CN112341212A - Nano silicon carbide ceramic sintering stabilizer and preparation method thereof - Google Patents

Nano silicon carbide ceramic sintering stabilizer and preparation method thereof Download PDF

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CN112341212A
CN112341212A CN202011206979.XA CN202011206979A CN112341212A CN 112341212 A CN112341212 A CN 112341212A CN 202011206979 A CN202011206979 A CN 202011206979A CN 112341212 A CN112341212 A CN 112341212A
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silicon carbide
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龚晔
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Changzhou Geoquin Nano New Materials Co ltd
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Abstract

The invention belongs to the technical field of ceramic materials, and particularly relates to a nano-scale silicon carbide ceramic sintering stabilizer and a preparation method thereof. The nano silicon carbide ceramic sintering stabilizer consists of water, anhydrous acetic acid, citric acid, nano yttrium oxide and nano graphene composite powder. The obtained stabilizer is used for preparing the nanoscale silicon carbide ceramic, is uniformly dispersed in silicon carbide powder, can reduce the sintering temperature, and improves the sintering uniformity of silicon carbide powder particles, so that the high temperature resistance, the bending strength and the density of the silicon carbide ceramic are improved, and the prepared silicon carbide ceramic has lower porosity and higher thermal conductivity.

Description

Nano silicon carbide ceramic sintering stabilizer and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a nano-scale silicon carbide ceramic sintering stabilizer and a preparation method thereof.
Background
The silicon carbide ceramic has excellent mechanical property, oxidation resistance, high abrasion resistance, low friction coefficient and the like. The silicon carbide ceramic has the greatest characteristics of high-temperature strength, the strength of a common ceramic material is obviously reduced at 1200-1400 ℃, and the silicon carbide ceramic not only has high room-temperature strength, corrosion resistance, wear resistance and low friction coefficient, but also has high-temperature strength and creep resistance. The use temperature can reach 1600 ℃, and the silicon carbide ceramic has higher heat conduction capability and is second to beryllium oxide ceramic in the ceramic, so the silicon carbide is widely applied to the fields of high-temperature bearings, bulletproof plates, nozzles, high-temperature corrosion-resistant components, high-temperature and high-frequency range electronic equipment components and the like.
Silicon carbide pressureless sintering is a common sintering mode, but pressureless sintering temperature is 2100-2200 ℃, energy consumption is high, cost is high, reducing temperature can cause binding force among silicon carbide ceramic particles to be reduced, density is reduced, and if the sintering temperature can be reduced, the silicon carbide pressureless sintering is suitable for mass production; the hot-pressing sintering process can only produce SiC parts with simple shapes, and the product quantity produced by the one-time hot-pressing sintering process is very small, thus being not beneficial to industrial production; the hot isostatic pressing sintering can obtain a compact phase product with a complex shape, and the product has good mechanical properties, but the hip sintering needs to be sealed and blank, and industrial production is difficult to realize; the reaction sintering temperature is low (1400-1600 ℃), complex products can be produced, and 8-20% of free silicon still remains in the blank, which limits the high-temperature mechanical properties of the silicon carbide and the application of the silicon carbide in strong acid and strong alkali.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nano-scale silicon carbide ceramic sintering stabilizer and a preparation method thereof.
The invention provides a nano-scale silicon carbide ceramic sintering stabilizer which is composed of water, anhydrous acetic acid, citric acid, nano-scale yttrium oxide and nano-scale graphene composite powder, wherein the mass part ratio of the water, the anhydrous acetic acid, the citric acid and the nano-scale composite powder is as follows: 50: (5-10): (1-2): 5.
the nano-scale composite powder consists of nano-scale yttrium oxide powder with the particle size of 20-40nm and nano-scale graphene powder with the particle size of 50-100nm, and the composite powder comprises the following components in percentage by mass: 60-80% of nano-scale yttrium oxide powder and 20-40% of nano-scale graphene powder.
The invention also provides a preparation method of the nano silicon carbide ceramic sintering stabilizer, which comprises the following steps:
(1) according to the metering ratio, adding deionized water, anhydrous acetic acid and citric acid, fully stirring and adding into a horizontal grinder;
(2) respectively weighing nanometer yttrium oxide powder with the particle size of 20-40nm and nanometer graphene powder with the particle size of 50-100nm according to the metering ratio, and adding the nanometer yttrium oxide powder and the nanometer graphene powder into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential and viscosity of the slurry Zata; thus obtaining the nano silicon carbide ceramic sintering stabilizer.
The nano-scale silicon carbide ceramic sintering stabilizer prepared by the method is used for preparing nano-scale silicon carbide ceramic, and the specific application method comprises the following steps:
(1) and according to the metering ratio, putting deionized water into a ball mill, taking D50: putting 3-5 micron silicon carbide powder into a ball mill for ball milling for 10 minutes;
the mass ratio of the silicon carbide powder to the water is 1: 1.5-2.5.
(2) Adding the obtained ceramic sintering stabilizer into a ball mill for ball milling for 2-4 hours;
the addition amount of the ceramic sintering stabilizer is 1-3% of the mass of the micron silicon carbide powder;
(3) granulating the mixture obtained in the step (2) by using a spray granulator to obtain a granulated particle size D50: 40 microns;
inlet temperature of the spray granulator: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 150-200 g/min.
(4) Putting the silicon carbide powder obtained in the step (3) into a steel die with the diameter of 30mm, pressurizing to 15Mpa on a press machine, and keeping for 10 minutes to form a blank with a certain shape;
(5) and putting the pressed blank into a vacuum sintering furnace for calcining.
Wherein the sintering process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa。
Has the advantages that:
(1) the sintering stabilizer provided by the invention is uniformly dispersed in the silicon carbide powder, can reduce the sintering temperature and improve the sintering uniformity of silicon carbide powder particles, thereby improving the high temperature resistance, bending strength and density of the silicon carbide ceramic.
(2) Anhydrous acetic acid and citric acid are adopted to adjust the isoelectric point of the stabilizer, and the Zata potential value of the stabilizer is improved.
(3) The prepared silicon carbide ceramic has lower porosity and higher thermal conductivity.
Drawings
FIG. 1 is an electron micrograph of a portion of a sintered silicon carbide ceramic part according to example 1;
FIG. 2 is an electron micrograph of a portion of a sintered silicon carbide ceramic part according to example 2;
FIG. 3 is an electron micrograph of a portion of a sintered silicon carbide ceramic part according to comparative example 1;
FIG. 4 is an electron micrograph of a portion of a sintered silicon carbide ceramic part of comparative example 2;
FIG. 5 is an electron micrograph of a portion of a sintered silicon carbide ceramic part of comparative example 3;
FIG. 6 is an electron micrograph of a portion of a sintered silicon carbide ceramic part of comparative example 4;
FIG. 7 is an electron micrograph of a portion of a sintered silicon carbide ceramic part of comparative example 5.
Detailed Description
The present invention is further described below with reference to examples, but is not limited thereto.
Example 1
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 20g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 80g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 20 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry to obtain a ceramic sintering stabilizer, and detecting the potential of the slurry Zata to be 80mv and the viscosity to be 2000 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 170g/min, particle size after granulation D50: 40 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 3.3g/cm3The bending strength is 650Mpa, the thermal conductivity is 210W/m.k, and the apparent porosity is less than or equal to 0.16%.
Example 2
(1) Adding 150g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 80g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 20 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 82mv and the viscosity to be 2150 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 150g/min, particle size after granulation D50: 43 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 3.2g/cm3Bending strength 640Mpa, thermal conductivity 205W/m.k, apparent porosity less than or equal to 0.17%.
Example 3
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata at 81mv and the viscosity at 2150 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 3.25g/cm3Bending strength 645Mpa, thermal conductivity 213W/m.k, apparent porosity less than or equal to 0.15%.
Example 4
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 20g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 83mv and the viscosity to be 2150 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 100ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 4 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is maintained at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1900 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphereNull condition 6X 10-2Pa, detection density of the ceramic part is 2.9g/cm3Bending strength 590MPa, thermal conductivity 203W/m.k, apparent porosity less than or equal to 0.18%.
Example 5
(1) Adding 200g of anhydrous acetic acid (98%) into 1L of deionized water, adding 40g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential 84mv and the viscosity 2230mpa.s of the slurry Zata;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2.5kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 100ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 4 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1900 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, and the sintering atmosphere is vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 3.3g/cm3The bending strength is 630MPa, the thermal conductivity is 215W/m.k, and the apparent porosity is less than or equal to 0.16 percent.
Example 6
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 70g of the mixture with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 30 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 83mv and the viscosity to be 2150 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 3kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 300ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 4 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1900 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, and the sintering atmosphere is vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 3.31g/cm3The bending strength is 630MPa, the thermal conductivity is 219W/m.k, and the apparent porosity is less than or equal to 0.17 percent.
Comparative example 1
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of particles with the particle size of 100-: 10-15m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 50mv and the viscosity to be 2000 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 170g/min, particle size after granulation D50: 40 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 2.5g/cm3Bending strength of 450Mpa, thermal conductivity of 65W/m.k, apparent porosity of 0.35% or less.
Comparative example 2
(1) Adding 130g of anhydrous acetic acid (98%) into 1L of deionized water, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential 42mv and the viscosity 1150mpa.s of the slurry Zata;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 36 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 2.1g/cm3Bending strength is 360Mpa, thermal conductivity is 115W/m.k, and apparent porosity is less than or equal to 0.45%.
Comparative example 3
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential 83mv and the viscosity 2250mpa.s of the slurry Zata;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 1000ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 2.2g/cm3The bending strength is 380MPa, the thermal conductivity is 106W/m.k, and the apparent porosity is less than or equal to 0.33 percent.
Comparative example 4
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of oxalic acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano graphene powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 25mv and the viscosity to be 550 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept between 0 ℃ and 800 ℃ for 30 minutes, and the temperature is kept between 800 ℃ and 1200 DEG CThe temperature is kept for 60 minutes, the temperature is kept at 1400 ℃ for 100 minutes at 1200 ℃ and 1700 ℃ for 10 hours at the temperature of 1400 ℃ and the heating rate is 10-20 ℃/min, and the sintering atmosphere is a vacuum condition of 6 multiplied by 10-2Pa, detection density of the ceramic part is 1.9g/cm3The bending strength is 320Mpa, the thermal conductivity is 95W/m.k, and the apparent porosity is less than or equal to 0.45 percent.
Comparative example 5
(1) Adding 100g of anhydrous acetic acid (98%) into 1L of deionized water, adding 30g of citric acid, fully stirring, and adding into a horizontal grinding machine;
(2) respectively weighing 60g of the powder with the particle size of 20-40nm and BET: 30-40m2Adding per gram of nano yttrium oxide powder and 40 grams of nano aluminum oxide powder composite powder with the grain diameter of 50-100nm into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotating speed is 2500r/min, and the grinding time is 2 hours; taking out the ground slurry, and detecting the potential of the slurry Zata to be 25mv and the viscosity to be 550 mpa.s;
(4) and 5kg of deionized water is taken and put into a ball mill, and D50: 2kg of 3-5 micron silicon carbide powder is put into a ball mill for ball milling for 10 minutes;
(5) adding 200ml of the ceramic sintering stabilizer obtained in the step (3) into a ball mill for ball milling for 2 hours;
(6) and (3) granulating the mixture obtained in the step (5) by using a spray granulator, wherein the inlet temperature is as follows: 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 200g/min, particle size after granulation D50: 38 microns;
(7) putting the silicon carbide powder obtained in the step (6) into a steel die with the diameter of 30mm, separating, and pressurizing to 15Mpa on a press machine for 10 minutes to form a blank with a certain shape;
(8) and placing the pressed blank body into a vacuum sintering furnace for calcination, wherein the calcination process comprises the following steps: the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1900 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, and the sintering atmosphere is vacuum condition of 6 x 10-2Pa, detection density of the ceramic part is 2.6g/cm3Bending strength 480Mpa, thermal conductivity 150W/m.k, apparent porosity less than or equal to 0.3%.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.

Claims (8)

1. The nano-scale silicon carbide ceramic sintering stabilizer is characterized by consisting of water, anhydrous acetic acid, citric acid, nano-scale yttrium oxide and nano-scale graphene composite powder, wherein the mass part ratio of the water, the anhydrous acetic acid, the citric acid and the nano-scale composite powder is as follows: 50: 5-10: 1-2: 5.
2. the nano-scale silicon carbide ceramic sintering stabilizer according to claim 1, wherein the nano-scale composite powder consists of nano-scale yttrium oxide powder with the particle size of 20-40nm and nano-scale graphene powder with the particle size of 50-100nm, and the composite powder comprises the following components in percentage by mass: 60-80% of nano-scale yttrium oxide powder and 20-40% of nano-scale graphene powder.
3. The preparation method of the nano-scale silicon carbide ceramic sintering stabilizer according to claim 1, characterized by comprising the following steps:
(1) according to the metering ratio, adding deionized water, anhydrous acetic acid and citric acid, fully stirring and adding into a horizontal grinder;
(2) respectively weighing nanometer yttrium oxide powder with the particle size of 20-40nm and nanometer graphene powder with the particle size of 50-100nm according to the metering ratio, and adding the nanometer yttrium oxide powder and the nanometer graphene powder into a horizontal grinding machine;
(3) starting grinding, wherein the grinding rotation speed is 2500-; taking out the ground slurry, and detecting the potential and viscosity of the slurry Zata; thus obtaining the nano silicon carbide ceramic sintering stabilizer.
4. A method for preparing nanoscale silicon carbide ceramic, which is characterized in that the stabilizer of claim 1 is used for preparing nanoscale silicon carbide ceramic, and the preparation method comprises the following steps:
(1) putting deionized water into a ball mill, taking D50: putting 3-5 micron silicon carbide powder into a ball mill for ball milling for 10 minutes;
(2) adding the ceramic sintering stabilizer into a ball mill for ball milling for 2-4 hours;
(3) granulating the mixture obtained in the step (2) by using a spray granulator to obtain a granulated particle size D50: 30-50 microns;
(4) putting the silicon carbide powder obtained in the step (3) into a steel die with the diameter of 30mm, pressurizing to 15Mpa on a press machine, and keeping for 10 minutes to form a blank with a certain shape;
(5) and putting the pressed blank into a vacuum sintering furnace for calcining.
5. The method for preparing nano-scale silicon carbide ceramic according to claim 4, wherein the mass ratio of the silicon carbide powder to the water in the step (1) is 1: 1.5-2.5.
6. The method for preparing nano-scale silicon carbide ceramic according to claim 4, wherein the addition amount of the ceramic sintering stabilizer in the step (2) is 1-3% of the mass of the micro-scale silicon carbide powder.
7. The method for preparing nanoscale silicon carbide ceramic according to claim 4, wherein the inlet temperature of the spray granulator in the step (3): 250 ℃, outlet temperature: 120 ℃, rotation speed of the atomizing disc: 25000r/min, flow rate: 150-200 g/min.
8. The method for preparing nanoscale silicon carbide ceramic according to claim 4, wherein the sintering process of step (5): the temperature is kept at 0-800 ℃ for 30 minutes, at 800-1200 ℃ for 60 minutes, at 1200-1400 ℃ for 100 minutes, at 1400-1700 ℃ for 10 hours, at a heating rate of 10-20 ℃/min, in a sintering atmosphere under a vacuum condition of 6 x 10-2Pa。
CN202011206979.XA 2020-11-03 2020-11-03 Nano silicon carbide ceramic sintering stabilizer and preparation method thereof Pending CN112341212A (en)

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