CN112759298A - Material for powder 3D printing test model and preparation method thereof - Google Patents

Material for powder 3D printing test model and preparation method thereof Download PDF

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CN112759298A
CN112759298A CN202110004608.1A CN202110004608A CN112759298A CN 112759298 A CN112759298 A CN 112759298A CN 202110004608 A CN202110004608 A CN 202110004608A CN 112759298 A CN112759298 A CN 112759298A
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powder
printing
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test
quartz sand
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CN112759298B (en
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刘雄飞
马国伟
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Hebei University of Technology
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/04Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
    • B33Y70/10Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034Physico-chemical characteristics of the mixtures
    • C04B2111/00181Mixtures specially adapted for three-dimensional printing (3DP), stereo-lithography or prototyping
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00991Uses not provided for elsewhere in C04B2111/00 for testing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention provides a material for a powder 3D printing test model and a preparation method thereof, wherein the material is prepared from the following materials: magnesium phosphate cement, a spreadability adjusting component, a cohesiveness adjusting component and a reinforcing component. The material has the characteristics of good forming strength, high condensation speed, high early strength, high printing precision and the like, can greatly improve the problem that the conveying, spraying and building processes of powder and liquid materials in the 3D printing of the traditional portland cement material and powder are difficult to adapt, can manufacture a cement space bracket structure with good mechanical property and printing precision, meets the requirements of copying and controlling a physical test model with a complex structure, effectively combines various mechanism researches with a test verification method, further verifies the reliability of a mechanism theory, and has a good application prospect.

Description

Material for powder 3D printing test model and preparation method thereof
Technical Field
The invention relates to a material for a powder 3D printing test model and a preparation method thereof, belonging to the field of novel building materials. The novel building material for the powder 3D printing test model is high in strength, high in stability, simple, convenient and quick in process and capable of being mechanically operated, and a reproducible and controllable physical test model can be flexibly printed. Compared with common energy consumption materials and traditional finite element simulation calculation methods, the method has the advantages of high strength, high toughness, intellectualization, high accuracy, high stability, flexible control of test model parameters, repeatable test verification and the like, meets the intelligent market requirements of various mechanism test researches, and has wide application prospects.
Background
The 3D printing technology is also called additive manufacturing technology, is born in the middle and later stages of the 20 th century and the 80 th era, is a technology which is opposite to a traditional material removing and processing method, is based on a three-dimensional digital model, and combines materials by using a layer-by-layer manufacturing mode by using adhesive materials such as powdered metal or plastic and the like, has great development potential in the current building field, the powdered 3D printing is a new emerging printing technology, and the printing materials are key influence factors influencing the development of the printing technology.
The powder material needs to be selected from materials which can be rapidly molded and have good moldability, at present, the mature application in 3D model printing is gypsum powder, which is the first material widely used for 3D powder printing, but the gypsum material mainly depends on import and is expensive, while the cement material is the main material in the current building, the invention focuses on the powder 3D printing cement material, but the cement material used in the current powder 3D printing generally has the problems of poor performance, low product strength, low printing precision and the like.
Magnesium Phosphate Cement (MPC) is a novel hydraulic cementing material formed by reburning MgO, phosphate, retarder and functional components, obtains strength through chemical reaction between magnesium oxide and phosphate, has the characteristic of chemically bonded ceramics, has the advantage of early strength and quick setting, can have demolding strength after placing a pouring test piece in air and curing for 3 hours, and can reach 40-60 MPa in 7 days. If the application of the magnesium phosphate cement in the 3DP printing technology is realized, the manufacturing cost of the model can be obviously reduced. However, most of the existing powder 3D printing materials are gypsum-based materials, and a small amount of geopolymer and ordinary portland cement are used, and these materials cannot meet the requirements of the 3D printing process on the performances of the materials, such as printability, spreadability, forming strength and the like, and the research on the application of quick-hardening cement, such as magnesium phosphate cement-based materials, in powder 3D printing is insufficient.
Due to the limitation of the prior art and materials, refined model tests cannot be performed in many fields in civil engineering, for example, research means in the field of geotechnical engineering mainly include theoretical research, numerical simulation and physical model tests. The theoretical method can only provide a theoretical solution of a stress field and a displacement field for engineering with simple configuration; a large number of theoretical assumptions are needed in numerical calculation, and a calculation model and the accuracy of the calculation model need to be verified; physical model tests can simulate more geological formations and more complex geological engineering in one model, avoiding mathematical and mechanical difficulties. If a controllable and reproducible model can be developed, the catastrophe mechanism of the complex geological structure under different working conditions can be researched, and the research result of regularity is obtained. At present, a three-dimensional complex geological structure model based on rock-like materials cannot be manufactured by manufacturing a physical model, and how to accurately and finely simulate the structural characteristics of a rock mass is an unsolved problem.
Disclosure of Invention
In order to solve the existing problems, break through the existing limitations, and fully utilize the excellent properties of fast hardening, early strength, high adhesion, small shrinkage performance and the like of magnesium phosphate cement, the invention aims to provide a material for a powder 3D printing test model and a preparation method thereof, which can meet the requirements of the performances of powder 3D printing printability, spreadability, forming strength and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the material for the powder 3D printing test model comprises a powder material and a binder, and is characterized in that the powder material comprises: phosphate material component, quartz sand, PVA, mineral admixture component and fiber reinforcement component;
the particle fineness of the phosphate material component is not more than the thickness of the 3D printing layer and is more than the particle fineness of the quartz sand;
the maximum particle size of the quartz sand is not more than 0.1mm, the minimum particle size is 0.03mm, and the quartz sand is distributed in a grading mode and accounts for 25-30% of the total mass of the powder;
the particle fineness of the PVA is smaller than that of the phosphate material component, and the PVA accounts for 3-8% of the total mass of the powder;
the particle fineness of the mineral admixture component is smaller than that of quartz sand and accounts for 5-10% of the total mass of the powder;
the fiber reinforced component accounts for 0.1-0.3% of the total mass of the powder.
The binder consists of 1, 2-propylene glycol, glycerol and water, wherein the 1, 2-propylene glycol and the glycerol account for 3-8% of the total mass of the binder, so that more water can be ensured to exist under the condition of sufficient viscosity, and the later-stage powder spreading and printing are facilitated.
The phosphate material comprises the following components: calcining MgO at 1600-; ammonium dihydrogen phosphate; the phosphate material component is obtained by ball milling natural dried dead burned MgO and ammonium dihydrogen phosphate for 20min at the rotating speed of 1100r by a planetary ball mill according to the mass ratio of 59:41, and the particle fineness is 150 meshes.
The quartz sand is a spreading adjusting component and is obtained by ball milling for 20min at the rotating speed of 1100r by a planetary ball mill, and the particle fineness is 200 meshes.
A bonding adjustment component: the bonding adjusting components comprise 1,2 propylene glycol, glycerol and polyvinyl alcohol (PVA), the 1,2 propylene glycol and the glycerol are used in the preparation of the bonding agent, the 2 liquids can improve the viscosity of the liquid, so that the bonding agent can be better sprayed out of a printing spray head, the ratio of the liquid to the bonding agent accounts for 3% -8% of the total mass of the bonding agent, the bonding agent is set according to the requirements of printing parameters, and the rest components in the bonding agent are water; the polyvinyl alcohol (PVA) is used in the preparation of powder materials, has good cohesive force, the cohesive strength is increased along with the increase of alcoholysis degree and polymerization degree, the PVA is 17-88 type, the particle fineness is 200 meshes, the proportion is 3% -8% of the total mass of the powder, the PVA has auxiliary cohesive action, the water consumption is relatively low, and the PVA is suitable for powder printing.
Mineral admixture component: the mineral admixture component is one or more of fly ash and silica fume, the particle fineness of the mineral admixture component is 325 meshes, the mineral admixture component is finer, and the mineral admixture component accounts for 5% -10% of the total mass of the powder;
the fiber reinforced component is a carbon nano tube, the length of the carbon nano tube is 7-30 mu m, the weight percentage of the carbon nano tube is 0.1-0.3 percent of the total mass of the powder, the wave-absorbing requirement can be met, and the adhesion is not easy to occur.
The invention also provides a preparation method of the material for the powder 3D printing test model, which comprises the following steps:
powder material: adding the dead burned MgO and ammonium dihydrogen phosphate into a stirrer, and stirring for 2-4 minutes; then, adding the quartz sand, the mineral admixture and PVA powder in the proportion, and continuing stirring for 1-3 minutes; finally, adding a fiber reinforced component, and stirring for 2-5 minutes to obtain a powder material for the powder 3D printing test model;
liquid material: adding weighed 1, 2-propylene glycol and glycerol into distilled water, and ultrasonically vibrating at 50Hz for 3 min;
adding the prepared powder material for the powder 3D printing test model into a powder feeding bin of a printer, and adding a liquid material into a printing ink box; printing by a powder 3D printing technology, printing a molded test piece according to 0.1mm of each layer, wherein the ink-jet height is 4-15mm, the printing speed is 6-10cm/s, the molded test piece is maintained in an outdoor environment for 7D to obtain the material for the test model, and the strength meets the test requirements.
The above preparation method enables to obtain a maximum model size of 1000 × 650 × 600 mm. The preparation method can be used for printing circular ring curved surface characteristic test pieces, fence test pieces, cuboid test pieces, crack structure test pieces and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the model material can be used for printing a powder 3D printing physical experiment model, and can prepare a repeatable and controllable powder 3D printing physical experiment model. The rapid-hardening early-strength cement material magnesium phosphate cement is utilized, and the spreading performance and the permeability of the material are improved by adding PVA (polyvinyl alcohol), so that the cement-based material has certain forming strength and printing precision to achieve the effect of printing in a powder printer, and the material has good forming strength, high printing precision and high apparent precision.
2. The material can be used for model printing with high precision requirements, such as the manufacture of complex fractured rock mass models, the printing precision is at least ensured to be 0.5mm, and the PVA which is a material component with good film forming property is adopted in the application, so that the permeability (penetration depth and penetration diameter) of the binder on the powder can be well regulated and controlled, and thus, the good printing precision and apparent precision are obtained; the material forming strength is high, the powder can be removed after 2min of printing, even the printed test piece can be taken out from the printer after 1min, and the phenomena of fragmentation and fracture surface can not occur.
3. The Magnesium Phosphate Cement (MPC) is successfully used in powder 3D printing, the MPC has excellent characteristics of early strength, quick setting and the like, compared with other cements such as silicate and the like, the early strength and the quick setting performance of the MPC meet the requirements of quick hardening, early strength and high bonding of materials required in the powder 3D printing technology, the powder can be printed for several minutes, the setting speed is quick setting, the setting can be carried out within half minute, the setting time can be controlled within a range from half minute to 20 minutes by adding a retarder, the setting can be carried out quickly in winter even 10 minutes, particularly, the magnesium ammonium phosphate cement can be selected to be quickly set, the magnesium phosphate cement is not easy to crack after maintenance, the structure of a finished product is taken out completely, the water consumption is low, and the MPC is very. The early strength 1d of the pouring piece can reach 27MPa, and the powder removing strength can be reached after the pouring piece is printed for 1 min.
4. The quartz sand with the grain diameter of 30-75 mu m and grading distribution is added into the material composition, so that the spreading performance and the printing performance of the powder material can be effectively improved; meanwhile, PVA is added to adjust permeability and film forming property, fly ash or silica fume is used for improving water resistance, and the added carbon nano tube is used for improving strength. The powder formed by the specific particle sizes has a synergistic effect, so that the application of the magnesium phosphate cement in powder 3D printing can be realized, and the printing precision and the apparent precision are high. The particle size screening of the material must be well controlled, because the powder 3D printing technology generally has a layer thickness of about 0.1mm, a 200-mesh sieve is required when the material, namely quartz sand, is prepared, because the 200-mesh sieve is 0.075mm, and other materials at least need to pass through the 0.1mm sieve, so that the material can be used in the powder 3D printing, the small particle size of the quartz sand can fill the pores between the materials, and the material is relatively compact. The quartz sand after ball milling is selected to be between 0.03mm and 0.075mm, if the quartz sand is too thin, the problem of agglomeration can occur, the powder is not favorable for spreading, and if the quartz sand is too thick, the phenomenon that the particle diameter is larger than the layer thickness and each layer is not good for spreading can be caused. The powder spread was continuous with the addition of the quartz sand within the ranges given in this application, with no intermittent "step effect".
5. The viscosity adjusting component adopts 17-88 type PVA which has high viscosity after being dissolved in water, and can well realize the layer-to-layer adhesion and improve the interlayer adhesion performance of a test piece. 17-88 first 17 represents an average degree of polymerization of 1700-1800 and 88 represents a degree of alcoholysis of 88%. + -. 2%. The water solubility of the polyvinyl alcohol is greatly different according to the alcoholysis degree, the product with the alcoholysis degree of 87-89% has the best water solubility, can be quickly dissolved in both cold water and hot water and shows the maximum solubility, so the alcoholysis degree is about 88; along with the increase of polymerization degree, molecular chains of PVA grow, the acting force between molecules is enhanced, the entanglement is increased, the water solubility of the PVA is gradually reduced, the viscosity of the solution is increased, and therefore 1700-1800 with medium average polymerization degree is selected, and the 17-88 type PVA is selected. Besides the advantage of high viscosity, PVA is selected by combining the characteristics of PVA and the specificity of the powder 3D printing technology because PVA has excellent film forming property which can prevent excessive penetration and rolling of a binder on powder, thereby improving the precision of powder 3D printing.
6. The introduction of the admixture of the fly ash and the silica fume mineral effectively improves the water resistance of the magnesium phosphate cement, so that a printed test piece can be subjected to steam curing, and the strength of the test piece is improved.
7. The carbon nanotube of the invention has the length of 7-30 μm, can improve the strength of the test piece and can also improve the wave-absorbing performance of the test piece.
Compared with the traditional powder 3D printing materials such as gypsum, geopolymer and the like, the Magnesium Phosphate Cement (MPC) material prepared by the method can realize early-strength and fast-setting printing effects and has high printing precision.
According to the best formula, for example 1, the compressive strength can reach 27MPa after curing for 7d, the gypsum-based material can only reach about 0.7MPa, the molding strength of a test piece printed by the material is better, the powder can be removed after printing for 2min, even the printed test piece can be taken out from a printer after 1min, the phenomena of fragmentation and fracture surface cannot occur, and the gypsum-based material can be subjected to powder removal operation after being placed for more than half an hour; the crack images show that 4 cracks with the widths of 0.1mm, 0.3mm, 0.5mm and 0.8mm are printed, powder cannot be removed when the crack images are 0.1mm, only surface powder can be removed when the crack images are 0.3mm, powder can be removed when the crack images are 0.5mm, the crack printing with the width of 0.5mm can be met, the cracks are communicated, the apparent precision is good after the powder is removed from the ring model, the apparent precision is high for a test piece printed by geopolymer powder 3D, and the surface of the test piece printed by geopolymer has obvious particles. The invention can print the test piece with the characteristics of the circular ring curved surface, and has higher precision and strength than the existing gypsum-based powder printing test piece, especially geopolymer powder printing test piece. The method meets the requirements of complex structure physical test model reproducibility and controllability, effectively combines various mechanism researches with test verification methods, further verifies the reliability of mechanism theory, and has good application prospect.
Drawings
FIG. 1 is a drawing of different types of powder 3D printed MPC coupons obtained in example 1 of the present invention.
Detailed Description
The present invention is further illustrated in detail below with reference to specific examples.
The material for the powder 3D printing test model is prepared from the following raw materials in parts by weight:
phosphate material composition: calcining MgO at 1600-; ammonium dihydrogen phosphate is analyzed and purified; the phosphate material component is obtained by ball milling natural dried dead burned MgO and ammonium dihydrogen phosphate for 20min at the rotating speed of 1100r by a planetary ball mill according to the mass ratio of 59:41, the particle fineness is 150 meshes and is not more than the thickness of a printed 3D layer;
spreading adjusting component: the spreadability adjusting component is quartz sand, is obtained by ball milling for 20min at the rotating speed of 1100r by a planetary ball mill, has the particle fineness of 200 meshes and the maximum particle size of 0.075mm (30-75 mu m), is distributed in a grading manner, reduces the porosity, has few impurities, does not change the acid-base environment of a system, and accounts for 25-30% of the total mass of the powder;
a bonding adjustment component: the bonding adjustment components comprise 1, 2-propylene glycol, glycerol and polyvinyl alcohol (PVA), the 1, 2-propylene glycol and the glycerol are used in the preparation of the bonding agent, the 2-liquid can improve the viscosity of the liquid, so that the bonding agent can be better sprayed out from a printing spray head, the bonding agent accounts for 3% -8% of the total mass of the bonding agent (the bonding agent consists of the 1, 2-propylene glycol, the glycerol and water), and the specific content can be set according to the requirement of printing parameters; the polyvinyl alcohol (PVA) is used in the preparation of powder materials, has good cohesive force, the cohesive strength is increased along with the increase of alcoholysis degree and polymerization degree, the used 17-88 type powder has the particle fineness of 200 meshes, the proportion is 3-8 percent of the total mass of the powder, the compressive strength is good, and the auxiliary cohesive effect is achieved;
mineral admixture component: the mineral admixture component is one or more of fly ash and silica fume, the particle fineness of the mineral admixture component is 325 meshes, and the mineral admixture component accounts for 5-10% of the total mass of the powder;
fiber reinforcement component: the fiber reinforced component is a carbon nano tube, the length of the carbon nano tube is 7-30 mu m, the wave absorbing requirement can be met, the carbon nano tube is too small and easy to adhere, and the carbon nano tube accounts for 0.1-0.3 percent of the total mass of the powder.
The raw materials used in the following examples are the same, only the mixing amount is different, the length of the carbon nanotube is 7 μm, and MgO is calcined at 1750 ℃ for 45 min; ammonium dihydrogen phosphate is analyzed and purified; the phosphate material component is formed by mixing natural dried dead burned MgO and ammonium dihydrogen phosphate according to the mass ratio of 59:41, and the particle fineness is 150 meshes after mixing; the mineral admixture component adopts fly ash, the particle fineness of the fly ash is 325 meshes, and the type of polyvinyl alcohol (PVA) is 17-88. The mass ratio of the 1, 2-propylene glycol to the glycerol in the adhesive is 1:1, and the total mass of the 1, 2-propylene glycol and the glycerol accounts for 5% of the total mass of the adhesive.
Comparative example 1
Drying and ball-milling 20% of quartz sand, wherein the ball-milling rotation speed is 1100r, the ball-milling time is 20min, and sieving the quartz sand by a 200-mesh sieve for later use; ball milling the dead burned magnesium oxide and ammonium dihydrogen phosphate at the ball milling rotation speed of 1100r for 20min, and sieving with a 150-mesh sieve for later use;
the dead burned magnesium oxide and the ammonium dihydrogen phosphate are mixed according to the mass ratio of 59:41, and finally adding 5 percent of 200-mesh polyvinyl alcohol, 5 percent of fly ash and 0.1 percent of carbon nano tube into a planetary mixer for mechanical stirring and mixing.
Comparative example 2
Drying and ball-milling 30% of quartz sand, wherein the ball-milling rotation speed is 1100r, the ball-milling time is 20min, and sieving the quartz sand by a 200-mesh sieve for later use; ball milling the dead burned magnesium oxide and ammonium dihydrogen phosphate at the ball milling rotation speed of 1100r for 20min, and sieving with a 150-mesh sieve for later use;
the dead burned magnesium oxide and the ammonium dihydrogen phosphate are mixed according to the mass ratio of 59:41, mixing; finally, 5% of 200-mesh polyvinyl alcohol, 15% of fly ash and 0.1% of carbon nano tube are added into a planetary mixer to be mechanically stirred and mixed.
Example 1
Drying and ball-milling 25% of quartz sand, wherein the ball-milling rotation speed is 1100r, the ball-milling time is 20min, and sieving the quartz sand by a 200-mesh sieve for later use; ball milling the dead burned magnesium oxide and ammonium dihydrogen phosphate at the ball milling rotation speed of 1100r for 20min, and sieving with a 150-mesh sieve for later use;
and (2) mixing the dead burned MgO sieved by the 150-mesh sieve with ammonium dihydrogen phosphate according to the mass ratio of 59:41, adding the mixture into a stirrer, and stirring for 3 minutes; then, adding 25% of quartz sand, 5% of fly ash and 5% of 200-mesh polyvinyl alcohol powder, and continuing stirring for 2 minutes; and finally, adding 0.1% of carbon nano tube, and stirring for 3 minutes to obtain the powder material for the powder 3D printing test model.
Liquid material: adding weighed 1, 2-propylene glycol and glycerol into distilled water, and ultrasonically vibrating at 50Hz for 3 min;
adding the prepared powder material for the powder 3D printing test model into a powder feeding bin of a printer, and adding a liquid material into a printing ink box; printing is carried out through a powder 3D printing technology, a formed test piece is printed according to 0.1mm of each layer, the ink-jet height is 10mm, the printing speed is 8cm/s, the formed test piece can be obtained after being maintained in the outdoor environment for 7D, and the strength meets the test requirements.
Example 2
The parts of this example were the same as example 1 except that the fly ash was added in an amount of 10% (wt).
Example 3
The present example is similar to example 1 except that the amount of carbon nanotubes added is 0.3% (wt).
Example 4
The present example was conducted in the same manner as example 1 except that the amount of silica sand added was 30 wt%.
Table 1: comparative examples 1-2 and examples 1-4 spreading and mechanical Properties
Name (R) Comparative example 1 Comparative example 2 Example 1 Example 2 Example 3 Example 4
Spreading performance Intermittent Intermittent (Continuous) (Continuous) (Continuous) (Continuous)
7d compressive strength/MPa 15 13 27 16 21 18
Experimental observation shows that the magnesium phosphate cement prepared in the embodiment 1 has the advantages of high setting speed, high early strength, high precision and good powder paving flatness, and meets the expected standards of experiments. Comparative example 1 the powder spreading performance was found to be seriously affected after the quartz sand content was reduced to 20%, but the early forming strength of the printed test piece was not greatly affected because the fly ash content was not very high; in comparative example 2, the content of quartz sand is increased to 30%, and the spreadability is continuous according to the proportion, but after the content of fly ash is increased to 15%, the spreading performance of powder is seriously affected, so that the precision of a printed test piece is reduced, the flatness of part of the printed test piece is reduced, the early molding strength is not enough, and the spreading performance is reduced, and the strength is the lowest; example 2, the content of the fly ash is increased to 10%, and it is found that the spreadability can be ensured, but the strength is reduced to a certain extent, and the strength requirement of a model material can be still met; example 3 increased the carbon nanotube content to 0.3%, and the compressive strength decreased compared to example 1, because the carbon nanotubes absorbed the water in the binder, and the water consumption for the powder hydration reaction was not sufficient, and the compressive strength decreased to some extent, but the spreadability and strength were still satisfactory under the formulation of example 3; in example 4, the content of the quartz sand was increased to 30%, and the other components were selected from the optimal solutions obtained in the above comparative tests, and it was found that the spreadability was continuously good, but the strength was somewhat reduced compared to example 1. By comparison, the formulation and materials used in example 1 were the best formulations for making a material for use in a powder 3D printing test model.
Example 5
The difference between the parts of this example and example 1 is that the mineral admixture component is selected to be silica fume, and the amount of silica fume added is 5%, so that the obtained model material can meet the requirement of continuous powder laying, and the 7d compressive strength is 21MPa which is relatively lower than that of example 1.
Example 6
The difference between each part of this example and example 1 is that the mineral admixture component is selected as a mixture of silica fume and fly ash, and the silica fume and fly ash are added according to a ratio of 1:1, so that the obtained model material can meet the 3D printing requirements.
The material for the model of the present application should eventually satisfy 3 basic properties: 1. continuity of powder laying; 2. the strength is not low, the 7d compressive strength reaches more than 10MPa, preferably 20-30MPa, powder falling does not occur, and printing and forming can be realized; 3. the precision is better, and the precision control is below 1mm, and the model material of printing is more accurate, is used for the crack preparation, and preferred precision 0.5 mm.
The preferred embodiments of the experiment have been described in detail, but the experiment is not limited to the details of the above embodiments, and it should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the experiment will not be described in detail in various possible combinations in order to avoid unnecessary repetition.
Nothing in this specification is said to apply to the prior art.

Claims (7)

1. The material for the powder 3D printing test model comprises a powder material and a binder, and is characterized in that the powder material comprises: phosphate material component, quartz sand, PVA, mineral admixture component and fiber reinforcement component;
the particle fineness of the phosphate material component is not more than the thickness of the 3D printing layer and is more than the particle fineness of the quartz sand;
the maximum particle size of the quartz sand is not more than 0.1mm, the minimum particle size is 0.03mm, and the quartz sand is distributed in a grading mode and accounts for 25-30% of the total mass of the powder;
the particle fineness of the PVA is smaller than that of the phosphate material component, and the PVA accounts for 3-8% of the total mass of the powder;
the particle fineness of the mineral admixture component is smaller than that of quartz sand and accounts for 5-10% of the total mass of the powder;
the fiber reinforced component accounts for 0.1-0.3% of the total mass of the powder.
2. The material for test patterns according to claim 1, wherein the binder is composed of 1,2 propylene glycol, glycerin and water, and the 1,2 propylene glycol and glycerin account for 3 to 8% by mass of the total mass of the binder.
3. The material for test patterns according to claim 1,
the phosphate material comprises the following components: calcining MgO at 1600-; ammonium dihydrogen phosphate; the phosphate material component is obtained by ball milling natural dried dead burned MgO and ammonium dihydrogen phosphate for 20min at the rotating speed of 1100r by a planetary ball mill according to the mass ratio of 59:41, and the particle fineness is 150 meshes;
the quartz sand is a spreadability adjusting component and is obtained by ball milling for 20min at the rotating speed of 1100r by a planetary ball mill, and the particle fineness is 200 meshes;
the PVA type is 17-88 type, and the particle fineness is 200 meshes;
the mineral admixture component is one or more of fly ash and silica fume, and the particle fineness is 325 meshes;
the fiber reinforced component is carbon nano tube with length of 7-30 μm.
4. A method for preparing a material for a powder 3D printing test model according to any one of claims 1 to 3, the method comprising the steps of:
powder material: adding the phosphate material components into a stirrer, and stirring for 2-4 minutes; then adding the quartz sand, the fly ash, the silica fume and the PVA powder in the proportion, and continuously stirring for 1-3 minutes; finally, adding the fiber reinforced component in the proportion, and stirring for 2-5 minutes to obtain a powder material for the powder 3D printing test model;
liquid material: adding weighed 1, 2-propylene glycol and glycerol into distilled water, and ultrasonically vibrating at 50Hz for 3 min;
adding the prepared powder material for the powder 3D printing test model into a powder feeding bin of a printer, and adding a liquid material into a printing ink box; printing by a powder 3D printing technology, printing a molded test piece according to 0.1mm of each layer, wherein the ink-jet height is 4-15mm, the printing speed is 6-10cm/s, and the molded test piece is maintained in an outdoor environment for 7D to obtain the material for the test model with the strength meeting the test requirements.
5. The method of claim 4, wherein the test pattern material has a pattern size of 1000 x 750 x 600mm3
6. The preparation method of claim 4, wherein the material for the test model can realize powder paving continuity, the 7d compressive strength is more than 10MPa, the printing precision is controlled below 1mm, preferably the precision is 0.5mm, and the material is used for manufacturing cracks.
7. The production method according to claim 4, wherein the method is applicable to printing of a toroidal surface property test piece, a fence test piece, a rectangular parallelepiped test piece, a fracture structure test piece.
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