CN114275793A - TiB2Powder preparation method - Google Patents
TiB2Powder preparation method Download PDFInfo
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- CN114275793A CN114275793A CN202111573794.7A CN202111573794A CN114275793A CN 114275793 A CN114275793 A CN 114275793A CN 202111573794 A CN202111573794 A CN 202111573794A CN 114275793 A CN114275793 A CN 114275793A
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Abstract
The application discloses a TiB2The powder preparation method comprises the following steps: preparing a boric acid mixed solution; preparing an organic titanium mixed solution; preparing boron-titanium mixed sol; preparing boron-titanium mixed gel; preparation of TiB2A precursor; preparation of TiB2And (3) powder. The application adopts a vacuum microwave oven to synthesize TiB2The powder has the advantages of low synthesis temperature, short synthesis time, high energy utilization rate, high heating efficiency, easy operation, no pollution and mild synthesis conditions.
Description
Technical Field
The application relates to the technical field of powder preparation, in particular to a TiB2A powder preparation method.
Background
Titanium diboride (TiB)2) The high-temperature-resistant high-strength alloy has the advantages of high melting point, high elasticity modulus, high hardness, high electrical conductivity, high thermal conductivity, low thermal expansion coefficient, good wear resistance, corrosion resistance, chemical stability and the like, is a high-potential ceramic material, and can be added into an alloy as reinforcing particles to form a composite material to improve the performance of the alloy. TiB2Whether used in the field of ceramic materials or composite materials, the microstructure of the materials andall the mechanical properties are affected by TiB2Influence of powder characteristics, thus on TiB2The activity, purity and grain diameter of the powder put forward higher requirements, and TiB with high activity, high purity and small grain diameter needs to be prepared2And (3) powder.
There are many synthetic TiB2The methods of (1) such as gas phase reaction method, electric heating, chemical vapor deposition, combustion synthesis method, etc., but these processes all require higher temperature or longer production period, and the synthesized powder usually has coarser particles and lower purity, and the powder is easy to agglomerate, which is not beneficial to improving the performance of the material.
Therefore, how to provide a TiB2The synthesis method can prepare TiB with high purity and small grain diameter2Powder, is a problem to be solved by those skilled in the art.
Disclosure of Invention
To solve the above technical problems, a first object of the present invention is to provide a TiB2A powder preparation method; the application adopts a vacuum microwave oven to synthesize TiB2The powder has the advantages of low synthesis temperature, short synthesis time, high energy utilization rate, high heating efficiency, easy operation, no pollution and mild synthesis conditions.
The technical scheme provided by the invention is as follows:
TiB2The powder preparation method comprises the following steps:
preparing a boric acid mixed solution: according to the molar ratio of boron to titanium of boric acid to butyl titanate (3.5-4.5) to 1, taking boric acid, according to the molar ratio of carbon to titanium of sucrose to butyl titanate (5-7) to 1, taking sucrose, and uniformly mixing boric acid, sucrose and ethanol to obtain a solution A;
preparing an organic titanium mixed solution: taking the butyl titanate according to the boron-titanium molar ratio of the boric acid to the butyl titanate; taking acetylacetone according to the mass ratio of the butyl titanate to the acetylacetone of (2.0-3.0) 1, and mixing the butyl titanate and the acetylacetone to form an organic titanium mixed solution, namely a solution B;
preparing boron-titanium mixed sol: mixing the solution A and the solution B to obtain boron-titanium mixed sol;
preparing boron-titanium mixed gel: carrying out heat treatment on the boron-titanium mixed sol at the temperature of 60-80 ℃ to obtain boron-titanium mixed gel;
preparation of TiB2Precursor: freeze-drying the boron-titanium mixed gel for 12-18h, and mechanically grinding to obtain TiB2A precursor;
preparation of TiB2Powder: mixing TiB2Heating the precursor to 650-700 ℃ in an inert atmosphere, preserving heat for 1-1.5h, continuing heating to 980-1050 ℃, preserving heat for 1-2h, and then cooling to room temperature along with the furnace to obtain TiB2And (3) powder.
Preferably, when preparing the boric acid mixed solution, mixing boric acid and sucrose to obtain a mixture, and adding ethanol into the mixture to prepare a mixed solution with the boric acid concentration of 3-8mol/L, namely the solution A.
Preferably, after adding ethanol, heating to 40-50 ℃, stirring, and preparing a mixed solution.
Preferably, acetylacetone is slowly added to the butyl titanate while stirring to form an organic titanium mixed solution.
Preferably, when preparing the boron-titanium mixed sol, the solution A is placed in an ultrasonic stirrer, the solution B is slowly poured into the ultrasonic stirrer, and the solution B is stirred for 1 to 1.5 hours to obtain the boron-titanium mixed sol.
Preferably, when preparing the boron-titanium mixed gel, the boron-titanium mixed sol is placed in an oven and is kept at the temperature of 60-80 ℃ for 2-3 h.
Preferably, TiB is prepared2And (3) placing the boron-titanium mixed gel into a vacuum freeze drying oven for freeze drying for 12-18h at-60 ℃ to-80 ℃.
Preferably, ball milling is carried out after freeze drying, the ball milling time is 24-36h, the ball milling speed is 800-.
Preferably, TiB is prepared2When in powder form, TiB is added2Placing the precursor in a vacuum microwave oven, filling argon, heating to 650-700 ℃, preserving heat for 1-1.5h, continuing heating to 980-1050 ℃, preserving heat for 1-2h, then cooling to room temperature along with the oven, then stopping filling argon, opening an oven door to obtain TiB2And (3) powder.
Preferably, the oxygen content in the furnace is kept between 180 and 220PPm after argon is filled.
The present application provides a TiB2The powder preparation method adopts a sol-gel microwave synthesis method, utilizes sucrose as a complexing agent to complex with boric acid to form a boric acid complex, and can improve the solubility of the boric acid; acetylacetone as a stabilizer to inhibit rapid hydrolysis of butyl titanate, prevent precipitation of metal oxides, form Ti (acac)2A chelate; ti (acac)2Mixing the chelate with boric acid complex to obtain sol, heat-treating the sol to obtain gel, drying the gel to form precursor, and preparing TiB under carbothermic reduction reaction2And (3) nano powder. The preparation method provided by the application and the prepared TiB2The nano powder particles reach the nano level, are in dispersion distribution and uniform dispersion, and the purity reaches more than 98%. Compared with other synthesis methods, the method for synthesizing the TiB by using the vacuum microwave oven2The powder has the advantages of low synthesis temperature, short synthesis time, high energy utilization rate, high heating efficiency, easy operation, no pollution and mild synthesis conditions.
In this application, the carbon-to-titanium molar ratio of sucrose to butyl titanate is calculated as the ratio of the number of moles of sucrose multiplied by 12 (since there are 12 carbon atoms in one molecule of sucrose) to the number of moles of butyl titanate.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a TiB prepared in example 1 of the present invention2A shape graph of the nano powder;
FIG. 2 shows TiB prepared in example 1 of the present invention2XRD pattern of nano powder;
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or be indirectly disposed on the other element; when an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, refer to an orientation or positional relationship illustrated in the drawings for convenience in describing the present application and to simplify description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present application.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, the meaning of a plurality of or a plurality of is two or more unless specifically limited otherwise.
It should be understood that the structures, ratios, sizes, and the like shown in the drawings are only used for matching the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the practical limit conditions of the present application, so that the modifications of the structures, the changes of the ratio relationships, or the adjustment of the sizes, do not have the technical essence, and the modifications, the changes of the ratio relationships, or the adjustment of the sizes, are all within the scope of the technical contents disclosed in the present application without affecting the efficacy and the achievable purpose of the present application.
Example 1
(1) Preparing a boric acid mixed solution: according to H3BO3(boric acid) and Ti (OC)4H9)4(Butyltitanate) 2.472g H was weighed at a boron-titanium molar ratio of 4:13BO3Press a C12H22O11The molar ratio of carbon to titanium of (sucrose) to butyl titanate is 6:1, and the ratio is 1.71g C12H22O11Is prepared from H3BO3And C12H22O11Mixing to obtain a mixture, adding 10ml of C2H5OH (ethanol), heating to 70 ℃, stirring until the mixture is completely dissolved to obtain a mixed solution with boric acid concentration of 4mol/L, namely solution A;
(2) preparing an organic titanium mixed solution: according to H3BO3With Ti (OC)4H9)4With a boron-titanium molar ratio of 4:1 3.399g of Ti (OC) were weighed4H9)4(ii) a Weighing 1.4g C5H8O2(acetylacetone) reaction of C5H8O2Slowly added to the stirring Ti (OC)4H9)4Forming an organic titanium mixed solution, namely a solution B;
(3) preparing boron-titanium mixed sol: placing the solution A in an ultrasonic stirrer, slowly pouring the solution B, and stirring for 1h to obtain boron-titanium mixed sol;
(4) preparing boron-titanium mixed gel: placing the boron-titanium mixed sol in a drying oven, and keeping the temperature at 80 ℃ for 2h to obtain boron-titanium mixed gel;
(5) preparation of TiB2Precursor: drying the boron-titanium mixed gel in a vacuum freeze drying oven at-60 ℃ for 12h, then putting the dried boron-titanium mixed gel into a centrifugal ball mill for ball milling, wherein the ball milling time is 24h, the ball milling speed is 800r/min, the cooling is suspended for 15min every 30min in the ball milling process, and the ball milled gel is sieved by a 100-mesh sieve to obtain TiB2Precursor powder;
(6) preparation of TiB2Powder: mixing TiB2Putting the precursor into a vacuum microwave oven, filling argon to keep the oxygen content in the oven at 200PPm, heating to 650 ℃, keeping the temperature for 1h, continuing heating to 980 ℃, keeping the temperature for 2h, then cooling to room temperature along with the oven, stopping filling argon, and opening an oven door to obtain TiB2And (3) nano powder.
Prepared TiB2The morphology of the nanopowder is shown in FIG. 1. The XRD pattern of the powder is shown in FIG. 2.
Example 2
(1) Preparing a boric acid mixed solution: according to H3BO3With Ti (OC)4H9)4The boron-titanium molar ratio of (B)/(B) was 3.5:1 and 2.163g H was weighed3BO3Press a C12H22O11With Ti (OC)4H9)4The molar ratio of carbon to titanium of (1) is 1.42g C12H22O11Is prepared from H3BO3And C12H22O11Mixing to obtain a mixture, adding 10ml of C2H5OH, heating to 70 ℃, stirring until the mixture is completely dissolved to obtain a mixed solution with boric acid concentration of 4mol/L, namely solution A;
(2) preparing an organic titanium mixed solution: according to H3BO3With Ti (OC)4H9)4With a boron-titanium molar ratio of 4:1 3.399g of Ti (OC) were weighed4H9)4(ii) a Weighing 1.36g C5H8O2Mixing C with5H8O2Slowly added to the stirring Ti (OC)4H9)4Forming an organic titanium mixed solution, namely a solution B;
(3) preparing boron-titanium mixed sol: placing the solution A in an ultrasonic stirrer, slowly pouring the solution B, and stirring for 1h to obtain boron-titanium mixed sol;
(4) preparing boron-titanium mixed gel: placing the boron-titanium mixed sol in a drying oven, and keeping the temperature at 80 ℃ for 2h to obtain boron-titanium mixed gel;
(5) preparation of TiB2Precursor: putting the boron-titanium mixed gel into a vacuum freeze drying oven to be dried at-60 ℃ 12h, drying, ball-milling in a centrifugal ball mill for 24h at a ball-milling speed of 800r/min, cooling for 15min when 30min is performed in the ball-milling process, and sieving with a 100-mesh sieve to obtain TiB2Precursor powder
(6)TiB2Powder synthesis: mixing TiB2Putting the precursor into a vacuum microwave oven, filling argon to keep the oxygen content in the oven at 200PPm, heating to 700 ℃, keeping the temperature for 1h, continuing heating to 1050 ℃, keeping the temperature for 2h, then cooling to room temperature along with the oven, stopping filling argon, and opening the oven door to obtain TiB2And (3) nano powder.
Comparative example 1
(1) Preparing a boric acid mixed solution: according to H3BO3With Ti (OC)4H9)4The boron-titanium molar ratio of 1.5458g H is weighed in a ratio of 2.5:13BO3Press a C6H14O6(sorbitol) with Ti (OC)4H9)4The molar ratio of carbon to titanium of (1) is 5:1 to 1.51g C6H14O6Is prepared from H3BO3And C6H14O6Mixing to obtain a mixture, adding 10ml of C2H5OH, heating to 70 ℃, stirring until the mixture is completely dissolved to obtain a mixed solution with the boric acid concentration of 2.5mol/L, namely solution A;
(2) preparing an organic titanium mixed solution: according to H3BO3With Ti (OC)4H9)4With a boron-titanium molar ratio of 2.5:1 3.403g of Ti (OC) were weighed out4H9)4(ii) a Weighing 1g C5H8O2Mixing C with5H8O2Slowly added to the stirring Ti (OC)4H9)4Forming an organic titanium mixed solution, namely a solution B;
(3) preparing boron-titanium mixed sol: placing the solution A in an ultrasonic stirrer, slowly pouring the solution B, and stirring for 1h to obtain boron-titanium mixed sol;
(4) preparing boron-titanium mixed gel: placing the boron-titanium mixed sol in a drying oven, and keeping the temperature at 70 ℃ for 7h to obtain boron-titanium mixed gel;
(5) system for makingPreparation of TiB2Precursor: drying the gel in an oven at 85 deg.C for 8h, heating the oven to 120 deg.C for 5h, grinding the dried gel, and sieving with 80 mesh sieve to obtain TiB2Precursor powder
(6) Preparation of TiB2Powder: mixing TiB2Putting the precursor into an atmosphere furnace, calcining at high temperature under the protection of argon, wherein the flow of the argon is 70ml/min, the heating system is to heat up from room temperature to the synthesis temperature (1500 ℃) at the speed of 4 ℃/min, preserving the heat at the synthesis temperature for 1.5h, then cooling to room temperature along with the furnace, stopping introducing the argon to obtain black powder, grinding the powder, sieving by a 100-mesh sieve to finally obtain TiB2And (3) nano powder.
TiB prepared for examples 1-2 and comparative example 12The nanopowder was tested as shown in the following table:
| purity of | Yield of powder | Whether or not to agglomerate | |
| Example 1 | 98.3％ | 85％ | Without agglomeration |
| Example 2 | 98.6％ | 83％ | Without agglomeration |
| Comparative example | 96.9％ | 67％ | With agglomeration |
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. TiB2The powder preparation method is characterized by comprising the following steps:
preparing a boric acid mixed solution: according to the molar ratio of boron to titanium of boric acid to butyl titanate (3.5-4.5) to 1, taking boric acid, according to the molar ratio of carbon to titanium of sucrose to butyl titanate (5-7) to 1, taking sucrose, and uniformly mixing boric acid, sucrose and ethanol to obtain a solution A;
preparing an organic titanium mixed solution: taking the butyl titanate according to the boron-titanium molar ratio of the boric acid to the butyl titanate; taking acetylacetone according to the mass ratio of the butyl titanate to the acetylacetone of (2.0-3.0) 1, and mixing the butyl titanate and the acetylacetone to form an organic titanium mixed solution, namely a solution B;
preparing boron-titanium mixed sol: mixing the solution A and the solution B to obtain boron-titanium mixed sol;
preparing boron-titanium mixed gel: carrying out heat treatment on the boron-titanium mixed sol at the temperature of 60-80 ℃ to obtain boron-titanium mixed gel;
preparation of TiB2Precursor: freeze-drying the boron-titanium mixed gel for 12-18h, and mechanically grinding to obtain TiB2A precursor;
preparation of TiB2Powder: mixing TiB2Heating the precursor to 650-700 ℃ in an inert atmosphere, preserving heat for 1-1.5h, continuing heating to 980-1050 ℃, preserving heat for 1-2h, and then cooling to room temperature along with the furnace to obtain TiB2And (3) powder.
2. The TiB of claim 12The powder preparation method is characterized in that when a boric acid mixed solution is prepared, boric acid and cane sugar are mixed to obtain a mixture, ethanol is added into the mixture to prepare a mixed solution with the boric acid concentration of 3-8mol/L, namely the solution A.
3. The TiB of claim 22The powder preparation method is characterized in that after ethanol is added, the mixture is heated to 40-50 ℃ and stirred to prepare a mixed solution.
4. The TiB of claim 12The powder preparation method is characterized in that acetylacetone is slowly added into butyl titanate which is being stirred to form an organic titanium mixed solution.
5. The TiB of claim 12The powder preparation method is characterized in that when preparing the boron-titanium mixed sol, the solution A is placed in an ultrasonic stirrer, the solution B is slowly poured in, and the stirring is carried out for 1-1.5h, so as to obtain the boron-titanium mixed sol.
6. The TiB of claim 12The preparation method of the powder is characterized in that when preparing the boron-titanium mixed gel, the boron-titanium mixed sol is placed in a drying oven, and the heat preservation is carried out for 2-3h at the temperature of 60-80 ℃.
7. The TiB of claim 12The powder preparation method is characterized in that TiB is prepared2And (3) placing the boron-titanium mixed gel into a vacuum freeze drying oven for freeze drying for 12-18h at-60 ℃ to-80 ℃.
8. TiB of any one of claims 1 or 72A method for preparing powder, which comprises the following steps,the method is characterized in that ball milling is carried out after freeze drying, the ball milling time is 24-36h, the ball milling speed is 800-1200r/min, cooling is suspended for 10-15min every 25-30min in the ball milling process, and the ball is sieved by a 125-mesh sieve with 100 meshes after the ball milling is finished.
9. The TiB of claim 12The powder preparation method is characterized in that TiB is prepared2When in powder form, TiB is added2Placing the precursor in a vacuum microwave oven, filling argon, heating to 650-700 ℃, preserving heat for 1-1.5h, continuing heating to 980-1050 ℃, preserving heat for 1-2h, then cooling to room temperature along with the oven, then stopping filling argon, opening an oven door to obtain TiB2And (3) powder.
10. The TiB of claim 92The powder preparation method is characterized in that the oxygen content in the furnace is kept at 180-220 PPm after argon is filled.
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Cited By (1)
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| CN114751752A (en) * | 2022-05-27 | 2022-07-15 | 中国科学院合肥物质科学研究院 | High-purity TiB2Ceramic nanosheet and preparation method thereof |
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