CN107686380A - A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating - Google Patents

A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating Download PDF

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Publication number
CN107686380A
CN107686380A CN201710724970.XA CN201710724970A CN107686380A CN 107686380 A CN107686380 A CN 107686380A CN 201710724970 A CN201710724970 A CN 201710724970A CN 107686380 A CN107686380 A CN 107686380A
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Prior art keywords
graphite
coating
described step
rotator
graphite rotator
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CN107686380B (en
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马北越
张亚然
苏畅
尹月
任鑫明
于景坤
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Northeastern University China
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Northeastern University China
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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
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/89Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • 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
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Structures Of Non-Positive Displacement Pumps (AREA)

Abstract

A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating, belong to metal bath purification and coating protection technical field.Specifically preparation method is:First, pre-oxidation treatment is carried out to graphite material, to obtain coarse surface;Then, graphite material is submerged with aluminium dihydrogen phosphate, to improve the inoxidizability of graphite rotator;Finally, in the multiple brushing slurry in graphite rotator top layer, make coating that there is certain thickness.The inoxidizability of graphite rotator is the method improve, extends the service life of graphite rotator, improves the purification of aluminum melt.And the technological operation is simple, and raw material is cheap and easy to get, production cost is reduced.

Description

A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating
Technical field
The invention belongs to metal bath purification and coating protection technical field, and in particular to a kind of aluminium melt purifying graphite The preparation method of rotor inoxidzable coating.
Background technology
Aluminum processing technology develops rapidly, increasingly harsh to the quality requirement of aluminum products.Aluminum melt is purified, eliminates aluminum products Internal flaw, it is always the focus of aluminium processing industry.In purification process technique, inert gas is blown using rotor It is the current international advanced aluminium liquid purification techniques of the next item up to remove hydrogen in aluminium liquid and oxide inclusion.
The degassing rotor being commonly used is graphite rotator, and carbon mass fraction is more than 99.9%, and carbon is in atmosphere The critical-temperature of oxidation is 400 DEG C, and the purification temperature of aluminum melt greatly exceed critical-temperature between 700~730 DEG C, Graphite oxidation causes the diameter of axle of armature spindle to be gradually reduced, final fracture, it is impossible to uses.Therefore, the anti-oxidant of graphite material is improved Performance is to improve the key of aluminium melt purifying.
The main path for improving the antioxygenic property of graphite rotator has:(1) from high-quality high purity graphite as rotor material. (2) inert gas shielding method.(3) coating protection method.(4) casing protection method etc..Wherein, coating protection method passes through in graphite rotator Brushing paint on surface, the oxygen in shroud air, prevents graphite rotator to be oxidized, and turn into a kind of effective processing method.
The content of the invention
In order to improve the antioxygenic property of graphite rotator, the present invention proposes a kind of aluminium melt purifying graphite rotator oxygen Change the preparation method of coating.The master operation of this method is as follows:First, pre-oxidation treatment is carried out to graphite material, it is thick to obtain Rough surface;Then, graphite material is submerged with aluminium dihydrogen phosphate, to improve the inoxidizability of graphite rotator;Finally, turn in graphite The multiple brushing slurry of sublist layer, makes coating have certain thickness.
A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating of the present invention, is carried out according to the following steps:
Step 1:Graphite pre-oxidation treatment
(1) after using alcohol washes graphite material, 5h is dried in an oven, then cool down 2h;
(2) graphite after cooling is placed in the high temperature furnace that temperature is 850 DEG C, pre-oxidizes 6min;
Step 2:Graphite impregnation processing
(1) with Al2O3Powder and phosphoric acid are waste aluminium dihydrogen phosphate;
(2) graphite material is submerged with aluminium dihydrogen phosphate, then is put in vavuum pump and is vacuumized;
(3) graphite material impregnated is placed in 120 DEG C of baking ovens and dries 5h;
Step 3:Apply brush applied coating
(1) with SiC powder, Al2O3Powder and additive A are coating material, configure coating slurry, the additive A in coating material Mass fraction be 10%~40%.
(2) repeatedly brushed on graphite rotator top layer after coating slurry is well mixed, all dried after brushing every time Or naturally dry processing.
In described step 1 (1), described graphite is common loose graphite;
Described oven drying temperature is 80 DEG C~150 DEG C;
In described step 1 (2), high temperature furnace is one kind in box resistance wire furnace, box silicon carbide rod furnace, tunnel cave;
In described step 2 (1), the raw material A l of aluminium dihydrogen phosphate is prepared2O3The amount proportioning of the material of powder and phosphoric acid is 1:6;
In described step 2 (2), the time that described vavuum pump vacuumizes is 5~30min;
In described step 3 (1), described additive A is Y2O3、MgO、TiO2、ZrSiO4In one or more;
In described step 3 (2), graphite rotator brushing number is 2~5 times;
The density of coating raw material differs, and coating will stir again before brushing every time;
The technique for brushing drying:After 100 DEG C of drying 1h, 1h is dried again at 200 DEG C,.
The beneficial effects of the present invention are:
1. a kind of aluminium melt purifying preparation method of graphite rotator inoxidzable coating of the present invention, effectively improves graphite The inoxidizability of rotor, the service life of graphite rotator is extended, improve the clean-up effect of aluminum melt.
2. a kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating of the present invention, utilizes phosphoric acid complex salt Solution carries out impregnation to graphite rotator, improves the inoxidizability of graphite rotator, improves rupture strength, enhances heat resistanceheat resistant Pinking.
A kind of 3. preparation method of aluminium melt purifying graphite rotator inoxidzable coating of the present invention, using coating protection Method, simple process is easy, is easy to industrialized production.
A kind of 4. preparation method of aluminium melt purifying graphite rotator inoxidzable coating of the present invention, using SiC powder, Al2O3 Powder and additive A are coating material, and wiping operation is simple, and raw material is cheap and easy to get, and production cost is greatly reduced.
Brief description of the drawings
Fig. 1 is the process chart of the present invention;
Embodiment
With reference to embodiment, the present invention is described in further detail.
In following examples, except special instruction, raw material is all from purchased in market.
In following examples, a kind of method process chart for improving aluminium melt purifying graphite rotator antioxygenic property is shown in Fig. 1.
Embodiment 1
A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating, is carried out according to the following steps:
Step 1:Graphite pre-oxidation treatment
(1) after using alcohol washes graphite material, 5h is dried in 120 DEG C of baking ovens, then cool down 2h;
(2) graphite after cooling is placed in the high temperature furnace that temperature is 850 DEG C, pre-oxidizes 6min;
Step 2:Graphite impregnation processing
(1) with Al2O3Powder and phosphoric acid are waste aluminium dihydrogen phosphate;
(2) graphite material is placed in large beaker and submerged with aluminium dihydrogen phosphate, then beaker is put in vavuum pump and vacuumized 15min;
(3) graphite material impregnated is placed in 120 DEG C of baking ovens and dries 5h;
Step 3:Apply brush applied coating
(1) with SiC powder, Al2O3Powder and additive Y2O3For coating material.Formula composition is (mass fraction, %):55% SiC-30%Al2O3- 15%Y2O3, according to this proportioning, configure coating slurry;
(2) brushed on graphite rotator top layer after coating slurry is well mixed, carried out after brushing every time at drying three times Reason, i.e., after 100 DEG C dry 1h, 1h is dried again at 200 DEG C.
After testing, after the graphite rotator after coating aoxidizes 300min at 900 DEG C, mass loss 7%, coating has been kept It is good;900 DEG C of thermal shock periods to room temperature reach 16 times;The newly-generated thing phase composition of coating is after oxidation 600min at 900 DEG C SiO2, the SiC components in coating and the O in air2Reaction generation SiO2Diaphragm, coating is reduced during oxidation experiment Peeling, significantly improve the antioxygenic property of graphite product.
Embodiment 2
A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating, with embodiment 1, difference is, Required additive A is MgO.
After testing, after the graphite rotator after coating aoxidizes 300min at 900 DEG C, mass loss 8%, coating has been kept It is good;900 DEG C of thermal shock periods to room temperature reach 12 times;The newly-generated thing phase composition of coating is after oxidation 600min at 900 DEG C SiO2, the SiC components in coating and the O in air2Reaction generation SiO2Diaphragm, coating is reduced during oxidation experiment Peeling probability, significantly improve the antioxygenic property of graphite product.
Embodiment 3
A kind of method for improving aluminium melt purifying graphite rotator antioxygenic property, with embodiment 1, difference is:
(1) additive A needed for is TiO2
(2) the formula composition of coating material is (mass fraction, %):45%SiC-40%Al2O3- 15%TiO2
After testing, after the graphite rotator after coating aoxidizes 300min at 900 DEG C, mass loss 5%, coating is almost kept It is intact, without big peeling;900 DEG C of thermal shock periods to room temperature reach 10 times;At 900 DEG C aoxidize 600min after coating new life It is SiO into thing phase composition2, the SiC components in coating and the O in air2Reaction generation SiO2Diaphragm, coating is reduced in oxygen Change the peeling probability in experimentation, significantly improve the antioxygenic property of graphite product.
Embodiment 4
A kind of preparation method of aluminium melt purifying graphite rotator inoxidzable coating, with embodiment 1, difference is:
(1) it is ZrSiO in required additive A4
(2) the formula composition of coating material is (mass fraction, %):45%SiC-40%Al2O3- 15%ZrSiO4
After testing, after the graphite rotator after coating aoxidizes 300min at 900 DEG C, mass loss 6%, coating is almost kept It is intact, without big peeling;900 DEG C of thermal shock periods to room temperature reach 13 times;After 900 DEG C aoxidize 600min, in component SiC also with O2Reaction generates SiO2, significantly improve the antioxygenic property of graphite product.

Claims (8)

1. a kind of aluminium melt purifying preparation method of graphite rotator inoxidzable coating, it is characterised in that carry out according to the following steps:
Step 1:Graphite pre-oxidation treatment
(1) after using alcohol washes graphite material, 5h is dried in an oven, then cool down 2h;Oven drying temperature is 80 DEG C~150 ℃;
(2) graphite after cooling is placed in the high temperature furnace that temperature is 850 DEG C, pre-oxidizes 6min;
Step 2:Graphite impregnation processing
(1) with Al2O3Powder and phosphoric acid are waste aluminium dihydrogen phosphate;In described step 2 (1), Al2O3The material of powder and phosphoric acid Amount proportioning be 1:6;
(2) graphite material is submerged with aluminium dihydrogen phosphate, then is put in vavuum pump and is vacuumized;
(3) graphite material impregnated is placed in 120 DEG C of baking ovens and dries 5h;
Step 3:Apply brush applied coating
(1) with SiC powder, Al2O3Powder and additive A are coating material, configure coating slurry, the additive A matter in coating material It is 10%~40% to measure fraction;
(2) 2~5 brushings are carried out after coating slurry is well mixed on graphite rotator top layer, all dried after brushing every time or Naturally dry processing;The technique for brushing drying:After 100 DEG C of drying 1h, 1h is dried again at 200 DEG C.
2. the method as described in claim 1, it is characterised in that in described step 1, described graphite is loose graphite.
3. method as claimed in claim 1 or 2, it is characterised in that in described step 1 (2), high temperature furnace is box resistance wire One kind in stove, box silicon carbide rod furnace, tunnel cave.
4. method as claimed in claim 1 or 2, it is characterised in that in described step 2 (2), described vavuum pump vacuumizes Time be 5~30min.
5. method as claimed in claim 3, it is characterised in that in described step 2 (2), what described vavuum pump vacuumized Time is 5~30min.
6. method as claimed in claim 1 or 2, it is characterised in that in described step 3 (1), described additive A is Y2O3、MgO、TiO2、ZrSiO4In one or more.
7. method as claimed in claim 3, it is characterised in that in described step 3 (1), described additive A is Y2O3、 MgO、TiO2、ZrSiO4In one or more.
8. method as claimed in claim 4, it is characterised in that in described step 3 (1), described additive A is Y2O3、 MgO、TiO2、ZrSiO4In one or more.
CN201710724970.XA 2017-08-22 2017-08-22 Preparation method of graphite rotor anti-oxidation coating for aluminum melt purification Active CN107686380B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108456005A (en) * 2018-04-20 2018-08-28 郑州大学 Graphite antioxidant coating and preparation method thereof
CN111362727A (en) * 2020-03-18 2020-07-03 德翼高科(杭州)科技有限公司 Phosphate anti-oxidation coating of carbon/carbon composite material and coating process thereof

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DE19652670C1 (en) * 1996-12-18 1998-02-05 Meierkord Karl Heinz Electric furnace for maintaining metal in molten state
CN201864764U (en) * 2010-11-10 2011-06-15 王丽珍 Graphite rotor used in aluminum liquid degasser

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19652670C1 (en) * 1996-12-18 1998-02-05 Meierkord Karl Heinz Electric furnace for maintaining metal in molten state
CN201864764U (en) * 2010-11-10 2011-06-15 王丽珍 Graphite rotor used in aluminum liquid degasser

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
王丽珍: "铝液除气机中的石墨转子强化工艺研究", 《新技术新工艺》 *
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108456005A (en) * 2018-04-20 2018-08-28 郑州大学 Graphite antioxidant coating and preparation method thereof
CN108456005B (en) * 2018-04-20 2021-04-27 郑州大学 Graphite oxidation resistant coating
CN111362727A (en) * 2020-03-18 2020-07-03 德翼高科(杭州)科技有限公司 Phosphate anti-oxidation coating of carbon/carbon composite material and coating process thereof
CN111362727B (en) * 2020-03-18 2022-05-10 德翼高科(杭州)科技有限公司 Phosphate anti-oxidation coating of carbon/carbon composite material and coating process thereof

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