by weight first, choose the electric-melting zirconia particle that 80 parts of particle diameters are 1mm, 25 parts of hematite powders, 2 Part aluminium powder, 3 parts of potassium chlorate mixing, is placed in a closed container, and is passed through the mixed gas of containment vessel volume 1/2 to it, its The volume ratio of oxygen and nitrogen is 1 in middle mixed gas:10;Gas to be mixed is passed through after end, the magnesium ribbon lighted is placed in close Close in container, the mixture in closed container is reacted after 2h, add when the temperature in closed container reaches 1000 DEG C, then to it Enter the lime powder of electric-melting zirconia granular mass 25%, stirring is well mixed it, it is 200r/min to control mixing speed, Mixing time is 30min;Then acetylene gas is passed through into closed container, is passed through once to it every 5min, 7 is passed through altogether It is secondary, and control to be passed through speed for 30mL/s, the temperature in closed container is improved to 1300 DEG C, after gas is passed through end, protect Warm 2h, then it is naturally cooled to room temperature;The mixture that room temperature is cooled in closed container is taken out, ball milling in ball mill is placed in Into 120 mesh powders, then it after its PDA glue mixing with powder quality 2%, will be placed in the baking oven that temperature is 80 DEG C Row drying 45min, you can obtain a kind of zircite product.The density of zircite product is 4.5g/cm3, normal temperature is resistance to be pressed on 370MPa, fusing point is at 3000 DEG C.Zircite product obtained above is used to make zirconium oxide abrasive material.Utilize the zirconium oxide The grinding-material that product is made has that hardness is big, wear rate is small, service life length, the pollution of grinding raw material can be greatly reduced.
Example 2
Count by weight first, choose the electric-melting zirconia particle that 70 parts of particle diameters are 0.5mm, 25 parts of hematite powders, 2 Part aluminium powder, 3 parts of potassium chlorate mixing, is placed in a closed container, and is passed through the mixed gas of containment vessel volume 1/2 to it, its The volume ratio of oxygen and nitrogen is 1 in middle mixed gas:9;Gas to be mixed is passed through after end, the magnesium ribbon lighted is placed in closed In container, the mixture in closed container is reacted after 2h, added when the temperature in closed container reaches 900 DEG C, then to it The lime powder of electric-melting zirconia granular mass 25%, stirring is well mixed it, and it is 100r/min to control mixing speed, is stirred The time is mixed for 25~30min;Then acetylene gas is passed through into closed container, is passed through once to it every 3min, 5 is passed through altogether It is secondary, and control to be passed through speed for 20mL/s, the temperature in closed container is improved to 1200 DEG C, after gas is passed through end, protect Warm 1h, then it is naturally cooled to room temperature;The mixture that room temperature is cooled in closed container is taken out, ball milling in ball mill is placed in Into 100 mesh powders, then it after its PDA glue mixing with powder quality 1%, will be placed in the baking oven that temperature is 70 DEG C Row drying 30min, you can obtain a kind of zircite product.The density of zircite product is 4g/cm3, normal temperature is resistance to be pressed on 250MPa, Fusing point is at 2700 DEG C.Zircite product obtained above is used to make zirconia coating material, applied to high-performance whirlpool Aero-engine is taken turns, and can be with high temperature resistant as coating material, temperature is up to 3000 DEG C.
Example 3
Count by weight first, choose the electric-melting zirconia particle that 75 parts of particle diameters are 0.6mm, 20 parts of hematite powders, 2 Part aluminium powder, 3 parts of potassium chlorate mixing, is placed in a closed container, and is passed through the mixed gas of containment vessel volume 1/2 to it, its The volume ratio of oxygen and nitrogen is 1 in middle mixed gas:9;Gas to be mixed is passed through after end, the magnesium ribbon lighted is placed in closed In container, the mixture in closed container is reacted after 2h, added when the temperature in closed container reaches 950 DEG C, then to it The lime powder of electric-melting zirconia granular mass 25%, stirring is well mixed it, and it is 150r/min to control mixing speed, is stirred The time is mixed for 27min;Then acetylene gas is passed through into closed container, is passed through once to it every 4min, is passed through altogether 6 times, And control to be passed through speed for 25mL/s, and the temperature in closed container is improved to 1250 DEG C, after gas is passed through end, insulation 1h, then it is naturally cooled to room temperature;The mixture that room temperature will be cooled in closed container takes out, be placed in ball mill ball milling into 110 mesh powders, then carried out after its PDA glue mixing with powder quality 1%, being placed in the baking oven that temperature is 75 DEG C Dry 40min, you can obtain a kind of zircite product.The density of zircite product is 4.2g/cm3, normal temperature is resistance to be pressed on 300MPa, Fusing point is at 2800 DEG C.Zircite product obtained above is used to make zirconium oxide abrasive material.Utilize the zircite product system Into grinding-material have that hardness is big, wear rate is small, service life length, the pollution of grinding raw material can be greatly reduced.

Claims (1)

1. a kind of preparation method of zircite product, it is characterised in that specifically preparation process is:
(1)Count by weight, choose the electric-melting zirconia particle that 70~80 parts of particle diameters are 0.5~1mm, 17~25 parts of bloodstone Powder, 1~2 part of aluminium powder, 2~3 parts of potassium chlorate mixing are placed in a closed container, and be passed through containment vessel volume 1/2 to it The volume ratio of oxygen and nitrogen is 1 in mixed gas, the mixed gas:9~1:10;
(2)Gas to be mixed is passed through after end, and the magnesium ribbon lighted is placed in closed container, makes the mixture in closed container anti- Answer after 1~2h, electric-melting zirconia granular mass is added when the temperature in closed container reaches 900~1000 DEG C, then to it 25% lime powder, stirring is well mixed it, and it is 100~200r/min control mixing speed, mixing time for 25~ 30min;
(3)Then acetylene gas is passed through into closed container, is passed through once to it every 3~5min, is passed through altogether 5~7 times, and Control to be passed through speed for 20~30mL/s, the temperature in closed container is improved to 1200~1300 DEG C, treat that gas is passed through end Afterwards, 1~2h is incubated, then it is naturally cooled to room temperature;
(4)The mixture that room temperature will be cooled in closed container takes out, and is placed in ball mill ball milling into 100~120 mesh powders, Again by after its PDA glue mixing with powder quality 1~2%, it is placed in the baking oven that temperature is 70~80 DEG C and is dried 30~45min, you can obtain a kind of zircite product.
CN201510791392.2A 2015-11-17 2015-11-17 A kind of preparation method of zircite product Active CN105384437B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002104877A (en) * 2000-09-27 2002-04-10 Moritex Corp Method of synthesizing heat-shrinkable oxide
CN103496974A (en) * 2013-09-25 2014-01-08 安徽巨盛新材料科技有限公司 Production process of zirconia ceramics
CN104591745A (en) * 2015-02-02 2015-05-06 厦门胜中流体控制技术有限公司 Raw material powder for zirconia ceramic part with high wear resistance and preparation method of raw material powder
CN104891857A (en) * 2015-05-26 2015-09-09 新化县众一陶瓷有限公司 Preparation method of stabilizer composite zirconium oxide powder

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