CN106830944B - Ceramic composite material and firing method and application thereof - Google Patents

Ceramic composite material and firing method and application thereof Download PDF

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Publication number
CN106830944B
CN106830944B CN201710157719.XA CN201710157719A CN106830944B CN 106830944 B CN106830944 B CN 106830944B CN 201710157719 A CN201710157719 A CN 201710157719A CN 106830944 B CN106830944 B CN 106830944B
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parts
ceramic composite
composite material
pumps
pump
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CN106830944A (en
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王征
王涛
王勇
王宇时
王雪莹
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Beijing Zhongxing Shiqiang Ceramic Bearing Co ltd
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Beijing Zhongxing Shiqiang Ceramic Bearing Co ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
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Abstract

The invention provides a ceramic composite material which is mainly prepared from the following raw materials: 5-30 parts of silicon nitride, 70-95 parts of silicon carbide and Al2O30.5-10 parts of, Y2O30.5-10 parts of Er2O3And/or Yb2O30.5-8 parts. The invention also provides a firing method of the ceramic composite material, which comprises the following steps: 1) mixing the raw materials for preparing the ceramic composite material, and adding absolute ethyl alcohol for grinding; 2) adding a binder and a dispersant into the ground mixture, uniformly mixing and stirring, then performing spray drying and granulation; 3) preparing the powder obtained after granulation into a biscuit; 4) and sintering the biscuit under high pressure in a high-purity inert gas environment. The invention also provides application of the ceramic composite material in preparation of various pumps, wherein the pumps comprise a full-ceramic canned motor pump, a magnetic pump, a vane pump, a gear pump, a cam rotor pump, a screw pump and an aluminum liquid delivery pump.

Description

Ceramic composite material and firing method and application thereof
Technical Field
The invention relates to the field of ceramic materials, in particular to a ceramic composite material and a firing method and application thereof
Background
With the development of science and technology, green and environment-friendly products are more and more concerned by various industries. At present, the high-end magnetic pumps, canned pumps, gear pumps, cam rotor pumps, metering pumps and other chemical pumps at home and abroad are manufactured by using pressureless sintered silicon carbide to manufacture parts such as ceramic sliding bearing assemblies, pump shafts and the like, and other parts of the pumps are also manufactured by using stainless steel, hastelloy, titanium alloy, carbon steel, cast iron and other materials. In the case of pumps which are used under severe environmental requirements such as wear resistance, corrosion resistance, high temperature resistance and the like and are proposed in the industries of sanitation, food, medicine and fine chemical industry, metal materials cannot meet the requirements. At present, pressureless sintered silicon carbide which is widely adopted at home and abroad has good wear resistance, corrosion resistance, performance and low price, but the silicon carbide is easy to break suddenly due to low strength, so that the whole equipment is damaged. At present, the silicon carbide is only limited to sliding bearings for various pumps and pump shafts and sintered without pressure, and large-size structural parts are difficult to sinter.
The invention aims to meet the requirements of pump components such as various pump bodies, impellers, cam rotors, gears, screw rods, plungers and the like, and solves the problems of improving the strength and hardness of the pump components, improving the toughness, improving the wear resistance of pump parts, prolonging the service life of the pump components and the like. A ceramic composite material is provided for manufacturing various pump components.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a ceramic composite material which has high bending strength, good fracture toughness, high microhardness and good corrosion resistance, and can be used in a corrosive or high-temperature environment to meet the requirements of various pump components such as pump bodies, impellers, cam rotors, gears, screw rods, plungers, etc.
The second purpose of the invention is to provide the firing method of the ceramic composite material, the method adopts high-pressure sintering, the density of the finished product of the fired product can be improved, and the parameters selected in the process are particularly suitable for firing for preparing the ceramic composite material provided by the invention.
The third purpose of the invention is to provide the application of the ceramic composite material in the preparation of pumps, and the material of the invention is suitable for preparing various pumps due to the good properties of the material.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
one aspect of the present invention relates to a ceramic composite material, which is mainly made of the following raw materials:
5-30 parts of silicon nitride,
70-95 parts of silicon carbide,
Al2O30.5 to 10 portions of the raw materials,
Y2O30.5 to 10 parts, and
Er2O3and/or Yb2O30.5-8 parts.
According to the ceramic composite material, silicon carbide is used as a main base material, the silicon carbide-based ceramic has the characteristics of corrosion resistance, high temperature resistance, thermal shock resistance, wear resistance, good thermal conductivity, light weight and the like, and a small amount of silicon nitride is added, so that the ceramic material can have good mechanical properties, thermal properties and chemical stability. The silicon carbide-silicon nitride composite ceramic material is a high-temperature structural ceramic, and is generally difficult to realize sintering densification2O3And Y2O3The sintering aid forms yttrium aluminum garnet in the sintering process, permeates into a surrounding matrix, can realize densification sintering at a lower temperature, improves the microstructure of the ceramic, endows the ceramic with better mechanical property, and does not influence the properties of other aspects of the ceramic, particularly the corrosion resistance and the mechanical property, in addition, the invention further adds Er2O3Or Yb2O3Or a mixture of the two, can further improve the mechanical properties of the ceramic material, particularly the bending strength and the fracture toughness.
Preferably, the ceramic composite material comprises the following components in parts by weight:
15-25 parts of silicon nitride;
75-85 parts of silicon carbide;
Al2O35-10 parts of (A) a water-soluble polymer,
Y2O35 to 10 parts, and
Er2O3and/or Yb2O34-6 parts.
Preferably, Al2O3And Y2O3In a weight ratio of 1: 1.
Preferably, the silicon nitride is α -Si3N4And/or β -Si3N4Preferably, the silicon nitride has a purity greater than 98% and a primary particle size less than 3 microns.
Preferably, the silicon carbide is alpha-SiC with a purity greater than 98% and a particle size of 0.5-1.5 microns.
Preferably, said Er2O3、Yb2O3、Al2O3And Y2O3The purity of the particles is respectively more than 99.99 percent and the particle size is respectively 0.5 to 1.5 microns.
The invention selects silicon carbide, silicon nitride and Er with specific purity and grain diameter range2O3、Yb2O3、Al2O3And Y2O3After the raw materials are uniformly mixed, the particles with different particle diameters can be well and compactly stacked, so that the forming rate of the biscuit can be improved after forming, the biscuit with higher density can be formed, and finally the density of the ceramic material is improved.
Another aspect of the present invention relates to a method for firing a ceramic composite, the method comprising the steps of:
1) mixing the raw materials for preparing the ceramic composite material, and adding absolute ethyl alcohol for grinding;
2) adding a binder and a dispersant into the ground mixture, uniformly mixing, carrying out spray drying, and granulating;
3) pressing and molding the powder obtained after granulation to prepare a biscuit;
4) and sintering the biscuit under high pressure in a high-purity inert gas environment.
The firing method adopted by the invention is characterized in that the added absolute ethyl alcohol is generally industrial grade 99.99% absolute ethyl alcohol, a proper amount of grinding is added, the amount of the grinding is the conventional amount in the field, the absolute ethyl alcohol can be added according to the needs by the technicians in the field, then stirring and grinding are carried out, the mixture is pumped into a spray granulation tower to be spray-dried and granulated, and the mixture is sieved by a sieve of 80-120 meshes through vibration. And the granules are molded after granulation, so that the granules after granulation have good fluidity and uniform size and are easy to fill uniformly. The method is firstly easy to reduce the porosity in the forming process, improve the density of the biscuit and enable the biscuit to have certain strength, secondly is easy to enable the density of the biscuit to be uniform and improve the forming rate, and is beneficial to improving the physical and chemical properties of the finished product in all aspects. The product molding can select compression molding or cold isostatic pressing molding or other molding modes according to the structure and the size of the prepared product. The formed biscuit can be processed or preprocessed according to the size and the shape. And products with larger sizes also need to be subjected to presintering and debonding, wherein the presintering is conventional presintering in the field, the presintering conditions can be selected by a person skilled in the art according to the needs, and then the presintering biscuit is placed into a pressure sintering furnace to be sintered in a high-purity inert gas environment.
Preferably, in the step 1), the grinding time is 10-20 h.
Preferably, the sintering process in the step 4) is to heat up to 1000-1200 ℃ at a speed of 10-20 ℃/min, then fill high-purity inert gas into the sintering furnace, keep the temperature, heat up to 1800-2000 ℃ at a speed of 10-25 ℃/min, and keep the temperature.
The sintering process adopted by the invention is a twice heating process, which is beneficial to improving the yield, and can improve the physical and chemical properties of the finally fired product, particularly the bending strength and the fracture toughness, and the twice heat preservation time can be determined according to the size and the dimension of the workpiece. The heat preservation time in the sintering process can be determined according to the size of the workpiece, and generally, the first heat preservation time is 60-120min, and the heat preservation time after temperature rise is 400-600 min.
Preferably, after the high-purity argon is filled, the pressure in the sintering furnace is 7.5-9 MPa.
The filling of the pure inert gas is helpful for the fired ceramic to have higher density and better applicability.
Another aspect of the invention relates to the use of the ceramic composite material in corrosion or high temperature resistant equipment or components; preferably, the ceramic composite material is used for manufacturing a pump body, pump parts, a shielding case and a magnetic driver; more preferably, the pump comprises an all-ceramic canned motor pump, a magnetic pump, a vane pump, a gear pump, a cam rotor pump, a screw pump and an aluminum liquid delivery pump.
The ceramic composite material has excellent chemical corrosion resistance, high temperature resistance, wear resistance and excellent mechanical properties, can be used in corrosive environments or high-temperature environments, mainly aims at certain special industries, adopts equipment or parts in environments which cannot be met by special materials such as stainless steel, titanium alloy and the like, is particularly suitable for equipment or parts in the chemical field and industries such as pharmacy, food, fine chemistry and the like, can be used for manufacturing pump bodies of various pumps and various parts for the pumps, such as impellers, pump shafts, cam rotor pumps, gears, gear shafts, screws and the like, and can also be manufactured into various parts such as isolating covers of ceramic composite materials, magnetic drivers of ceramic composite materials and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. in the ceramic composite material, silicon nitride component and Al are added into silicon carbide material2O3-Y2O3-Er2O3-Yb2O3The multi-element sintering aid enables the ceramic material to have good mechanical properties while having corrosion resistance, high temperature resistance and wear resistance of common silicon carbide ceramic materials;
2. the ceramic composite material can realize compact sintering at a lower temperature;
3. the process adopts a secondary sintering mode, enables the ceramic material components to be fully sintered through a specific temperature rise curve, and enables the prepared ceramic product to have higher sintering density through a gas-phase high-pressure sintering mode;
4. the ceramic of the present invention has excellent corrosion resistance, high temperature resistance, wear resistance, strength, toughness and density, so that it has wide application range, and is especially suitable for preparing pumps under various special conditions.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The composition ratio of silicon nitride and silicon carbide used in this example is: weighing Si3N4The powder accounts for 10 percent of the weight, and the silicon carbide SiC powder accounts for 90 percent of the weight. Additive Al2O3And Y2O3The addition amount of the modifier is 0.5 percent of the total weight of the silicon carbide and the silicon nitride, and the modifier Yb2O3The addition amount of (B) is 0.5% of the total weight of silicon carbide and silicon nitride, and the purity is 99.99%.
Wherein the silicon nitride is α -Si3N4The purity of the silicon nitride is more than 98 percent, and the original particle size is less than 3 microns.
The silicon carbide is alpha-SiC, the purity is more than 98%, and the granularity is 0.5-1.5 microns.
The manufacturing process comprises the following steps:
1. firstly, the powder, the additive and the toughening agent are respectively weighed according to the component proportion and added into a stirring mill of silicon nitride, and a proper amount of silicon nitride balls are added. Adding a proper amount of industrial grade 99.99% absolute ethyl alcohol, stirring and grinding for 10 hours, directly sending the mixture into a spray granulation tower through a diaphragm pump for spray drying granulation, and sieving the granules by a vibrating sieve with a sieve of 80-120 meshes for later use.
2. The product molding can select compression molding and cold isostatic pressing molding according to the structure and the size of the pump, and the pressure can be controlled at 180-250 MPa. The formed biscuit can be processed or preprocessed according to the size and the shape. And (3) presintering and debonding products with larger sizes, then putting the presintering biscuit into a pneumatic sintering furnace for pneumatic sintering, heating to 1000 ℃ at the heating speed of 10 ℃/min, introducing high-purity argon or high-purity nitrogen to ensure that the pressure in the furnace reaches 7.5MPa, preserving the heat for 60 minutes, then heating to 1800 ℃ at the heating speed of 10 ℃/min, and keeping the pressure in the furnace at 7.5MPa, and preserving the heat for 400 minutes.
The main performance indexes of the composite ceramic product are 740MPa of bending strength and 7.5MPa of fracture toughness HV 2750. Density 3.25g/cm3。
Example 2
The composition ratio of silicon nitride and silicon carbide used in the experiment is as follows:weighing Si3N425% of powder and 75% of silicon carbide SiC powder. Additive Al2O3And Y2O3The addition amount of the silicon carbide and the silicon nitride is 2.5 percent of the total weight of the silicon carbide and the silicon nitride, and the modifier is erbium oxide Er2O3The addition amount of (B) is 1.5% of the total weight of silicon carbide and silicon nitride, and the purity is 99.99%.
Wherein the silicon nitride is α -Si3N4The purity of the silicon nitride is more than 98 percent, and the original particle size is less than 3 microns.
The silicon carbide is alpha-SiC, the purity is more than 98%, and the granularity is 0.5-1 micron.
The manufacturing process comprises the following steps:
1. firstly, the powder, the additive and the toughening agent are respectively weighed according to the component proportion and added into a stirring mill of silicon nitride, and a proper amount of silicon nitride balls are added. Adding a proper amount of industrial grade 99.99% absolute ethyl alcohol, stirring and grinding for 15-20 hours. Directly sending into a spray granulation tower through a diaphragm pump for spray drying granulation, and sieving through a vibrating sieve with a sieve of 80-120 meshes for later use.
2. The product molding can select compression molding and cold isostatic pressing molding according to the structure and the size of the pump, and the pressure can be controlled at 180-250 MPa. The formed biscuit can be processed or preprocessed according to the size and the shape. And (3) presintering and debonding products with larger sizes, then putting the presintering biscuit into a pneumatic sintering furnace for pneumatic sintering, heating to 1200 ℃ at the heating speed of 20 ℃/min, introducing high-purity argon or high-purity nitrogen to keep the temperature of the furnace pressure at 8MPa for 120 minutes, heating to 2000 ℃ at the heating speed of 25 ℃/min, keeping the pressure in the furnace at 8MPa, and keeping the temperature for 600 minutes.
The main performance indexes of the composite ceramic product are bending strength 780MPa and fracture toughness 7.9MPa microhardness HV 2430. Density 3.41g/cm3。
Example 3
The composition ratio of silicon nitride and silicon carbide used in the experiment is as follows: weighing Si3N45% of powder and 95% of silicon carbide SiC powder. Additive Al2O3And Y2O3The addition amount of the modifier is 10 percent of the total weight of the silicon carbide and the silicon nitride, and the modifier Er2O3And Yb2O3The addition amount of the silicon carbide is 4 percent of the total weight of the silicon carbide and the silicon nitride, and the purity is 99.99 percent.
The silicon carbide alpha-SiC is obtained, the purity of the silicon nitride is more than 98%, and the original particle size is less than 3 microns.
The silicon nitride is α -Si3N4And β -Si3N4The mixture of (1) has a purity of greater than 98% and a particle size of 0.5-1 micron.
The manufacturing process comprises the following steps:
1. firstly, the powder, the additive and the toughening agent are respectively weighed according to the component proportion and added into a stirring mill of silicon nitride, and a proper amount of silicon nitride balls are added. Adding a proper amount of industrial grade 99.99% absolute ethyl alcohol, stirring and grinding for 15-20 hours. Directly sending into a spray granulation tower through a diaphragm pump for spray drying granulation, and sieving through a vibrating screen and a 80-mesh sieve for later use.
2. The product molding can select compression molding and cold isostatic pressing molding according to the structure and the size of the pump, and the pressure can be controlled at 180-250 MPa. The formed biscuit can be processed or preprocessed according to the size and the shape. And (3) presintering and debonding products with larger sizes, then putting the presintering biscuit into a pneumatic sintering furnace for pneumatic sintering, heating to 1200 ℃ at the heating speed of 15 ℃/min, introducing high-purity argon or high-purity nitrogen to ensure that the pressure in the furnace reaches 8.5MPa, preserving the heat for 100 minutes, then heating to 2000 ℃ at the heating speed of 15 ℃/min, and keeping the pressure in the furnace at 8.5MPa, and preserving the heat for 600 minutes.
The main performance indexes of the composite ceramic product are obtained, namely the bending strength of 841MPa and the fracture toughness of 8.3MPa, and the microhardness of HV 2857. Density 3.58g/cm3。
Example 4
The composition ratio of silicon nitride and silicon carbide used in the experiment is as follows: weighing Si3N430% of powder and 70% of silicon carbide SiC powder. Additive Al2O3And Y2O3Is added toThe addition amount of the modifier Er is 5 percent of the total weight of the silicon carbide and the silicon nitride2O3And Yb2O3The addition amount of the silicon carbide is 3 percent of the total weight of the silicon carbide and the silicon nitride, and the purity is 99.99 percent.
Wherein the silicon nitride is α -Si3N4The purity of the silicon nitride is more than 98 percent, and the original particle size is less than 3 microns.
The silicon carbide is alpha-SiC, the purity is more than 98%, and the granularity is 1-1.5 microns.
The manufacturing process comprises the following steps:
1. firstly, the powder, the additive and the toughening agent are respectively weighed according to the component proportion and added into a stirring mill of silicon nitride, and a proper amount of silicon nitride balls are added. Adding a proper amount of industrial grade 99.99% absolute ethyl alcohol, stirring and grinding for 15-20 hours. Directly sending into a spray granulation tower through a diaphragm pump for spray drying granulation, and sieving through a vibrating screen and a 80-mesh sieve for later use.
2. The product molding can select compression molding and cold isostatic pressing molding according to the structure and the size of the pump, and the pressure can be controlled at 180-250 MPa. The formed biscuit can be processed or preprocessed according to the size and the shape. And (3) presintering and debonding products with larger sizes, then putting the presintering biscuit into a pneumatic sintering furnace for pneumatic sintering, heating to 1100 ℃ at a heating speed of 10 ℃/min, introducing high-purity argon or high-purity nitrogen to ensure that the pressure in the furnace reaches 7.5MPa, preserving the heat for 110 minutes, then heating to 1800 ℃ at a speed of 25 ℃/min, and keeping the pressure in the furnace at 7.5MPa, and preserving the heat for 500 minutes.
The main performance indexes of the composite ceramic product are bending strength 827MPa and fracture toughness 8.3MPa microhardness HV 2695. Density 3.29g/cm3。
Example 5
The composition ratio of silicon nitride and silicon carbide used in the experiment is as follows: weighing Si3N415% of powder and 85% of silicon carbide SiC powder. Additive Al2O3And Y2O3The addition amount of the modifier is 5 percent of the total weight of the silicon carbide and the silicon nitride, and the modifier Er2O3And Yb2O3The addition amount of the silicon carbide is 2 percent of the total weight of the silicon carbide and the silicon nitride, and the purity is 99.99 percent.
Wherein the silicon nitride is α -Si3N4The purity of the silicon nitride is more than 98 percent, and the original particle size is less than 3 microns.
The silicon carbide is alpha-SiC, the purity is more than 98%, and the granularity is 1-1.5 microns.
The manufacturing process comprises the following steps:
1. firstly, the powder, the additive and the toughening agent are respectively weighed according to the component proportion and added into a stirring mill of silicon nitride, and a proper amount of silicon nitride balls are added. Adding a proper amount of industrial grade 99.99% absolute ethyl alcohol, stirring and grinding for 15-20 hours. Directly sending into a spray granulation tower through a diaphragm pump for spray drying granulation, and sieving through a vibrating screen and a 80-mesh sieve for later use.
2. The product molding can select compression molding and cold isostatic pressing molding according to the structure and the size of the pump, and the pressure can be controlled at 180-250 MPa. The formed biscuit can be processed or preprocessed according to the size and the shape. And (3) presintering and debonding products with larger sizes, then putting the presintering biscuit into a pneumatic sintering furnace for pneumatic sintering, heating to 1100 ℃ at a heating speed of 15 ℃/min, introducing high-purity argon or high-purity nitrogen to ensure that the pressure in the furnace reaches 8MPa, preserving the heat for 100 minutes, then heating to 1900 ℃ at a speed of 20 ℃/min, and keeping the pressure in the furnace at 8MPa, and preserving the heat for 500 minutes.
The main performance indexes of the composite ceramic product, namely the bending strength of 793MPa and the fracture toughness of 8.2MPa are HV 2516. Density 3.29g/cm3。
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims (9)

1. A method of firing a ceramic composite, the method comprising the steps of:
1) mixing the raw materials for preparing the ceramic composite material, and adding absolute ethyl alcohol for grinding;
2) adding a binder and a dispersant into the ground mixture, uniformly mixing, carrying out spray drying, and granulating;
3) pressing and molding the powder obtained after granulation to prepare a biscuit;
4) sintering the biscuit under high pressure in a high-purity inert gas environment; the sintering process in the step 4) is that high-purity inert gas is filled into the sintering furnace after the temperature is raised to 1000-1200 ℃ at the speed of 10-20 ℃/min, the temperature is preserved, and then the temperature is raised to 1800-2000 ℃ at the speed of 10-25 ℃/min, and the temperature is preserved;
the ceramic composite material is mainly prepared from the following raw materials:
5-30 parts of silicon nitride,
70-95 parts of silicon carbide,
Al2O30.5 to 10 portions of the raw materials,
Y2O30.5 to 10 parts, and
Er2O3and/or Yb2O30.5-8 parts;
the purity of the silicon nitride is more than 98 percent, and the original particle size is less than 3 microns;
the silicon carbide is alpha-SiC, the purity is more than 98%, and the granularity is 0.5-1.5 microns;
the Er2O3、Yb2O3、Al2O3And Y2O3The purity of the particles is respectively more than 99.99 percent and the particle size is respectively 0.5 to 1.5 microns.
2. The method of claim 1, wherein the ceramic composite comprises the following components in parts by weight:
15-25 parts of silicon nitride;
75-85 parts of silicon carbide;
Al2O35-10 parts of (A) a water-soluble polymer,
Y2O35 to 10 parts, and
Er2O3and/or Yb2O34-6 parts.
3. The method of claim 1, wherein Al is2O3And Y2O3In a weight ratio of 1: 1.
4. The method of claim 1, wherein the silicon nitride is α -Si3N4And/or β -Si3N4。
5. The method as claimed in claim 1, wherein the grinding time in step 1) is 10-20 h.
6. The method of claim 1, wherein after the high purity argon gas is introduced, the pressure in the sintering furnace is maintained at 7.5 to 9 Mpa.
7. Use of the ceramic composite material prepared by the method for firing a ceramic composite material according to any one of claims 1 to 6 for equipment or parts resistant to corrosion or high temperatures.
8. Use according to claim 7, wherein the ceramic composite material is used to form pump bodies, pump components, shielding cages, and magnetic drives.
9. The use of claim 8, wherein the pumps comprise all-ceramic canned pumps, magnetic pumps, vane pumps, gear pumps, lobe rotor pumps, screw pumps and aluminium liquid transfer pumps.
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