CN110843085A - Method for manufacturing gypsum mold and method for manufacturing fused quartz ceramic radome by using gypsum mold - Google Patents

Method for manufacturing gypsum mold and method for manufacturing fused quartz ceramic radome by using gypsum mold Download PDF

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Publication number
CN110843085A
CN110843085A CN201911200152.5A CN201911200152A CN110843085A CN 110843085 A CN110843085 A CN 110843085A CN 201911200152 A CN201911200152 A CN 201911200152A CN 110843085 A CN110843085 A CN 110843085A
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China
Prior art keywords
gypsum
cellulose
nano
ball milling
fused quartz
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CN201911200152.5A
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Chinese (zh)
Inventor
慈吉良
王涛
吕毅
张天翔
赵英民
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Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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Priority to CN201911200152.5A priority Critical patent/CN110843085A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/34Moulds, cores, or mandrels of special material, e.g. destructible materials
    • B28B7/344Moulds, cores, or mandrels of special material, e.g. destructible materials from absorbent or liquid- or gas-permeable materials, e.g. plaster moulds in general
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/26Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B28B1/261Moulds therefor
    • B28B1/262Mould materials; Manufacture of moulds or parts thereof
    • B28B1/264Plaster
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/52Producing shaped prefabricated articles from the material specially adapted for producing articles from mixtures containing fibres, e.g. asbestos cement
    • B28B1/525Producing shaped prefabricated articles from the material specially adapted for producing articles from mixtures containing fibres, e.g. asbestos cement containing organic fibres, e.g. wood fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • B28B17/02Conditioning the material prior to shaping
    • B28B17/023Conditioning gypsum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/34Moulds, cores, or mandrels of special material, e.g. destructible materials
    • B28B7/346Manufacture of moulds
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01QANTENNAS, i.e. RADIO AERIALS
    • H01Q1/00Details of, or arrangements associated with, antennas
    • H01Q1/42Housings not intimately mechanically associated with radiating elements, e.g. radome

Abstract

The invention relates to a method for manufacturing a plaster mold and a method for manufacturing a fused quartz ceramic radome by using the plaster mold. The method comprises the following steps: (1) preparing nano-cellulose by ball milling: mixing the fiber raw material and a solvent, and then carrying out ball milling to obtain a nano-cellulose suspension with the size of 20-100 nm; (2) dispersing: carrying out ultrasonic dispersion on the nano cellulose suspension obtained in the step (1) to obtain a dispersion liquid; (3) curing and forming: and (3) mixing the dispersion liquid obtained in the step (2) with gypsum powder, then pouring the mixture into a mould, curing and drying to obtain the gypsum mould. The gypsum mold provided by the invention can bear higher grouting pressure, so that the grouting forming speed is increased, the working efficiency is improved, and the density of a fused quartz ceramic blank can be improved under higher grouting pressure, so that a quartz ceramic finished product with higher density and bending strength is obtained.

Description

Method for manufacturing gypsum mold and method for manufacturing fused quartz ceramic radome by using gypsum mold
Technical Field
The invention relates to the technical field of a fused quartz ceramic radome, in particular to a manufacturing method of a gypsum mold and a method for manufacturing the fused quartz ceramic radome by using the gypsum mold.
Background
At present, a slip casting method is widely used for producing the fused quartz ceramic radome, and gypsum has good water absorption and demoulding performance, so that a free-form ceramic blank can be prepared according to requirements, and the gypsum is usually adopted as a slip casting mould. In the production of the traditional gypsum mould, gypsum powder is dispersed in water to obtain gypsum slurry, and the gypsum slurry is injected into the mould to be dried and solidified to obtain the gypsum mould. In the grouting process, after the fused quartz slurry is added into a gypsum mold, water in the slurry is discharged through the capillary action of gypsum pores, so that fused quartz particles are separated out and molded along the gypsum wall, and the radome green body is obtained. Compared with normal pressure grouting, by applying external pressure, fused quartz particles can be stacked more tightly, the prepared ceramic blank is more compact, and the ceramic finished product obtained after drying and sintering has higher density and bending strength. However, the strength of the plaster mold is low, and the grouting pressure is only 0.1-0.3 MPa.
Therefore, a material with higher compressive strength is sought to be used as a pressure grouting mold, and the pressure grouting mold is still an important research direction in the field of preparing the quartz ceramic radome by pressure grouting.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention aims to solve the following problems: how to prepare a gypsum mould with high compressive strength for preparing a fused quartz ceramic radome by a high-pressure grouting method.
In order to solve the technical problems, the invention provides the following technical scheme:
a method of manufacturing a gypsum mold, the method comprising the steps of:
(1) preparing nano-cellulose by ball milling: mixing the fiber raw material and a solvent, and then carrying out ball milling to obtain a nano-cellulose suspension with the size of 20-100 nm;
(2) dispersing: carrying out ultrasonic dispersion on the nano-cellulose suspension obtained in the step (1) to obtain a nano-cellulose dispersion liquid;
(3) curing and forming: and (3) mixing the dispersion liquid obtained in the step (2) with gypsum powder, then pouring the mixture into a mould, curing and drying to obtain the gypsum mould.
Preferably, the fiber raw material comprises any one or more of absorbent cotton, cotton linter, CF11 cellulose and corncob cellulose; preferably, the mass ratio of the fiber raw material to the solvent is (1-10): (1000-2000); and/or
The solvent is a sulfuric acid aqueous solution with the concentration of 2-5 wt%.
Preferably, when the ball milling is carried out, the mass ratio of large, medium and small milling balls is 1 (2-4) to (1-3);
preferably, the ball-to-feed ratio is (1-3): 1.
preferably, when the ball milling is carried out, the ball milling rotating speed is 300 and 1000 rpm; and/or
The ball milling time is 4-6 h.
Preferably, when the ultrasound is performed, the ultrasound power is 300-900W.
Preferably, the mass ratio of the nano-cellulose dispersion liquid to the gypsum powder is 1: (1-1.5).
Preferably, the curing is carried out at room temperature, preferably for a period of 20-24 hours; and/or
The drying is carried out at a temperature below 50 ℃, preferably at a temperature of 35-40 ℃.
Preferably, the plaster mold has a compressive strength of 0.4 to 0.8 MPa.
A method of making a fused silica ceramic radome, the method comprising the steps of:
(1) manufacturing a gypsum mould according to the method provided by the invention;
(2) mixing fused quartz sand and water, ball-milling into slurry, injecting the slurry into a gypsum mold, adjusting the pressure to 0.4-0.8MPa to obtain a fused quartz blank, then demolding, taking out, drying and calcining to obtain the fused quartz ceramic radome.
Preferably, the drying is performed at 120-; and/or
The calcination was carried out at 1100 ℃ and 1300 ℃.
Advantageous effects
The technical scheme of the invention has the following advantages:
the gypsum mold provided by the invention can bear higher grouting pressure, so that the grouting forming speed is increased, the working efficiency is improved, and the density of a fused quartz ceramic blank can be improved under higher grouting pressure, so that a quartz ceramic finished product with higher density and bending strength is obtained.
The preparation method provided by the invention has the advantages of simplicity, easiness in implementation, low cost, no pollution and the like
The raw materials for preparing the nano-cellulose have wide sources and low price.
Drawings
Fig. 1 is a TEM photograph of the nanocellulose prepared in example 2.
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 clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The present invention provides a method for manufacturing a gypsum mold, which uses nanocellulose as a reinforcing phase to reinforce the strength of gypsum, and since nanocellulose has extremely high strength and a large number of hydroxyl groups on the surface of nanocellulose can form strong interaction with gypsum particles, the strength of gypsum is increased, and the mold manufactured by using the gypsum meets the requirement of bearing higher grouting pressure. Specifically, the manufacturing method provided by the invention comprises the following steps:
(1) preparing nano-cellulose by ball milling: mixing the fiber raw material and a solvent, and then carrying out ball milling to obtain a nano-cellulose suspension with the size of 20-100 nm; destroying the structure of the fiber raw material by ball milling to obtain solution containing nano-cellulose; in addition, the invention also compares the reinforcing effect of the nanocellulose with different sizes obtained by different ball milling processes, and finds that the reinforcing effect on the gypsum mould is the best when the size of the cellulose is 20-50 nm;
(2) dispersing: carrying out ultrasonic dispersion on the nano-cellulose suspension obtained in the step (1) to obtain a nano-cellulose dispersion liquid;
(3) curing and forming: and (3) mixing the dispersion liquid obtained in the step (2) with gypsum powder, then pouring the mixture into a mould, curing and drying to obtain the gypsum mould. It should be noted that the mold used in the manufacturing method of the present invention is an existing mold, and reference may be made to the prior art in this field, and the present invention will not be described in detail in its structure.
The raw materials for preparing the nano-cellulose have wide sources and low price, and include but are not limited to any one or more of absorbent cotton, cotton linter, CF11 cellulose, corn cob cellulose and the like.
The present invention makes intensive research on the technological conditions of ball milling. The ball milling process affects the size of the obtained cellulose, and in order to obtain nano-cellulose with the size meeting the requirement, the better ball milling process conditions are as follows:
when ball milling is carried out, the mass ratio of the fiber raw materials to the solvent is (1-10): (1000-2000).
When ball milling is carried out, the mass ratio of large, medium and small grinding balls is 1 (2-4) to (1-3); the diameters of the large, medium and small grinding balls are respectively 30mm, 20mm and 10 mm.
The ball milling is carried out at a ball-to-feed ratio of (1-3):1, for example, 1:1, 2:1, 3: 1.
When the ball milling is carried out, the ball milling rotation speed is 300-1000rpm, for example, 300rpm, 400rpm, 500rpm, 600rpm, 700rpm, 800rpm, 900rpm, 1000rpm can be set;
the ball milling time is 4-6h, for example, 4h, 5h and 6 h.
When ball milling is carried out, the solvent added during ball milling is 2-5 wt% sulfuric acid aqueous solution, and the sulfuric acid aqueous solution with the concentration can better destroy the structure of the fiber raw material to obtain the nano-cellulose. After the ball milling is finished, the ball milling product can be repeatedly washed by distilled water, for example, 5 times, and finally the nano cellulose suspension containing 20-100nm is obtained.
The invention adopts wet ball milling to ball mill fiber raw materials, the solvent adopts 2-5 wt% sulfuric acid water solution, the material-liquid ratio is (1-10): (1000-2000), the ball-material ratio is (1-3):1, the mass ratio of large, medium and small grinding balls is 1 (2-4): (1-3), the ball-milling rotating speed is 300-1000rpm, the ball-milling time is 4-6h, and the nano-cellulose with the size characteristic of 20-100nm is obtained with high efficiency.
In some preferred embodiments, the ultrasound power is 300-900W, for example, 300W, 400W, 500W, 600W, 700W, 800W, 900W.
In some preferred embodiments, the mass ratio of the nanocellulose dispersion to the landplaster is 1: (1-1.5). The dispersion is reduced and agglomeration occurs due to the overhigh content of the nano-cellulose; the content of the nano-cellulose is too low, and the reinforcing effect on the gypsum is reduced.
In some preferred embodiments, the curing is performed at room temperature, preferably for a period of 20-24 hours, for example, 20 hours, 21 hours, 22 hours, 23 hours, 24 hours.
In some preferred embodiments, the drying is performed at less than 50 ℃, preferably at 35-40 ℃ (e.g., may be 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃).
More fully, the present invention provides a method of manufacture comprising:
(1) preparing nano-cellulose by ball milling: mixing a fiber raw material and a sulfuric acid aqueous solution with the concentration of 2-5 wt%, performing ball milling, and repeatedly washing by using distilled water to obtain a nano-cellulose suspension with the size of 20-100 nm; the fiber raw material comprises any one or more of absorbent cotton, cotton linter, CF11 cellulose and corncob cellulose; preferably, the mass ratio of the fiber raw material to the solvent is (1-10): (1000-2000); when ball milling is carried out, the mass ratio of large, medium and small grinding balls is 1:2: 1.5; the ball material ratio is (1-3): 1; when ball milling is carried out, the ball milling rotating speed is 300-; the ball milling time is 4-6 h;
(2) dispersing: carrying out ultrasonic dispersion on the nano cellulose suspension obtained in the step (1) to obtain a dispersion liquid; the ultrasonic power is 300-900W;
(3) curing and forming: mixing the dispersion liquid obtained in the step (2) with gypsum powder, wherein the mass ratio of the nano cellulose dispersion liquid to the gypsum powder is 1: (1-1.5), then pouring into a mould, curing, drying, and carrying out the curing at room temperature, wherein the curing time is preferably 20-24h, and the drying is carried out at the temperature of below 50 ℃, preferably at the temperature of 35-40 ℃, so as to obtain the gypsum mould. The plaster mold has the compression strength of 0.4-0.8MPa through detection.
In the second aspect, the invention provides a method for manufacturing a fused quartz ceramic radome, the method utilizes the gypsum mold provided in the first aspect of the invention as a molding device, compared with the traditional gypsum, the nano-cellulose reinforced gypsum can bear higher grouting pressure, so that the grouting molding speed is increased, the working efficiency is improved, and the density of a fused quartz ceramic blank can be improved under higher grouting pressure, so that a quartz ceramic finished product with higher density and mechanical property is obtained. Specifically, the method comprises the following steps:
mixing fused quartz sand and water, ball-milling into slurry, injecting the slurry into a gypsum mold, adjusting the pressure to 0.4-0.8MPa to obtain a fused quartz blank, then demolding, taking out, drying and calcining to obtain the fused quartz ceramic radome, wherein the drying is preferably carried out at the temperature of 120-140 ℃ (for example, 120 ℃, 130 ℃, 140 ℃) and the calcining is preferably carried out at the temperature of 1100-1300 ℃ (for example, 1100 ℃, 1200 ℃, 1300 ℃).
The following are examples of the present invention.
Example 1
S1, preparation of nano-cellulose: adding cotton linters and a 2 wt% sulfuric acid aqueous solution into a ball milling tank, adding large, medium and small grinding balls, wherein the diameters of the large, medium and small grinding balls are respectively 30mm, 20mm and 10mm, setting the rotating speed of the ball mill to 300rpm, and flushing for 5 times by using distilled water after ball milling for 4 hours to obtain a dispersion solution 1; wherein the mass ratio of the cotton linters to the aqueous solution is 1:2000, the ball-to-material ratio is 1.3:1, and the ratio of the large balls to the small balls to the medium balls is 1:2: 1.5; and (3) placing the dispersion liquid 1 in a beaker, placing an ultrasonic probe 1.5cm below the liquid level in the beaker, setting the ultrasonic power at 300W, and carrying out ultrasonic treatment for 30min to obtain the nano-cellulose dispersion liquid 2.
S2, preparation of a gypsum mold: adding gypsum powder and the nano-cellulose dispersion liquid 2 into a stirring barrel, wherein the mass ratio of the nano-cellulose dispersion liquid 2 to the gypsum powder is 1:1, stirring for 3min, pouring into a gypsum forming mold, drying and curing at room temperature for 24h, then removing the gypsum forming mold, and drying gypsum in an oven at 35 ℃ for 24h to obtain a dried gypsum mold; the detection proves that the compression strength of the gypsum mould is 0.6 MPa.
S3, preparing a fused quartz ceramic pressure grouting blank: adding fused quartz sand and water into a ball mill, adding grinding balls, and performing ball milling to obtain fused quartz slurry. Connecting the gypsum mould, the feeding device and the pressing device, pouring the slurry into a cavity of the gypsum mould, connecting a nitrogen cylinder, adjusting the pressure to 0.5MPa, absorbing the moisture in the slurry by the gypsum mould through capillary action to obtain a fused quartz blank, and then demoulding and taking out. And (3) putting the blank into an oven to be dried for 24h at 120 ℃, and then sintering for 2h at 1200 ℃ to obtain the fused quartz ceramic.
The method can perform slip casting under higher slip casting pressure, the slip casting speed is accelerated, the working efficiency is improved, and the density of the fused quartz ceramic blank can be improved under higher slip casting pressure, so that a quartz ceramic finished product with higher density and mechanical property is obtained. The detection shows that the finally prepared fused quartz ceramic product has the density of 1.98g/cm3The flexural strength was 64.7 MPa.
Example 2
S1, preparation of nano-cellulose: adding absorbent cotton and a 2 wt% sulfuric acid aqueous solution into a ball milling tank, adding large, medium and small grinding balls, wherein the diameters of the large, medium and small grinding balls are 30mm, 20mm and 10mm respectively, setting the rotating speed of the ball mill at 500rpm, and flushing the ball mill for 4 hours by distilled water for 5 times to obtain a dispersion liquid 1. Wherein the mass ratio of the absorbent cotton to the aqueous solution is 1:1000, the ball-to-material ratio is 1.5:1, and the ratio of the large balls to the small balls to the medium balls is 1: 2.5: 1; and (3) placing the dispersion liquid 1 in a beaker, placing an ultrasonic probe 1.5cm below the liquid level in the beaker, setting the ultrasonic power to 900W, and carrying out ultrasonic treatment for 40min to obtain the nano-cellulose dispersion liquid 2. The morphology of the prepared nanocellulose is shown in figure 1.
S2, preparation of a gypsum mold: adding gypsum powder and the nano-cellulose dispersion liquid 2 into a stirring barrel, wherein the mass ratio of the nano-cellulose dispersion liquid 2 to the gypsum powder is 1:1.5, stirring for 5min, pouring into a gypsum forming mold, drying and curing at room temperature for 24h, then removing the gypsum forming mold, and drying gypsum in an oven at 35 ℃ for 12h to obtain a dried gypsum mold; the detection proves that the compression strength of the gypsum mould is 0.8 MPa.
S3, preparing a fused quartz ceramic pressure grouting blank: adding fused quartz sand and water into a ball mill, adding grinding balls, and performing ball milling to obtain fused quartz slurry. Connecting the gypsum mould, the feeding device and the pressing device, pouring the slurry into a cavity of the gypsum mould, connecting a nitrogen cylinder, adjusting the pressure to 0.6MPa, absorbing the moisture in the slurry by the gypsum mould through capillary action to obtain a fused quartz blank, and then demoulding and taking out. And (3) putting the blank into an oven to be dried for 12h at the temperature of 110 ℃, and then sintering for 6h at the temperature of 1200 ℃ to obtain the fused quartz ceramic.
The method can perform slip casting under higher slip casting pressure, the slip casting speed is accelerated, the working efficiency is improved, and the density of the fused quartz ceramic blank can be improved under higher slip casting pressure, so that a quartz ceramic finished product with higher density and mechanical property is obtained. The detection shows that the density of the finally prepared fused quartz ceramic product is 1.97g/cm3The flexural strength was 72.8 MPa.
Example 3
S1, preparation of nano-cellulose: adding absorbent cotton and a 2 wt% sulfuric acid aqueous solution into a ball milling tank, adding large, medium and small grinding balls, wherein the diameters of the large, medium and small grinding balls are 30mm, 20mm and 10mm respectively, setting the rotating speed of the ball mill at 400rpm, and flushing the ball mill for 5 hours by distilled water for 5 times to obtain a dispersion liquid 1. Wherein the mass ratio of the absorbent cotton to the aqueous solution is 2:1500, the ball-to-material ratio is 2:1, and the ratio of the large balls to the small balls to the medium balls is 1: 3: 2; and (3) placing the dispersion liquid 1 in a beaker, placing an ultrasonic probe 1.5cm below the liquid level in the beaker, setting the ultrasonic power at 600W, and carrying out ultrasonic treatment for 40min to obtain the nano-cellulose dispersion liquid 2.
S2, preparation of a gypsum mold: adding gypsum powder and the nano-cellulose dispersion liquid 2 into a stirring barrel, wherein the mass ratio of the nano-cellulose dispersion liquid 2 to the gypsum powder is 1:1, stirring for 5min, pouring into a gypsum forming mold, drying and curing at room temperature for 24h, then removing the gypsum forming mold, and drying gypsum in an oven at 40 ℃ for 12h to obtain a dried gypsum mold; the detection proves that the compression strength of the gypsum mould is 0.6 MPa.
S3, preparing a fused quartz ceramic pressure grouting blank: adding fused quartz sand and water into a ball mill, adding grinding balls, and performing ball milling to obtain fused quartz slurry. Connecting the gypsum mould, the feeding device and the pressing device, pouring the slurry into a cavity of the gypsum mould, connecting a nitrogen cylinder, adjusting the pressure to 0.5MPa, absorbing the moisture in the slurry by the gypsum mould through capillary action to obtain a fused quartz blank, and then demoulding and taking out. And (3) putting the blank into an oven to be dried for 12h at the temperature of 110 ℃, and then sintering for 6h at the temperature of 1150 ℃ to obtain the fused quartz ceramic.
The method can perform slip casting under higher slip casting pressure, the slip casting speed is accelerated, the working efficiency is improved, and the density of the fused quartz ceramic blank can be improved under higher slip casting pressure, so that a quartz ceramic finished product with higher density and mechanical property is obtained. The detection shows that the density of the finally prepared fused quartz ceramic product is 1.97g/cm3The flexural strength was 64.9 MPa.
Example 4
S1, preparation of nano-cellulose: adding absorbent cotton and a 2 wt% sulfuric acid aqueous solution into a ball milling tank, adding large, medium and small grinding balls, wherein the diameters of the large, medium and small grinding balls are 30mm, 20mm and 10mm respectively, setting the rotating speed of the ball mill at 400rpm, and flushing the ball mill for 5 hours by distilled water for 5 times to obtain a dispersion liquid 1. Wherein the mass ratio of the absorbent cotton to the aqueous solution is 10:2000, the ball-material ratio is 2:1, and the ratio of the large balls to the small balls to the medium balls is 1: 3: 2; and (3) placing the dispersion liquid 1 in a beaker, placing an ultrasonic probe 1.5cm below the liquid level in the beaker, setting the ultrasonic power at 600W, and carrying out ultrasonic treatment for 40min to obtain the nano-cellulose dispersion liquid 2.
S2, preparation of a gypsum mold: adding gypsum powder and the nano-cellulose dispersion liquid 2 into a stirring barrel, wherein the mass ratio of the nano-cellulose dispersion liquid 2 to the gypsum powder is 0.6:1, stirring for 5min, pouring into a gypsum forming mold, drying and curing at room temperature for 24h, then removing the gypsum forming mold, and drying gypsum in an oven at 40 ℃ for 12h to obtain a dried gypsum mold; through detection, the compression strength of the gypsum mold is only 0.3MPa, and the gypsum mold cannot bear higher grouting pressure.
Example 5
S1, preparation of nano-cellulose: adding absorbent cotton and a 2 wt% sulfuric acid aqueous solution into a ball milling tank, adding large, medium and small grinding balls, wherein the diameters of the large, medium and small grinding balls are 30mm, 20mm and 10mm respectively, setting the rotating speed of the ball mill at 400rpm, and flushing the ball mill for 5 hours by distilled water for 5 times to obtain a dispersion liquid 1. Wherein the mass ratio of the absorbent cotton to the aqueous solution is 1:1800, the ball-material ratio is 2:1, and the ratio of the large balls to the small balls to the medium balls is 1: 3: 2; and (3) placing the dispersion liquid 1 in a beaker, placing an ultrasonic probe 1.5cm below the liquid level in the beaker, setting the ultrasonic power at 600W, and carrying out ultrasonic treatment for 40min to obtain the nano-cellulose dispersion liquid 2.
S2, preparation of a gypsum mold: adding the gypsum powder and the nano-cellulose dispersion liquid 2 into a stirring barrel, wherein the mass ratio of the nano-cellulose dispersion liquid 2 to the gypsum powder is 1.5:1, stirring for 5min, pouring into a gypsum forming die, and observing fiber floc with naked eyes, which shows that the dispersion performance of the nano-cellulose is poor.
And (3) after drying and curing for 24h at room temperature, dismantling the gypsum forming mold, and drying the gypsum in an oven at 40 ℃ for 12h to obtain the dried gypsum mold. The detection proves that the compression strength of the gypsum mould is 0.4MPa, and the unexpected remarkable improvement does not occur.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method of manufacturing a plaster mold, comprising the steps of:
(1) preparing nano-cellulose by ball milling: mixing the fiber raw material and a solvent, and then carrying out ball milling to obtain a nano-cellulose suspension with the size of 20-100 nm;
(2) dispersing: carrying out ultrasonic dispersion on the nano-cellulose suspension obtained in the step (1) to obtain a nano-cellulose dispersion liquid;
(3) curing and forming: and (3) mixing the dispersion liquid obtained in the step (2) with gypsum powder, then pouring the mixture into a mould, curing and drying to obtain the gypsum mould.
2. The method of claim 1,
the fiber raw material comprises any one or more of absorbent cotton, cotton linter, CF11 cellulose and corncob cellulose; preferably, the mass ratio of the fiber raw material to the solvent is (1-10): (1000-2000); and/or
The solvent is a sulfuric acid aqueous solution with the concentration of 2-5 wt%.
3. The method of claim 2,
when ball milling is carried out, the mass ratio of large, medium and small grinding balls is 1 (2-4) to (1-3);
preferably, the ball-to-feed ratio is (1-3): 1.
4. the method of claim 3,
when ball milling is carried out, the ball milling rotating speed is 300-; and/or
The ball milling time is 4-6 h.
5. The method according to any one of claims 1 to 4,
when ultrasonic treatment is carried out, the ultrasonic power is 300-900W.
6. The method according to any one of claims 1 to 5,
the mass ratio of the nano cellulose dispersion liquid to the gypsum powder is 1: (1-1.5).
7. The method according to any one of claims 1 to 6,
the curing is carried out at room temperature, and the curing time is preferably 20-24 h; and/or
The drying is carried out at a temperature below 50 ℃, preferably at a temperature of 35-40 ℃.
8. The method according to any one of claims 1 to 7,
the plaster mold has a compressive strength of 0.4-0.8 MPa.
9. A method of making a fused silica ceramic radome, comprising the steps of:
(1) a gypsum mould made according to the method of any one of claims 1 to 8;
(2) mixing fused quartz sand and water, ball-milling into slurry, injecting the slurry into a gypsum mold, adjusting the pressure to 0.4-0.8MPa to obtain a fused quartz blank, then demolding, taking out, drying and calcining to obtain the fused quartz ceramic radome.
10. The method of claim 9,
the drying is carried out at the temperature of 120-140 ℃; and/or
The calcination was carried out at 1100 ℃ and 1300 ℃.
CN201911200152.5A 2019-11-29 2019-11-29 Method for manufacturing gypsum mold and method for manufacturing fused quartz ceramic radome by using gypsum mold Pending CN110843085A (en)

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CA1282578C (en) * 1985-05-30 1991-04-09 Fritz Faessle Procedure for the production of moulds, patterns and tools made from plaster-based and cement-based materials
CN101204830A (en) * 2007-12-18 2008-06-25 中国科学院上海硅酸盐研究所 Plaster mould for ceramic grout fashioned improved and producing method with same
CN107032771A (en) * 2017-03-17 2017-08-11 邹亚静 A kind of manufacture method of quartz ceramic crucible
RU2644453C1 (en) * 2016-11-14 2018-02-12 Акционерное общество "Обнинское научно-производственное предприятие "Технология" им. А.Г. Ромашина" Quartz ceramic antenna fairing of a missile and the method of its manufacture
CN108911664A (en) * 2018-07-11 2018-11-30 中国船舶重工集团公司第七二五研究所 The preparation method of nanometer scale ceramics powder pressure injection forming high strength gypsum mould
CN110330350A (en) * 2019-07-25 2019-10-15 武汉理工大学 A kind of preparation method of fiber reinforced alumina ceramics

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1282578C (en) * 1985-05-30 1991-04-09 Fritz Faessle Procedure for the production of moulds, patterns and tools made from plaster-based and cement-based materials
CN101204830A (en) * 2007-12-18 2008-06-25 中国科学院上海硅酸盐研究所 Plaster mould for ceramic grout fashioned improved and producing method with same
RU2644453C1 (en) * 2016-11-14 2018-02-12 Акционерное общество "Обнинское научно-производственное предприятие "Технология" им. А.Г. Ромашина" Quartz ceramic antenna fairing of a missile and the method of its manufacture
CN107032771A (en) * 2017-03-17 2017-08-11 邹亚静 A kind of manufacture method of quartz ceramic crucible
CN108911664A (en) * 2018-07-11 2018-11-30 中国船舶重工集团公司第七二五研究所 The preparation method of nanometer scale ceramics powder pressure injection forming high strength gypsum mould
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