CN117263718B - Foam ceramic similar material and preparation method, production device and application thereof - Google Patents

Foam ceramic similar material and preparation method, production device and application thereof Download PDF

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CN117263718B
CN117263718B CN202311191963.XA CN202311191963A CN117263718B CN 117263718 B CN117263718 B CN 117263718B CN 202311191963 A CN202311191963 A CN 202311191963A CN 117263718 B CN117263718 B CN 117263718B
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microwave
similar material
sintering
stirring
mixing
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CN117263718A (en
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张希巍
薛淳元
李广波
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Shandong Gold Mining Technology Co ltd Filling Engineering Laboratory Branch
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Shandong Gold Mining Technology Co ltd Filling Engineering Laboratory Branch
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    • 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
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Abstract

The invention provides a foam ceramic similar material, a preparation method, a production device and application thereof, comprising the following steps: (1) Uniformly mixing aggregate, cementing material and water to prepare suspension; (2) Heating and standing the suspension by microwaves, adding a nonionic surfactant, and uniformly mixing to obtain foaming slurry; (3) And after layering and printing the foaming slurry through a 3D printing module, pouring the foaming slurry into a visual microwave shielding box body to prepare the foam ceramic similar material. The invention has the advantages of easily obtained raw materials, simple method and capability of obtaining the foam ceramic similar material with excellent performance.

Description

Foam ceramic similar material and preparation method, production device and application thereof
Technical Field
The invention relates to the technical field of similar model tests, in particular to a foam ceramic similar material, a preparation method, a production device and application thereof.
Background
Deep tunnel/tunnel excavation unloading often induces high-intensity dynamic disasters, causes a large amount of casualties and great economic property loss, and becomes a key problem affecting the safe construction of tunnel/tunnel engineering. In order to simulate and monitor the deep engineering disaster inoculation process, a large-scale three-dimensional similar material physical model test is often used for carrying out related tests, and a physical model sample similar to an engineering rock mass is scaled down, so that the method is a solution based on a similarity theory. The preparation of the low-strength and high-brittleness material suitable for the physical model test is a precondition for researching deep hard rock engineering disasters.
At present, most of experimental researches are only to add cement cementing materials into common powdery aggregates (quartz sand, barite, bentonite, mine tailings, building solid wastes and the like) so as to increase the compressive strength of simulated similar materials, and the materials cannot realize the balance of low strength and high brittleness. At present, the three-dimensional physical model test is adopted to simulate rock burst, the loading mode is unreasonable, the excavation mode is not in accordance with the actual and other problems, so that the simulated rock burst phenomenon is almost indistinguishable from the conventional destruction phenomenon, and in order to break through the physical simulation test of rock burst, a brittleness similar criterion suitable for rock burst is firstly established, and a similar material with low strength and high brittleness is developed.
The foamed ceramic is a porous material which is prepared by taking minerals, pure substances or solid wastes as main raw materials and adding a proper amount of additives by adopting different preparation processes, and generally has the excellent characteristics of low strength, high brittleness, low density, high porosity, high temperature resistance, corrosion resistance, high thermal stability and the like, and has better association degree with a rock-soil similar model material. The existing foam ceramic preparation process generally adopts high-temperature sintering, the preparation of raw material ends is complex, and high-pressure curing is often required; the material is densified at a high temperature of more than 1000 ℃, so that the energy consumption is high and the cost is high; the pore diameter and the distribution of the product are difficult to control, and have great influence on the product performance.
Therefore, the material proportion is required to be optimized, the process route is improved, and the microwave cold sintering technology is innovated to adapt to the mechanical properties of similar foam ceramic materials, so that the simulation of the engineering characteristics of deep rock mass is realized.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation process of a cold-sintered foam ceramic similar material, which realizes multiple action coupling of ceramic hardening, cement bonding, foaming reaction, fiber fleece, cold sintering densification and the like through preferable material proportion, adopts a microwave cold sintering process, has excellent performance of low strength and high brittleness, optimally designs a microwave heating structure, innovates a pressureless mixed cold sintering process, simultaneously increases the slurry in-situ solidification function, improves the low-temperature heating densification efficiency, accelerates the gas expansion foaming effect, and realizes stable and efficient operation of similar material preparation.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A process for preparing the cold-sintered foam ceramic similar material includes such steps as preparing gold ore tailings and lithium-porcelain clay as aggregate, high-strength gypsum and cement as cementing material, adding water, stirring, mixing, adding a small amount of non-ionic surfactant, and adding aggregate: the content of the cementing material is controlled at 30: about 1, controlling the water content to be about 20% -28%, and optimally controlling the ratio of the gold mine tailings to the lithium porcelain clay to be 1:1, optimally controlling the ratio of the high-strength gypsum to the cement to be 1.5:1, the brittleness of the similar material is improved, and the strength of the material is reduced.
The preparation process of the cold-sintered foam ceramic similar material mainly has the following characteristics:
A key technology for microwave cold sintering of foamed ceramics. The invention firstly utilizes the two-section microwave auxiliary stirring foaming technology to stir and activate the first-section aggregate of the raw materials, and the second-section microwave stirring foaming is carried out, wherein the first-section aggregate stirring is used for homogenizing the aggregate and is uniform, and the low-speed stirring can further homogenize the incoming materials; the two-stage microwave stirring is foaming, heating and enhancing fluidity, and the foaming effect is better only after the former stage is uniformly stirred and then the high-speed stirring is carried out; the second section uses microwaves, so that the heating foaming effect is better, the cementing material is not in a slurry state before high-temperature sintering, the yield stress can be reduced to accelerate the flow due to proper heating, meanwhile, the microwave heating only needs an external microwave heating plate, the temperature conduction is uniform from inside to outside, and the effect is better than that of the traditional heating from outside to inside. Through two-stage stirring foaming, a biscuit with good microcosmic uniformity and higher density is obtained, and then the biscuit is printed and sintered simultaneously through a 3D printing module and a microwave heating module, so that the functions of in-situ pouring of a sample, in-situ rapid solidification of slurry, high-efficiency microwave cold sintering, microwave radiation prevention, multi-station continuous production and the like are realized, and the visualized shielding box body is optimally designed, so that the microwave radiation can be shielded, and the preparation process can be monitored in real time.
The ceramic material is suitable for microwave cold sintering. The invention selects gold mine tailings and clay as aggregate, has wide raw material sources and low cost, and is favorable for microcosmic densification, temperature reduction and sintering time reduction. The granularity of the gold ore tailings is similar to that of fine sand, and the gold ore tailings are economical and environment-friendly as substitutes of siliceous raw materials; the fluxing effect of the lithium porcelain stone is obvious, and the sintering temperature can be effectively reduced by adding a proper amount of the lithium porcelain stone. By matching the microwave cold sintering process, effective heat treatment is provided for mineral raw materials at lower temperature and sintering time, microwave energy is directly converted into heat in the material, and the internal and volume heating of the material is facilitated, so that temperature gradient and reverse heating flow are formed, physical properties equivalent to those of conventional sintering are obtained, and high thermal stress which can damage ceramics is not generated.
The pressureless microwave cold sintering preparation process. Pouring the foamed slurry into a visual shielding box body through a 3D printing module, marking each 10-50cm as a layer, continuously working the 3D printing module to print a second layer after the first layer is poured, presintering the first layer at a low temperature of 60-80 ℃ by a microwave heating module to promote rapid solidification of the slurry, stable expansion of foam and dissolution and precipitation of particles, then carrying out cold sintering for 1h within a temperature range of 250-300 ℃, heating at a rate of 10 ℃/min, promoting water evaporation, crystal growth and material densification, and repeating the steps to realize layered continuous sintering after the first layer sintering is completed. Compared with the traditional sintering process, the method has the advantages that the pressure is not needed to be dense, the high-temperature energy consumption is not needed, and the continuous, efficient, clean and environment-friendly mixed cold sintering process is realized.
A light, low-strength and high-brittleness functionally similar material. The invention has the excellent properties of low density, low strength and high brittleness, generates a compact porous gel structure through the foaming expansion effect, effectively reduces the density and the dead weight of the material, and is beneficial to the preparation and the transportation of the ultra-large similar material model; meanwhile, the proportion of the cementing material is optimized (the proportion of the cementing material in the prior art is approximately 5:1-10:1), so that the brittleness of similar materials is improved, and meanwhile, the strength of the materials is reduced; the microwave cold sintering technology promotes the particle densification, gas expansion foaming, clay hardening and cement hydration, accelerates the formation of the strength of the material, improves the brittleness of the material and reduces the density of the material.
A light-weight low-strength high-brittleness energy evaluation method. Before each test of printing similar material model, a batch of standard components with the thickness of 50mm multiplied by 100mm are required to be synchronously printed for performance test and evaluation, and firstly, density test is carried out to ensure that the density of a sample is in the range of 900-1200 kg/m 3; then, carrying out wave velocity test to ensure that the wave velocity of the sample is in the range of 1200-1600 m/s; then, carrying out uniaxial compressive strength test to ensure that the uniaxial strength of the sample is in the range of 1 MPa-3 MPa and the peak strain is between 0.1% and 1%; the cold-sintered foam ceramic similar material meeting the parameter requirements is beneficial to the preparation of a large-volume similar material model, and the obtained product has the excellent properties of low density, low strength, high brittleness and high heat resistance.
The invention has at least the following beneficial effects:
① The raw materials are cheap and easy to obtain, and the finished product has the excellent properties of low density, low strength and high brittleness; ② The multi-station continuous and accurate preparation is simple and easy, and the period is short; ③ In-situ microwave assisted rapid hardening and solidification are carried out, so that a biscuit with good microcosmic uniformity and higher density is obtained; ④ The microwave cold sintering process reduces energy consumption and cost; ⑤ The pressureless mixed sintering process controls the foaming efficiency and microstructure.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process route diagram for the preparation of materials according to the present invention.
FIG. 2 is a schematic diagram showing the operation of the microwave heating sample preparation device of the present invention.
FIG. 3 is a graph of performance versus moisture content for different bone cement ratios of the present invention.
FIG. 4 is a graph showing the comparison of the properties of the ceramic foam material obtained in example 1 of the present invention with conventional three-dimensional ceramic foam materials.
In the figure, 1-gold mine tailings and lithium porcelain clay aggregates; 2-collecting hoppers; 3-a weighing feeder; 4, water sump; 5-a metering pump; 6-cementing bin; 7-a double-tube spiral weighing feeder; 8-a first-level aggregate activation stirring barrel; 9-a secondary microwave foaming mixer; 10-a visual shielding box body; 11-3D printing module; 12-a microwave heating module.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
As shown in fig. 1-4, the preparation process of the cold-sintering foam ceramic similar material comprises the steps of selecting gold mine tailings and lithium porcelain stone clay as aggregate, taking high-strength gypsum and cement as cementing materials, adding water, stirring and mixing, and adding a small amount of nonionic surfactant, wherein the aggregate comprises the following components: the content of the cementing material is controlled at 30:1, controlling the water content to be 24wt%, and controlling the ratio of gold mine tailings to lithium porcelain clay to be 1:1, controlling the proportion of the high-strength gypsum to the cement to be 1.5:1, the brittleness of the similar material is improved, and the strength of the material is reduced.
The invention comprises a microwave heating sample preparation device, which mainly comprises a visual shielding box body 10, a microwave heating module 12 and a 3D printing module 11, wherein the bottom of the visual shielding box body 10 is a metal plate, and the other five surfaces are toughened glass shielding plates with metal grids, so that the microwave heating sample preparation device can shield microwave radiation and monitor the preparation process in real time; the microwave heating module 12 slides up and down in the vertical direction of the box body by virtue of the sliding block, and is provided with four microwave heating plates which move synchronously, so that the microwave heating modules can be sintered step by step along with the printing progress; the 3D printing module 11 is inlaid under the upper shielding plate, can move vertically with the upper shielding plate, and can also move freely in the horizontal plane of the upper shielding plate.
Because the microwave shielding box body around is motionless, upper shield plate because the promotion of high needs to remove, consequently with 3D printing module synchronous motion can guarantee the cavity integrality.
The device provided by the invention realizes the functions of in-situ pouring of a sample, in-situ rapid solidification of slurry, efficient microwave cold sintering, microwave radiation prevention and multi-station continuous production.
The preparation method comprises the following steps:
1. the method comprises the steps of collecting gold mine tailings and lithium porcelain clay aggregate 1 which are piled up in a dry mode through a collecting hopper 2, and then throwing the aggregate into a primary aggregate activation stirring barrel through a weighing feeder 3;
2. The outlet of the water sump 4 is connected with the metering pump 5, so that the water quantity entering the primary aggregate activation stirring barrel 8 can be accurately controlled, the concentration in the primary aggregate activation stirring barrel 8 is accurately controlled, and the flushing work of the stirring barrel after feeding can be completed through the water sump pipeline.
3. The high-strength gypsum and cement are used as cementing materials, a small amount of nonionic surfactant is added, the cementing materials are stored in a cementing bin 6 after being proportioned, a level gauge is arranged in the cementing bin for real-time detection and measurement, the proportioning is controlled by a plate gate valve, and the cementing materials are uniformly added into a primary aggregate activation stirring barrel 8 according to the preset proportioning after being conveyed and measured by a double-pipe spiral weighing feeder 7;
4. in the primary aggregate activation stirring barrel 8, quartz sand and barite powder aggregate, water, high-strength gypsum and cement binder aggregate and the mixture are stirred at a low speed (500 rpm) according to a set mortar-sand ratio, promoting alkaline activation:
5. The obtained suspension was added to a secondary microwave foaming mixer 9, the suspension was first allowed to stand and solidify for 2 hours under microwave low temperature heating (75 ℃), then a nonionic surfactant (0.2 wt%) was added, and the partially hardened suspension was foamed by high speed mechanical stirring (2000 rpm);
6. pouring the foamed slurry into a visual shielding box 10 through a 3D printing module 11, marking each 50cm as one layer, continuing to work the 3D printing module to print a second layer after the first layer is poured, and heating the first layer at a low temperature of 60-80 ℃ by a microwave heating module 12 to promote rapid solidification of the slurry, stable expansion of foam and dissolution and precipitation of particles;
7. Then cold sintering is carried out for 1h at the temperature of 280 ℃, the heating rate is 10 ℃/min, the evaporation of water, the growth of crystals and the densification of the material are promoted, and the sintering of the first layer is completed.
And (3) repeating the steps 6 and 7 to realize layered continuous sintering until the preparation of the cold-sintered foam ceramic material is completed.
As can be seen from fig. 3, by studying the properties of the obtained material under different bone cement ratios and different water contents, it can be found that the bone cement ratio has a positive correlation with the uniaxial compressive strength of the material, and that the larger the bone cement ratio is, the higher the uniaxial compressive strength is, and the water content has a negative correlation with the uniaxial compressive strength of the material, and the smaller the water content is, the higher the uniaxial compressive strength is.
Example two
The other is the same as the first embodiment except that: (1) The two-section stirring is changed into one-section stirring, the suspension is not prepared and the suspension is heated by microwave, namely, quartz sand, barite powder aggregate, water, high-strength gypsum, cement cementing material and nonionic surfactant are mixed and stirred at high speed according to a set lime-sand ratio in a primary aggregate activation stirring barrel; (2) In the layering continuous sintering process, the 3D printing module directly performs cold sintering without low-temperature heating after printing, namely, the 3D printing module continuously works to print the second layer after the first layer is poured, and the microwave heating module 12 performs cold sintering on the first layer within the temperature range of 280 ℃.
Meanwhile, in order to illustrate the superior properties of the foamed ceramic material obtained by the invention, quartz sand is taken as aggregate, gypsum and cement are taken as cementing materials, and the conventional three-dimensional similar material is prepared by a conventional method (i.e. without foaming and sintering) according to the raw material proportion of the foamed ceramic material. Similar materials ideal in the art should be characterized by high brittleness (simulating small rock peak strain), low strength (matching existing low loading capacity), low density (ease of transportation), low wave speed (rapid prediction of other properties by non-destructive testing).
Comparing the performance of the cold-sintered foam ceramic material obtained in the example 1 with that of a conventional three-dimensional similar material, the density, the wave velocity, the uniaxial strength and the peak strain of the material obtained in the invention are all obviously lower than those of the existing material, which proves that the material obtained in the invention has more excellent performance.
Comparing the materials obtained in the first and second embodiments, it was found that the change of foaming mode and sintering process resulted in uneven pore distribution, higher density, higher strength, higher peak strain, and the material was similar to plastic material rather than brittle, and the performance was deteriorated in all aspects.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (6)

1. The preparation method of the foam ceramic similar material is characterized by comprising the following steps of:
(1) Uniformly mixing aggregate, cementing material and water to prepare suspension;
The aggregate is gold mine tailings and lithium porcelain stones, and the mass ratio of the gold mine tailings to the lithium porcelain stones is 2:3-3:2;
(2) Heating and standing the suspension by microwaves, adding a nonionic surfactant, and uniformly mixing to obtain foaming slurry;
(3) After layering and printing the foaming slurry through a 3D printing module, pouring the foaming slurry into a visual microwave shielding box body to prepare a foam ceramic similar material;
Wherein:
in the step (1), the cementing material is selected from high-strength gypsum and cement, and the mass ratio of the high-strength gypsum to the cement is 1:1-2:1; the mass ratio of the aggregate to the cementing material is 20:1-40:1;
In the step (2), the temperature of microwave heating is 70-80 ℃, and the standing time is 1.5-2 hours;
In the step (3), after each layer is printed by the 3D printing module, microwave preheating is carried out on the layer; then microwave cold sintering is carried out; the temperature of microwave preheating is 60-80 ℃, and the time of microwave preheating is 1-1.5 h; the temperature of the microwave cold sintering is 250-300 ℃, and the time of the microwave cold sintering is 1-1.5 h; and printing and sintering the next layer after the cold sintering of each layer is finished, so as to realize layered continuous sintering.
2. The method according to claim 1, wherein,
In the step (1), the water content in the suspension is 20-28 wt%; mixing and stirring, wherein the speed of mixing and stirring is 400-600rpm; the mixing and stirring time is 20-30 min.
3. The method according to claim 1, wherein,
In the step (2), the nonionic surfactant is selected from at least one of polyoxyethylene derivatives, alkyl alcohol amides and polyol monofatty acid esters; the mass ratio of the aggregate to the nonionic surfactant is 1000:1-3000:1;
In the foaming slurry, the concentration of the nonionic surfactant is 0.1-0.3 wt%;
Mixing and stirring, wherein the speed of mixing and stirring is 1500 rpm-2000 rpm; the mixing and stirring time is 20-30 min.
4. The method according to claim 1, wherein,
In the step (3), the heating rate of the microwave cold sintering is 10-20 ℃ per minute.
5. A ceramic foam material according to any one of the preceding claims 1 to 4,
The strength of the foam ceramic similar material is 1-3 MPa, and the peak strain is 0.1-1%;
The density of the sample is 900-1200 Within the range;
the wave speed of the sample is in the range of 1200-1600 m/s.
6. Use of a ceramic foam similar material prepared by the preparation method according to any one of claims 1 to 4 or a ceramic foam similar material according to claim 5 as a three-dimensional similar material physical model for researching deep hard rock engineering disaster simulation.
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