CN103936428A - Preparation method of rapid molding powder material used for three dimensional printing - Google Patents

Abstract

The invention discloses a method for preparing powder materials for three-dimensional printing rapid prototyping, which is characterized in that the method includes pretreatment of powder materials and preparation of molding materials, wherein the pretreatment of powder materials: mixing 88% to 96% of powder materials with 4 %~12% of 3-aminopropyltriethoxysilane is mixed and ground at a speed of 500~1000 rpm for 2~6 hours to obtain a pretreated powder material; add 50%~70% water according to the mass percentage concentration, add 0.5%~1.0% polyoxyethylene lauryl ether, stir to dissolve, then add 2%~10% polyvinyl alcohol, heat to dissolve, add 25%~40% pretreatment powder material, stir and mix evenly, put Put it into a grinding machine, mix and grind at room temperature for 10-15 hours, and then spray dry to obtain a rapid prototyping powder material. The material does not need to be sprayed with a binder and can be directly molded by heating at 85-100°C and pressure within the range of 1MPa-10MPa. The preparation process is simple, the conditions are easy to control, the production cost is low, and it is easy for industrial production.

Description

A preparation method for three-dimensional printing rapid prototyping powder material

the

technical field

The invention relates to a preparation method for three-dimensional printing rapid prototyping powder materials, belonging to the field of rapid prototyping materials, in particular to a preparation process for three-dimensional printing rapid prototyping alumina, silicon carbide and ceramic powder materials.

Background technique

Rapid prototyping technology, also known as Rapid Prototyping Manufacturing (RPM) technology, was born in the late 1980s. It is a high-tech manufacturing technology based on material accumulation method and is considered to be a major achievement in the manufacturing field in recent years. It integrates mechanical engineering, CAD, reverse engineering technology, layered manufacturing technology, numerical control technology, material science, and laser technology, and can automatically, directly, quickly and accurately transform design ideas into prototypes with certain functions or directly manufacture parts , so as to provide a high-efficiency and low-cost realization means for parts prototype production and verification of new design ideas. That is, rapid prototyping technology is to use the data of three-dimensional CAD to accumulate layers of materials into solid prototypes through rapid prototyping machines.

3D printing (Three Dimonsion Printing, referred to as 3DP) is a rapid prototyping technology that can divide the 3D model data designed by the computer into layer model data, and build specific raw materials layer by layer until the entire entity is constructed. 3DP molding has the advantages of low cost, no pollution in the working process, and fast molding speed.

3D printing technologies include 3DP technology, FDM fusion lamination molding technology, SLA stereolithography technology, SLS selective laser sintering technology, DLP laser molding technology and UV ultraviolet molding technology. The most widely used is FDM3D printing technology. This technology can be used in the home. It is easy to operate and the materials used are generally available. The products printed by this technology are also close to our daily necessities. The materials used are mainly environmentally friendly polymer materials. Such as: PLA, PCL PHA PBS PA ABS PC PS POM PVC, because this technology is generally printed on the desktop, the smell produced by the molten polymer material or the harmful substances produced by decomposition directly contact with our people, which is easy to cause Security Question. Suitable materials can be selected for industrial parts and other parts that require a certain strength function.

In the field of existing molding materials, SLS rapid prototyping technology has a wide range of applications in the field of rapid prototyping because of its advantages such as diverse sources of raw materials and short construction time of parts. Chinese invention patent CN1379061A discloses a nylon powder material used for laser sintering molding products. Through chemical synthesis and process improvement, the surface of the nylon powder material is treated to obtain excellent sintering performance, high strength molding products, and good toughness. The product simplifies the preparation process of laser sintered nylon material and reduces the cost. However, there are many shortcomings in the SLS process that seriously limit the further application and popularization of SLS; thus, the use of molding materials based on the SLS process is also limited.

The 3DP process is similar to the SLS process, both of which are formed by powder materials. The difference is that the powder materials of the 3DP process are not connected by layer-by-layer laser sintering, but are bonded with an adhesive (such as silica gel) under the action of the nozzle. "Print" the section information of the part on the powder material. Since 3DP is molded by spraying the adhesive through the nozzle, the cost of using complex and expensive sintering equipment such as lasers is avoided, which is conducive to the use and promotion of rapid prototyping technology. Chinese invention patent CN102093646 B discloses a preparation method for three-dimensional printing rapid prototyping materials, which is to carry out a series of modifications on powder materials to obtain modified powder materials A, and modify powder materials A and binder B during use Matching.

Due to the large particle size of the 3DP rapid prototyping material powder, it is difficult to form thin-walled parts, the forming accuracy of tiny parts is not high enough, and the surface has a relatively rough feeling; in addition, because the binder is not strong enough, there is a low strength of the formed part Waiting is not enough. In addition, the 3DP molding materials currently sold in the market are basically monopolized by foreign companies, and the price is high, which seriously restricts the promotion and popularization of 3DP molding technology in my country.

In the present invention, the superfine powder material can reach the submicron level or even nanometer level by surface dispersion modification of the powder material, and the powder material with uniform particle size is obtained; starting from the formula of powder modification, the obtained powder material can It can be formed directly under pressure without spraying adhesive, which greatly simplifies the procedure. The obtained product not only has high strength, but also makes it possible to realize the molding of thin-walled tiny parts on a 3DP rapid prototyping machine; in addition, the method provided by this patent is simple and low in cost.

Contents of the invention

The purpose of the present invention is to provide a preparation method for three-dimensional printing rapid prototyping powder material, rapid prototyping powder can be directly molded without spraying binder;

The purpose of the present invention is achieved through the following technical solutions.

A preparation method for three-dimensional printing rapid prototyping powder material, characterized in that the method has the following process steps:

(1) Powder material pretreatment: In the grinder, add 4%~12% of 3-aminopropyltriethoxysilane according to the mass percentage concentration, add 88%~96% of powder material, the The sum is 100%, turn on the grinder at a speed of 500~1000 rpm, grind at room temperature for 2~6 hours, and obtain the pretreated powder material;

(2) Preparation of rapid prototyping powder materials: In the reactor, add 50%~70% water according to the mass percentage concentration, add 0.5%~1.0% polyoxyethylene lauryl ether, stir to dissolve, and then add 2%~10% After heating to dissolve the polyvinyl alcohol, add 25%~40% pretreatment powder material, the sum of each component is 100%, stir and mix evenly, put it into a grinder, mix and grind at room temperature for 10~15 hours, and then Spray drying to obtain rapid prototyping powder material, the particle size of the obtained rapid prototyping powder material is in the range of 200~600nm;

The powder material described in step (1) is alumina, silicon carbide, zirconia, ceramic powder, and the particle size of the powder material is within the range of 100-500nm;

In the spray drying described in step (2), the inlet air temperature is controlled within the range of 120-180°C.

The particle size test method of the present invention is the particle size equivalent diameter measured by a laser particle size analyzer.

Another object of the present invention is to provide a kind of application that is used for the molding of three-dimensional printing rapid prototyping powder material on three-dimensional printer. In the X and Y directions of the horizontal plane (the X and Y directions represent the horizontal and vertical directions of the horizontal plane, respectively), and then descend to a certain height in the vertical Z direction of the plane. Then spread the rapid prototyping powder material on the next layer, and repeat this process. After all the materials are added, the temperature rises to 85~100℃, and the pressure can be directly formed within the range of 1MPa~10MPa.

Compared with the prior art, the present invention has the following advantages and beneficial effects:

(1) The rapid prototyping powder material obtained by the present invention does not need to be sprayed with binder, and can be directly formed by heating at 85-100°C and pressure within the range of 1MPa-10MPa.

(2) The present invention obtains a rapid prototyping powder material, the particles can reach submicron or even nanometer level, and has the characteristics of small median diameter, narrow particle size distribution range, and stable properties; thin-walled models can be manufactured from this rapid prototyping powder material Or small parts, the manufactured products have the characteristics of high surface gloss, good strength and high precision.

(3) The rapid prototyping powder material obtained by the present invention has the advantages of simple preparation process, easy control of conditions, low production cost, and easy industrial production.

(4) The rapid prototyping powder material obtained by the present invention can be effectively prototyped on a three-dimensional printer, and can be applied to various types of three-dimensional printers.

Detailed ways

Example 1

(1) Pretreatment of silicon carbide powder materials: In the grinder, add 7g of 3-aminopropyltriethoxysilane, add 93g of silicon carbide, turn on the grinder at 1000 rpm, grind at room temperature for 4 hours, Obtain pretreated silicon carbide powder material;

(2) Preparation of rapid prototyping silicon carbide powder material: In the reactor, add 60g of water, add 0.8g of polyoxyethylene lauryl ether, stir to dissolve, then add 6g of polyvinyl alcohol, heat to dissolve, add 33.2g The pretreated silicon carbide powder material was stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 12 hours, and then spray-dried to obtain a rapid prototyping silicon carbide powder material.

Example 2

(1) Pretreatment of silicon carbide powder materials: In the grinder, add 12g of 3-aminopropyltriethoxysilane, add 88g of silicon carbide, turn on the grinder at a speed of 500 rpm, and grind at room temperature for 6h to obtain Pretreatment of silicon carbide powder materials;

(2) Preparation of rapid prototyping silicon carbide powder material: In the reactor, add 66.5g of water, add 0.5g of polyoxyethylene lauryl ether, stir to dissolve, then add 8g of polyvinyl alcohol, heat to dissolve, add 25g The pretreated silicon carbide powder material was stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 10 h, and then spray-dried to obtain a rapid prototyping silicon carbide powder material.

Example 3

(1) Pretreatment of silicon carbide powder material: In the grinder, add 4g of 3-aminopropyltriethoxysilane, add 96g of silicon carbide, turn on the grinder at 800 rpm, grind at room temperature for 5 hours, and get Pretreatment of silicon carbide powder materials;

(2) Preparation of rapid prototyping silicon carbide powder material: In the reactor, add 50g of water, add 1.0g of polyoxyethylene lauryl ether, stir to dissolve, then add 10g of polyvinyl alcohol, heat to dissolve, add 39g of The silicon carbide powder material was pretreated, stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 15 hours, and then spray-dried to obtain a rapid prototyping silicon carbide powder material.

Example 4

(1) Pretreatment of silicon carbide powder materials: In the grinder, add 10g of 3-aminopropyltriethoxysilane, add 90g of silicon carbide, turn on the grinder at a speed of 1000 rpm, and grind at room temperature for 2 hours. Obtain pretreated silicon carbide powder material;

(2) Preparation of rapid prototyping silicon carbide powder material: In the reactor, add 70g of water, add 1.0g of polyoxyethylene lauryl ether, stir to dissolve, then add 2g of polyvinyl alcohol, heat to dissolve, add 27g of The silicon carbide powder material was pretreated, stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 14 hours, and then spray-dried to obtain a rapid prototyping silicon carbide powder material.

Example 5

(1) Pretreatment of aluminum oxide powder material: In the grinder, add 7g of 3-aminopropyltriethoxysilane, add 93g of aluminum oxide, turn on the grinder at 500 rpm, room temperature Grind for 4 h to obtain pretreated aluminum oxide powder material;

(2) Preparation of aluminum oxide powder material for rapid prototyping: In the reactor, add 60g of water, add 0.8g of polyoxyethylene lauryl ether, stir to dissolve, then add 6g of polyvinyl alcohol, heat to dissolve, add 33.2g of the pretreated aluminum oxide powder material was stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 12 hours, and then spray-dried to obtain a rapid prototyping aluminum oxide powder material.

Example 6

(1) Pretreatment of aluminum oxide powder material: In the grinder, add 10g of 3-aminopropyltriethoxysilane, add 90g of aluminum oxide, turn on the grinder at 800 rpm, room temperature Grind for 3 h to obtain pretreated aluminum oxide powder material;

(2) Preparation of aluminum oxide powder material for rapid prototyping: In the reactor, add 55g of water, add 1.0g of polyoxyethylene lauryl ether, stir to dissolve, then add 4g of polyvinyl alcohol, heat to dissolve, add 40g of pretreated aluminum oxide powder material was stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 11 h, and then spray-dried to obtain rapid forming aluminum oxide powder material.

Example 7

(1) Pretreatment of zirconia powder material: In the grinder, add 7g of 3-aminopropyltriethoxysilane, add 93g of zirconia, turn on the grinder at 1000 rpm, and grind at room temperature for 4 h, obtaining pretreated zirconia powder material;

(2) Preparation of rapid prototyping zirconia powder material: In the reactor, add 60g of water, add 0.8g of polyoxyethylene lauryl ether, stir to dissolve, then add 6g of polyvinyl alcohol, heat to dissolve, add 33.2 g of pretreated zirconia powder material, stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 12 h, and then spray-dried to obtain rapid prototyping zirconia powder material.

Example 8

(1) Pretreatment of zirconia powder material: In the grinder, add 9g of 3-aminopropyltriethoxysilane, add 91g of zirconia, turn on the grinder at a speed of 500 rpm, and grind at room temperature for 5 h, obtaining pretreated zirconia powder material;

(2) Preparation of rapid prototyping zirconia powder material: In the reactor, add 65g of water, add 0.5g of polyoxyethylene lauryl ether, stir to dissolve, then add 5g of polyvinyl alcohol, heat to dissolve, add 29.5 g of pretreated zirconia powder material, stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 13 h, and then spray-dried to obtain rapid prototyping zirconia powder material.

Example 9

(1) Pretreatment of ceramic powder materials: In the grinder, add 7g of 3-aminopropyltriethoxysilane, add 93g of ceramic powder, turn on the grinder at 800 rpm, grind at room temperature for 4 hours, and get Pretreatment of ceramic powder materials;

(2) Preparation of rapid prototyping ceramic powder materials: In the reactor, add 60g of water, add 0.8g of polyoxyethylene lauryl ether, stir to dissolve, then add 6g of polyvinyl alcohol, heat to dissolve, add 33.2g of Pretreat the ceramic powder material, stir and mix evenly, put it into a grinder, mix and grind at room temperature for 12 hours, and then spray dry to obtain a rapid prototyping ceramic powder material.

Example 10

(1) Pretreatment of ceramic powder materials: In the grinder, add 11g of 3-aminopropyltriethoxysilane, add 89g of ceramic powder, turn on the grinder at 1000 rpm, grind at room temperature for 2 hours, and get Pretreatment of ceramic powder materials;

(2) Preparation of rapid prototyping ceramic powder materials: In the reactor, add 65g of water, add 0.5g of polyoxyethylene lauryl ether, stir to dissolve, then add 4.5g of polyvinyl alcohol, heat to dissolve, add 30g of The ceramic powder material is pretreated, stirred and mixed evenly, put into a grinder, mixed and ground at room temperature for 15 hours, and then spray-dried to obtain a rapid prototyping ceramic powder material.

Method of use: Take the rapid prototyping powder material synthesized in the example and place it on the three-dimensional printing rapid prototyping machine, in the X and Y directions of the horizontal plane of the evenly spread rapid prototyping powder material (the X and Y directions represent the horizontal and vertical directions of the horizontal plane respectively) , and then descend to a certain height in the vertical Z direction of the plane. Then spread the rapid prototyping powder material on the next layer, and repeat this process. After all the materials are added, the temperature rises to 85~100℃, and the pressure can be directly formed within the range of 1MPa~10MPa. The obtained product has high pressure resistance and good gloss.

Claims (5)

1. for a preparation method for rapid three dimensional printing forming powdered material, it is characterized in that, the method has following processing step:

(1) powdered material pre-treatment: in shredder, add 4% ~ 12% APTES by mass percentage concentration, add 88% ~ 96% powdered material, each component sum is absolutely, open shredder rotating speed at 500 ~ 1000 revs/min, grinding at room temperature 2 ~ 6 h, obtain pre-treatment powdered material;

(2) rapid shaping powdered material preparation: in reactor, add 50% ~ 70% water by mass percentage concentration, add 0.5% ~ 1.0% polyoxyethylene laurel ether, stirring and dissolving, add again 2% ~ 10% polyvinyl alcohol, after heating is dissolved it, add 25% ~ 40% pre-treatment powdered material, each component sum is absolutely, is uniformly mixed, and puts into shredder, normal temperature mixed grinding 10 ~ 15 h, then spraying is dry, obtains rapid shaping powdered material, and the particle diameter of the rapid shaping powdered material obtaining is within the scope of 200 ~ 600nm.

2. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: described powdered material is alchlor, silicon carbide, zirconium dioxide, ceramics powder.

3. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: the particle diameter of described powdered material is within the scope of 100 ~ 500nm.

4. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: dry in the spraying described in step (2), inlet temperature is controlled within the scope of 120 ~ 180 DEG C.

5. the rapid shaping powdered material of preparing according to claim 1 application in moulding on three-dimensional printer.