CN103771856A - Preparation method of Al2O3-TiB2 composite ceramic powder - Google Patents
Preparation method of Al2O3-TiB2 composite ceramic powder Download PDFInfo
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- CN103771856A CN103771856A CN201410057691.9A CN201410057691A CN103771856A CN 103771856 A CN103771856 A CN 103771856A CN 201410057691 A CN201410057691 A CN 201410057691A CN 103771856 A CN103771856 A CN 103771856A
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Abstract
The invention discloses a preparation method of Al2O3-TiB2 composite ceramic powder, and belongs to the technical field of ceramic material preparation. The preparation method comprises the following steps: fully mixing 32-38 wt.% of Al powder, 34-40 wt.% of CaSO4 powder, 12-18 wt.% of TiO2 powder and 10-16 wt.% of B2O3 powder, compacting the mixture, scattering pyrophoric powder on the surface of the compacted mixture, igniting, and carrying out self-propagating high-temperature reaction, thus obtaining mixed particles; and grinding the mixed particles, adding a carbonate solution, reacting for 5-10 minutes, then adding hydrochloric acid, reacting for 5-10 minutes, centrifuging, washing, and drying, thus obtaining the Al2O3-TiB2 composite ceramic powder. The preparation method is simple to operate, rapid in reaction, high in preparation efficiency and low in energy consumption and cost; equipment used in the method is simple; the prepared Al2O3-TiB2 composite ceramic powder has relatively high purity, relatively good quality and high industrial popularization value.
Description
Technical field
The invention belongs to ceramic materials preparation technology field, be specifically related to a kind of Al
2o
3-TiB
2the preparation method of composite ceramic powder.
Background technology
Ceramic powder belongs to a kind of nonmetal multifunctional material, and main component is Al
2o
3and SiO
2, thering is excellent dispersiveness and suspension, good covering power and chemical stability possess good plasticity-and thermotolerance simultaneously; Can also instead of titanium white powder, and can eliminate the light flocculation phenomenon of titanium dioxide.Thereby ceramic powder is at building coating, in industrial coating and civilian coating, is used widely.TiB
2because of it, to have fusing point high, and the feature such as hardness is large, and antioxidant property is good, and erosion resistance is strong, and heat-conductivity conducting is good, is widely used in the field such as mechanically resistant material and conducting ceramic material.With Al
2o
3in stupalith for main body, add TiB
2made composite ceramic material is collection compact grained Al
2o
3ceramic and the TiB with " three-dimensional continuity "
2be integrated, aspect mould manufacture and hard alloy coating, having a good application prospect.
At present, domesticly obtain very large breakthrough preparing aspect composite ceramics, the composite ceramics excellent property of producing, but exist technological process loaded down with trivial details, produce the problems such as cost is higher.As adopt the preparation method of the disclosed aluminium oxide-titanium oxide composite ceramic powder of patent 201010177581.8, although obtained the good composite ceramic powder of flowing property, but need to pass through that high speed centrifugation, spraying are dry, the technological process such as high temperature sintering and plasma spheroidization, preparation process relatively redundant and complicated and cost does not have controlled yet.In patent 2011102030264.3, adopt chemical process to prepare zirconium white and alumina composite ceramic, some pharmaceutical chemicalss that use are as harmful and be not easy to process to environment in concentrated hydrochloric acid, and do not meet environmental protection concept.
Produce Al
2o
3-TiB
2the key of composite ceramic powder is TiB
2the preparation of powder.At present, preparation TiB
2method mainly contain magnesium heat from spreading reduction method, fused salt electrolysis process and carbothermic method.The method of patent 01128497.8 disclosed preparation of high-purity titanium biboride, although compared with the synthetic TiB of SHS simple substance
2cost is low, and still whole reaction process need to be carried out under the protection of argon gas, and production technique is still relatively loaded down with trivial details.The preparation method of patent 201010227287.3 disclosed nano titanium diboride polycrystalline powders, utilizes magnesium heat to produce the higher TiB of purity from epidemic techniques
2powder, but the hot self-propagating reaction of this magnesium not only need to carry out under argon shield atmosphere, but also must utilize 500 tons of tabletting machine pressurize for some time, the technological process of whole preparation is relatively complicated, does not also give effective control on cost.The disclosed High Temperature High Pressure of patent 201210048082.8 is prepared the method for TiB2, and using titanium valve and boron powder as starting material, and the price of boron powder is higher and need under High Temperature High Pressure, carry out, and preparation cost is higher.And the synthetic titanium diboride ceramic powder of disclosed low-temperature solid-phase method in patent 201310168396.6, although simplified technical process, and the powder purity obtaining is higher, but the method is used micron-sized boron powder as starting material, does not overcome the defect that preparation cost is high.
Summary of the invention
Technical problem to be solved by this invention is to overcome to prepare at present the process redundant and complicated existing in composite ceramic powder, produces the more high defect of cost, utilizes self propagating high temperature synthetic technology, and a kind of easy and simple to handle, preparation Al that energy consumption is low, with low cost is provided
2o
3-TiB
2the method of composite ceramic powder.
A kind of Al
2o
3-TiB
2the preparation method of composite ceramic powder, comprises the following steps:
(1) by the Al powder of 32-38wt.%, the CaSO of 34-40 wt.%
4powder, the TiO of 12-18 wt.%
2the B of powder and 10-16 wt.%
2o
3after powder fully mixes, compacting, sprinkles pyrophoric powders on its surface, ignites, and carries out self propagating high temperature reaction, obtains composite grain;
(2) composite grain of being prepared by step (1) grinds, and adding concentration is the carbonate solution reaction 5-10 minute of 0.5-1.0mol/L, then adds 10%-20% hydrochloric acid reaction 5-10 minute, separates, and washing, dries, and obtains Al
2o
3-TiB
2composite ceramic powder.
The fineness of the Al powder in described step (1) is 200 orders.
Pyrophoric powders in described step (1) is fire powder.
Igniting in described step (1) ignited for magnesium rod.
Carbonate solution in described step (2) is Na
2cO
3solution or K
2cO
3solution.
Washing in described step (2) is that distilled water wash is to neutral.
Drying condition in described step (2) is: bake out temperature 100-110 ℃, drying time 0.5-1.0h.
Principle of the present invention is: self propagating high temperature reacts by two process implementations, is first aluminium powder and calcium sulfate reaction, and reaction formula is: 8Al+3CaSO
4=3CaS+4Al
2o
3, producing a large amount of heats, these heats impel aluminium, boron oxide and titanium oxide reaction, and reaction formula is: 10Al+3B
2o
3+ 3TiO
2=5Al
2o
3+ 3TiB
2, the surrounding at reactor after having reacted obtains composite grain, composite grain is collected and used mortar grind into powder with container.Then add M
2cO
3solution, the reaction of generation is: M
2cO
3+ CaSO
4=CaCO
3↓+M
2sO
4; And there is following reaction: CaCO after adding hydrochloric acid
3+ 2HCI=CO
2↑+CaCl
2+ H
2o and CaS+2HCl=CaCl
2+ H
2s ↑; The reaction of aluminium and calcium sulfate is the thermopositive reaction that produces amount of heat, and the hot conditions that the heat of generation is built provides condition with reacting of titanium oxide exactly to aluminium, boron oxide, and this reaction can be carried out; The Al that this reaction produces simultaneously
2o
3for composite ceramic powder of the present invention one of main component.The effect of dilute hydrochloric acid has the following aspects, makes on the one hand sulfurated lime rapidly and acid-respons generation gas and salt, is to eliminate because excessive calcium sulfate reacts the calcium carbonate impurity generating with sodium carbonate on the other hand, is also due to TiB in addition
2not with the characteristic of hydrochloric acid reaction.Being washed with distilled water to neutral object is not introduce chlorine element impurity.
Preparation Al provided by the invention
2o
3-TiB
2as shown in Figure 1, as shown in Figure 1, preparation process is simple for the schema of composite ceramic powder, and raw material is simple and easy to get.
The present invention utilizes self propagating high temperature synthetic technology to prepare Al
2o
3-TiB
2composite ceramic powder, the reaction times is short, and preparation efficiency is high, and energy consumption is low, has good industrial application value.
Tool of the present invention has the following advantages and beneficial effect:
1. the present invention has realized the reasonable utilization of resource, and energy consumption is little, with low cost.Use the reaction of aluminium and calcium sulfate not only to provide sufficient heat to the preparation of TiB2, abundant alumina substrate be provided to the ceramic powder of preparation simultaneously, reaction product aluminum oxide arrived rational utilization; Reaction is without other external energy supplies, and the heat being produced by reaction itself directly maintains the carrying out of reaction, and the aluminium powder of use, calcium sulfate, titanium oxide, boron oxide easily obtain, and cost compare is cheap.
2. present device is simple and easy, simple to operate.Only need to load the graphite jig of powder, without other large-scale equipment.Operating process is powdered reaction, collects grinding, hydrochloric acid removal of impurities, neutral processing and dry.
3. the present invention is swift in response, and preparation efficiency is higher.Self-propagating reaction process is only about 10 seconds, just can carry out afterwards follow-up grinding, removal of impurities and drying and processing at once.
4. the ceramic powder purity that prepared by the present invention is higher.Whole process product only has CaS to be impurity and may to contain a small amount of CaSO
4remnants, by adding a small amount of NaCO
3reaction, then utilizes dilute hydrochloric acid immersion and filtration subsequently just can process and obtains the composite ceramic powder that purity is higher.
Accompanying drawing explanation
Fig. 1 is preparation Al
2o
3-TiB
2the schema of composite ceramic powder.
Fig. 2 is the device schematic diagram of the self propagating high temperature reaction of embodiment 1, and wherein 1 is magnesium rod, and 2 is fire powder, and 3 is plumbago crucible, and 4 is reaction powder.
Fig. 3 is the prepared Al of embodiment 1
2o
3-TiB
2the XRD figure of composite ceramic powder.
Embodiment
Below in conjunction with embodiment, the present invention is done to further detailed description, but embodiments of the present invention are not limited to this.If no special instructions, the chemical using in following embodiment is analytical reagent.
By the Al powder of 32g (fineness is 200 orders), 38gCaSO
4powder, 14gTiO
2powder and 16gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck medicine fire powder (its setting drawing as shown in Figure 2) on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the NaCO of 0.5mol/L
3solution, to not having powder, fully reacts 10 minutes, then adds the dilute hydrochloric acid of 50mL 10% to react 10 minutes, and reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 110 ℃, dries 0.5 hour, finally makes Al
2o
3-TiB
2composite ceramic powder.By the Al making
2o
3-TiB
2composite ceramic powder carries out XRD test.XRD test result as shown in Figure 3, has shown Al in figure
2o
3and TiB
2characteristic peak, preparation powder be Al
2o
3-TiB
2composite ceramic powder.
By the Al powder of 34g (fineness is 200 orders), 40gCaSO
4powder, 12gTiO
2powder and 14gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck fire powder on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the NaCO of 0.5mol/L
3solution, to not having powder, fully reacts 10 minutes, then adds the dilute hydrochloric acid of 50mL 10% to react 10 minutes, and reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 110 ℃, dries 0.5 hour, makes Al
2o
3-TiB
2composite ceramic powder.
By the Al powder of 36g (fineness is 200 orders), 36gCaSO
4powder, 18gTiO
2powder and 10gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck fire powder on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the NaCO of 0.5mol/L
3solution, to not having powder, fully reacts 10 minutes, then adds the dilute hydrochloric acid of 50mL 10% to react 10 minutes, and reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 110 ℃, dries 0.5 hour, makes Al
2o
3-TiB
2composite ceramic powder.
By the Al powder of 38g (fineness is 200 orders), 34gCaSO
4powder, 16gTiO
2powder and 12gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck fire powder on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the NaCO of 0.5mol/L
3solution, to not having powder, fully reacts 10 minutes, then adds the dilute hydrochloric acid of 50mL10% to react 10 minutes, and reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 110 ℃, dries 0.5 hour, finally makes Al
2o
3-TiB
2composite ceramic powder.
Embodiment 5
By the Al powder of 32g (fineness is 200 orders), 38gCaSO
4powder, 14gTiO
2powder 16gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck fire powder on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the NaCO of 0.7mol/L
3solution, to not having powder, fully reacts 8 minutes, then adds the dilute hydrochloric acid reaction 8 minutes of 75mlL15%, after reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 105 ℃, dries 0.8 hour, finally makes Al
2o
3-TiB
2composite ceramic powder.
Embodiment 6
By the Al powder of 32g (fineness is 200 orders), 38gCaSO
4powder, 14gTiO
2powder and 16gB
2o
3powder is loaded in meal mixer, mix, then mixture is put into plumbago crucible, slightly after compacting, sprinkle one deck fire powder on mixture surface, light magnesium rod with lighter for ignition and ignite, mixed powder carries out self propagating high temperature reaction, after having reacted, generates composite grain in plumbago crucible surrounding.The composite grain of the generation of surrounding is collected, use mortar grind into powder, add the K of 1.0mol/L
2cO
3solution, to not having powder, fully reacts 5 minutes, then adds the dilute hydrochloric acid of 100mL20% to react 5 minutes, and reacted solution is filtered.The powder arriving filtering cleans to neutral with distilled water, then in the dryer of 100 ℃, dries 1.0 hours, finally makes Al
2o
3-TiB
2composite ceramic powder.
Above embodiments of the present invention are explained in detail, but ratio of the present invention is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, can also under the prerequisite that does not depart from aim of the present invention, makes a variety of changes.
Claims (7)
1. an Al
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that comprising the following steps:
(1) by the Al powder of 32-38wt.%, the CaSO of 34-40 wt.%
4powder, the TiO of 12-18 wt.%
2the B of powder and 10-16 wt.%
2o
3after powder fully mixes, compacting, sprinkles pyrophoric powders on its surface, ignites, and carries out self propagating high temperature reaction, obtains composite grain;
(2) composite grain of being prepared by step (1), grinds, and adding concentration is the carbonate solution reaction 5-10 minute of 0.5-1.0mol/L, then adds 10%-20% hydrochloric acid reaction 5-10 minute, separates, and washing, dries, and obtains Al
2o
3-TiB
2composite ceramic powder.
2. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: the fineness of the Al powder in described step (1) is 200 orders.
3. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: the pyrophoric powders in described step (1) is fire powder.
4. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: igniting in described step (1) ignited for magnesium rod.
5. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: the carbonate solution in described step (2) is Na
2cO
3solution or K
2cO
3solution.
6. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: the washing in described step (2) is that distilled water wash is to neutral.
7. a kind of Al according to claim 1
2o
3-TiB
2the preparation method of composite ceramic powder, is characterized in that: the drying condition in described step (2) is: bake out temperature 100-110 ℃, drying time 0.5-1.0h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445378A (en) * | 2014-12-17 | 2015-03-25 | 武汉大学 | Synthesis method of stannic oxide microrods |
| CN105905931A (en) * | 2016-04-20 | 2016-08-31 | 武汉大学 | Method of synthesizing spherical aluminum oxide nano-particles through self-propagation reaction |
| CN105984875A (en) * | 2015-01-30 | 2016-10-05 | 中国人民解放军军械工程学院 | Preparation method of TiB2 nano-wire array |
| CN108794928A (en) * | 2018-06-22 | 2018-11-13 | 安徽索亚装饰材料有限公司 | A kind of anti-mildew PVC foam Wallpaper paste material |
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| CN1152562A (en) * | 1996-10-30 | 1997-06-25 | 大连理工大学 | Method of preparing (AlxOx+TiBx) foamed ceramic filter by self-overgrowth high-temp. synthesis control |
| CN101301552A (en) * | 2008-07-08 | 2008-11-12 | 山东科技大学 | TiB2-Al2O3 compound filter material and preparation thereof |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
-
2014
- 2014-02-20 CN CN201410057691.9A patent/CN103771856B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152562A (en) * | 1996-10-30 | 1997-06-25 | 大连理工大学 | Method of preparing (AlxOx+TiBx) foamed ceramic filter by self-overgrowth high-temp. synthesis control |
| CN101301552A (en) * | 2008-07-08 | 2008-11-12 | 山东科技大学 | TiB2-Al2O3 compound filter material and preparation thereof |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445378A (en) * | 2014-12-17 | 2015-03-25 | 武汉大学 | Synthesis method of stannic oxide microrods |
| CN105984875A (en) * | 2015-01-30 | 2016-10-05 | 中国人民解放军军械工程学院 | Preparation method of TiB2 nano-wire array |
| CN105905931A (en) * | 2016-04-20 | 2016-08-31 | 武汉大学 | Method of synthesizing spherical aluminum oxide nano-particles through self-propagation reaction |
| CN105905931B (en) * | 2016-04-20 | 2017-08-25 | 武汉大学 | A kind of method of utilization Self-propagating Reaction Synthesis spherical alumina nano particle |
| CN108794928A (en) * | 2018-06-22 | 2018-11-13 | 安徽索亚装饰材料有限公司 | A kind of anti-mildew PVC foam Wallpaper paste material |
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