Preparation Method and Application of a Nano-Additive Material Composite Powder

Abstract

The present invention relates to the technical field of nano-additive materials, and specifically relates to a preparation method and application of a nano-additive material composite powder, which includes the following steps: Weigh raw materials according to parts by weight: 45-50 parts of Al powder, 5-7 parts of Ni powder, 8-12 parts of nano-enhanced modified particles, and 10-15 parts of a ball matching agent based on ball milling. The nano-additive material composite powder of the present invention uses Al powder and Ni powder in combination, and at the same time, the added nano-enhanced modified particles and the ball matching agent based on ball milling are coordinated and matched. After ball milling treatment, laser melting, and finally heat improvement treatment, the mechanical properties, wear resistance, and elongation of the obtained nano-additive material are coordinately improved, and at the same time, the product has remarkable effects of anti-impact and anti-thermal-cold change stability.

Description

Technical Field

[0001] The present invention relates to the technical field of nano-additive materials, and particularly relates to a preparation method and application of a nano-additive material composite powder. Background Art

[0002] Additive manufacturing is a new manufacturing technology that integrates technologies such as lasers, precision transmissions, and CAD / CAM. By using a fine laser focusing spot, powder is melted layer by layer and stacked to achieve additive manufacturing, enabling the forming and manufacturing of metal parts with arbitrarily complex shapes. Existing nano-additive products have poor mechanical strength properties, low wear resistance and elongation rate at the same time. It is difficult for products to achieve the coordination of mechanical properties, wear resistance and elongation rate. At the same time, the products have poor impact resistance and thermal and cold stability, which further limits the use efficiency of the products. Summary of the Invention

[0003] Aiming at the defects of the existing technology, the purpose of the present invention is to provide a preparation method and application of a nano-additive material composite powder to solve the problems raised in the above background art.

[0004] The present invention adopts the following technical solutions to solve the technical problems:

[0005] The present invention provides a preparation method of a nano-additive material composite powder, comprising the following steps:

[0006] Step 1: Weigh raw materials according to parts by weight:

[0007] 45 - 50 parts of Al powder, 5 - 7 parts of Ni powder, 8 - 12 parts of nano-enhanced modification particles, and 10 - 15 parts of a ball matching agent based on ball milling;

[0008] Step 2: Feed the above raw materials into a ball mill for wet ball milling treatment. The ball milling speed is 1000 r / min, and the ball milling time is 1 h. After the ball milling is completed, perform suction filtration and drying until the moisture content is lower than 5%;

[0009] Step 3: Prepare an additive material from the product of Step 2 by selective laser melting;

[0010] Step 4: Perform thermal improvement treatment on the additive material, and finally ball mill it into powder and pass through a 200-mesh sieve to obtain the nano-additive material composite powder.

[0011] Preferably, the energy density of selective laser melting is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts planar row-by-row scanning and layer-by-layer scanning, and the energy density fluctuation of each layer is 20 J / m.

[0012] Preferably, the specific steps of the thermal improvement treatment are: first increase the temperature to 350°C at a rate of 2-5°C / min, keep warm for 2h, then reduce the temperature to 220°C at a rate of 3°C / min, keep warm for 1h, and finally air cool to room temperature.

[0013] Preferably, the preparation method of the nano-enhanced modified particles is:

[0014] S01: Stir TiC in a sufficient amount of acid solution, then wash, filter and dry. Preheat the dried TiC powder at 55-60°C for 1h to obtain preheated TiC powder.

[0015] S02: adding 3-5 parts by weight of cerium oxide and 1-3 parts by weight of silicon nitride to 5-8 parts by weight of 5% urea solution and mixing them thoroughly to obtain a first conditioning solution;

[0016] 3-5 parts by weight of magnesium fluoride, 1-3 parts by weight of silane coupling agent KH550 and 4-7 parts by weight of sodium dodecyl sulfate solution are mixed to obtain a second conditioning solution;

[0017] S03: the first conditioning liquid and the second conditioning liquid are stirred and mixed in a weight ratio of 3:5 to obtain a cerium-doped conditioning liquid;

[0018] S04: subjecting the preheated TiC powder and the cerium-doped conditioning liquid to ultrasonic modification in a weight ratio of 4:7, and after the ultrasonic modification is completed, filtering and drying are performed to obtain a modified TiC agent;

[0019] The conditioned TiC agent and the reinforcing agent were mixed and ball-milled in a weight ratio of 5:3 at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling was completed, the particles were filtered and dried to obtain nano-enhanced modified particles.

[0020] Preferably, the acid solution is a sulfuric acid solution with a mass fraction of 5%; the mass fraction of the sodium dodecyl sulfate solution is 3-5%.

[0021] The nano-enhanced modified particles use TiC through acid solution and preheating treatment to optimize the activity efficiency of TiC, and then use cerium-doped conditioning liquid for ultrasonic improvement treatment. The first conditioning liquid and the second conditioning liquid in the cerium-doped conditioning liquid are mutually adjusted and improved. The first conditioning liquid is mixed with cerium oxide, silicon nitride and 5% by mass urea solution. The magnesium fluoride, silane coupling agent KH550 and sodium dodecyl sulfate solution in the second conditioning liquid are mixed and blended. Through the coordination and synergy between the raw materials, cerium oxide, silicon nitride and magnesium fluoride are blended into the TiC system, and then the conditioned TiC agent is further added to the product system, so that the performance of the product is further improved. The boron oxide, sodium silicate solution and nano-silica sol in the reinforcing agent are coordinated with each other, and then zirconium oxide and dopamine hydrochloride solution are blended and improved. Cobalt oxide is used to blend raw materials such as boron oxide, and the conditioned TiC agent is further matched, so that the performance coordination and performance stability of the product are further improved.

[0022] Preferably, the ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic treatment is performed for 20 minutes.

[0023] Preferably, the preparation method of the enhancer is:

[0024] The boron oxide, sodium silicate solution and nano-silica sol are mixed and ball-milled in a weight ratio of (3-5): (7-11): 2, with a ball-milling speed of 1000 r / min for 2 hours, and the ball-milling is completed to obtain a compounding agent;

[0025] 4-7 parts by weight of the compounding agent, 1-2 parts by weight of zirconium oxide and 5-8 parts by weight of dopamine hydrochloride solution are fully mixed to obtain a reinforcing agent.

[0026] Preferably, the mass fraction of the sodium silicate solution is 5-8%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

[0027] By combining zirconium oxide with dopamine hydrochloride solution and a compounding agent, the compounding agent is improved by mixing boron oxide, sodium silicate solution and nano-silica sol. Through the coordinated optimization between the raw materials, the reinforcing agent is further enhanced and improved into the system, so that the performance of the product is further optimized and improved.

[0028] Preferably, the preparation method of the ball formulation based on ball milling is:

[0029] S11: preparing a chitosan solution with a mass fraction of 3-5% and a sodium alginate solution with a mass fraction of 2-5%;

[0030] S12: First, stir 3 - 5 parts of Ta powder in 5 - 8 parts of sodium alginate solution at a first - stage stirring speed of 550 - 600 r / min for 15 min. Subsequently, add 2 - 3 parts of chitosan solution and 1 - 2 parts of sodium carboxymethylcellulose, and perform second - stage stirring at a stirring speed of 300 - 350 r / min for 40 - 50 min to obtain a ball - matching agent based on ball - milling.

[0031] The ball - matching agent based on ball - milling is prepared by blending Ta powder with sodium alginate solution, chitosan solution and sodium carboxymethylcellulose. Through the coordination of raw materials, the effect of the ball - matching agent based on ball - milling combined with nano - enhanced modification particles is more significant. And after being blended into the system by the ball - matching agent based on ball - milling, the improvement effect of the interfacial property between product raw materials is more obvious, thus further improving the performance of the product.

[0032] The present invention also provides an application of a preparation method of a nano - additive material composite powder in laser melting additive manufacturing.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] The nano - additive material composite powder of the present invention is prepared by using Al powder and Ni powder in combination, and at the same time adding nano - enhanced modification particles and the ball - matching agent based on ball - milling for coordination. After ball - milling treatment, laser melting, and finally heat improvement treatment, the mechanical properties, wear resistance and elongation of the obtained nano - additive material are coordinately improved, and at the same time, the product has significant anti - impact, anti - thermal - cold - change stability effects. Specific Embodiments

[0035] The following describes the technical solutions in the embodiments of the present invention clearly and completely with reference to specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of them. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0036] A preparation method of a nano - additive material composite powder in this embodiment includes the following steps:

[0037] Step 1: Weigh raw materials according to parts by weight:

[0038] 45 - 50 parts of Al powder, 5 - 7 parts of Ni powder, 8 - 12 parts of nano - enhanced modification particles and 10 - 15 parts of the ball - matching agent based on ball - milling;

[0039] Step 2: Feed the above - mentioned raw materials into a ball mill for wet ball - milling treatment at a ball - milling speed of 1000 r / min for 1 h. After ball - milling, perform suction filtration and drying until the moisture content is lower than 5%.

[0040] Step 3: Prepare the additive material by selective laser melting of the product of Step 2;

[0041] Step 4: Perform thermal improvement treatment on the additive material, and finally ball mill it into powder and pass through 200 meshes to obtain the nano-additive material composite powder.

[0042] In this example, the energy density of selective laser melting is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts planar line-by-line scanning and layer-by-layer scanning, and the energy density fluctuation of each layer is 20 J / m;

[0043] The specific steps of the thermal improvement treatment are as follows: First, heat it up to 350 °C at a rate of 2-5 °C / min, keep it warm for 2 h, then cool it down to 220 °C at a rate of 3 °C / min, keep it warm for 1 h, and finally air-cool it to room temperature.

[0044] The preparation method of the nano-enhanced modified particles in this example is as follows:

[0045] S01: First, stir TiC sufficiently in a sufficient amount of acid solution, then wash it with water, filter it by suction, and dry it. Then preheat the dried TiC powder at 55-60 °C for 1 h to obtain the preheated TiC powder;

[0046] S02: Add 3-5 parts by weight of cerium oxide and 1-3 parts by weight of silicon nitride to 5-8 parts by weight of a 5% urea solution by mass and mix well to obtain the first conditioning liquid;

[0047] Add 3-5 parts by weight of magnesium fluoride, 1-3 parts by weight of silane coupling agent KH550 and 4-7 parts by weight of sodium dodecyl sulfate solution and mix well to obtain the second conditioning liquid;

[0048] S03: Stir and mix the first conditioning liquid and the second conditioning liquid evenly according to the weight ratio of 3:5 to obtain the cerium-doped conditioning liquid;

[0049] S04: Perform ultrasonic modification treatment on the preheated TiC powder and the cerium-doped conditioning liquid according to the weight ratio of 4:7. After the ultrasonic treatment is completed, filter it by suction and dry it to obtain the conditioned TiC agent;

[0050] Mix the conditioned TiC agent and the reinforcing agent evenly according to the weight ratio of 5:3 and perform ball milling treatment. The ball milling speed is 1500 r / min, and the ball milling time is 2 h. After the ball milling is completed, filter it by suction and dry it to obtain the nano-enhanced modified particles.

[0051] The acid solution in this example is a 5% sulfuric acid solution by mass; the mass fraction of the sodium dodecyl sulfate solution is 3-5%.

[0052] The ultrasonic power of the ultrasonic modification treatment in this example is 350-400 W, and the ultrasonic treatment time is 20 min.

[0053] The preparation method of the enhancer of this embodiment is:

[0054] The boron oxide, sodium silicate solution and nano-silica sol are mixed and ball-milled in a weight ratio of (3-5): (7-11): 2, with a ball-milling speed of 1000 r / min for 2 hours, and the ball-milling is completed to obtain a compounding agent;

[0055] 4-7 parts by weight of the compounding agent, 1-2 parts by weight of zirconium oxide and 5-8 parts by weight of dopamine hydrochloride solution are fully mixed to obtain a reinforcing agent.

[0056] The mass fraction of the sodium silicate solution in this embodiment is 5-8%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

[0057] The preparation method of the ball preparation based on ball milling of this embodiment is:

[0058] S11: preparing a chitosan solution with a mass fraction of 3-5% and a sodium alginate solution with a mass fraction of 2-5%;

[0059] S12: 3-5 parts of Ta powder are stirred in 5-8 parts of sodium alginate solution, and then 2-3 parts of chitosan solution and 1-2 parts of sodium carboxymethyl cellulose are added, and stirred in the second stage to obtain a ball formulation based on ball milling.

[0060] The stirring speed of the first-stage stirring treatment in this embodiment is 550-600 r / min, and the stirring is for 15 minutes; the stirring speed of the second-stage stirring treatment is 300-350 r / min, and the stirring is for 40-50 minutes.

[0061] The present embodiment provides a method for preparing a nano-additive material composite powder and its application in laser melting additive manufacturing.

[0062] Example 1

[0063] A method for preparing a nano-additive material composite powder of this embodiment includes the following steps:

[0064] Step 1: Weigh the raw materials by weight:

[0065] 45 parts of Al powder, 5 parts of Ni powder, 8 parts of nano-enhanced modified particles and 10 parts of ball preparation based on ball milling;

[0066] Step 2: feeding the above raw materials into a ball mill for wet ball milling, with a ball milling speed of 1000r / min and ball milling for 1h. After the ball milling is completed, filtering and drying are performed until the moisture content is less than 5%;

[0067] Step 3: preparing additive material by selective laser melting the product of step 2;

[0068] Step 4: The additive material is subjected to thermal improvement treatment, and finally ball-milled into powder, and then passed through 200 meshes to obtain nano-additive material composite powder.

[0069] The energy density of the selective laser melting in this embodiment is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts plane line-by-line scanning and layer-by-layer scanning, and the energy density of each layer fluctuates by 20 J / m;

[0070] The specific steps of thermal improvement treatment are: first increase the temperature to 350°C at a rate of 2°C / min, keep warm for 2 hours, then reduce the temperature to 220°C at a rate of 3°C / min, keep warm for 1 hour, and finally air cool to room temperature.

[0071] The preparation method of the nano-enhanced modified particles of this embodiment is:

[0072] S01: Stir TiC in a sufficient amount of acid solution, then wash, filter and dry. Preheat the dried TiC powder at 55°C for 1h to obtain preheated TiC powder.

[0073] S02: adding 3 parts by weight of cerium oxide and 1 part by weight of silicon nitride to 5 parts by weight of 5% urea solution and mixing them thoroughly to obtain a first conditioning solution;

[0074] 3 parts by weight of magnesium fluoride, 1 part by weight of silane coupling agent KH550 and 4 parts by weight of sodium dodecyl sulfate solution are mixed to obtain a second conditioning solution;

[0075] S03: the first conditioning liquid and the second conditioning liquid are stirred and mixed in a weight ratio of 3:5 to obtain a cerium-doped conditioning liquid;

[0076] S04: subjecting the preheated TiC powder and the cerium-doped conditioning liquid to ultrasonic modification in a weight ratio of 4:7, and after the ultrasonic modification is completed, filtering and drying are performed to obtain a modified TiC agent;

[0077] The conditioned TiC agent and the reinforcing agent were mixed and ball-milled in a weight ratio of 5:3 at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling was completed, the particles were filtered and dried to obtain nano-enhanced modified particles.

[0078] The acid solution in this embodiment is a sulfuric acid solution with a mass fraction of 5%; the mass fraction of the sodium dodecyl sulfate solution is 3%.

[0079] The ultrasonic power of the ultrasonic modification treatment in this embodiment is 350W, and the ultrasonic treatment is carried out for 20 minutes.

[0080] The preparation method of the enhancer of this embodiment is:

[0081] The boron oxide, sodium silicate solution and nano silica sol were mixed and ball-milled in a weight ratio of 3:7:2, with a ball-milling speed of 1000 r / min for 2 h to obtain a compounding agent;

[0082] 4 parts by weight of the compounding agent, 1 part by weight of zirconium oxide and 5 parts by weight of dopamine hydrochloride solution were fully mixed to obtain a reinforcing agent.

[0083] The mass fraction of the sodium silicate solution in this embodiment is 5%; the mass fraction of the dopamine hydrochloride solution is 2%.

[0084] The preparation method of the ball preparation based on ball milling of this embodiment is:

[0085] S11: preparing a 3% by mass chitosan solution and a 2% by mass sodium alginate solution;

[0086] S12: 3 parts of Ta powder are added to 5 parts of sodium alginate solution for primary stirring treatment, and then 2 parts of chitosan solution and 1 part of sodium carboxymethyl cellulose are added for secondary stirring treatment to obtain a ball formulation based on ball milling.

[0087] The stirring speed of the first-stage stirring treatment in this embodiment is 550 r / min, and the stirring is for 15 min; the stirring speed of the second-stage stirring treatment is 300 r / min, and the stirring is for 40 min.

[0088] The present embodiment provides a method for preparing a nano-additive material composite powder and its application in laser melting additive manufacturing.

[0089] Example 2

[0090] A method for preparing a nano-additive material composite powder of this embodiment includes the following steps:

[0091] Step 1: Weigh the raw materials by weight:

[0092] 50 parts of Al powder, 7 parts of Ni powder, 12 parts of nano-enhanced modified particles and 15 parts of ball preparation based on ball milling;

[0093] Step 2: feeding the above raw materials into a ball mill for wet ball milling, with a ball milling speed of 1000r / min and ball milling for 1h. After the ball milling is completed, filtering and drying are performed until the moisture content is less than 5%;

[0094] Step 3: preparing additive material by selective laser melting the product of step 2;

[0095] Step 4: The additive material is subjected to thermal improvement treatment, and finally ball-milled into powder, and then passed through 200 meshes to obtain nano-additive material composite powder.

[0096] The energy density of the selective laser melting in this embodiment is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts plane line-by-line scanning and layer-by-layer scanning, and the energy density of each layer fluctuates by 20 J / m;

[0097] The specific steps of thermal improvement treatment are: first increase the temperature to 350°C at a rate of 5°C / min, keep warm for 2 hours, then reduce the temperature to 220°C at a rate of 3°C / min, keep warm for 1 hour, and finally air cool to room temperature.

[0098] The preparation method of the nano-enhanced modified particles of this embodiment is:

[0099] S01: Stir TiC in a sufficient amount of acid solution, then wash, filter and dry. Preheat the dried TiC powder at 60°C for 1h to obtain preheated TiC powder.

[0100] S02: adding 5 parts by weight of cerium oxide and 3 parts by weight of silicon nitride to 8 parts by weight of 5% urea solution and mixing them thoroughly to obtain a first conditioning solution;

[0101] 5 parts by weight of magnesium fluoride, 3 parts by weight of silane coupling agent KH550 and 7 parts by weight of sodium dodecyl sulfate solution are mixed to obtain a second conditioning solution;

[0102] S03: the first conditioning liquid and the second conditioning liquid are stirred and mixed in a weight ratio of 3:5 to obtain a cerium-doped conditioning liquid;

[0103] S04: subjecting the preheated TiC powder and the cerium-doped conditioning liquid to ultrasonic modification in a weight ratio of 4:7, and after the ultrasonic modification is completed, filtering and drying are performed to obtain a modified TiC agent;

[0104] The conditioned TiC agent and the reinforcing agent were mixed and ball-milled in a weight ratio of 5:3 at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling was completed, the particles were filtered and dried to obtain nano-enhanced modified particles.

[0105] The acid solution in this embodiment is a sulfuric acid solution with a mass fraction of 5%; the mass fraction of the sodium dodecyl sulfate solution is 5%.

[0106] The ultrasonic power of the ultrasonic modification treatment in this embodiment is 400W, and the ultrasonic treatment is performed for 20 minutes.

[0107] The preparation method of the enhancer of this embodiment is:

[0108] The boron oxide, sodium silicate solution and nano silica sol were mixed and ball-milled in a weight ratio of 5:11:2, with a ball-milling speed of 1000 r / min for 2 h to obtain a compounding agent;

[0109] Mix 7 parts by weight of a compounding agent, 2 parts by weight of zirconia, and 8 parts by weight of dopamine hydrochloride solution thoroughly to obtain a reinforcing agent.

[0110] In this example, the mass fraction of the sodium silicate solution is 8%; the mass fraction of the dopamine hydrochloride solution is 5%.

[0111] The preparation method of the ball compounding agent based on ball milling in this example is as follows:

[0112] S11: Prepare a chitosan solution with a mass fraction of 5% and a sodium alginate solution with a mass fraction of 5%;

[0113] S12: First-stage stir 5 parts of Ta powder in 8 parts of sodium alginate solution, then add 3 parts of chitosan solution and 2 parts of sodium carboxymethylcellulose, and perform second-stage stirring to obtain a ball compounding agent based on ball milling.

[0114] In this example, the stirring speed of the first-stage stirring treatment is 600 r / min, and the stirring time is 15 min; the stirring speed of the second-stage stirring treatment is 350 r / min, and the stirring time is 50 min.

[0115] The preparation method of a nano-additive material composite powder in this example is applied in laser melting additive manufacturing.

[0116] Example 3

[0117] The preparation method of a nano-additive material composite powder in this example includes the following steps:

[0118] Step 1: Weigh the raw materials according to parts by weight:

[0119] 47.5 parts of Al powder, 6 parts of Ni powder, 10 parts of nano-reinforced modified particles, and 12.5 parts of a ball compounding agent based on ball milling;

[0120] Step 2: Feed the above raw materials into a ball mill for wet ball milling treatment. The ball milling speed is 1000 r / min, and the ball milling time is 1 h. After the ball milling is completed, perform suction filtration and drying until the moisture content is lower than 5%;

[0121] Step 3: Prepare an additive material by selective laser melting for the product of Step 2;

[0122] Step 4: Perform heat improvement treatment on the additive material, and finally ball mill it into powder and pass through a 200-mesh sieve to obtain the nano-additive material composite powder.

[0123] In this example, the energy density of selective laser melting is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts planar progressive scanning and layer-by-layer scanning, and the energy density fluctuation of each layer is 20 J / m;

[0124] The specific steps of thermal improvement treatment are: first increase the temperature to 350°C at a rate of 2-5°C / min, keep warm for 2 hours, then reduce the temperature to 220°C at a rate of 3°C / min, keep warm for 1 hour, and finally air cool to room temperature.

[0125] The preparation method of the nano-enhanced modified particles of this embodiment is:

[0126] S01: Stir TiC in a sufficient amount of acid solution, then wash, filter and dry. Preheat the dried TiC powder at 57.5°C for 1h to obtain preheated TiC powder.

[0127] S02: adding 4 parts by weight of cerium oxide and 2 parts by weight of silicon nitride to 6.5 parts by weight of 5% urea solution and mixing them thoroughly to obtain a first conditioning solution;

[0128] 4 parts by weight of magnesium fluoride, 2 parts by weight of silane coupling agent KH550 and 5.5 parts by weight of sodium dodecyl sulfate solution are mixed to obtain a second conditioning solution;

[0129] S03: the first conditioning liquid and the second conditioning liquid are stirred and mixed in a weight ratio of 3:5 to obtain a cerium-doped conditioning liquid;

[0130] S04: subjecting the preheated TiC powder and the cerium-doped conditioning liquid to ultrasonic modification in a weight ratio of 4:7, and after the ultrasonic modification is completed, filtering and drying are performed to obtain a modified TiC agent;

[0131] The conditioned TiC agent and the reinforcing agent were mixed and ball-milled in a weight ratio of 5:3 at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling was completed, the particles were filtered and dried to obtain nano-enhanced modified particles.

[0132] The acid solution in this embodiment is a sulfuric acid solution with a mass fraction of 5%; the mass fraction of the sodium dodecyl sulfate solution is 4%.

[0133] The ultrasonic power of the ultrasonic modification treatment in this embodiment is 375W, and the ultrasonic treatment is carried out for 20 minutes.

[0134] The preparation method of the enhancer of this embodiment is:

[0135] The boron oxide, sodium silicate solution and nano silica sol were mixed and ball-milled in a weight ratio of 4:9:2, with a ball-milling speed of 1000 r / min for 2 h to obtain a compounding agent;

[0136] 5.5 parts by weight of the compounding agent, 1.5 parts by weight of zirconium oxide and 6.5 parts by weight of dopamine hydrochloride solution were fully mixed to obtain a reinforcing agent.

[0137] The mass fraction of the sodium silicate solution in this embodiment is 6.5%; the mass fraction of the dopamine hydrochloride solution is 3.5%.

[0138] The preparation method of the ball compounding agent based on ball milling in this embodiment is as follows:

[0139] S11: Prepare a chitosan solution with a mass fraction of 4% and a sodium alginate solution with a mass fraction of 3.5%;

[0140] S12: First-stage stir 4 parts of Ta powder in 6.5 parts of sodium alginate solution, then add 2.5 parts of chitosan solution and 1.5 parts of sodium carboxymethylcellulose, and perform second-stage stirring to obtain the ball compounding agent based on ball milling.

[0141] In this embodiment, the stirring speed of the first-stage stirring treatment is 570 r / min, and the stirring time is 15 min; the stirring speed of the second-stage stirring treatment is 325 r / min, and the stirring time is 45 min.

[0142] The preparation method of a nano-additive material composite powder in this embodiment is applied in laser melting additive manufacturing.

[0143] Comparative Example 1

[0144] The difference from Example 3 is that no nano-enhancing and modifying particles are added.

[0145] Comparative Example 2

[0146] The difference from Example 3 is that no conditioned TiC agent is added in the preparation of the nano-enhancing and modifying particles.

[0147] Comparative Example 3

[0148] The difference from Example 3 is that no preheated TiC powder is added in the preparation of the conditioned TiC agent.

[0149] Comparative Example 4

[0150] The difference from Example 3 is that no cerium-doped conditioning solution is added in the preparation of the conditioned TiC agent.

[0151] Comparative Example 5

[0152] The difference from Example 3 is that no first conditioning solution is added in the preparation of the cerium-doped conditioning solution.

[0153] Comparative Example 6

[0154] The difference from Example 3 is that no cerium oxide and silicon nitride are added in the first conditioning solution.

[0155] Comparative Example 7

[0156] The difference from Example 3 is that no second conditioning solution is added in the preparation of the cerium-doped conditioning solution.

[0157] Comparative Example 8

[0158] Different from Example 3, magnesium fluoride and silane coupling agent KH550 were not added to the second conditioning solution.

[0159] Comparative Example 9

[0160] Different from Example 3, no reinforcing agent was added in the preparation of nano-enhanced modified particles.

[0161] Comparative Example 10

[0162] Different from Example 3, the ball matching agent based on ball milling was not added.

[0163] Comparative Example 11

[0164] Different from Example 3, Ta powder and chitosan solution were not added in the preparation of the ball matching agent based on ball milling.

[0165] Under conventional conditions, the products of Examples 1-3 and Comparative Examples 1-11 were tested for their strength, wear resistance (friction and wear test was carried out with a friction and wear testing machine, and the test conditions were: loading load 10 kg, wear time 30 min, wear frequency 10 HAZ, and the counter-material was GCr15 steel ball (55 HRC)) and elongation performance; 50 J / cm

[0166] The products were impacted for 1 h with an impact toughness of 50 J / cm, and at the same time, the products were heated to 150 °C, held for 1 h, then cooled with 5 °C water for 2 h, then cooled to -20 °C, held for 1 h, and then warmed back with 50 °C water for 2 h. The above was one cycle, and the cycle was repeated 10 times to test the impact resistance and thermal shock stability of the products; The performance test is shown in Table 1 below. Table 1 is the performance test table of strength, wear resistance and elongation.

[0167] Table 1:

[0168]

[0169] It can be seen from Examples 1-3 and Comparative Examples 1-11 that

[0170] Under conventional conditions, the product of Example 3 of the present invention has excellent tensile strength performance, and at the same time has excellent wear resistance and elongation performance. The strength, wear resistance and elongation performance of the product can be coordinately improved, and the product still has excellent performance under impact resistance and thermal shock conditions, and the performance stability is strong;

[0171] It can be seen from Comparative Examples 1-11 and Example 3 that if one of the nano-enhanced modified particles or the ball matching agent based on ball milling is not added in the present invention, the performance of the product deteriorates significantly. By using the two in coordinated cooperation and synergistic effect, the performance effect of the product is remarkable;

[0172] The performance of the products showed a trend of deterioration to varying degrees when no conditioned TiC agent was added to the preparation of the nano-reinforced modified particles, no preheated TiC powder was added to the preparation of the conditioned TiC agent, no cerium-doped conditioning liquid was added to the preparation of the cerium-doped conditioning liquid, no first conditioning liquid was added to the preparation of the cerium-doped conditioning liquid, no cerium oxide and silicon nitride were added to the first conditioning liquid, no second conditioning liquid was added to the preparation of the cerium-doped conditioning liquid, and no magnesium fluoride and silane coupling agent KH550 were added to the second conditioning liquid; and the performance of the products showed a relatively obvious trend of deterioration when no reinforcing agent was added to the preparation of the nano-reinforced modified particles;

[0173] The cerium-doped conditioning liquid prepared by combining the first conditioning liquid and the second conditioning liquid obtained by the specific method of the present invention, and the conditioned TiC agent obtained by combining with the specific preheated TiC powder, have the most significant product performance effects. At the same time, the performance effects of the products made by combining the conditioned TiC agent obtained by the method of the present invention and the nano-reinforced modified particles are the most significant. At the same time, Ta powder and chitosan solution are not added in the preparation of the ball preparation based on ball milling, and the performance of the product also shows a relatively obvious trend of deterioration.

[0174] Since the enhancer has a significant impact on the performance of the product, further research is needed:

[0175] The preparation method of the enhancer is:

[0176] The boron oxide, sodium silicate solution and nano silica sol were mixed and ball-milled in a weight ratio of 4:9:2, with a ball-milling speed of 1000 r / min for 2 h to obtain a compounding agent;

[0177] 5.5 parts by weight of the compounding agent, 1.5 parts by weight of zirconium oxide and 6.5 parts by weight of dopamine hydrochloride solution were fully mixed to obtain a reinforcing agent.

[0178] The mass fraction of the sodium silicate solution in this embodiment is 6.5%; the mass fraction of the dopamine hydrochloride solution is 3.5%.

[0179] Experimental Example 1

[0180] The same as Example 3, except that zirconium oxide was not added in the preparation of the reinforcing agent.

[0181] Experimental Example 2

[0182] The same as Example 3, except that no dopamine hydrochloride solution was added in the preparation of the enhancer.

[0183] Experimental Example 3

[0184] The same as Example 3, except that boron oxide was not added in the preparation of the compounding agent.

[0185] Experimental Example 4

[0186] Same as Example 3, except that sodium silicate solution and nano-silica sol were not added in the preparation of the compounding agent.

[0187] Experimental Example 5

[0188] Same as Example 3, except that the mass fraction of the sodium silicate solution was 4%; the mass fraction of the dopamine hydrochloride solution was 6%.

[0189] The performance tests of the products in Experimental Examples 1-5 are shown in Table 2 below. Table 2 is a test table for the influence of the preparation of the enhancer on the product performance;

[0190] Table 2:

[0191]

[0192] It can be seen from Experimental Examples 1-5 that when zirconia was not added in the preparation of the enhancer, the performance of the product deteriorated significantly. At the same time, when boron oxide was not added in the preparation of the compounding agent, the performance effect of the product was poor. In addition, when dopamine hydrochloride solution was not added in the preparation of the enhancer and sodium silicate solution and nano-silica sol were not added in the preparation of the compounding agent, the performance of the product showed a trend of deterioration to varying degrees. The performance effect of the product was the most significant when the enhancer obtained by using a specific compounding agent in combination with specific raw materials. In addition, when the mass fraction of the sodium silicate solution was 4%; the mass fraction of the dopamine hydrochloride solution was 6%, the performance of the product also showed a trend of deterioration. Only within the specific mass fraction range of the present invention, the performance effect of the product was the most obvious.

Claims

1. A method for preparing a nano-additive material composite powder, characterized in that: The following steps are involved: Step 1: Weigh the raw materials by weight: 45-50 parts of Al powder, 5-7 parts of Ni powder, 8-12 parts of nano-enhanced modified particles and 10-15 parts of ball preparation based on ball milling; Step 2: feeding the above raw materials into a ball mill for wet ball milling, with a ball milling speed of 1000r / min and ball milling for 1h. After the ball milling is completed, filtering and drying are performed until the moisture content is less than 5%; Step 3: preparing additive material by selective laser melting the product of step 2; Step 4: The additive material is subjected to thermal improvement treatment, and finally ball-milled into powder, and then passed through 200 meshes to obtain nano-additive material composite powder; The preparation method of nano-enhanced modified particles is: S01: Stir TiC in a sufficient amount of acid solution, then wash, filter and dry. Preheat the dried TiC powder at 55-60°C for 1h to obtain preheated TiC powder. S02: adding 3-5 parts by weight of cerium oxide and 1-3 parts by weight of silicon nitride to 5-8 parts by weight of 5% urea solution and mixing them thoroughly to obtain a first conditioning solution; 3-5 parts by weight of magnesium fluoride, 1-3 parts by weight of silane coupling agent KH550 and 4-7 parts by weight of sodium dodecyl sulfate solution are mixed to obtain a second conditioning solution; S03: the first conditioning liquid and the second conditioning liquid are stirred and mixed in a weight ratio of 3:5 to obtain a cerium-doped conditioning liquid; S04: subjecting the preheated TiC powder and the cerium-doped conditioning liquid to ultrasonic modification in a weight ratio of 4:7, and after the ultrasonic modification is completed, filtering and drying are performed to obtain a modified TiC agent; The conditioned TiC agent and the reinforcing agent were mixed and ball-milled in a weight ratio of 5:3, with a ball-milling speed of 1500 r / min for 2 h. After the ball-milling was completed, the mixture was filtered and dried to obtain nano-enhanced modified particles. The preparation method of the enhancer is: The boron oxide, sodium silicate solution and nano-silica sol are mixed and ball-milled in a weight ratio of (3-5): (7-11): 2, with a ball-milling speed of 1000 r / min for 2 hours, and the ball-milling is completed to obtain a compounding agent; 4-7 parts by weight of a compounding agent, 1-2 parts by weight of zirconium oxide and 5-8 parts by weight of a dopamine hydrochloride solution are fully mixed to obtain a reinforcing agent; The preparation method of the ball preparation based on ball milling is: S11: preparing a chitosan solution with a mass fraction of 3-5% and a sodium alginate solution with a mass fraction of 2-5%; S12: 3-5 parts of Ta powder are stirred in 5-8 parts of sodium alginate solution, and then 2-3 parts of chitosan solution and 1-2 parts of sodium carboxymethyl cellulose are added, and stirred in the second stage to obtain a ball formulation based on ball milling.

2. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The energy density of selective laser melting is 90 J / m, and the scanning speed is 1000 mm / s; and the selective laser melting method adopts plane line-by-line scanning and layer-by-layer scanning, and the energy density of each layer fluctuates by 20 J / m.

3. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The specific steps of the thermal improvement treatment are: first increase the temperature to 350°C at a rate of 2-5°C / min, keep it warm for 2h, then reduce the temperature to 220°C at a rate of 3°C / min, keep it warm for 1h, and finally air cool to room temperature.

4. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The acid solution is a sulfuric acid solution with a mass fraction of 5%; the mass fraction of the sodium dodecyl sulfate solution is 3-5%.

5. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic treatment lasts for 20 minutes.

6. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The mass fraction of the sodium silicate solution is 5-8%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

7. The method for preparing a nano-additive material composite powder according to claim 1, characterized in that: The stirring speed of the first-stage stirring treatment is 550-600r / min, and the stirring is for 15 minutes; the stirring speed of the second-stage stirring treatment is 300-350r / min, and the stirring is for 40-50 minutes.

8. Application of the method for preparing the nano-additive material composite powder according to any one of claims 1 to 7 in laser melting additive.

Images