CN114985727A - In-situ synthesis enhanced additive composite powder, preparation method and application - Google Patents
In-situ synthesis enhanced additive composite powder, preparation method and application Download PDFInfo
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Abstract
The invention discloses an in-situ synthesis enhanced additive composite powder, a preparation method and application thereof 2 Coating the powder with graphene sol, and adding TiO 2 And carrying out vacuum mechanical ball milling and mixing on the @ graphene sol coated powder and the aluminum alloy powder to prepare the in-situ synthesis enhanced additive composite powder for additive manufacturing. When the powder material prepared by the method is applied to laser processing and forming, the graphene and the powder materialTiO 2 Can be closely contacted and fully reacted in the aluminum melt to synthesize Al in situ 2 O 3 And TiC ceramic reinforcement, can improve the laser energy utilization rate of the aluminum alloy powder apparently; the in-situ synthesized reinforcement is more beneficial to improving the comprehensive performance of the composite material, and the preparation process is clean and pollution-free.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, relates to a preparation technology of additive manufacturing powder, and particularly relates to in-situ synthesis enhanced additive composite powder, a preparation method and application.
Background
Light high-strength materials represented by aluminum alloy have great application requirements in the fields of national defense and military industry, aerospace, automobile manufacturing, energy and power and the like. The ceramic reinforced aluminum-based composite material formed based on the method combines the beneficial properties of the ceramic body and the aluminum alloy matrix, and is paid close attention to the technical field of engineering by the characteristics of high specific strength, high specific stiffness, low density, good corrosion resistance, good wear resistance and the like. In the face of the increasingly complex structural design of advanced manufacturing parts, the defects of traditional die forming preparation methods such as casting, extrusion, forging blank making and the like are obvious, such as low degree of freedom, long processing period, separation of preparation and forming processes and the like, and various severe efficiency requirements are difficult to meet, and the production application of the composite material is limited to a certain extent.
The laser additive manufacturing (3D printing) technology can plan a scanning path according to two-dimensional contour information of a three-dimensional model section, and powder or wire materials are melted by high-energy density laser beams and are stacked layer by layer to be solidified into a three-dimensional entity for realizing direct near-net forming of parts with complex structures. For a long time, when the multiphase ceramic reinforced aluminum matrix composite is prepared by a laser additive manufacturing technology, an external reinforced phase method is mainly adopted to directly mechanically mix ceramic particles with aluminum alloy powder, or different types of nano ceramic particles are introduced in a gas atomization powder making process, so that the preparation of the powder for the multiphase ceramic reinforced aluminum matrix composite is realized. The ceramic reinforcement is selected from lattice-matched refractory metal oxides, carbides, borides, nitrides, etc., such as Al 2 O 3 、SiC、B 4 C、ZrH 2 、TiC、TiN、TiB 2 、ZrB 2 A plurality of combinations of (a). However, although the external reinforcing phase method can improve part of performance indexes of the composite material, the wettability between the ectopic reinforcement and the matrix is poor, the interface bonding strength is too low, andthe difference of thermal expansion coefficient and the like inevitably deteriorates other properties of the composite material, so that the post-treatment cost is increased, and the rapid preparation and production of the composite reinforced material are not facilitated.
The common principle of preparing in-situ composite material by laser additive manufacturing in the prior art is that the traditional fusion casting method is combined with atomization powder preparation by means of potassium fluoborate (KBF) 4 ) Or potassium fluorozirconate (K) 2 ZrF 6 ) With potassium fluorotitanate (K) 2 TiF 6 ) Carrying out mixed fluoride salt reaction, TiB 2 Or ZrB 2 The ceramic reinforcement particles are formed in situ in the aluminum melt to prepare a composite casting blank, and the casting blank is further prepared into in-situ composite material powder by a vacuum gas atomization method. Because a series of metallurgical processes such as refining, slagging-off and the like are involved, KBF 4 And K 2 ZrF 6 The fluorine salt is easy to decompose or hydrolyze to form highly toxic substances to pollute the environment, the powder preparation process is time-consuming and labor-consuming and is only limited to synthesize an in-situ ceramic phase. The ceramic reinforcement synthesized in situ by the method is easy to deviate and the size is not easy to control, and is not beneficial to improving the comprehensive performance of the aluminum matrix composite.
Disclosure of Invention
Aiming at the problems that the multi-ceramic reinforcement of the aluminum-based composite material synthesized in situ by laser 3D printing in the prior art can not be prepared simultaneously and refractory borides (TiB and TiB) are difficult to be prepared at the present stage 2 、ZrB 2 ) Or the defects of the preparation method of the carbide (TiC) ceramic reinforced aluminum-based composite material powder, and provides a method for preparing sol-coated composite powder for laser 3D printing in-situ synthesis 2 Coating the powder with graphene sol, and adding TiO 2 And carrying out vacuum mechanical ball milling and mixing on the @ graphene sol coated powder and the aluminum alloy powder to prepare the in-situ synthesized enhanced additive composite powder. When the composite powder material prepared by the method is applied to laser 3D printing processing, graphene and TiO are used 2 Can be closely contacted and fully reacted in the aluminum meltSite-synthesized Al 2 O 3 And a TiC ceramic reinforcement, which not only can remarkably improve the laser energy utilization rate of the aluminum alloy powder; and the in-situ self-generated reinforcement is more beneficial to improving the comprehensive performance of the composite material, and any preparation process is clean and pollution-free.
A preparation method of in-situ synthesized enhanced additive composite powder comprises the following specific steps:
(1) synchronously and slowly dripping a titanium source precursor and a hydrolysis inhibitor into deionized water, adjusting the pH value of the system to 2.5-3.5 by adopting an acid solution under the condition of continuous stirring, and continuously performing hydrolysis reaction to form titanium dioxide sol;
(2) adding single-layer graphene powder into titanium dioxide sol and uniformly dispersing to ensure that the surface of the single-layer graphene powder is uniformly coated with the titanium dioxide sol, and aging at room temperature, drying, grinding and screening to obtain TiO 2 @ graphene sol-coated powder;
(3) mixing TiO with 2 The in-situ synthesis enhanced additive composite powder for additive manufacturing is obtained by carrying out ball-milling mixing treatment on the @ graphene sol coated powder and aluminum alloy powder.
Preferably, in the step (1), the titanium source precursor is titanate.
Further preferably, the titanate is selected from one or more of ethyl titanate, propyl titanate and butyl titanate.
Preferably, in the step (1), the hydrolysis inhibitor is a mixed solution of absolute ethyl alcohol and glacial acetic acid, and the glacial acetic acid accounts for 15-25% of the total volume of the mixed solution.
Preferably, in the step (1), the volume ratio of the titanium source precursor to the deionized water to the hydrolysis inhibitor is 1:2: 3.8-1: 2: 4.2.
Preferably, in the step (1), the acid solution is a dilute nitric acid solution, and the hydrolysis duration is 7-10 h.
Preferably, in the step (2), the single-layer graphene powder is lamellar powder, the diameter of each layer is 1-5 μm, and the thickness of each layer is 0.8-1.2 nm.
Preferably, in the step (2), TiO2@ graphene sol is coated on TiO in the powder 2 The mass ratio to graphene was 20: 3.
Preferably, in the step (2), the room-temperature aging time is 1-3 d.
Preferably, in the step (2), the drying temperature is 60-80 ℃, and the drying time is 4-8 h.
Preferably, in the step (2), the grinding process is performed in a small planetary high-throughput ball mill, the grinding medium is stainless steel grinding balls, the size ratio of phi 3 to phi 5 to phi 10 is 2 to 1, the ball-to-material ratio is 5 to 1-8 to 1, the fixed rotation speed in a vacuum environment is 300-450 rpm, the ball milling is paused for 5min for 30min each time, and the total grinding time is 4-5 h.
Preferably, in step (2), the sieving treatment preferably has a plate diameter of not more than 7 μm and no significant agglomeration of TiO 2 @ graphene sol-coated powder.
Preferably, in the step (3), the aluminum alloy powder is spherical powder, and the particle size is 5-165 μm.
Preferably, in the step (3), TiO in the reinforced additive composite powder is synthesized in situ 2 The mass fraction of the @ graphene powder is 1-6%.
Preferably, in the step (3), the particle size of the aluminum alloy powder used for the laser melting 3D printing process is 5-75 μm; the particle size of the aluminum alloy powder used in the laser near-net-shape 3D printing process is 75-165 micrometers.
Further preferably, the aluminum alloy powder is AlSi7Mg alloy powder, AlSi10Mg alloy powder and Al-12Si alloy powder, or other aluminum alloy powder suitable for laser additive manufacturing techniques.
More preferably, the AlSi7Mg alloy powder comprises, by mass, 6.5-7.5% of Si, 0.25-0.45% of Mg, less than or equal to 0.4% of Fe, less than or equal to 0.3% of Mn, less than or equal to 0.25% of Cu, less than or equal to 0.2% of Ti, less than or equal to 0.25% of Zn, less than or equal to 0.01% of Sn, and the balance of Al.
More preferably, the AlSi10Mg alloy powder comprises, by mass, 9.5-10.5% of Si, 0.15-0.45% of Mg, less than or equal to 0.45% of Fe, less than or equal to 0.4% of Mn, less than or equal to 0.05% of Cu, less than or equal to 0.1% of Ti, less than or equal to 0.1% of Zn, less than or equal to 0.05% of Sn, and the balance of Al.
More preferably, the Al-12Si alloy powder comprises, by mass, 10.5-13.5% of Si, less than or equal to 0.1% of Mg, less than or equal to 0.65% of Fe, less than or equal to 0.5% of Mn, less than or equal to 0.05% of Cu, less than or equal to 0.15% of Ti, less than or equal to 0.15% of Zn, less than or equal to 0.05% of Sn, and the balance of Al.
Preferably, in the mechanical ball milling and mixing process in the step (3), the ball milling medium is stainless steel balls, the size ratio of phi 5 to phi 10 is 2:1, the ball-material ratio is 2: 1-4: 1, the fixed rotation speed in a vacuum environment is 250-350 rpm, and the total ball milling and mixing time is 2-3 hours;
preferably, the TiO is 2 @ graphene sol coated TiO in powder 2 The powder is A-type anatase powder or R-type rutile powder.
The invention also discloses in-situ synthesis enhanced additive composite powder which is characterized by being prepared by the preparation method.
The invention also protects the application of the in-situ synthesized enhanced additive composite powder, which is characterized in that: the method is used for preparing the high-performance two-phase ceramic reinforced aluminum matrix composite material by laser 3D printing.
The reaction equation of the laser in-situ synthesis reinforcing phase related by the invention is as follows:
The sol-coated composite powder prepared by the method is used for in-situ synthesis of high-performance dual-phase ceramic reinforced aluminum-based composite material TiO through laser 3D printing 2 The @ graphene sol coated powder (titanium dioxide sol is uniformly coated on the surface of single-layer graphene powder) is subjected to in-situ chemical reaction with an aluminum melt under the radiation of a high-energy-density laser beam, and two expected ceramic bodies Al are instantly synthesized in situ in an aluminum matrix of the composite reinforced material 2 O 3 And TiC to form high-performance biphase ceramic reinforcement which can be further combustedThe proportion of the authigenic ceramic reinforcement in the prepared aluminum-based composite material is accurately regulated and controlled by the stoichiometric ratio of the synthetic chemical reaction.
The preparation principle of the in-situ synthesis enhanced additive composite powder is as follows: titanate is used as a titanium source precursor of titanium dioxide sol formed by a chemical method, a mixed solution of absolute ethyl alcohol and glacial acetic acid is used as a specific hydrolysis inhibitor, a thin layer of titanium dioxide sol is coated on the surface of a graphene sheet, standing is carried out to solidify the titanium dioxide sol into a gel film, and then the coated powder is uniformly dispersed in aluminum alloy powder to prepare TiO for additive manufacturing 2 @ graphene sol-coated powder, TiO 2 In the process of melting the @ graphene sol-coated powder by high-temperature laser, graphene and TiO on the surface layer 2 The gel films react with each other in the aluminum melt to synthesize the ceramic reinforcement Al through self-propagating combustion 2 O 3 And TiC.
The beneficial effects of the invention are:
(1) the invention synthesizes the enhanced additive composite powder in situ, wherein the surface of the graphene layer sheet is tightly coated with a thin TiO layer 2 The gel film is fully contacted with the aluminum melt and reacts with the aluminum melt together in the additive manufacturing, processing and forming process, so that the combustion synthesis efficiency is improved, and the formed metallurgical bonding can effectively improve the wettability and the interface strength between the reinforcing phase and the matrix phase;
(2) in the in-situ synthesized enhanced additive composite powder, the surface is coated with TiO 2 The graphene layer of the gel film has extremely high laser absorption rate, so that the infrared laser energy utilization rate of the whole aluminum alloy powder material can be remarkably improved, and the temperature field distribution of an instantaneous liquid molten pool is more uniform so as to improve the fusion quality;
(3) the method does not generate environmental pollutants in the preparation stage, and the in-situ authigenic double-phase ceramic has small particle size, thereby being beneficial to improving the comprehensive performance of the composite material.
Drawings
FIG. 1 is a process flow diagram for preparing composite powder for laser additive manufacturing in situ synthesis;
fig. 2 is a microscopic topography of the dual-phase ceramic reinforced aluminum matrix composite prepared by in-situ synthesis of the reinforced additive composite powder in the laser additive manufacturing of example 1.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which will assist those skilled in the art in further understanding the present invention, but are not intended to limit the present invention in any way. It should be noted that various modifications and improvements can be made without departing from the spirit of the invention and still fall within the scope of the invention.
Example 1: a preparation method of in-situ synthesized enhanced additive composite powder (see figure 1) comprises the following specific steps:
(1) slowly and synchronously dripping ethyl titanate serving as a titanium source precursor and a specific hydrolysis inhibitor into deionized water, uniformly mixing under the condition of continuous stirring, adjusting the pH value of a system to 3 by adopting a dilute nitric acid solution, heating the solution to 60 ℃, and continuously carrying out hydrolysis reaction for 10 hours to obtain light yellow transparent titanium dioxide sol; wherein the specific hydrolysis inhibitor is a mixed solution of absolute ethyl alcohol and glacial acetic acid, the glacial acetic acid accounts for 15% of the total volume of the mixed solution, and the volume ratio of the titanium ethyl titanate source precursor, the deionized water and the specific hydrolysis inhibitor is 1:2: 3.8;
(2) adding monolayer lamellar graphene powder into titanium dioxide sol and uniformly dispersing to ensure that the titanium dioxide sol is uniformly coated on the surface of the graphene layer, aging at room temperature for 2d, heating at 80 ℃ and drying in vacuum for 4h, mechanically grinding and preferably screening with the sheet diameter not more than 7 mu m to prepare TiO 2 @ graphene sol-coated powder; wherein the single-layer graphene powder is lamellar powder, the purity is not lower than 99.99%, the average sheet diameter is 2 μm, the average layer thickness is 1.2nm, and the TiO is 2 @ graphene sol coated TiO in powder 2 The mass ratio of the graphene to the graphene is 20: 3; the grinding process is carried out in a small planetary high-flux ball mill, the grinding medium is stainless steel grinding balls, the size ratio of phi 3 to phi 5 to phi 10 is 2 to 1, the ball-material ratio is 8 to 1, the fixed rotating speed in a vacuum environment is 400rpm, the ball milling is paused for 5min every 30min, so as to avoid advanced reaction caused by overhigh temperature of powder, and the total grinding time is 5 h;
(3) will be provided withTiO 2 Putting the @ graphene composite powder and the AlSi10Mg alloy powder into a planetary ball mill, and performing ball-milling mixing treatment to prepare in-situ synthesis enhanced additive composite powder; wherein TiO in the enhanced additive composite powder is synthesized in situ 2 The mass fraction of the @ graphene sol-coated powder is 1%, the AlSi10Mg alloy powder is spherical powder, the average particle size is 35.5 μm, and in mass percent, the AlSi10Mg alloy powder contains 9.97% of Si, 0.4% of Mg, 0.05% of Fe, 0.04% of Mn, 0.015% of Cu, 0.01% of Ti, 0.014% of Zn, 0.02% of Sn, and the balance of Al; in the ball milling and mixing process, a ball milling medium is stainless steel balls, the size ratio of phi 5 to phi 10 is 2:1, the ball material ratio is 2:1, the fixed rotating speed in a vacuum environment is 250rpm, and the total mixing time is 2.5 h;
in this example, the composite powder for laser additive manufacturing in-situ synthesis is processed and formed by a high-energy laser beam, and then self-propagating combustion is performed to synthesize a dual-phase ceramic reinforcement (Al) 2 O 3 + TiC) mass content of 1%;
in this embodiment, the in-situ synthesized reinforced composite powder is manufactured by laser additive, and the microscopic morphology of the in-situ synthesized dual-phase ceramic reinforced aluminum-based composite material is shown in fig. 2, and as can be seen from fig. 2, after the composite powder is melted by high-temperature laser and rapidly solidified, the micron-sized rod-like TiC and Al are formed 2 O 3 A ceramic phase.
Example 2: a preparation method of in-situ synthesized enhanced additive composite powder (see figure 1) comprises the following specific steps:
(1) slowly dripping butyl titanate serving as a titanium source precursor and a specific hydrolysis inhibitor into deionized water synchronously, uniformly mixing under the condition of continuous stirring, adjusting the pH value of the system to 2.5 by adopting a dilute nitric acid solution, heating the solution to 55 ℃, and continuously carrying out hydrolysis reaction for 7 hours to obtain light yellow transparent titanium dioxide sol; wherein the specific hydrolysis inhibitor is a mixed solution of absolute ethyl alcohol and glacial acetic acid, the glacial acetic acid accounts for 25 percent of the total volume of the mixed solution, and the volume ratio of the titanium ethyl titanate source precursor, the deionized water and the specific hydrolysis inhibitor is 1:2: 4;
(2) adding the monolayer lamellar graphene powder into the titanium dioxide sol and uniformly dispersing to ensure that the titanium dioxideUniformly coating titanium oxide sol on the surface of a graphene layer sheet, sequentially aging at room temperature for 3d, heating at 65 ℃ and vacuum drying for 8h, mechanically grinding and preferably screening with the sheet diameter not more than 7 mu m to obtain TiO 2 @ graphene sol-coated powder; wherein the single-layer graphene powder is lamellar powder, the purity is not lower than 99.99%, the average sheet diameter is 5 μm, the average layer thickness is 0.8nm, and the TiO is 2 @ graphene sol coated TiO in powder 2 The mass ratio of the graphene to the graphene is 20: 3; the grinding process is carried out in a small planetary high-flux ball mill, grinding media are stainless steel grinding balls, the size ratio of phi 3 to phi 5 to phi 10 is 2:1:1, the ball-material ratio is 5:1, the fixed rotating speed in a vacuum environment is 450rpm, each ball mill is paused for 5min for 30min, advanced reaction caused by overhigh temperature of powder is avoided, and the total grinding time is 4 h;
(3) adding TiO into the mixture 2 Putting the @ graphene composite powder and Al-12Si alloy powder into a planetary ball mill for ball milling and mixing treatment to prepare in-situ synthesized enhanced additive composite powder; wherein TiO in the enhanced additive composite powder is synthesized in situ 2 The mass fraction of the @ graphene sol-coated powder is 6%, the Al-12Si alloy powder is spherical powder, the average particle size is 85.5 microns, and the mass percentage of Si in the Al-12Si alloy powder is 11.75%, Mg is 0.01%, Fe is 0.45%, Mn is 0.15%, Cu is 0.025%, Ti is 0.015%, Zn is 0.09%, Sn is 0.03%, and the balance is Al; in the ball milling and mixing process, a ball milling medium is stainless steel balls, the size ratio of phi 5 to phi 10 is 2 to 1, the ball-material ratio is 3 to 1, the fixed rotating speed in a vacuum environment is 350rpm, and the total mixing time is 2 hours;
the in-situ synthesized reinforced additive composite powder prepared in the embodiment is processed and formed by a high-energy laser beam, and then self-propagating combustion is performed to synthesize a dual-phase ceramic reinforcement (Al) 2 O 3 + TiC) 6% by mass.
Example 3: a preparation method of in-situ synthesized enhanced additive composite powder (see figure 1) comprises the following specific steps:
(1) slowly and synchronously dripping propyl titanate serving as a titanium source precursor and a specific hydrolysis inhibitor into deionized water, uniformly mixing under the condition of continuous stirring, adjusting the pH value of a system to 2 by adopting a dilute nitric acid solution, heating the solution to 60 ℃, and continuously carrying out hydrolysis reaction for 9 hours to obtain light yellow transparent titanium dioxide sol; wherein the specific hydrolysis inhibitor is a mixed solution of absolute ethyl alcohol and glacial acetic acid, the glacial acetic acid accounts for 20% of the total volume of the mixed solution, and the volume ratio of the titanium ethyl titanate source precursor, the deionized water and the specific hydrolysis inhibitor is 1:2: 4.2;
(2) adding monolayer lamellar graphene powder into titanium dioxide sol and uniformly dispersing to ensure that the titanium dioxide sol is uniformly coated on the surface of the graphene layer, sequentially aging at room temperature for 1d, heating at 70 ℃ and vacuum drying for 6h, mechanically grinding and preferably screening with the sheet diameter not more than 7 mu m to prepare TiO 2 @ graphene sol-coated powder; wherein the single-layer graphene powder is lamellar powder, the purity is not lower than 99.99%, the average sheet diameter is 1 μm, the average layer thickness is 1nm, and the TiO is 2 @ graphene sol coated TiO in powder 2 The mass ratio of the graphene to the graphene is 20: 3; the grinding process is carried out in a small planetary high-flux ball mill, the grinding medium is stainless steel grinding balls, the size ratio of phi 3 to phi 5 to phi 10 is 2 to 1, the ball-material ratio is 6 to 1, the fixed rotating speed in a vacuum environment is 300rpm, the ball milling is paused for 5min every 30min, so as to avoid advanced reaction caused by overhigh temperature of powder, and the total grinding time is 5 h;
(3) adding TiO into the mixture 2 Putting the @ graphene composite powder and AlSi7Mg alloy powder into a planetary ball mill for ball milling and mixing treatment to prepare in-situ synthesized enhanced additive composite powder; wherein TiO in the enhanced additive composite powder is synthesized in situ 2 The mass fraction of the @ graphene sol-coated powder was 4%, the AlSi7Mg alloy powder was a spherical powder having an average particle diameter of 37.5 μm, and in mass percentage, the AlSi7Mg alloy powder contained 6.97% of Si, 0.35% of Mg, 0.09% of Fe, 0.13% of Mn, 0.015% of Cu, 0.02% of Ti, 0.025% of Zn, 0.01% of Sn, and the balance Al; in the ball milling and mixing process, a ball milling medium is stainless steel balls, the size ratio of phi 5 to phi 10 is 2 to 1, the ball-material ratio is 4 to 1, the fixed rotating speed in a vacuum environment is 300rpm, and the total mixing time is 3 hours;
in the embodiment, the enhanced additive composite powder synthesized in situ is processed and formed by a high-energy laser beamSelf-propagating combustion synthesis of dual-phase ceramic reinforcement (Al) 2 O 3 + TiC) content of 4% by mass.
While particular embodiments of the present invention have been described, it is to be understood that the invention is not limited to the precise embodiments described, and that various changes and modifications may be effected therein by one skilled in the art within the scope of the appended claims and the scope of the invention is to be accorded the full scope of the claims.
Claims (10)
1. The preparation method of the in-situ synthesized enhanced additive composite powder is characterized by comprising the following specific steps of:
(1) synchronously and slowly dripping a titanium source precursor and a hydrolysis inhibitor into deionized water, adjusting the pH value of the system to 2.5-3.5 by adopting an acid solution under the condition of continuous stirring, and continuously performing hydrolysis reaction to form titanium dioxide sol;
(2) adding single-layer graphene powder into titanium dioxide sol and uniformly dispersing to ensure that the surface of the single-layer graphene powder is uniformly coated with the titanium dioxide sol, and aging at room temperature, drying, grinding and screening to obtain TiO 2 @ graphene sol-coated powder;
(3) adding TiO into the mixture 2 The @ graphene sol coated powder and the aluminum alloy powder are subjected to ball milling mixing treatment to obtain the in-situ synthesis enhanced additive composite powder for additive manufacturing.
2. The method for preparing the reinforced additive composite powder synthesized in situ according to claim 1, wherein the method comprises the following steps: in the step (1), the titanium source precursor is titanate;
the titanate is one or more of ethyl titanate, propyl titanate and butyl titanate.
3. The method for preparing the reinforced additive composite powder synthesized in situ according to claim 1, wherein the method comprises the following steps: in the step (1), the hydrolysis inhibitor is a mixed solution of absolute ethyl alcohol and glacial acetic acid, and the glacial acetic acid accounts for 15-25% of the total volume of the mixed solution;
the volume ratio of the titanium source precursor to the deionized water to the hydrolysis inhibitor is 1:2: 3.8-1: 2: 4.2;
the acid solution is a dilute nitric acid solution, and the hydrolysis duration is 7-10 h.
4. The method for preparing the reinforced additive composite powder synthesized in situ according to claim 1, wherein the method comprises the following steps: in the step (2), the single-layer graphene powder is lamellar powder, the diameter of each lamellar is 1-5 microns, and the thickness of each layer is 0.8-1.2 nm;
TiO 2 @ graphene sol coated TiO in powder 2 The mass ratio to graphene was 20: 3.
5. The method for preparing the in-situ synthesized reinforced additive composite powder according to claim 1, wherein the method comprises the following steps: in the step (2), the room temperature aging time is 1-3 d; the drying temperature is 60-80 ℃.
6. The method for preparing the reinforced additive composite powder synthesized in situ according to claim 1, wherein the method comprises the following steps: in the step (3), the aluminum alloy powder is spherical powder, and the particle size is 5-165 micrometers;
TiO in the in-situ synthesized enhanced additive composite powder 2 The mass fraction of the @ graphene sol coated powder is 1-6%.
7. The method for preparing the reinforced additive composite powder synthesized in situ according to claim 1, wherein the method comprises the following steps: in the step (3), the aluminum alloy powder is any one or more of AlSi7Mg alloy powder, AlSi10Mg alloy powder and Al-12Si alloy powder.
8. The method for preparing in-situ synthesis reinforced additive composite powder according to claim 7, wherein the method comprises the following steps:
measured by mass percent
6.5-7.5% of Si, 0.25-0.45% of Mg, less than or equal to 0.4% of Fe, less than or equal to 0.3% of Mn, less than or equal to 0.25% of Cu, less than or equal to 0.2% of Ti, less than or equal to 0.25% of Zn, less than or equal to 0.01% of Sn and the balance of Al in the AlSi7Mg alloy powder;
9.5-10.5% of Si, 0.15-0.45% of Mg, less than or equal to 0.45% of Fe, less than or equal to 0.4% of Mn, less than or equal to 0.05% of Cu, less than or equal to 0.1% of Ti, less than or equal to 0.1% of Zn, less than or equal to 0.05% of Sn and the balance of Al in the AlSi10Mg alloy powder;
10.5-13.5% of Si, less than or equal to 0.1% of Mg, less than or equal to 0.65% of Fe, less than or equal to 0.5% of Mn, less than or equal to 0.05% of Cu, less than or equal to 0.15% of Ti, less than or equal to 0.15% of Zn, less than or equal to 0.05% of Sn and the balance of Al in the Al-12Si alloy powder.
9. An in-situ synthesized reinforced additive composite powder, which is prepared by the preparation method of any one of claims 1 to 8.
10. Use of the in-situ synthesized reinforced additive composite powder prepared by the preparation method according to any one of claims 1 to 8, wherein the preparation method comprises the following steps: the method is used for preparing the high-performance double-phase ceramic reinforced aluminum matrix composite material by laser 3D printing.
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