CN112159215A - Long-wave low-temperature 3D printing ceramic material and product processing method - Google Patents

Long-wave low-temperature 3D printing ceramic material and product processing method Download PDF

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CN112159215A
CN112159215A CN202011029959.XA CN202011029959A CN112159215A CN 112159215 A CN112159215 A CN 112159215A CN 202011029959 A CN202011029959 A CN 202011029959A CN 112159215 A CN112159215 A CN 112159215A
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ceramic
temperature
long
printing
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赵喆
李鸣
姜焱林
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Jiaxing Raoji Technology Co ltd
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Jiaxing Raoji Technology Co ltd
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    • B28—WORKING CEMENT, CLAY, OR STONE
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    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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Abstract

The invention relates to the technical field of 3D ceramic printing, in particular to a long-wave low-temperature 3D printing ceramic material which is prepared from the following raw materials in parts by weight: 90-120 parts of ceramic powder, 25-40 parts of light-cured resin prepolymer, 20-35 parts of reactive diluent and sintered5-12 parts of an auxiliary agent, 0.1-0.4 part of a photoinitiator, 0.015-0.045 part of a polymerization inhibitor, 2.5-5.5 parts of a dispersing agent and 0-4 parts of a defoaming agent; the sintering aid is composed of the following raw materials in parts by weight: 8-12 parts of CaO, 1-5 parts of MgO and SiO25 to 9 parts of TiO21-7 parts. By adding the sintering aid and refining the grain diameter of the ceramic powder, the sintering temperature of the ceramic is reduced, and the ceramic is gradually photocured from deep to shallow through three times of sub-bands, so that the obtained product has low porosity and good mechanical property.

Description

Long-wave low-temperature 3D printing ceramic material and product processing method
Technical Field
The invention relates to the technical field of 3D ceramic printing, in particular to a long-wave low-temperature 3D printing ceramic material and a product processing method.
Background
The appearance of the 3D printing and forming technology enables the production and manufacturing of ceramics to be changed innovatively, and the original material reduction manufacturing is changed into material increase manufacturing in the preparation process. The forming method for preparing the ceramic product through 3D printing mainly comprises heating curing, oxidation curing and photocuring, wherein the photocuring forming curing speed is high, the organic volatile matter is less, the energy utilization rate is high, and the forming method is an energy-saving, environment-friendly and efficient curing forming method.
After the material is solidified, the biscuit needs to be sintered, in the traditional process, the sintering temperature is high, the mechanical property of the material is poor, and in addition, the high temperature causes serious damage to the refractory bricks of the kiln.
Therefore, we propose a long-wave low-temperature 3D printing ceramic material and a product processing method to solve the above problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a long-wave low-temperature 3D printing ceramic material and a product processing method.
The long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 90-120 parts of ceramic powder, 25-40 parts of a photo-curing resin prepolymer, 20-35 parts of a reactive diluent, 5-12 parts of a sintering aid, 0.1-0.4 part of a photoinitiator, 0.015-0.045 part of a polymerization inhibitor, 2.5-5.5 parts of a dispersant and 0-4 parts of an antifoaming agent; the sintering aid is composed of the following raw materials in parts by weight: 8-12 parts of CaO, 1-5 parts of MgO and SiO25 to 9 parts of TiO21-7 parts; the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
Preferably, the ceramic powder consists of the following raw materials in parts by weight: al (Al)2O395 to 99 parts of Na20.1 to 0.5 part of O and Fe2O30.01 to 0.05 portion.
Preferably, the light-cured resin prepolymer is prepared from the following raw materials in parts by weight: 25-40 parts of polyether acrylate, 20-35 parts of epoxy acrylate, 15-25 parts of polyurethane acrylate and 5-10 parts of polyester acrylate.
Preferably, the photoinitiator is one or more of 369, 651, 784, 819, ITX, TPO and TPO-L.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating LED light with the wavelength of 460-480 nm for 2-4S for first curing, and then standing for 3-10 min;
s3, irradiating for 4-6S by using LED light with the wavelength of 400-420 nm, curing for the second time, and then standing for 3-10 min;
s4, irradiating for 2-4S by using LED light with the wavelength of 350-370 nm, and curing for the third time to obtain a ceramic biscuit;
and S5, degreasing the biscuit, and sintering at 1500-1600 ℃ for 1.5-3 h to obtain the 3D printing ceramic product.
Preferably, the power of the LED lamp in the step S2 is 800mW/cm2～1200mW/cm2。
Preferably, the power of the LED lamp in the step S3 is 1000mW/cm2～1400mW/cm2。
Preferably, the power of the LED lamp in the step S4 is 1200mW/cm2～1600mW/cm2。
The invention has the beneficial effects that:
1. by adding the sintering aid and refining the grain diameter of the ceramic powder, the sintering temperature of the ceramic is reduced, the compactness of the ceramic product is improved, and the loss of the refractory bricks of the kiln is effectively reduced.
2. Through three wave band-splitting light curing step by step from deep to shallow, the ceramic filler is firstly supported without collapse and then is leveled step by step from deep to shallow, and the obtained product has low porosity and good mechanical property.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The first embodiment is as follows:
the long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 100 parts of ceramic powder, 25 parts of a light-cured resin prepolymer, 20 parts of an active diluent, 7 parts of a sintering aid, 0.3 part of a photoinitiator, 0.015 part of a polymerization inhibitor, 3 parts of a dispersing agent and 2 parts of a defoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: CaO 8 parts, MgO 5 parts, SiO29 parts of TiO22 parts of (1);
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O398 portions of Na20.2 part of O and Fe2O30.015 part, wherein the light-cured resin prepolymer comprises the following raw materials in parts by weight: 30 parts of polyether acrylate, 35 parts of epoxy acrylate, 25 parts of polyurethane acrylate and 5 parts of polyester acrylate, wherein the types of the photoinitiator are 369 and 784 and TPO, and the mass of the photoinitiator is equal to that of the photoinitiator 369, 784 and TPO.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating for 3S by using LED light with the wavelength of 470nm, curing for the first time, and then standing for 5 min;
s3, irradiating for 5S by using LED light with the wavelength of 410nm, curing for the second time, and then standing for 5 min;
s4, irradiating for 3S by using LED light with the wavelength of 360nm, and curing for the third time to obtain a ceramic biscuit;
and S5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1500 ℃ for 3h to obtain the 3D printing ceramic product.
In this embodiment, the power of the LED lamp in the step S2 is 1000mW/cm2And the power of the LED lamp in the step S3 is 1200mW/cm2And the power of the LED lamp in the step S4 is 1450mW/cm2。
Example two:
the long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 100 parts of ceramic powder, 35 parts of light-cured resin prepolymer, 32 parts of reactive diluent, 7 parts of sintering aid, 0.3 part of photoinitiator, 0.015 part of polymerization inhibitor, 3 parts of dispersant and 2 parts of defoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: CaO 9 parts, MgO 3 parts, SiO25 parts of TiO23 parts of a mixture;
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O398 portions of Na20.2 part of O and Fe2O30.015 part, wherein the light-cured resin prepolymer comprises the following raw materials in parts by weight: 40 parts of polyether acrylate, 30 parts of epoxy acrylate, 20 parts of polyurethane acrylate and 10 parts of polyester acrylate, wherein the types of the photoinitiator are 651 and 819, and the TPO-L, 651 and 819 are equal to the TPO-L in mass.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating for 3S by using LED light with the wavelength of 460nm, carrying out primary curing, and then standing for 5 min;
s3, irradiating for 5S by using LED light with the wavelength of 400nm, curing for the second time, and then standing for 5 min;
s4, irradiating for 3S by using LED light with the wavelength of 350nm, and curing for the third time to obtain a ceramic biscuit;
and S5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1525 ℃ for 2.8h to obtain the 3D printing ceramic product.
In this embodiment, the power of the LED lamp in the step S2 is 1000mW/cm2And the power of the LED lamp in the step S3 is 1200mW/cm2And the power of the LED lamp in the step S4 is 1450mW/cm2。
Example three:
the long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 100 parts of ceramic powder, 30 parts of a light-cured resin prepolymer, 25 parts of an active diluent, 8 parts of a sintering aid, 0.3 part of a photoinitiator, 0.015 part of a polymerization inhibitor, 3 parts of a dispersing agent and 2 parts of a defoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: CaO 10 parts, MgO 3 parts, SiO25 parts of TiO24 parts of a mixture;
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O398 portions of Na20.2 part of O and Fe2O30.015 part, wherein the light-cured resin prepolymer comprises the following raw materials in parts by weight: 35 parts of polyether acrylate, 25 parts of epoxy acrylate, 25 parts of polyurethane acrylate and 10 parts of polyester acrylate, wherein the types of the photoinitiator are 651 and 784 and TPO, and the mass of the photoinitiator is equal to that of the photoinitiator 651 and 784.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating for 3S by using LED light with the wavelength of 470nm, curing for the first time, and then standing for 5 min;
s3, irradiating for 5S by using LED light with the wavelength of 410nm, curing for the second time, and then standing for 5 min;
s4, irradiating for 3S by using LED light with the wavelength of 360nm, and curing for the third time to obtain a ceramic biscuit;
and S5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1550 ℃ for 2.5h to obtain the 3D printing ceramic product.
In this embodiment, the power of the LED lamp in the step S2 is 1000mW/cm2And the power of the LED lamp in the step S3 is 1200mW/cm2And the power of the LED lamp in the step S4 is 1450mW/cm2。
Example four:
the long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 95 parts of ceramic powder, 30 parts of a photo-curing resin prepolymer, 30 parts of an active diluent, 5 parts of a sintering aid, 0.25 part of a photoinitiator, 0.025 part of a polymerization inhibitor, 3 parts of a dispersant and 2 parts of an antifoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: 11 parts of CaO, 4 parts of MgO and SiO25 parts of TiO23 parts of a mixture;
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O397 parts of Na20.5 part of O and Fe2O30.05 part of light-cured resin prepolymer, wherein the light-cured resin prepolymer is prepared from the following raw materials in parts by weight: 35 parts of polyether acrylate, 25 parts of epoxy acrylate, 25 parts of polyurethane acrylate and 10 parts of polyester acrylate, wherein the types of the photoinitiator are 651 and 784 and TPO-L, and the mass of the photoinitiator is equal to that of the photoinitiator 651 and 784.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating for 3S by using LED light with the wavelength of 480nm, curing for the first time, and then standing for 5 min;
s3, irradiating for 5S by using LED light with the wavelength of 420nm, curing for the second time, and then standing for 5 min;
s4, irradiating for 3S by using LED light with the wavelength of 370nm, and curing for the third time to obtain a ceramic biscuit;
and S5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1575 ℃ for 2h to obtain the 3D printing ceramic product.
In this embodiment, the power of the LED lamp in the step S2 is 1000mW/cm2And the power of the LED lamp in the step S3 is 1200mW/cm2And the power of the LED lamp in the step S4 is 1450mW/cm2。
Example five:
the long-wave low-temperature 3D printing ceramic material is prepared from the following raw materials in parts by weight: 95 parts of ceramic powder, 35 parts of a light-cured resin prepolymer, 35 parts of an active diluent, 8 parts of a sintering aid, 0.3 part of a photoinitiator, 0.015 part of a polymerization inhibitor, 3 parts of a dispersing agent and 2 parts of a defoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: CaO 10 parts, MgO 1 parts, SiO29 parts of TiO23.5 parts;
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O398 portions of Na20.3 part of O and Fe2O30.03 part of light-cured resin prepolymer, wherein the light-cured resin prepolymer is prepared from the following raw materials in parts by weight: 35 parts of polyether acrylate, 25 parts of epoxy acrylate, 25 parts of polyurethane acrylate and 10 parts of polyester acrylate, wherein the types of the photoinitiator are 369 and 819 and TPO-L, and the weight of the photoinitiator is equal to that of the photoinitiator 369, 819 and TPO-L.
A processing method of a long-wave low-temperature 3D printed ceramic product comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating for 3S by using LED light with the wavelength of 480nm, curing for the first time, and then standing for 5 min;
s3, irradiating for 5S by using LED light with the wavelength of 420nm, curing for the second time, and then standing for 5 min;
s4, irradiating for 3S by using LED light with the wavelength of 370nm, and curing for the third time to obtain a ceramic biscuit;
and S5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1600 ℃ for 1.5h to obtain the 3D printing ceramic product.
In this embodiment, the power of the LED lamp in the step S2 is 1000mW/cm2And the power of the LED lamp in the step S3 is 1200mW/cm2And the power of the LED lamp in the step S4 is 1450mW/cm2。
Comparative example:
the 3D printing ceramic material is composed of the following raw materials in parts by weight: 100 parts of ceramic powder, 30 parts of a light-cured resin prepolymer, 25 parts of an active diluent, 0.3 part of a photoinitiator, 0.015 part of a polymerization inhibitor, 3 parts of a dispersant and 2 parts of a defoaming agent;
the grain diameter of the ceramic powder is between 5 and 12 mu m.
In the embodiment, the ceramic powder comprises the following raw materials in parts by weight: al (Al)2O399 parts of Na20.3 part of O and Fe2O30.03 part of the photo-curing resin prepolymer is epoxy acrylate, and the type of the photoinitiator is 369.
A3D printing ceramic product processing method comprises the following steps:
s1, loading the material into a 3D printer for printing;
s2, adopting the power with the wavelength of 360nm of 1200mW/cm2Irradiating the LED light for 11s, and curing to obtain a ceramic biscuit;
s5, slowly heating the ceramic biscuit to 650 ℃, heating for 1.5h, degreasing, and sintering at 1660 ℃ for 1.5h to obtain the 3D printing ceramic product.
The ceramic products of the first to fifth examples and the comparative example were tested for relative density and compressive strength, and the results were as follows:
serial number Relative density Compressive strength (MPa)
Example one 97.7％ 62.3
Example two 98.1％ 64.5
EXAMPLE III 98.5％ 68.3
Example four 97.2％ 59.8
EXAMPLE five 98.9％ 71.2
Comparative example 95.2％ 38.5
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (8)

1. The long-wave low-temperature 3D printing ceramic material is characterized by comprising the following raw materials in parts by weight: 90-120 parts of ceramic powder, 25-40 parts of a photo-curing resin prepolymer, 20-35 parts of a reactive diluent, 5-12 parts of a sintering aid, 0.1-0.4 part of a photoinitiator, 0.015-0.045 part of a polymerization inhibitor, 2.5-5.5 parts of a dispersant and 0-4 parts of an antifoaming agent;
the sintering aid is composed of the following raw materials in parts by weight: 8-12 parts of CaO, 1-5 parts of MgO and SiO25 to 9 parts of TiO21-7 parts;
the grain diameter of the ceramic powder is between 0.8 and 4 mu m, and the grain diameter of the sintering aid is between 2.5 and 3.5 mu m.
2. The long-wave low-temperature 3D printing ceramic material as claimed in claim 1, wherein the ceramic powder is composed of the following raw materials in parts by weight: al (Al)2O395 to 99 parts of Na20.1 to 0.5 part of O and Fe2O30.01 to 0.05 portion.
3. The long-wave low-temperature 3D printing ceramic material according to claim 1, wherein the light-cured resin prepolymer is prepared from the following raw materials in parts by weight: 25-40 parts of polyether acrylate, 20-35 parts of epoxy acrylate, 15-25 parts of polyurethane acrylate and 5-10 parts of polyester acrylate.
4. The long-wave low-temperature 3D printing ceramic material according to claim 3, wherein the photoinitiator is one or more of model number 369, 651, 784, 819, ITX, TPO-L.
5. A processing method of a long-wave low-temperature 3D printed ceramic product is characterized by comprising the following steps:
s1, loading the material into a 3D printer for printing;
s2, irradiating LED light with the wavelength of 460-480 nm for 2-4S for first curing, and then standing for 3-10 min;
s3, irradiating for 4-6S by using LED light with the wavelength of 400-420 nm, curing for the second time, and then standing for 3-10 min;
s4, irradiating for 2-4S by using LED light with the wavelength of 350-370 nm, and curing for the third time to obtain a ceramic biscuit;
and S5, degreasing the biscuit, and sintering at 1500-1600 ℃ for 1.5-3 h to obtain the 3D printing ceramic product.
6. The method for processing a long-wave low-temperature 3D printed ceramic product according to claim 5, wherein the power of the LED lamp in the step S2 is 800mW/cm2～1200mW/cm2。
7. The method for processing a long-wave low-temperature 3D printed ceramic product according to claim 5, wherein the power of the LED lamp in the step S3 is 1000mW/cm2～1400mW/cm2。
8. The method for processing a long-wave low-temperature 3D printed ceramic product according to claim 5, wherein the power of the LED lamp in the step S4 is 1200mW/cm2～1600mW/cm2。
CN202011029959.XA 2020-09-27 2020-09-27 Long-wave low-temperature 3D printing ceramic material and product processing method Pending CN112159215A (en)

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