CN104190161B - The motlten metal ceramic filter that comprises Graphene - Google Patents
The motlten metal ceramic filter that comprises Graphene Download PDFInfo
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Abstract
The invention provides a kind of ceramic filter for filtering molten metal, main raw materials is refractory material, binding agent and Graphene. Wherein, in refractory material, at least comprise part ceramic material. In the present invention, introduce Graphene, improved mechanical strength and the thermal shock resistance of filter.
Description
Technical field
The present invention relates to a kind of ceramic filter that is suitable for filtering molten metal, be mainly used in casting industry.
Background technology
The purification of molten metal plays an important role to the mechanical property that improves foundry goods. Purify for molten metal at presentFilter is ceramic filter, can effectively intercept and capture the objectionable impurities in molten metal and molten metal is become from turbulent flowLaminar flow, plays and purifies and homogeneous effect. Ceramic filter can be divided into ceramic foam filter and straight hole according to structureCeramic filter. All almost ceramic foam filter for the filter of cast steel at present. In all meltingsMetal is with in the middle of foam filter, and the highest with the requirement of foam filter for cast steel, this is due to cast steel meltingMetal has higher melt temperature. At this temperature, filter need to keep enough mechanical strength, heat resistanceheat resistantPinking and lower specific heat capacity. Wherein, the factor that affects thermal shock resistance comprise material thermal coefficient of expansion, leadHot coefficient, material inherent strength, fracture toughness etc. Generally speaking, thermal coefficient of expansion is less, material Yin WenduThe Volume Changes changing and cause is little, and the temperature stress of corresponding generation is little, and thermal shock resistance is better; Thermal conductivity is large,The temperature difference of material internal is less, and the stress difference being caused by the temperature difference is less, and thermal shock resistance is better; Material inherent strengthHigher, bear thermal stress and the intensity of unlikely destruction is larger, good thermal shock. For ceramic material,The internal organizational structure of material and geometry are also influence factors. Generally speaking, material structure is relatively loose,Have certain porosity, have suitable micro-crack to exist, can improve energy to failure, make material under thermal shock notCause destroyed. But material structure is relatively loose, also can reduce the mechanical strength of material, therefore at filterBetween mechanical strength and thermal shock resistance, easily there is contradiction.
In prior art, having had a large amount of open source literatures is the technological improvements about motlten metal ceramic filter,These improvement are to be mainly to improve mechanical strength and the thermal shock resistance of filter, for example CN1449312A,CN101257957A, EP1421042A1 are disclosed.
Summary of the invention
The present invention proposes a kind of new solution, with improve simultaneously the cast steel mechanical strength of ceramic filter andThermal shock resistance.
Novel filtering material, it,, taking refractory material as material of main part, adds new material---Graphene with andHis binding agent and additive be by high-speed mixing, and the steps such as moulding, dry, sintering, make a kind of excellent performanceCeramic filter material. This material has excellent refractoriness, elevated temperature strength, thermal shock resistance and chemical stabilityEtc. advantage, be suitable for the filtration of molten steel, iron liquid, non-ferrous alloy liquid etc., be especially applicable to filtering all kinds of steel-castingsFilter.
The invention still further relates to the manufacture method of described filter, comprise successively step below:
(1) will comprise refractory material, binding agent, Graphene and liquid-carrier raw material and mix, make slurry;
(2) this slurry is coated with to a disposable mould;
(3) material after dry being coated with, obtains preform;
(4) this preform is carried out to anaerobic sintering and make foam filter.
Graphene of the present invention is Multi-layer graphite sheet composition, and its thickness is at 0.5-3nm, by adopting stoneChina ink alkene, significantly improves product properties.
Detailed description of the invention
Term " Graphene " in the present invention refers to the Graphene of individual layer or multiple-layer overlapped, in the situation of multilayerUnder, its number of plies is no more than 30 layers, is preferably no more than 20 layers, more preferably no more than 10 layers. In current one-tenthThis consideration, is not used the Graphene of individual layer in embodiments of the invention. In the following embodiment of the present invention, useGraphene be the Graphene of producing and selling by Shengquan Group Co. Ltd., Jinan, its number of plies is at 3-10Between layer, thickness is between 0.5-10 nanometer, preferably between 1-3 nanometer. Chinese patent application201210367072.0 number, recorded Graphene for No. 201410308860.1, the 201410398232.7thProduction method, the content of its disclosure is incorporated to herein with reform. The consumption of Graphene needn't exceed 10% conventionally,Even do not exceed 5%, for example 1%, 2%, 3%. Preferred embodiment, the consumption of Graphene is fire-resistantThe 0.5-2% of material.
The group that can select freely following material to form for refractory material of the present invention: zirconia, zirconia, zirconiumYing Fen, silica, aluminium oxide, corundum, titanium oxide, carbide (as, carborundum, zirconium carbide, titanium carbide,Calcium carbide, aluminium carbide), nitrate (nitric acid silicon and aluminum nitrate), nickel oxide, chromium oxide, magnesia, Mo LaiStone, talcum, feldspar, pyrophillite, wollastonite, spinelle, andalusite, kyanite, sillimanite, spodumene,Alumina, fused alumina zirconia, zirconium mullite, fire clay, graphite, anthracite, coke, active carbon, graphite-oxygenChange magnesium, graphite-zirconia.
Conventionally, the consumption of refractory material is by mass between 70-90%, preferably between 70-80%. Fire-resistantMaterial comprises zirconia, zirconia, zirconium English powder, silica, aluminium oxide, corundum, titanium oxide, carbonization conventionallyThing (as, carborundum, zirconium carbide, titanium carbide, calcium carbide, aluminium carbide), nitrate (nitric acid silicon and nitric acidAluminium), nickel oxide, chromium oxide, magnesia, mullite, talcum, feldspar, pyrophillite, wollastonite, point be brilliantIn stone, andalusite, kyanite, sillimanite, spodumene, alumina, fused alumina zirconia, zirconium mullite, fire clayOne or more. In another embodiment, refractory material further comprises graphite, anthracite, JiaoOne or more in charcoal, active carbon are as the second composition. A part for refractory material is favourable with this material with carbon elementIn the thermal coefficient of expansion and the thermal conductivity factor that reduce filter, thereby be conducive to improve thermal shock resistance. In this situationUnder, this second composition accounts for the 1-30% of refractory material, preferably 5-25%, more preferably 10-20%.
In the present invention, the effect of binding agent is to make to comprise refractory material, Graphene and liquid-carrier (normallyWater) slurry there is suitable caking property so that slurry has formability, can make preform. ?In a kind of embodiment, binding agent comprise a kind of in Alusil, aluminium colloidal sol, Zirconium colloidal sol, ρ-aluminium oxide orPerson is multiple. A kind of better mode is, binding agent forms the organic poly-of carbon while being pitch, tar or pyrolysisCompound, for example phenolic resins. This binding agent provides preferably caking property on the one hand, has higher after firingCarbon yield. These binding agents all can be buied from market. The consumption of binding agent account for refractory material, binding agent andThe 8-30% of Graphene three gross weight, preferably 10-20%.
In the present invention, the liquid-carrier that is used to form slurry is generally water, uses other liquid as first but do not get rid ofAlcohol, ethanol and isopropyl alcohol.
In the time addressing composition of raw materials, all do not comprise the amount of liquid-carrier herein, only consider refractory material, stoneThe amount of China ink alkene and binding agent. The present invention does not get rid of in raw material yet and introduces other a small amount of functional aids. For example,In one embodiment of the invention, added a small amount of lignin, it is by quantity not sufficient 3%, and for example 1%,This is in order to reduce amount of water, improves product strength simultaneously; In another embodiment, added a small amount of carbon fibreDimension, it uses quantity not sufficient 1%, and this is in order to ensure product high-temperature behavior, simultaneously little on amount of water impact. CanOther auxiliary agents for example thickener, dispersant, the surfactant introduced. The consumption of these functional aids needs onlyBe no more than 10% of total amount, for example 8%, 6%, 3% and even 1% or lower, all should be understood to thisThe detailed description of the invention of inventive concept, or improved embodiment.
Filter of the present invention can be prepared to the form into a kind of open cell porous material. Open cell porous material isRefer to a kind of hole that comprises rule, regular, the irregular or random distribution of part in solid material, these Kong WeirongMelt the passage of metal. Can all or part of interactive exchange maybe can there be multiple passages in these holes, make motlten metalPass through. The size in hole own and shape can be rules or irregular. For example, these holes can be by a series of flatThe passage of row, can linearly pass this solid material, and these passages have the cross section of any needs, for example, and circleShape, ellipse, triangle interconnecting channel etc., and the poroid distribution similar to natural foam.
The present invention has further comprised a kind of manufacture and has been applicable to the method for the filter of filtering molten metal, this filtrationDevice comprises refractory material, binding agent and Graphene. This preparation method comprises by refractory material, binding agent, stoneThe mixture of China ink alkene composition is shaped to the preform of required shape, then through oversintering, obtains filter.
Can prepare straight hole filter with above-mentioned raw materials, method is: in a model, comprise by compressing oneThe mixture of refractory material, binding agent, Graphene makes it to become pan or sheet, then uses a kind of combinedPin or combined bar pierce through compressor, have just produced like this aperture on the cross section of pan or sheet.These apertures are likely pentagonal. And aperture is preferably in the surface of compressor with a kind of grill-shaped of ruleFormula is arranged. Another kind of product similarly can be a kind of by refractory material, binding agent, Graphene by extrudingThe mixture of composition is produced. Preferably in mixture, add a kind of liquid and/or some other additiveMixture is more easily pushed, after extrusion process completes, make to push with a kind of mould of being furnished with axle shape compositionDeposits yields aperture. Often use this extrusion process in this industry. Use this extrusion process can obtain directlyThe preform of pass filter.
Can also make ceramic foam filter with above-mentioned material. The method comprises the steps: that (1) will compriseRefractory material, binding agent, Graphene and liquid-carrier raw material mix, and make slurry; (2) this slurry is coated withTo a disposable mould; (3) material (4) after dry being coated with is if needs then carry out once or manyInferior refractory material and/or binding agent are coated with, and then are dried, and obtain preform; (5) by this preformationType body carries out sintering and makes foam filter.
May also need to add surfactant, addition is total weight of solids several percentage points, for example 1-6%, to improve the mobility of slurry and the wetability to disposable mould. Can also use dispersant, at potteryIt is very common that porcelain powder uses dispersant in mixing. Conventional dispersant is various dispersions conventional in this areaAgent, for example calgon, sodium phosphate trimer, polyacrylamide or sulfonic acid substance (as sodium alkyl sulfonate,Sodium metnylene bis-naphthalene sulfonate). Can also use thickener: xanthans, starch, CMC, bentonite, clay,PVA, PVB etc.
In the preparation process of slurry, can use efficient blender that the solid in slurry and liquid are mixed.Because Graphene is nanoscale, for graphene uniform is dispersed in slurry, can adopt ultrasonic wave, ball millingMachine or high speed dispersor mix.
Above-mentioned disposable mould is the foamed material with network-like skeleton, can adhere to above-mentioned slurry of the present invention,Form preform. This disposable mould can vapor away in follow-up high-temperature process, or major part is wavedSend out, and carbon wherein left behind with the form of active carbon. Typical foamed material be polyurethane foam,Polystyrene foam, polyethylene. Can slurry be executed by means such as dipping, roller coat, brushing, sprayingsBe added on disposable mould, and carry out appropriateness extruding, for example, make it pass through two rollers that relatively roll, squeeze outUnnecessary slurry. Preferably, in order to optimize the performance that is coated with of slurry, can in slurry, add forming agent. Allusion quotationThe forming agent of type is polyvinyl alcohol, and its addition is 0.05-2.0%.
After being coated with, disposable mould is dried, if need to be further coated with, until reach requiredThickness. Material after being coated with is preferably under higher temperature dry, removes all residual volatile matters, obtains pre-Formed body.
Obtaining above-mentionedly with disposable mould with not after the preform with disposable mould, needing sintering preformedBody. Be preferably in to be no more than at 1000 DEG C and carry out sintering, be more preferably no more than 950 DEG C. Sintering is to lackUnder oxygen atmosphere, carry out, for example, in an inert " anaerobic " atmosphere, in nitrogen or argon atmospher, or in vacuumOr " reducing atmosphere ", in hydrogen and/or carbon monoxide and/or coal gas (mixture of namely for methane and hydrogen) atmosphere.Mode as an alternative, there is lower sintering preform in the medium that can reduce, for example, removes with carbon (graphite)Partly or entirely oxygen.
Before sintering, the foam that moulding slurry or painting hang up properly is general at least part of dry, as, at 100～200 DEG CBetween be dried (150 DEG C according to appointment).
Sintering is generally to carry out in a drying oven or kiln, but also can use the thermal source of other form to carry outSintering, as the microwave that carries out wireless frequency heating.
The present invention is taking cheap recyclable materials---and Graphene is prepared filter for molten metal, root as primary raw materialThe filter obtaining according to the present invention is suitable for filtering multiple motlten metal, is particularly suited for filtering the gold such as molten iron, aluminium alloyBelong to liquid. Preparation method is simple, greatly reduces product cost, is suitable for smelting, foundary industry uses in a large number.
Embodiment 1:
Alumina powder: 81%
Graphene: 10%
Aluminium sol adhesive: 9%
Carbon fiber: 0.5% (based on first three items gross weight)
Above-mentioned material is all commercially available material, and described ratio is all percentage by weight. In above-mentioned powder, needAdd and account for the xanthans of powder gross weight 0.2% and 20% water. Slurry is powder with an efficient blenderMaterial and water are mixed. This slurry is used for being coated with polyurethane foam. Then at 1000 DEG C under oxygen-free atmosphereCarry out sintering.
The filter size of making by this formula is 50 × 50 × 15mm, has filtered 50kg steel at 1650 DEG CWater, result is that this filter has withstood this testing conditions, and on request molten steel is filtered.
Through detecting with anti-folding instrument, the rupture strength of screen pack is 1.60 ± 0.2Mpa.
The same specification filter of preparing under similarity condition, does not add Graphene, at 1650 DEG C, has only filtered, just there is breakage in 40kg molten steel. Through with the detection of anti-folding instrument, the rupture strength of screen pack is 1.20 ±0.3Mpa。
Embodiment 2
Schmigel: 18%
Mullite: 50%
Silicon powder: 5%
Alusil solution: 20%
Lignin: 1.0%
Carbon fiber: 1.0%
Graphene: 5%
In above-mentioned powder, need to add 12% water. Slurry is mixed to powder and water with an efficient blenderClose and make. This slurry is used for being coated with polyurethane foam. Then under oxygen-free atmosphere, carry out sintering at 1000 DEG C.The filter size of making by this formula is 50 × 50 × 15mm, has filtered 50kg molten steel at 1650 DEG C,Result is that this filter has withstood this testing conditions, and on request molten steel is filtered.
The same specification filter of preparing under similarity condition, does not add Graphene, at 1650 DEG C, has only filtered, just there is breakage in 39kg molten steel.
Embodiment 3
Zirconium mullite: 62%
ρ-aluminium oxide: 5%
Coke blacking: 11%
Graphene: 2%
Phenolic resins: 20%
In above-mentioned powder, need to add and account for the calgon of powder gross weight 2% and 15% water. To starchMaterial is infused in compression in a model and makes it to become pan, then uses a kind of combined needle-penetration compressor, thisSample has just produced aperture on the cross section of pan, has obtained a kind of straight pass filter. Then at 150 DEG CUnder be dried, and in carbon monoxide atmosphere, carry out sintering at 1100 DEG C.
The filter obtaining has filtered 50Kg molten steel at 1650 DEG C, and result is that this filter has stood thisTesting conditions. The same specification filter of preparing under similarity condition, does not add Graphene, at 1650 DEG C onlyFilter 35kg molten steel, just occurred breakage.
Embodiment 4
Calcined bauxite in powder: 70%
Clay powder: 15%
Graphene: 1%
Alusil: 14%
In above-mentioned powder, need to add and account for the calgon of powder gross weight 2% and 18% water. SlurryPowder and water are mixed with an efficient blender. This slurry is used for being coated with polyurethane foam. ThenUnder 1100 DEG C of carbon monoxide atmospheres, carry out sintering.
The filter size of making by this formula is 50 × 50 × 15mm, has filtered 50kg iron at 1500 DEG CWater, result is that this filter has withstood this testing conditions, and on request molten steel is filtered.Comparative example:
Calcined bauxite in powder: 70%
Clay powder: 15%
Graphite: 1%
Alusil: 14%
In above-mentioned powder, need to add and account for the calgon of powder gross weight 2% and 18% water. SlurryPowder and water are mixed with an efficient blender. This slurry is used for being coated with polyurethane foam. ThenUnder 1100 DEG C of carbon monoxide atmospheres, carry out sintering.
The filter size of making by this formula is 50 × 50 × 15mm, has only filtered 20kg at 1500 DEG CMolten iron, this filter is unable to bear the filtration of 50 kilograms of molten iron, and broken product introduction iron liquid does not rise and has beenThe effect of filter.
Claims (9)
1. for the ceramic filter of filtering molten metal, main raw materials be refractory material, binding agent andGraphene, the thickness of described Graphene is at 0.5-3nm.
2. filter claimed in claim 1, wherein, in mass, refractory material accounts for 70-90% to described raw material,Binding agent accounts for 8-30%; Graphene accounts for 0.1-10%.
3. filter claimed in claim 1, wherein, refractory material is selected from: zirconium English powder, silica, aluminium oxide,Corundum, titanium oxide, carborundum, zirconium carbide, titanium carbide, calcium carbide, aluminium carbide, nitric acid silicon, nitric acidAluminium, nickel oxide, chromium oxide, magnesia, mullite, talcum, feldspar, pyrophillite, wollastonite, pointSpar, andalusite, kyanite, sillimanite, spodumene, alumina, fused alumina zirconia, zirconium mullite, fire-resistantClay, graphite, anthracite, coke, active carbon, graphite-magnesia, graphite-zirconia.
4. filter claimed in claim 3, wherein, in described refractory material a part be selected from graphite, anthracite,Coke, active carbon.
5. filter claimed in claim 4, wherein, the 1-30% that a described part is refractory material.
6. filter claimed in claim 1, wherein, described binding agent is rich carbon organic matter, it is pitch, JiaoWhen oil and pyrolysis, form the organic polymer of carbon.
7. filter claimed in claim 6, wherein, described binding agent is phenolic resins.
8. filter claimed in claim 1, wherein, described binding agent be Alusil, aluminium colloidal sol, Zirconium colloidal sol,One or more in ρ-aluminium oxide.
9. filter claimed in claim 1, wherein, described Graphene accounts for 0.5-2%.
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