CN111498849B - Aluminothermic reduction preparation of Ti2Method for preparing AlC ceramic powder - Google Patents

Aluminothermic reduction preparation of Ti2Method for preparing AlC ceramic powder Download PDF

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CN111498849B
CN111498849B CN202010515242.XA CN202010515242A CN111498849B CN 111498849 B CN111498849 B CN 111498849B CN 202010515242 A CN202010515242 A CN 202010515242A CN 111498849 B CN111498849 B CN 111498849B
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赵坤
李言栋
张晓东
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Yangtze Normal University
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Abstract

The invention discloses a method for preparing Ti by aluminothermic reduction2The method for preparing AlC ceramic powder is characterized by taking fluotitanate, aluminum powder and activated carbon powder with the mass ratio of 1 (0.16-0.38) to 0.02-0.05 as raw materials, mixing and grinding the raw materials, and then carrying out thermal reduction reaction andand after vacuum distillation, removing impurities to obtain the product. The method has the advantages of simple raw material requirement, wide source, lower cost, shorter process flow, higher reaction efficiency, better controllability, full-element utilization and the like.

Description

Aluminothermic reduction preparation of Ti2AlC ceramicsMethod for producing powder
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a method for preparing Ti by aluminothermic reduction2A method for preparing AlC ceramic powder.
Background
In recent years, with the rapid development of social economy, people have more and more extensive demands on ceramic materials, and the ceramic materials are inorganic non-metallic materials with the advantages of high melting point, high hardness, high wear resistance, high oxidation resistance and the like. It can be used for construction and cutter materials, and ceramics also have certain special properties, so it can be used as functional material. The ceramic powder is a material for preparing ceramic products, and good ceramic products are prepared by adopting the ceramic powder, so that more exquisite appearance and excellent performance can be obtained.
Mn +1AXn (MAX phase for short) ceramics are ternary carbon/nitride ceramics with a nano-layered structure, wherein M represents a transition metal element, A represents a main group element, X is carbon or nitrogen element, and n is generally 1-3. The MAX ceramic has the characteristics of ceramic and metal, such as high strength, high electric and thermal conductivity, corrosion resistance, oxidation resistance, excellent processability and the like. Ti2AlC (titanium aluminum carbide) ceramic is taken as a typical 211-phase MAX ceramic, is a laminar machinable conductive ceramic, has low density and low expansion coefficient, high elastic modulus and high mechanical strength, good oxidation resistance, thermal shock resistance, chemical and thermal corrosion resistance, damage resistance at high temperature and certain self-repairing capability, and has great application potential in the technical fields of nuclear power, aerospace and extreme working environments. At present, Ti2The preparation process of AlC mainly comprises hot-pressing sintering (HP), reaction hot-pressing sintering technology (RHP), Hot Isostatic Pressing (HIP), Spark Plasma Sintering (SPS), self-propagating reaction, self-propagating quasi-hot isostatic pressing technology (SPS/PHIP) and the like.
But Ti is prepared at the present stage2The AlC basically adopts metal powder, carbon powder or carbide as raw materials, so that the raw material cost and the process cost are high, the further expanded production is limited, and the Ti is further limited2More widespread use of AlC.
For example, CN105271232A discloses a method for preparing Ti based on ultrasonic-assisted thermal explosion reaction2The AlC method is that Ti powder, Al powder and graphite powder are used as raw materials, and the ternary Ti with the main phase is prepared by ultrasonic thermal explosion reaction2Reaction products of AlC. The method utilizes ultrasonic-assisted thermal explosion reaction, and can rapidly prepare relatively pure Ti under the condition of low temperature2And (4) AlC. Therefore, although the preparation process is relatively quick, the method still directly adopts metal powder as a raw material and adopts ultrasonic-assisted thermal explosion as a preparation process, and the defects of high raw material cost and high process cost still exist.
Therefore, how to design a Ti with simple requirements on raw materials, lower cost, simple process and higher reaction efficiency2The preparation process of AlC ceramic powder becomes a problem to be considered and solved by the technical personnel in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problems to be solved by the invention are as follows: how to provide a method for preparing Ti by aluminothermic reduction with simple raw material requirement, wide source, lower cost, shorter process flow, higher reaction efficiency and better controllability2A method for preparing AlC ceramic powder.
In order to solve the technical problems, the invention adopts the following technical scheme:
aluminothermic reduction preparation of Ti2The method for preparing the AlC ceramic powder is characterized in that fluotitanate, aluminum powder and activated carbon powder with the mass ratio of 1 (0.16-0.38) to (0.02-0.05) are used as raw materials, and are obtained by mixing and grinding the raw materials, carrying out thermal reduction reaction and vacuum distillation and then removing impurities;
wherein the reaction formula of the thermal reduction reaction is as follows:
when the sodium fluotitanate is used as the raw material,
6Na2TiF6+11Al+3C＝3Ti2AlC+12NaF+8AlF3 (1)
xNaF+yAlF3＝NaxAlyFx+3ywherein 0 is<x≤12，0<y≤8 (2)
Alternatively, when potassium fluotitanate is used as a raw material,
6K2TiF6+11Al+3C＝3Ti2AlC+12KF+8AlF3 (3)
mKF+nAlF3＝KmAlnFm+3nwherein 0 is<m≤12，0<n≤8 (4)。
Thus, in this embodiment, the raw materials can be prepared according to the above reaction formula, wherein the fluorotitanate is a major raw material, and includes, but is not limited to, sodium fluorotitanate and potassium fluorotitanate. Thus, the fluorine-containing titanate is directly used as a raw material source, the raw material proportion and the specific process are controlled, and the Ti is prepared by thermal reduction reaction2AlC products. Therefore, the raw materials are simple in requirement, wide in source and lower in cost, and Ti can be prepared by means of short-process steps2AlC ceramic powder. Meanwhile, other reaction byproducts can be recycled, so that the utilization efficiency of the raw materials is improved.
Preferably, the fluotitanate is sodium fluotitanate. This is due to the difference in atomic weight of sodium and potassium, which means that a lower proportion of sodium salts is required to produce the same weight of ceramic powder. And, sodium salt has the same high wettability and non-hygroscopic property as potassium salt, even sodium salt has higher stability. In addition, the by-product generated by adopting the sodium salt is sodium cryolite derivative, and the industrial value of the sodium cryolite derivative is higher than that of potassium cryolite. Thus, sodium fluorotitanate may be more advantageous as a raw material than potassium fluorotitanate.
As an optimization, the method specifically comprises the following steps:
step 1: mixing sodium fluotitanate, aluminum powder and activated carbon powder which meet the proportion requirement, wet grinding, drying the slurry, and dry grinding and activating in vacuum or inert atmosphere;
step 2: putting the mixed and ground material into a mold, and cold-pressing under the condition of 40-120MPa to obtain a green body;
and step 3: placing the green body in a vacuum reduction furnace for thermal reduction at the temperature of 800-1500 ℃ and the vacuum degree of 10-4-10Pa, reduction time 1-6 hours;
and 4, step 4: after the reduction is finished, controlling the temperature to be 1000-;
and 5: cooling the distilled product to room temperature along with the furnace under the vacuum or argon condition to obtain the porous agglomerate Ti2Peeling AlC crude product, crushing and grinding into powder, sieving the obtained powder, pickling, washing with water and drying to obtain purified Ti2AlC powder.
In the detailed steps, the first step adopts wet grinding to realize the full mixing of the raw material components under the condition of bulk particles, and has the effect of removing trace soluble impurities possibly existing in the raw materials; then, after drying, grinding is realized by adopting a dry grinding mode, under the protection condition of vacuum or inert atmosphere, proper grinding time is selected, the activity of the raw material components can be improved on the basis of the wet grinding process, the aim of further refining and increasing the activity is achieved, and the efficiency of the subsequent reduction reaction can be effectively improved; in the second step, the raw materials after mixing and grinding are firstly subjected to cold pressing to obtain green bodies, and proper cold pressing conditions are selected, so that the contact area among particles to be reacted of the raw material components can be greatly increased, and the reduction efficiency and the product generation rate can be greatly increased. However, it is not preferable to form a preform under an excessive pressure because it affects the escape of distillation components in the subsequent distillation process.
Preferably, in the step 1, the mass ratio of the sodium fluorotitanate, the aluminum powder and the activated carbon powder is 1:0.248: 0.029.
A large number of experiments prove that the preferable proportion can achieve better preparation effect.
In the step 1, the wet grinding time of the material is 2-8 hours, preferably 4 hours, and the dry grinding time is 4-12 hours, preferably 8 hours.
A large number of comparison experiments prove that better mixing and activating effects can be achieved by adopting the optimized combined grinding time parameters.
Preferably, in the step 2, the green body is obtained by cold pressing under the condition of 50 MPa.
Experiments prove that the cold pressing with the pressure parameters has a good effect.
As an optimization, the aboveIn step 3, the reduction temperature is 1250 ℃ and the vacuum degree is 10-3Pa, reduction time 3 hours. The effect can be optimized.
Preferably, in step 4, the vacuum distillation is carried out at 1200 ℃ for 5 hours. This allows the effect to be optimised.
In the above step 4, the distillation product obtained is mainly Na3AlF6Sodium hexafluoroaluminate, Na5Al3F14(Cone cryolite) and NaAlF4(single cryolite) and a mixture containing small amounts of low valent titanium compounds and fluoride, wherein the titanium content is 3% to 8%.
Therefore, as optimization, the distillation product obtained in the step 4 can be further subjected to the following steps of titanium element recovery and cryolite component purification treatment: step 6, grinding the distillation product into powder, adding aluminum scraps or aluminum-titanium intermediate alloy scraps, placing the powder in a reduction furnace, and preserving heat for 1-5 hours at the temperature of 850-; after cooling, the upper layer product is white molten salt, and the lower layer product is the aluminum-titanium intermediate alloy.
In the secondary aluminothermic reduction process of the distillation product, the component of the obtained upper-layer molten salt is Na3AlF6Sodium hexafluoroaluminate, Na5Al3F14(Cone cryolite) and NaAlF4The mixture of (single cryolite) belongs to cryolite series products, so the pure molten salt component obtained after the secondary reduction can be called as cryolite component, and the molecular ratio of the cryolite component is 2.10-2.85.
The principle of the secondary reduction process as the recycling process of the distillation product is that the high-vapor-pressure titanium-containing compound in the distillation product is re-reduced by adopting the reducing component aluminum in the pure aluminum or the aluminum-titanium intermediate alloy, and the titanium element in the distillation product is finally Al3The form of Ti is present in the metal melt. Thus, the titanium element in the distillation product can be completely extracted, and the preparation of Ti by aluminothermic reduction is realized2Closed-loop recovery processing of waste products in AlC ceramic powder process to obtain byproductsThe cryolite component and the aluminum-titanium intermediate alloy achieve the complete utilization of reaction raw materials, no waste products are generated in the whole process, and the environment-friendly performance of the process and the utilization efficiency of the reaction raw materials are greatly improved.
In the secondary aluminothermic reduction process of the distillation product, the mixture ratio of the raw materials is controlled, and the distillation product is aluminum scrap or aluminum-titanium intermediate alloy which is 1 (0.2-5). The aluminum-titanium intermediate alloy can be recycled, and is subjected to secondary thermal reduction treatment with distillation products obtained in different batches of experiments, so that closed-loop control is realized.
After the distillation product is subjected to secondary aluminothermic reduction, the first titanium-containing percentage of the obtained aluminum-titanium intermediate alloy is 0.6-16%; the cryolite component contains less than 0.0005% of titanium by mass, so that the cryolite component can completely reach the application standard of industrial products.
From the above description of the specific steps and principles, it can be seen that the method of the present invention is simple in operation, short in process flow, and obtains Ti2The AlC powder has high purity, adjustable granularity, easily controlled ratio of titanium to aluminum to carbon in the reaction process, low cost of raw materials and high component purity of the by-product cryolite, and can be used as an aluminum industrial electrolyte.
In conclusion, the method has the advantages of simple raw material requirement, wide source, lower cost, shorter process flow, higher reaction efficiency, better controllability, no waste gas or waste residue generated in the whole process, full element utilization in the whole process and the like.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention in a specific embodiment.
FIG. 2 is an XRD pattern of the ceramic powder obtained in example 1.
FIG. 3 is a photograph showing the pure cryolite fraction after the secondary reduction obtained in example 3.
FIG. 4 is a photograph showing the appearance of the Al-Ti master alloy obtained in example 3.
FIG. 5 is an SEM image of the Al-Ti master alloy obtained in example 4.
Fig. 6 is a table listing the results of XRF component analysis of cryolite compositions obtained in example 3.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The specific implementation mode is as follows: aluminothermic reduction preparation of Ti2The flow of the method for preparing the AlC ceramic powder is shown in figure 1 and comprises the following steps:
step 1: mixing sodium fluotitanate, aluminum powder and activated carbon powder which meet the requirement of the proportion of 1 (0.16-0.38) (0.02-0.05), wet grinding the mixture for 2-8 hours, drying the slurry after wet grinding, and then dry grinding and activating the slurry in vacuum or inert atmosphere for 4-12 hours;
step 2: putting the mixed and ground material into a mold, and cold-pressing under the condition of 40-120MPa to obtain a green body;
and step 3: placing the green body in a vacuum reduction furnace for thermal reduction at the temperature of 800-1500 ℃ and the vacuum degree of 10-4-10Pa, reduction time 1-6 hours;
and 4, step 4: after the reduction is finished, controlling the temperature to be 1000-;
and 5: cooling the distilled product to room temperature along with the furnace under the vacuum or argon condition to obtain the porous agglomerate Ti2Peeling AlC crude product, crushing and grinding into powder, sieving the obtained powder, pickling, washing with water and drying to obtain purified Ti2AlC powder;
step 6, grinding the distillation product into powder, adding aluminum scraps or aluminum-titanium intermediate alloy scraps, placing the powder in a reduction furnace, and preserving heat for 1-5 hours at the temperature of 850-; after cooling, the upper layer product is a white cryolite component, can be used as a solvent for the aluminum electrolysis industry after being ground, and the lower layer product is an aluminum-titanium intermediate alloy; in the secondary aluminothermic reduction process of the distillation product, the mixture ratio of the raw materials is controlled, and the distillation product is aluminum scrap or aluminum-titanium intermediate alloy which is 1 (0.2-5). Wherein the aluminum-titanium intermediate alloy can be repeatedly recycled and the distillation product is subjected to secondary thermal reduction treatment, so that closed-loop control is realized.
Wherein the purity of the sodium fluotitanate is more than 99.5 percent, and the granularity is 25-120 mu m. The purity of the aluminum powder is more than 99.9 percent, and the oxygen content is less than 0.2 percent. The purity of the activated carbon powder is more than 99 percent, and the apparent relative density is 0.08-0.45.
The raw materials of sodium fluotitanate, aluminum powder and activated carbon powder are firstly mixed according to the proportion, wet grinding is carried out in an absolute ethyl alcohol medium to form raw material slurry, then vacuum drying is carried out on the raw material slurry, and the dried powder is placed in ball milling equipment in a vacuum or inert gas environment for dry milling.
Wherein the distillation product mainly comprises cryolite, concryolite and single cryolite, and a small amount of mixture of incompletely reduced low-valence titanium fluoride salt; after the secondary reduction, the titanium element in the distillation product is completely extracted in the form of aluminum-titanium intermediate alloy, and a pure cryolite component is generated, wherein the molecular ratio of the pure cryolite component is 2.10-2.85.
The results of the present invention are further verified below by means of several groups of specific examples. Each example was carried out in accordance with the following specific procedures and parameter conditions, except that the limitations of the above-described embodiments were satisfied.
Example 1
On the basis of satisfying the above-described embodiments, the following requirements are fulfilled: mixing 300 g of sodium fluotitanate, 74.3 g of aluminum powder and 8.8 g of activated carbon powder, carrying out wet grinding for 4 hours by adopting a planetary ball mill in an anhydrous ethanol medium at a material-ball ratio of 2:1, and then carrying out vacuum drying for 12 hours at the temperature of 60 ℃; placing the dried mixed material into a high-energy ball mill, and performing high-energy activation for 8 hours in a high-purity argon atmosphere; placing the activated mixed material in a steel mould, and cold-pressing the mixed material into a blank under the pressure of 50 MPa; then the blank is put into a reduction furnace and is thermally reduced under the vacuum condition, the reduction temperature is 1250 ℃, and the vacuum degree is 10-3Pa, the reduction time is 3 hours; and after the reduction process is finished, starting a vacuum system for vacuum distillation, setting the distillation temperature to be 1200 ℃, carrying out distillation for 5 hours, closing a control system after the distillation is finished, and cooling the materials to room temperature along with the furnace under the vacuum condition to obtain 87.7 g of a reduced crude product and 293.4 g of a distillation product.
Peeling the crude product, and crushingGrinding into particles with the particle size of less than 75 mu m, placing the particles in 8 percent hydrochloric acid solution for acid washing, then washing with deionized water, and finally drying in vacuum at 60 ℃ to obtain Ti2The XRD analysis result of AlC ceramic powder is shown in FIG. 2, and it can be seen from FIG. 2 that the main phase of the product is Ti2AlC but with a small number of minute impurity peaks, resulting in Ti2The purity of AlC is more than 96 percent.
Example 2
On the basis of satisfying the above-described embodiments, the following requirements are fulfilled: mixing 616.3 g of sodium fluotitanate, 152.5 g of aluminum powder and 18.1 g of activated carbon powder, carrying out wet grinding for 5 hours by adopting a planetary ball mill in an anhydrous ethanol medium at a material-ball ratio of 2:1, and then carrying out vacuum drying for 16 hours at the temperature of 60 ℃; then placing the dried mixed material into a high-energy ball mill to carry out high-energy activation for 10 hours under the vacuum condition; placing the activated mixed material in a steel mould, and cold-pressing the mixed material into a blank under the pressure of 50 MPa; then the blank is put into a reduction furnace and is thermally reduced under the vacuum condition, the reduction temperature is 1250 ℃, and the vacuum degree is 10-3Pa, the reduction time is 4 hours; and after the reduction process is finished, starting a vacuum system for vacuum distillation, wherein the distillation time is 7 hours, closing the control system after the distillation is finished, and cooling the materials to room temperature along with the furnace under the argon condition to obtain 191.3 g of a reduction crude product and 592.9 g of a distillation product.
Peeling the crude product, crushing and grinding the crude product into particles with the particle size of less than 75 mu m, placing the particles into 8 percent hydrochloric acid solution for acid washing, then adopting deionized water for water washing, and finally obtaining Ti with the purity of about 95 percent after vacuum drying at 60 DEG C2AlC ceramic powder.
Example 3
The distillation products obtained in the examples 1 and 2 are used as raw materials, aluminum scraps with the granularity less than 5mm are used as reducing agents, and the secondary thermal reduction is carried out to prepare pure cryolite and aluminum-titanium intermediate alloy. The method specifically comprises the following steps: grinding 420 g of distillation product to a particle size of less than 1mm, mixing and pressing 120 g of aluminum scraps as a reducing agent into a cluster, placing the cluster in a reducing furnace, heating to 1200 ℃ under the protection of argon, preserving heat for 3 hours, and cooling to room temperature along with the furnace; the product was removed and separated, with the upper layer being a white pure cryolite fraction with a theoretical mass of 413.4 g and a cryolite molecular ratio of 2.4, and XRF analysis results for the cryolite fraction being shown in the composition list of fig. 6. A photograph of the cryolite fraction obtained after the second thermal reduction is shown in fig. 3. As can be seen from FIGS. 3 and 6, the cryolite produced in example 3 of the present invention meets the national standard GB/T4291-. The lower layer is massive aluminum-titanium intermediate alloy with the mass of 126.6 g; the photo of the appearance of the obtained aluminum-titanium master alloy is shown in FIG. 4.
Example 4
The method is the same as example 3 except that the distilled product obtained in example 2 is used as a raw material, and the method is different in that pure cryolite and Al-Ti intermediate alloy are prepared by secondary thermal reduction using Al-Ti intermediate alloy scrap containing 10.9 wt% of Ti as a reducing agent. The specific process is as follows: grinding 300 g of distillation product until the granularity is less than 1mm, mixing 120 g of aluminum-titanium intermediate alloy scraps with the granularity less than 1mm, pressing into a cluster, placing the cluster in a reduction furnace, heating to 1200 ℃ under the protection of argon, preserving heat for 3 hours, and cooling to room temperature along with the furnace; taking out the product and separating, wherein the upper layer is white pure cryolite component, the theoretical mass is 297.2 g, and the molecular ratio of the cryolite is 2.4; the lower layer is massive aluminum-titanium intermediate alloy with the mass of 122.8 g. The SEM image of the obtained al-ti master alloy is shown in fig. 5.

Claims (7)

1. Aluminothermic reduction preparation of Ti2The method for preparing the AlC ceramic powder is characterized in that fluotitanate, aluminum powder and activated carbon powder with the mass ratio of 1 (0.16-0.38) to 0.02-0.05 are used as raw materials, and are obtained by mixing and grinding, carrying out thermal reduction reaction and vacuum distillation and then removing impurities;
sodium fluorotitanate is selected as fluorotitanate;
wherein the reaction formula of the thermal reduction reaction is as follows:
6Na2TiF6+11Al+3C=3Ti2AlC+12NaF+8AlF3 (1)
xNaF+yAlF3=NaxAlyFx+3y wherein 0 is<x≤12，0<y≤8 (2)
The method specifically comprises the following steps:
step 1: mixing sodium fluotitanate, aluminum powder and activated carbon powder which meet the proportion requirement, wet grinding, drying the slurry, and dry grinding and activating in inert atmosphere;
step 2: putting the mixed and ground material into a mold, and cold-pressing under the condition of 40-120MPa to obtain a green body;
and step 3: placing the green body in a vacuum reduction furnace for thermal reduction at the temperature of 800-oC, vacuum degree of 10−4-10Pa, reduction time 1-6 hours;
and 4, step 4: after the reduction is finished, controlling the temperature to be 1000-;
and 5: cooling the distilled product to room temperature along with the furnace under the vacuum or argon condition to obtain the porous agglomerate Ti2Peeling AlC crude product, crushing and grinding into powder, sieving the obtained powder, pickling, washing with water and drying to obtain purified Ti2AlC powder.
2. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing AlC ceramic powder is characterized in that in the step 1, the mass ratio of the sodium fluotitanate, the aluminum powder and the activated carbon powder is preferably 1:0.248: 0.029.
3. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing the AlC ceramic powder is characterized in that in the step 1, the wet grinding time of the material is 2-8 hours, the optimal time is 4 hours, and the dry grinding time is 4-12 hours, the optimal time is 8 hours.
4. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing the AlC ceramic powder is characterized in that in the step 2, a green body is obtained by cold pressing under the condition of 50 MPa.
5. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing AlC ceramic powder is characterized in that in the step 3, the reduction temperature is 1250 ℃, and the vacuum degree is 10−3Pa, reduction time 3 hours.
6. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing AlC ceramic powder is characterized in that in the step 4, vacuum distillation is carried out at the temperature of 1200 ℃, and the distillation time is 5 hours.
7. Thermite reduction process for preparing Ti as claimed in claim 12The method for preparing AlC ceramic powder is characterized by also comprising the step 6 of grinding the distillation product into powder, adding aluminum scraps or aluminum-titanium intermediate alloy scraps, placing the powder in a reduction furnace, preserving heat for 1-5 hours at the temperature of 850-; after cooling, the upper layer product is a white cryolite component, can be used as a solvent for the aluminum electrolysis industry after being ground, and the lower layer product is an aluminum-titanium intermediate alloy; in the secondary thermal reduction process of the distillation product, the mixture ratio of the raw materials is controlled, and the distillation product is aluminum scrap or aluminum-titanium intermediate alloy scrap =1 (0.2-5).
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