CN106830944A - A kind of ceramic composite and its method for cooking and application - Google Patents

A kind of ceramic composite and its method for cooking and application Download PDF

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Publication number
CN106830944A
CN106830944A CN201710157719.XA CN201710157719A CN106830944A CN 106830944 A CN106830944 A CN 106830944A CN 201710157719 A CN201710157719 A CN 201710157719A CN 106830944 A CN106830944 A CN 106830944A
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China
Prior art keywords
pump
parts
ceramic composite
silicon nitride
carborundum
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CN201710157719.XA
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Chinese (zh)
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CN106830944B (en
Inventor
王征
王涛
王勇
王宇时
王雪莹
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Beijing Zhong Xing Shi Qiang Ceramic Bearing Co Ltd
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Beijing Zhong Xing Shi Qiang 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 kind of ceramic composite, the ceramic composite is mainly made up of following raw material：5 30 parts of silicon nitride, 70 95 parts of carborundum, Al2O30.5 10 parts, Y2O30.5 10 parts, and Er2O3And/or Yb2O30.5 8 parts.Present invention also offers the method for cooking of the ceramic composite, the method includes：1) the raw material mixing of ceramic composite will be prepared, adds absolute ethyl alcohol to be ground；2) it is spray-dried again to addition binding agent in the mixture after grinding and dispersant and after carrying out mixing and stirring, is granulated；3) powder obtained after granulation is made biscuit；4) biscuit described in high-pressure sinter under high purity inert gas environment.Present invention also offers application of the ceramic composite in various pumps are prepared, the pump includes complete ceramic screened pump, magnetic drive pump, vane pump, gear pump, lobed rotor pump, screw pump and aluminium liquid delivery pump.

Description

A kind of ceramic composite and its method for cooking and application
Technical field
The present invention relates to ceramic material field, in particular to a kind of ceramic composite and its method for cooking and should With
Background technology
With the development of science and technology, the product of environmental type is increasingly paid close attention to by every profession and trade.At present both at home and abroad The chemical pumps such as high-end magnetic drive pump, canned motor pump, gear pump, lobed rotor pump, measuring pump are largely using the manufacture of pressureless sintering carborundum The part such as ceramic slide bearing component and pump shaft, other parts of pump still use stainless steel, breathe out tin alloy, titanium alloy, carbon steel, The material manufactures such as cast iron.Wear-resistant, corrosion-resistant, high temperature resistant proposed in face of the industry of health, food, medicine and fine chemistry industry etc. To the pump used under environmental requirement exacting terms, metal material cannot meet its requirement.And a large amount of uses both at home and abroad at present Pressureless sintering carborundum is although wear-resistant, corrosion-resistant, function admirable, and price is relatively low, but because the intensity of carborundum is relatively low, its Easily there is fracture suddenly, cause integral device to damage.Only it is confined to be used on the sliding bearing of various pumps and pump shaft at present Pressureless sintering carborundum, and large-sized structural member sintering is difficult.
The present invention is the need for meeting the parts of pump such as the various pump housings, impeller, cam follower, gear, sieve bar, plunger, to carry The problems such as intensity, hardness, the toughness that improves, wearability and service life of raising pump parts of the part of pump high.There is provided a kind of For manufacturing the ceramic composite of various pump parts.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of ceramic composite, and ceramic composite bending strength is high, fracture Good toughness, microhardness are high, good corrosion resistance, its can be used for that corrosivity is strong or high temperature in the environment of, meet the various pump housings, The need for the parts of pump such as impeller, cam follower, gear, sieve bar, plunger.
The second object of the present invention is the method for cooking for providing the ceramic composite, and the method selects high pressure combustion Knot, it is possible to increase the density of the finished product of burned product, the parameter selected in technique is particularly suitable for preparing the ceramics of present invention offer The firing of composite.
The third object of the present invention is the application for providing the ceramic composite in pump is prepared, material of the invention Because its multiple performance is good, it is suitable for preparing various pumps.
In order to realize above-mentioned purpose of the invention, spy uses following technical scheme：
One aspect of the present invention is related to a kind of ceramic composite, and the ceramic composite is main by following raw material system Into：
Silicon nitride 5-30 parts,
Carborundum 70-95 parts,
Al2O30.5-10 parts,
Y2O30.5-10 parts, and
Er2O3And/or Yb2O30.5-8 parts.
Ceramic composite of the invention, is main base material with carborundum, and types of silicon carbide-based ceramics has corrosion-resistant, resistance to height Temperature, anti-thermal shock, wear-resistant, heat conductivity be good and the features such as light weight, while a small amount of silicon nitride of addition, can assign pottery The good mechanical property of ceramic material, thermal property and chemical stability.Silicon-carbide-silicon nitride composite ceramic material is high temperature knot Structure ceramic, usual sintering densification relatively difficult to achieve the characteristics of the present invention is for silicon-carbide-silicon nitride base material, adds Al2O3With Y2O3Sintering aid, forms yttrium-aluminium-garnet during sintering, in penetrating into the matrix of surrounding, can be at a lower temperature Densification sintering is realized, improves the heterogeneous microstructure of ceramics, assign ceramics preferably mechanical property, and do not interfere with ceramics Other side performance particularly corrosion resistance and mechanical property, in addition, the present invention is further by adding Er2O3Or Yb2O3, or the mixture of both, can further improve the mechanical property of ceramic material, particularly bending strength and fracture Toughness.
Preferably, the ceramic composite includes following components by weight：
Silicon nitride 15-25 parts；
Carborundum 75-85 parts；
Al2O35-10 parts,
Y2O35-10 parts, and
Er2O3And/or Yb2O34-6 parts.
Preferably, Al2O3And Y2O3Weight ratio be 1:1.
Preferably, the silicon nitride is α-Si3N4And/or β-Si3N4, it is preferable that the purity of the silicon nitride is more than 98%, original particle size is less than 3 microns.
Preferably, the carborundum is α-SiC, and purity is 0.5-1.5 microns more than 98%, granularity.
Preferably, the Er2O3、Yb2O3、Al2O3And Y2O3Purity be respectively greater than 99.99%, granularity respectively 0.5- 1.5 microns.
Carborundum, silicon nitride, the Er of the selected certain pure of the present invention and particle size range2O3、Yb2O3、Al2O3And Y2O3, these After well mixed, the particle of its different-grain diameter can be realized preferably more densely piling up raw material, and then after shaping, can The ratio of briquetting of biscuit is improved, and forms the biscuit of higher density, the final density for improving ceramic material.
The method for cooking of the described ceramic composite of another aspect of the present invention design, methods described includes following step Suddenly：
1) the raw material mixing of ceramic composite will be prepared, adds absolute ethyl alcohol to be ground；
2) to binding agent and dispersant is added in the mixture after grinding, it is well mixed and is spray-dried, granulates；
3) the powder pressing shaping that will be obtained after granulation, is made biscuit；
4) biscuit described in high-pressure sinter under high purity inert gas environment.
The method for cooking that the present invention is used, the absolute ethyl alcohol of addition is generally the 99.99% of technical grade absolute ethyl alcohol, plus Enter and be ground in right amount, its consumption is the conventional amount used of this area, those skilled in the art can be added as needed, afterwards It is stirred grinding, then pumps into and be spray-dried in mist projection granulating tower, granulates, then sieved by vibrated 80--120 mesh. It is molded after granulation, the mobility of particle after granulation is good, and size is more homogeneous, easily filling is uniform.This method is first It is easy to reduce porosity in forming process, improves the density of biscuit, and make biscuit that there is certain intensity, next to that is easy to make Blank density is uniform, improves ratio of briquetting, is advantageous for improving finished product physicochemical property in every respect again.Formed product can be with root According to the structure snd size size of prepared product, compression molding or cold isostatic compaction, or other molding modes are selected.Into Biscuit after type can be machined or preprocessing according to size shape size.Larger-size product also needs to carry out pre-sintering The conventional pre-sintering in this area is become in unsticking, the pre-burning, and pre-sintered condition those skilled in the art can be carried out as needed , then be put into pre-sintered biscuit in gas pressure sintering stove by selection, is sintered under high-purity inert gas environment.
Preferably, the step 1) in, the time of the grinding is 10-20h.
Preferably, the step 4) described in sintering process be that 1000C-1200 is warming up to the speed of 10-20 DEG C/min High purity inert gas are filled with DEG C backward sintering furnace, are incubated, then 1800-2000 DEG C is warmed up to the speed of 10-25 DEG C/min, protected Temperature.
For temperature-rise period twice, one is advantageous for raising yield rate to the sintering process that uses of the present invention, and two is to improve The physicochemical property of the final product fired, particularly bending strength and fracture toughness, soaking time can be according to workpiece twice Size and size determine.Soaking time in sintering process can be determined according to the size of workpiece, it is generally the case that first The time of secondary insulation is 60-120min, and the soaking time after intensification is 400-600min.
Preferably, after being filled with high-purity argon gas, the air pressure in sintering furnace is 7.5-9Mpa.
Being filled with the inert gas of purity helps to fire finished product ceramics with density higher, and application is more preferable.
Another aspect of the present invention is related to the ceramic composite in corrosion-resistant or resistant to elevated temperatures equipment or parts side The application in face；Preferably, the ceramic composite is used to be made the pump housing, pump parts, cage and magnetically-actuated Device；It is furthermore preferred that the pump includes complete ceramic screened pump, magnetic drive pump, vane pump, gear pump, lobed rotor pump, screw pump and aluminium Liquid delivery pump.
Ceramic composite of the present invention has the corrosivity of very excellent chemical-resistant resistance, high temperature resistant, wear-resisting Outstanding mechanical property is undermined, be can be used for in corrosive environment or in the environment of high temperature, it is special mainly for some Industry is planted, equipment or parts in the environment of cannot being met using special materials such as stainless steel and titanium alloys are particularly suitable for Some equipment or parts of the industry such as chemical field and pharmacy, food, fine chemistry industry, for example, can be used to manufacture various pumps The various parts of the pump housing and pump, such as impeller, pump shaft, lobed rotor pump, gear and gear shaft, screw rod, can also be made pottery Various parts such as cage, the ceramic composite magnetic driver of porcelain composite.
Compared with prior art, beneficial effects of the present invention are：
1. in ceramic composite of the invention, nitridation silicon components and Al are added in carbofrax material2O3-Y2O3- Er2O3-Yb2O3Polynary sintering aid so that ceramic material the corrosion resistance with general thyrite, high temperature resistant, While wear resistance, with good mechanical property；
2. ceramic composite of the invention, can at a lower temperature realize that compactness is sintered；
3. technique of the invention enables ceramic material component by the way of double sintering by specific heating curve Enough fully sintering, and by way of gas-phase high pressure is sintered so that the ceramic being made has sintered density higher；
4. of the invention ceramic because having good corrosion resistance, high temperature resistant, wear resistance, intensity, toughness and density, because And there is broad range of application, it is particularly suitable for pump class of the application and preparation under the conditions of various special types.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, are The conventional products that can be obtained by commercially available purchase.
Embodiment 1
The composition ratio of silicon nitride used by the present embodiment and carborundum is classified as：Weigh Si3N4Powder is weight 10%, carborundum SiC powders are weight 90%.Additive A l2O3And Y2O3Addition be the 0.5% of carborundum and silicon nitride gross weight, be modified Agent Yb2O3Addition be the 0.5% of carborundum and silicon nitride gross weight, purity 99.99%.
Wherein, the silicon nitride is α-Si3N4, the purity of the silicon nitride is less than 3 microns more than 98%, original particle size.
The carborundum is α-SiC, and purity is 0.5-1.5 microns more than 98%, granularity.
Its manufacture craft is as follows：
The 1st, above-mentioned powder and additive and toughener are weighed into the stirring of silicon nitride by component ratio respectively first In mill, appropriate silicon nitride ball is added.Add the absolute ethyl alcohol of technical grade 99.99% appropriate, be stirred grinding 10 hours, directly Connecting during membrane pump is sent to mist projection granulating tower carries out spray drying granulation, standby 80---120 mesh sieves are sieved through by vibration With.
2nd, formed product can select compression molding and cold isostatic compaction, pressure according to the structure snd size size of pump Can control in 180-250MPa.Biscuit after shaping can be machined or preprocessing according to size shape size.Size Larger product also needs to carry out pre-sintered unsticking, and then pre-sintered biscuit is put into gas pressure sintering stove carries out gas pressure sintering, Programming rate is 10 DEG C/min, is warmed up to 1000 DEG C, is filled with high-purity argon gas or high pure nitrogen, furnace pressure is reached 7.5MPa and protects Temperature 60 minutes, is then warmed up to 1800 DEG C with the speed of 10 DEG C/min again, and keeps furnace pressure 7.5MPa, is incubated 400 minutes.
Obtain the main performance index of composite ceramic articles, bending strength 740MPa, fracture toughness 7.5MPa microhardnesses HV2750.Density 3.25g/cm3。
Embodiment 2
The composition ratio of silicon nitride and carborundum is classified as used by this experiment：Weigh Si3N4Powder is weight 25%, carborundum SiC Powder is weight 75%.Additive A l2O3And Y2O3Addition be the 2.5% of carborundum and silicon nitride gross weight, modifying agent oxidation Erbium Er2O3Addition be the 1.5% of carborundum and silicon nitride gross weight, purity 99.99%.
Wherein, the silicon nitride is α-Si3N4, the purity of the silicon nitride is less than 3 microns more than 98%, original particle size.
The carborundum is α-SiC, and purity is 0.5-1 microns more than 98%, granularity.
Its manufacture craft is as follows：
The 1st, above-mentioned powder and additive and toughener are weighed into the stirring of silicon nitride by component ratio respectively first In mill, appropriate silicon nitride ball is added.The absolute ethyl alcohol for adding technical grade 99.99% is appropriate, is stirred grinding 15-20 small When.Directly being sent in mist projection granulating tower by membrane pump carries out spray drying granulation, and 80--120 mesh sieves are being sieved through by vibration It is standby.
2nd, formed product can select compression molding and cold isostatic compaction, pressure according to the structure snd size size of pump Can control in 180-250MPa.Biscuit after shaping can be machined or preprocessing according to size shape size.Size Larger product also needs to carry out pre-sintered unsticking, and then pre-sintered biscuit is put into gas pressure sintering stove carries out gas pressure sintering, Programming rate is 20 DEG C/min, is warmed up to 1200 DEG C, is filled with high-purity argon gas or high pure nitrogen, furnace pressure is reached 8MPa and is incubated 120 minutes, then again with 25 DEG C/min, speed be warmed up to 2000 DEG C, and keep furnace pressure 8MPa, be incubated 600 minutes.
Obtain the main performance index of composite ceramic articles, bending strength 780MPa, fracture toughness 7.9MPa microhardnesses HV2430.Density 3.41g/cm3。
Embodiment 3
The composition ratio of silicon nitride and carborundum is classified as used by this experiment：Weigh Si3N4Powder is weight 5%, carborundum SiC Powder is weight 95%.Additive A l2O3And Y2O3Addition be the 10% of carborundum and silicon nitride gross weight, modifying agent Er2O3 And Yb2O3Addition be the 4% of carborundum and silicon nitride gross weight, purity 99.99%.
Wherein, described is carborundum α-SiC, and the purity of the silicon nitride is less than 3 microns more than 98%, original particle size.
The silicon nitride is α-Si3N4With β-Si3N4Mixture, purity is more than 98%, granularity is 0.5-1 microns.
Its manufacture craft is as follows：
The 1st, above-mentioned powder and additive and toughener are weighed into the stirring of silicon nitride by component ratio respectively first In mill, appropriate silicon nitride ball is added.The absolute ethyl alcohol for adding technical grade 99.99% is appropriate, is stirred grinding 15-20 small When.Directly being sent in mist projection granulating tower by membrane pump carries out spray drying granulation, standby 80 mesh sieves are sieved through by vibration.
2nd, formed product can select compression molding and cold isostatic compaction, pressure according to the structure snd size size of pump Can control in 180-250MPa.Biscuit after shaping can be machined or preprocessing according to size shape size.Size Larger product also needs to carry out pre-sintered unsticking, and then pre-sintered biscuit is put into gas pressure sintering stove carries out gas pressure sintering, Programming rate is 15 DEG C/min, is warmed up to 1200 DEG C, is filled with high-purity argon gas or high pure nitrogen, furnace pressure is reached 8.5MPa and protects Temperature 100 minutes, then again with 15 DEG C/min, speed be warmed up to 2000 DEG C, and keep furnace pressure 8.5MPa, be incubated 600 points Clock.
Obtain the main performance index of composite ceramic articles, bending strength 841MPa, fracture toughness 8.3MPa microhardnesses HV2857.Density 3.58g/cm3。
Embodiment 4
The composition ratio of silicon nitride and carborundum is classified as used by this experiment：Weigh Si3N4Powder is weight 30%, carborundum SiC Powder is weight 70%.Additive A l2O3And Y2O3Addition be the 5% of carborundum and silicon nitride gross weight, modifying agent Er2O3With Yb2O3Addition be the 3% of carborundum and silicon nitride gross weight, purity 99.99%.
Wherein, the silicon nitride is α-Si3N4, the purity of the silicon nitride is less than 3 microns more than 98%, original particle size.
The carborundum is α-SiC, and purity is 1-1.5 microns more than 98%, granularity.
Its manufacture craft is as follows：
The 1st, above-mentioned powder and additive and toughener are weighed into the stirring of silicon nitride by component ratio respectively first In mill, appropriate silicon nitride ball is added.The absolute ethyl alcohol for adding technical grade 99.99% is appropriate, is stirred grinding 15-20 small When.Directly being sent in mist projection granulating tower by membrane pump carries out spray drying granulation, standby 80 mesh sieves are sieved through by vibration.
2nd, formed product can select compression molding and cold isostatic compaction, pressure according to the structure snd size size of pump Can control in 180-250MPa.Biscuit after shaping can be machined or preprocessing according to size shape size.Size Larger product also needs to carry out pre-sintered unsticking, and then pre-sintered biscuit is put into gas pressure sintering stove carries out gas pressure sintering, Programming rate is 10 DEG C/min, is warmed up to 1100 DEG C, is filled with high-purity argon gas or high pure nitrogen, furnace pressure is reached 7.5MPa and protects Temperature 110 minutes, then again with 25 DEG C/min, speed be warmed up to 1800 DEG C, and keep furnace pressure 7.5MPa, be incubated 500 points Clock.
Obtain the main performance index of composite ceramic articles, bending strength 827MPa, fracture toughness 8.3MPa microhardnesses HV2695.Density 3.29g/cm3。
Embodiment 5
The composition ratio of silicon nitride and carborundum is classified as used by this experiment：Weigh Si3N4Powder is weight 15%, carborundum SiC Powder is weight 85%.Additive A l2O3And Y2O3Addition be the 5% of carborundum and silicon nitride gross weight, modifying agent Er2O3With Yb2O3Addition be the 2% of carborundum and silicon nitride gross weight, purity 99.99%.
Wherein, the silicon nitride is α-Si3N4, the purity of the silicon nitride is less than 3 microns more than 98%, original particle size.
The carborundum is α-SiC, and purity is 1-1.5 microns more than 98%, granularity.
Its manufacture craft is as follows：
The 1st, above-mentioned powder and additive and toughener are weighed into the stirring of silicon nitride by component ratio respectively first In mill, appropriate silicon nitride ball is added.The absolute ethyl alcohol for adding technical grade 99.99% is appropriate, is stirred grinding 15-20 small When.Directly being sent in mist projection granulating tower by membrane pump carries out spray drying granulation, standby 80 mesh sieves are sieved through by vibration.
2nd, formed product can select compression molding and cold isostatic compaction, pressure according to the structure snd size size of pump Can control in 180-250MPa.Biscuit after shaping can be machined or preprocessing according to size shape size.Size Larger product also needs to carry out pre-sintered unsticking, and then pre-sintered biscuit is put into gas pressure sintering stove carries out gas pressure sintering, Programming rate is 15 DEG C/min, is warmed up to 1100 DEG C, is filled with high-purity argon gas or high pure nitrogen, furnace pressure is reached 8MPa and is incubated 100 minutes, then again with 20 DEG C/min, speed be warmed up to 1900 DEG C, and keep furnace pressure 8MPa, be incubated 500 minutes.
Obtain the main performance index of composite ceramic articles, bending strength 793MPa, fracture toughness 8.2MPa microhardnesses HV2516.Density 3.29g/cm3。
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that without departing substantially from of the invention Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims Including belonging to all such changes and modifications in the scope of the invention.

Claims (10)

1. a kind of ceramic composite, it is characterised in that the ceramic composite is mainly made up of following raw material：
Silicon nitride 5-30 parts,
Carborundum 70-95 parts,
Al2O30.5-10 parts,
Y2O30.5-10 parts, and
Er2O3And/or Yb2O30.5-8 parts.
2. ceramic composite according to claim 1, it is characterised in that the ceramic composite is included by weight The following components of meter：
Silicon nitride 15-25 parts；
Carborundum 75-85 parts；
Al2O35-10 parts,
Y2O35-10 parts, and
Er2O3And/or Yb2O34-6 parts；
Preferably, Al2O3And Y2O3Weight ratio be 1:1.
3. ceramic composite according to claim 1, it is characterised in that the silicon nitride is α-Si3N4And/or β- Si3N4, it is preferable that the purity of the silicon nitride is more than 98%, and original particle size is less than 3 microns.
4. ceramic composite according to claim 1, it is characterised in that the carborundum is α-SiC, purity is more than 98%, granularity is 0.5-1.5 microns.
5. ceramic composite according to claim 1, it is characterised in that the Er2O3、Yb2O3、Al2O3And Y2O3It is pure Degree is respectively greater than 99.99%, granularity and is respectively 0.5-1.5 microns.
6. the method for cooking of the ceramic composite in claim 1-5 described in any one, it is characterised in that methods described bag Include following steps：
1) the raw material mixing of ceramic composite will be prepared, adds absolute ethyl alcohol to be ground；
2) to binding agent and dispersant is added in the mixture after grinding, it is well mixed and is spray-dried, granulates；
3) the powder pressing shaping that will be obtained after granulation, is made biscuit；
4) biscuit described in high-pressure sinter under high purity inert gas environment.
7. method according to claim 6, it is characterised in that the step 1) in, the time of the grinding is 10-20h.
8. method according to claim 6, it is characterised in that the step 4) described in sintering process be, with 10-20 DEG C/speed of min is warming up in 1000 DEG C -1200 DEG C backward sintering furnaces and is filled with high purity inert gas, be incubated, then with 10-25 DEG C/ The speed of min is warmed up to 1800-2000 DEG C, insulation.
9. method according to claim 8, it is characterised in that after being filled with high-purity argon gas, keeps the air pressure in sintering furnace to be 7.5-9Mpa。
10. the ceramic composite in claim 1-5 described in any one is in corrosion-resistant or resistant to elevated temperatures equipment or parts The application of aspect；
Preferably, the ceramic composite is used to be made the pump housing, pump parts, cage and magnetic driver；
It is furthermore preferred that the pump include complete ceramic screened pump, magnetic drive pump, vane pump, gear pump, lobed rotor pump, screw pump and Aluminium liquid delivery pump.
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CN109592984A (en) * 2017-09-30 2019-04-09 中国科学院上海硅酸盐研究所 A kind of highly thermally conductive, high resistance liquid phase sintering silicon carbide ceramic and preparation method thereof
CN109592984B (en) * 2017-09-30 2021-06-15 中国科学院上海硅酸盐研究所 High-thermal-conductivity and high-resistance liquid-phase sintered silicon carbide ceramic and preparation method thereof
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CN113372096A (en) * 2020-03-09 2021-09-10 江苏省宜兴非金属化工机械厂有限公司 Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product
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