CN109336612B - Preparation method of superfine titanium carbonitride powder - Google Patents
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Abstract
The invention discloses a preparation method of superfine titanium carbonitride powder, belonging to the technical field of nano ceramic powder preparation, comprising the following steps: s1, finely grinding titanium dioxide and carbon black in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture; s2, drying the mixture, and granulating to obtain mixed material particles; s3, feeding the mixed material particles into a continuous graphite carbon tube furnace for carbonitriding treatment, and controlling reaction temperature and reaction atmosphere to obtain a titanium carbonitride crude product; and S4, removing free carbon and impurities from the titanium carbonitride crude product to obtain a titanium carbonitride product. The method for preparing the titanium carbonitride has the advantages of low cost, high yield and high product purity.
Description
Technical Field
The invention belongs to the technical field of nano ceramic powder preparation, and particularly relates to a preparation method of ultrafine titanium carbonitride powder.
Background
Titanium carbide is a steel gray crystal with metallic luster, the crystal structure belongs to a typical NaCl structure, and the lattice constant a =0.4320 nm. The density of the titanium carbide at 20 ℃ is 4.91g/cm3, the melting point is 3150 +/-10 ℃, the boiling point is 4300 ℃, the Mohs hardness is 9.5, and the hardness is second only to diamond. The titanium carbide has good heat transfer performance and electric conductivity, and the electric conductivity is reduced along with the increase of temperature, which shows that the titanium carbide has the property of metal. Titanium carbide also has excellent oxidation resistance, chemical stability and thermal stability, and can be widely applied to the electronic, chemical and microelectronic industries.
Titanium carbonitride is a single compound formed by continuous solid solution of titanium carbide and titanium nitride, the crystal structure of titanium carbonitride is similar to that of titanium carbide, and part of C atoms in titanium carbide are replaced by N atoms. The lattice constant of titanium carbonitride is intermediate between that of titanium carbide and titanium nitride, and as the C content decreases, the lattice constant decreases accordingly. The C atoms in titanium carbide can be replaced by N atoms in any proportion, forming the continuous solid solution ti (clxny), (0< x <1, 0< y <1), the properties change with x, the hardness of the material decreases with increasing x and the toughness improves. Titanium carbonitride is a non-oxide ceramic material with excellent performance as a continuous solid solution of titanium carbide and titanium nitride, and has the characteristics of high melting point, high hardness, corrosion resistance and good oxidation resistance, so the titanium carbonitride is widely applied to the fields of mechanical chemistry, automobile manufacturing, aerospace and the like. The titanium carbonitride-based hard alloy cutter has high strength, high hardness, good oxidation resistance and good heat conduction performance, so that the adopted titanium carbonitride-based hard alloy cutter has better wear resistance, size precision and surface quality of a processed workpiece than the workpiece processed by the WC or TiC-based hard alloy cutter.
The preparation method of the titanium carbonitride comprises the following steps: high-temperature diffusion of titanium carbide and titanium nitride, high-temperature nitridation, self-propagating high-temperature synthesis, ammonolysis and mechanical alloying. Some of the above methods for preparing titanium carbonitride have the disadvantages of high production cost, low product yield and low product purity, and the realization of industrial large-scale production has certain difficulty.
Disclosure of Invention
In order to solve the defects of high production cost, low product yield and low product purity in the prior art, the invention provides a preparation method of ultrafine titanium carbonitride powder.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of superfine titanium carbonitride powder is characterized by comprising the following steps: the method comprises the following steps:
s1, finely grinding titanium dioxide and carbon black in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture;
s2, drying the mixture, and granulating to obtain mixed material particles;
s3, feeding the mixed material particles into a continuous graphite carbon tube furnace for carbonitriding treatment, and controlling reaction temperature and reaction atmosphere to obtain a titanium carbonitride crude product;
and S4, removing free carbon and impurities from the titanium carbonitride crude product to obtain a titanium carbonitride product.
Preferably, in the step S1, the adding amount of the paraffin is 2% to 6% of the total weight of the titanium dioxide and the carbon black, the filling coefficient during ball milling is 50%, the solid-liquid ratio is 1:1, and the ball-to-material ratio is 3: 1.
Preferably, in the step S1, the mass ratio of the carbon black to the titanium dioxide is 1: 2-4.
Preferably, in the step S2, the particle size of the mixture particles is 0.5 to 1.0 mm.
Preferably, in the step S3, the temperature is controlled to be 1500-1600 ℃ per belt, 1400-1500 ℃ per belt, 1300-1400 ℃ per belt, and the carbonization boat pushing speed is controlled to be 15-25 min per boat; and controlling the carbonization atmosphere to be a nitrogen atmosphere, introducing nitrogen into the furnace tail of the carbon tube furnace, and controlling the flow of the nitrogen to be 300-600 mL/h.
Preferably, in the step S4, the crude titanium carbonitride product is subjected to air classification to remove free carbon therein, and then is sieved by ultrasonic vibration to remove impurities therein, thereby obtaining the titanium carbonitride product.
The invention has the beneficial effects that:
(1) according to the invention, titanium dioxide and carbon black are used as raw materials, a titanium carbonitride crude product is obtained through mixing, granulating and carbonitriding, and superfine titanium carbonitride powder can be obtained through airflow classification, ultrasonic vibration screening treatment and impurity removal, wherein the price of titanium dioxide and carbon black is low, so that the cost is effectively reduced;
(2) the invention adopts three-belt heating to carry out carbonitriding treatment, the reaction temperature gradient can be effectively and real-timely adjusted through the heating mode, the reaction atmosphere in the furnace can be effectively adjusted through the mode of introducing nitrogen to the furnace tail, and the reaction time is controlled through adjusting the boat pushing speed, thereby accurately controlling the C/N and the granularity of the titanium carbonitride product, improving the product purity and highly concentrating the granularity of the product;
(3) according to the invention, the impurities are removed by air classification and ultrasonic vibration screening, so that free carbon and impurities can be effectively removed, the loss of titanium carbonitride is avoided, and the product yield is improved;
(4) the invention has the comprehensive effect of the optimized measures, continuous production, high yield, timely and dynamic adjustment of the process adjustment, and random inspection of the product quality during the production process, and not only can obtain the superfine titanium carbonitride powder with stable C/N and granularity, the granularity reaches below 500nm, but also the recovery rate of titanium reaches more than 90 percent.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. All other embodiments that can be obtained by a person skilled in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
Example one
A preparation method of superfine titanium carbonitride powder comprises the following steps:
s1: firstly, blending carbon black and titanium dioxide according to the weight ratio of 1:2, wherein the titanium dioxide is anatase titanium dioxide, the purity of the titanium dioxide is 99%, the C content in the carbon black is 98.5%, then feeding the blended raw materials into a ball mill, fully ball-milling in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture, the paraffin is added according to the total weight of the carbon black and the titanium dioxide of 3%, the filling coefficient is 50%, the solid-liquid ratio is 1:1, and the ball-material ratio is 3: 1;
s2: drying the mixture, and then granulating through a granulator to obtain mixed granules, wherein the granularity of the mixed granules is controlled to be 0.5-1.0 mm;
s3: loading the mixed material particles into a boat, and sending the boat into a carbonization furnace for carbonization treatment to obtain a titanium carbonitride crude product, wherein the carbonization treatment conditions are that the temperature is controlled to 1600 ℃ in one zone, 1480 ℃ in the second zone, 1380 ℃ in the third zone, the boat pushing speed is 25 min/boat, the carbonization atmosphere is controlled to be nitrogen atmosphere, nitrogen is introduced into the tail of a carbon tube furnace, and the nitrogen flow is 300 ml/h;
s4: and (3) feeding the titanium carbonitride crude product into an airflow classifier for crushing and grading, performing ultrasonic vibration screening on the graded material, wherein the screening aperture is 200 meshes, and removing free carbon and impurities through airflow classification and ultrasonic vibration screening to obtain a superfine titanium carbonitride product, wherein the granularity of the titanium carbonitride is 0.4 +/-0.05 mu m.
Example two
A preparation method of superfine titanium carbonitride powder comprises the following steps:
s1: firstly, blending carbon black and titanium dioxide according to the weight ratio of 1:3, wherein the titanium dioxide is anatase titanium dioxide, the purity of the titanium dioxide is 99%, the C content in the carbon black is 98.5%, then feeding the blended raw materials into a ball mill, fully ball-milling in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture, the paraffin is added according to the weight ratio of 3% of the total weight of the carbon black and the titanium dioxide, the filling coefficient is 50%, the solid-liquid ratio is 1:1, and the ball-material ratio is 3: 1;
s2: drying the mixture, and then granulating through a granulator to obtain mixed granules, wherein the granularity of the mixed granules is controlled to be 0.5-1.0 mm;
s3: loading the mixed material particles into a boat, sending the boat into a carbonization furnace for carbonization treatment to obtain a titanium carbonitride crude product, controlling the carbonization treatment temperature to be 1580 ℃ in one band, 1450 ℃ in the second band, 1350 ℃ in the third band, pushing the boat at a speed of 15 min/boat, controlling the carbonization atmosphere to be a nitrogen atmosphere, and introducing nitrogen into the furnace tail of a carbon tube furnace at a nitrogen flow rate of 500 ml/h;
s4: and (3) feeding the titanium carbonitride crude product into an airflow classifier for crushing and classifying, and performing ultrasonic vibration screening on the classified material, wherein the screening aperture is 325 meshes. Removing free carbon and impurities by air classification and ultrasonic vibration sieving to obtain the superfine titanium carbonitride product, wherein the granularity of the titanium carbonitride is 0.2 +/-0.05 mu m.
EXAMPLE III
A preparation method of superfine titanium carbonitride powder comprises the following steps:
s1: firstly, blending carbon black and titanium dioxide according to the weight ratio of 1:4, wherein the titanium dioxide is anatase titanium dioxide, the purity of the titanium dioxide is 99%, the C content in the carbon black is 98.5%, then feeding the blended raw materials into a ball mill, fully ball-milling in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture, the paraffin is added according to the total weight of the carbon black and the titanium dioxide of 3%, the filling coefficient is 50%, the solid-liquid ratio is 1:1, and the ball-material ratio is 3: 1;
s2: drying the mixture, and then granulating through a granulator to obtain mixed granules, wherein the granularity of the mixed granules is controlled to be 0.5-1.0 mm;
s3: loading the mixed material particles into a boat, and sending the boat into a carbonization furnace for carbonization treatment to obtain a titanium carbonitride crude product, wherein the carbonization treatment conditions are that the temperature is controlled to be 1500 ℃ in one zone, 1400 ℃ in the second zone, 1300 ℃ in the third zone, the boat pushing speed is 20 min/boat, the carbonization atmosphere is controlled to be nitrogen atmosphere, nitrogen is introduced into the furnace tail of a carbon tube furnace, and the nitrogen flow is 600 ml/h;
s4: and (3) feeding the titanium carbonitride crude product into an airflow classifier for crushing and classifying, performing ultrasonic vibration screening on the classified material, wherein the screening aperture is 200 meshes, and removing free carbon and impurities through airflow classification and ultrasonic vibration screening to obtain the superfine titanium carbonitride product. The titanium carbonitride particle size is 0.4 +/-0.05 mu m.
Examples of the experiments
S1: firstly, 10kg of carbon black and 40kg of titanium dioxide are mixed, the titanium dioxide is anatase titanium dioxide, the purity of the titanium dioxide is 99%, the C content in the carbon black is 98.5%, then the mixed raw materials are fed into a ball mill, and are fully ball-milled and uniformly mixed in 50kg of absolute ethyl alcohol added with 1.5kg of paraffin wax to obtain a mixture, the filling coefficient is 50%, and the ball-to-material ratio is 3: 1;
s2: drying the mixture, and then granulating through a granulator to obtain mixed granules, wherein the granularity of the mixed granules is controlled to be 0.5-1.0 mm;
s3: loading the mixed material particles into a boat, and sending the boat into a carbonization furnace for carbonization treatment to obtain a titanium carbonitride crude product, wherein the carbonization treatment conditions are that the temperature is controlled to be 1500 ℃ in one zone, 1400 ℃ in the second zone, 1300 ℃ in the third zone, the boat pushing speed is 20 min/boat, the carbonization atmosphere is controlled to be nitrogen atmosphere, nitrogen is introduced into the furnace tail of a carbon tube furnace, and the nitrogen flow is 600 mL/h;
s4: and (3) feeding the titanium carbonitride crude product into an airflow classifier for crushing and classifying, performing ultrasonic vibration screening on the classified material, wherein the screening aperture is 200 meshes, and removing free carbon and impurities through airflow classification and ultrasonic vibration screening to obtain the superfine titanium carbonitride product.
Through detection, 25kg of the obtained superfine titanium carbide product is obtained, the yield is 50%, the granularity of the obtained superfine titanium carbide product is 350-450 nm, and the product purity is 99.1%.
Claims (4)
1. A preparation method of superfine titanium carbonitride powder is characterized by comprising the following steps: the method comprises the following steps:
s1, finely grinding titanium dioxide and carbon black in absolute ethyl alcohol added with paraffin and uniformly mixing to obtain a mixture;
s2, drying the mixture, and granulating to obtain mixed material particles;
s3, sending the mixed material particles into a continuous graphite carbon tube furnace for carbonitriding treatment, and controlling reaction temperature and reaction atmosphere to obtain a titanium carbonitride crude product, wherein the specific contents are as follows: the temperature is controlled to be 1500-1600 ℃ per belt, 1400-1500 ℃ per belt, 1300-1400 ℃ per belt, and the carbonization boat pushing speed is controlled to be 15-25 min per boat; controlling the carbonization atmosphere to be a nitrogen atmosphere, introducing nitrogen into the furnace tail of the carbon tube furnace, and controlling the flow of the nitrogen to be 300-600 mL/h;
s4, removing free carbon and impurities from the titanium carbonitride crude product to obtain a titanium carbonitride product, which specifically comprises the following steps: and (3) carrying out air flow classification on the titanium carbonitride crude product to remove free carbon in the titanium carbonitride crude product, and then removing impurities in the titanium carbonitride crude product through ultrasonic vibration screening to obtain the titanium carbonitride product.
2. The method for preparing ultrafine titanium carbonitride powder according to claim 1, characterized in that: in the step S1, the adding amount of the paraffin is 2-6% of the total weight of the titanium dioxide and the carbon black, the filling coefficient during ball milling is 50%, the solid-liquid ratio is 1:1, and the ball-material ratio is 3: 1.
3. The method for preparing ultrafine titanium carbonitride powder according to claim 1, characterized in that: in the step S1, the mass ratio of the carbon black to the titanium dioxide is 1: 2-4.
4. The method for preparing ultrafine titanium carbonitride powder according to claim 1, characterized in that: in the step S2, the granularity of the mixed material particles is 0.5-1.0 mm.
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| CN109852871B (en) * | 2019-01-31 | 2021-02-05 | 株洲华斯盛高科材料有限公司 | Nitrogen-containing steel bonded hard alloy prepared from titanium nitride carbide |
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| CN112357896B (en) * | 2020-11-23 | 2022-05-27 | 株洲昊坤硬质材料有限公司 | Preparation method of superfine titanium carbonitride |
| CN115385697B (en) * | 2022-08-24 | 2023-06-23 | 湖南昊坤硬质新材料有限公司 | Production process of high-nitrogen titanium carbide nitride |
| CN116477626B (en) * | 2023-03-22 | 2024-09-24 | 常熟市电力耐磨合金铸造有限公司 | Superfine TiC powder with low oxygen content and preparation method thereof |
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Denomination of invention: A preparation method of ultrafine titanium carbonitride powder Effective date of registration: 20220630 Granted publication date: 20210507 Pledgee: Huishang Bank Co.,Ltd. Chengdu Jinsha sub branch Pledgor: CHENGDU MET-CERAMICS ADVANCED MATERIALS Co.,Ltd. Registration number: Y2022510000179 |