CN107445636A - A kind of alumina-based nano composite ceramic die material and preparation method thereof - Google Patents

A kind of alumina-based nano composite ceramic die material and preparation method thereof Download PDF

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CN107445636A
CN107445636A CN201710799333.9A CN201710799333A CN107445636A CN 107445636 A CN107445636 A CN 107445636A CN 201710799333 A CN201710799333 A CN 201710799333A CN 107445636 A CN107445636 A CN 107445636A
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oxide
alumina
composite ceramic
nano composite
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刘浩
张君
张欢芬
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Suzhou Hao Yan Precision Mold Ltd Co
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Suzhou Hao Yan Precision Mold Ltd Co
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Abstract

The invention provides a kind of alumina-based nano composite ceramic die material and preparation method thereof, the raw material of the composite includes：13 parts of aluminum oxide, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide, zinc oxide, molybdenum, magnesia and nickel.Its preparation method is first to add to aluminum oxide suspending liquid A is made in absolute ethyl alcohol；Lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol again suspension B is made；Suspending liquid A and suspension B are mixed, add molybdenum, magnesia, nickel, ultrasonic disperse, then mixing suspension is poured into ball grinder, dry to be placed under the conditions of 100 DEG C using sintered carbide ball mechanical ball mill lapping liquid and be dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, produce.Compared with aluminium oxide ceramics mold materials, composite ceramic die material of the invention has more preferable comprehensive mechanical property and excellent properties of antifriction and wear resistance.

Description

A kind of alumina-based nano composite ceramic die material and preparation method thereof
Technical field
The present invention relates to a kind of ceramic die material, and in particular to a kind of alumina-based nano composite ceramic die material and Its preparation method.
Background technology
Mold materials commonly used in production are mainly mould steel, hard alloy and cermet etc. at present, due to it In use there is deformation, cause product size stability and surface quality to decline, and its hardness, anti-wear performance are It is difficult to meet the needs of actual production, thus the mold use life-span is relatively low.From raising mold use performance and used life Set out, utilize the advantages of nano composite ceramic room temperature and high temperature hardness are high, wearability is good, elevated temperature strength is high, development of new nanometer Composite ceramic die.Work out the nano combined pottery for preparing the high-temperature behavior with high intensity, high tenacity, high-wearing feature and protrusion The design of porcelain mold material component, microstructure and the technology of technological design；Study the microcosmic knot of nano composite ceramic mould material Structure and mechanical property feature and its changing rule, nano composite ceramic mould material is analyzed with reference to the raising of comprehensive mechanical property Toughening and strengthening.
With the rapid development of production, plastic working proposes higher requirement to mold materials.Existing ceramic die Material has been difficult to meet the conditions of work such as high temperature drawing, high speed stamping, the Research Thinking new as one, nano ceramic material It is combined with mould design and manufacture technology, the height of nano material high intensity, high tenacity, high-wearing feature and protrusion can be given full play to The advantages such as warm nature energy, so as to develop a kind of novel nano composite ceramic die.The material is by with its excellent physical and mechanical property And performance, nano composite ceramic mould is used widely in fields such as plastic workings, and produce good economic effect Benefit and social benefit, have broad application prospects.
The content of the invention
Present invention aim to address the technical problem that existing ceramic die material toughness is very poor, there is provided a kind of alumina base Nano composite ceramic mould material and preparation method thereof.
A kind of alumina-based nano composite ceramic die material, raw material include in parts by weight：Aluminum oxide 80-100 parts, ovum Phosphatidase 0 .8-1.5 parts, carborundum 12-18 parts, calcium sulfate crystal whiskers 18-22 parts, zirconium oxide 2-4 parts, titanium oxide 3-5 parts, zinc oxide 0.8-2.5 parts, molybdenum 1-3 parts, magnesia 0.5-1.2 parts, nickel 1-3 parts.
Preferably, the particle diameter of the aluminum oxide is in 20-80nm.
Preferably, the particle diameter of the carborundum is in 5-10nm.
Preferably, the particle diameter of the zirconium oxide, titanium oxide and zinc oxide is in 10-20nm.
Preferably, the titania addition silica.
The preparation method of above-mentioned alumina-based nano composite ceramic die material, comprises the following steps：
Step 1, aluminum oxide is added in absolute ethyl alcohol, ultrasonic disperse, add dispersant polyethylene glycol, stirring, regulation pH to 3.5-4.0 obtain suspending liquid A；
Step 2, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol, ultrasound It is scattered, dispersant polyethylene glycol is added, stirring, pH to 3.5-4.0 is adjusted, obtains suspension B；
Step 3, suspending liquid A and suspension B are mixed, adds molybdenum, magnesia, nickel, ultrasonic disperse, adjust pH to 3.5-4.0, obtain To mixing suspension；
Step 4, mixing suspension is poured into ball grinder, using sintered carbide ball mechanical ball mill 50h, mixing suspension and hard The mass ratio of alloying pellet is 1：10, obtain lapping liquid；
Step 5, lapping liquid is dried and is placed under the conditions of 100 DEG C and is dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, i.e., .
Preferably, the dispersant polyethylene glycol is PEG2000.
Preferably, NH is used in step 1, step 2, step 34OH adjusts pH.
The present invention is using aluminum oxide as matrix, and addition carborundum, calcium sulfate crystal whiskers, zirconium oxide are as enhancing phase, with titanium oxide It is stabilizer with zinc oxide, using molybdenum, nickel, magnesia is compound is used as sintering aid.Carborundum, calcium sulfate crystal whiskers, zirconium oxide plus Enter, typical transgranular/intergranular hybrid architecture can be formed with zirconium oxide, crackle expands to the path of intergranular again from intergranular to transgranular Exhibition, consumes more energies to failure, the fracture mode along crystalline substance/transcrystalline mixing is formd, so as to greatly improve the comprehensive of composite Close mechanical property；Molybdenum, nickel, magnesia are compound to be used as sintering aid, can reduce sintering temperature, prevent growing up for crystal grain；With oxygen It is stabilizer to change titanium and zinc oxide, can play a part of refining matrix grain, and transgranular nano particle makes matrix grain more Refinement, further functions as the effect of crystal grain refinement Strengthening and Toughening.Compared with aluminium oxide ceramics mold materials, composite ceramics of the invention Mold materials have more preferable comprehensive mechanical property and excellent properties of antifriction and wear resistance, available for make extrusion die, drawing die with And the ceramic tool and mould such as cutting tool.
Embodiment
Embodiment 1
A kind of alumina-based nano composite ceramic die material, raw material include in parts by weight：80 parts of aluminum oxide, lecithin 0.8 Part, 12 parts of carborundum, 18 parts of calcium sulfate crystal whiskers, 2 parts of zirconium oxide, 3 parts of titanium oxide, 0.8 part of zinc oxide, 1 part of molybdenum, magnesia 0.5 Part, 1 part of nickel.
Wherein, the particle diameter of the aluminum oxide is in 20-80nm；The particle diameter of the carborundum is in 5-10nm；The zirconium oxide, oxygen Change the particle diameter of titanium and zinc oxide in 10-20nm.
The titania addition silica, specific method of modifying are as follows：Titanium oxide is made into 20g/L suspension, The pH value of suspension is adjusted to 10 with 0.5M sodium hydroxide solutions, ultrasonic disperse, 85 DEG C are warming up to, to suspension under stirring condition 1mol/L sodium silicate aqueous solution is added dropwise in liquid, the dosage of sodium metasilicate is m (SiO2):m(TiO2)=1:4, after dripping off, 85 DEG C of reactions 30-40min, reaction solution pH to 7.0 is adjusted with 1mol/L dilute sulfuric acid, filtering, removing soluble-salt is washed with deionized, 2h is calcined at 700 DEG C, that is, obtains the titanium oxide doped with silica.
The preparation method of above-mentioned alumina-based nano composite ceramic die material, comprises the following steps：
Step 1, aluminum oxide is added in absolute ethyl alcohol, concentration 1wt.%, ultrasonic disperse, adds dispersant polyethylene glycol 2000 1wt.%, stirring, using NH4OH adjusts pH to 3.5-4.0, obtains suspending liquid A；
Step 2, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol, concentration For 2wt.%, ultrasonic disperse, dispersant polyethylene glycol 2000 4wt.% is added, stirring, pH to 3.5-4.0 is adjusted, obtains suspension B；
Step 3, suspending liquid A and suspension B are mixed, adds molybdenum, magnesia, nickel, ultrasonic disperse, using NH4OH adjust pH to 3.5-4.0 obtain mixing suspension；
Step 4, mixing suspension is poured into ball grinder, using sintered carbide ball mechanical ball mill 50h, mixing suspension and hard The mass ratio of alloying pellet is 1：10, obtain lapping liquid；
Step 5, lapping liquid is dried and is placed under the conditions of 100 DEG C and is dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, i.e., .
The mechanical property of gained composite is bending strength 808MPa, fracture toughness 8.4MPam1/2, hardness 16.7GPa, its comprehensive mechanical property are better than single-phase alumina material.
In the case where normal load 50N~150N, friction rotating speed are 70r/min and 140r/min dry friction, composite compares oxygen Changing aluminium ceramics has relatively low wear rate.
Embodiment 2
A kind of alumina-based nano composite ceramic die material, raw material include in parts by weight：90 parts of aluminum oxide, lecithin 1.1 Part, 15 parts of carborundum, 20 parts of calcium sulfate crystal whiskers, 3 parts of zirconium oxide, 4 parts of titanium oxide, 1.8 parts of zinc oxide, 2 parts of molybdenum, magnesia 0.8 Part, 2 parts of nickel.
Wherein, the particle diameter of the aluminum oxide is in 20-80nm；The particle diameter of the carborundum is in 5-10nm；The zirconium oxide, oxygen Change the particle diameter of titanium and zinc oxide in 10-20nm.
The titania addition silica, specific method of modifying are as follows：Titanium oxide is made into 20g/L suspension, The pH value of suspension is adjusted to 10 with 0.5M sodium hydroxide solutions, ultrasonic disperse, 85 DEG C are warming up to, to suspension under stirring condition 1mol/L sodium silicate aqueous solution is added dropwise in liquid, the dosage of sodium metasilicate is m (SiO2):m(TiO2)=1:4, after dripping off, 85 DEG C of reactions 30-40min, reaction solution pH to 7.0 is adjusted with 1mol/L dilute sulfuric acid, filtering, removing soluble-salt is washed with deionized, 2h is calcined at 700 DEG C, that is, obtains the titanium oxide doped with silica.
The preparation method of above-mentioned alumina-based nano composite ceramic die material, comprises the following steps：
Step 1, aluminum oxide is added in absolute ethyl alcohol, concentration 1wt.%, ultrasonic disperse, adds dispersant polyethylene glycol 2000 1wt.%, stirring, using NH4OH adjusts pH to 3.5-4.0, obtains suspending liquid A；
Step 2, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol, concentration For 2wt.%, ultrasonic disperse, dispersant polyethylene glycol 2000 4wt.% is added, stirring, pH to 3.5-4.0 is adjusted, obtains suspension B；
Step 3, suspending liquid A and suspension B are mixed, adds molybdenum, magnesia, nickel, ultrasonic disperse, using NH4OH adjust pH to 3.5-4.0 obtain mixing suspension；
Step 4, mixing suspension is poured into ball grinder, using sintered carbide ball mechanical ball mill 50h, mixing suspension and hard The mass ratio of alloying pellet is 1：10, obtain lapping liquid；
Step 5, lapping liquid is dried and is placed under the conditions of 100 DEG C and is dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, i.e., .
The mechanical property of gained composite is bending strength 814MPa, fracture toughness 8.7MPam1/2, hardness 16.3GPa, its comprehensive mechanical property are better than single-phase alumina material.
In the case where normal load 50N~150N, friction rotating speed are 70r/min and 140r/min dry friction, composite compares oxygen Changing aluminium ceramics has relatively low wear rate.
Embodiment 3
A kind of alumina-based nano composite ceramic die material, raw material include in parts by weight：100 parts of aluminum oxide, lecithin 1.5 Part, 18 parts of carborundum, 22 parts of calcium sulfate crystal whiskers, 4 parts of zirconium oxide, 5 parts of titanium oxide, 2.5 parts of zinc oxide, 3 parts of molybdenum, magnesia 1.2 Part, 3 parts of nickel.
Wherein, the particle diameter of the aluminum oxide is in 20-80nm；The particle diameter of the carborundum is in 5-10nm；The zirconium oxide, oxygen Change the particle diameter of titanium and zinc oxide in 10-20nm.
The titania addition silica, specific method of modifying are as follows：Titanium oxide is made into 20g/L suspension, The pH value of suspension is adjusted to 10 with 0.5M sodium hydroxide solutions, ultrasonic disperse, 85 DEG C are warming up to, to suspension under stirring condition 1mol/L sodium silicate aqueous solution is added dropwise in liquid, the dosage of sodium metasilicate is m (SiO2):m(TiO2)=1:4, after dripping off, 85 DEG C of reactions 30-40min, reaction solution pH to 7.0 is adjusted with 1mol/L dilute sulfuric acid, filtering, removing soluble-salt is washed with deionized, 2h is calcined at 700 DEG C, that is, obtains the titanium oxide doped with silica.
The preparation method of above-mentioned alumina-based nano composite ceramic die material, comprises the following steps：
Step 1, aluminum oxide is added in absolute ethyl alcohol, concentration 1wt.%, ultrasonic disperse, adds dispersant polyethylene glycol 2000 1wt.%, stirring, using NH4OH adjusts pH to 3.5-4.0, obtains suspending liquid A；
Step 2, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol, concentration For 2wt.%, ultrasonic disperse, dispersant polyethylene glycol 2000 4wt.% is added, stirring, pH to 3.5-4.0 is adjusted, obtains suspension B；
Step 3, suspending liquid A and suspension B are mixed, adds molybdenum, magnesia, nickel, ultrasonic disperse, using NH4OH adjust pH to 3.5-4.0 obtain mixing suspension；
Step 4, mixing suspension is poured into ball grinder, using sintered carbide ball mechanical ball mill 50h, mixing suspension and hard The mass ratio of alloying pellet is 1：10, obtain lapping liquid；
Step 5, lapping liquid is dried and is placed under the conditions of 100 DEG C and is dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, i.e., .
The mechanical property of gained composite is bending strength 798MPa, fracture toughness 8.1MPam1/2, hardness 15.8GPa, its comprehensive mechanical property are better than single-phase alumina material.
In the case where normal load 50N~150N, friction rotating speed are 70r/min and 140r/min dry friction, composite compares oxygen Changing aluminium ceramics has relatively low wear rate.

Claims (8)

  1. A kind of 1. alumina-based nano composite ceramic die material, it is characterised in that：Raw material includes in parts by weight：Aluminum oxide 80-100 parts, lecithin 0.8-1.5 parts, carborundum 12-18 parts, calcium sulfate crystal whiskers 18-22 parts, zirconium oxide 2-4 parts, titanium oxide 3- 5 parts, zinc oxide 0.8-2.5 parts, molybdenum 1-3 parts, magnesia 0.5-1.2 parts, nickel 1-3 parts.
  2. 2. alumina-based nano composite ceramic die material according to claim 1, it is characterised in that：The aluminum oxide Particle diameter is in 20-80nm.
  3. 3. alumina-based nano composite ceramic die material according to claim 1, it is characterised in that：The carborundum Particle diameter is in 5-10nm.
  4. 4. alumina-based nano composite ceramic die material according to claim 1, it is characterised in that：The zirconium oxide, The particle diameter of titanium oxide and zinc oxide is in 10-20nm.
  5. 5. alumina-based nano composite ceramic die material according to claim 1, it is characterised in that：The titanium oxide is mixed Miscellaneous silica.
  6. 6. the preparation method of the alumina-based nano composite ceramic die material described in claim 1, it is characterised in that：Including with Lower step：
    Step 1, aluminum oxide is added in absolute ethyl alcohol, ultrasonic disperse, add dispersant polyethylene glycol, stirring, regulation pH to 3.5-4.0 obtain suspending liquid A；
    Step 2, lecithin, carborundum, calcium sulfate crystal whiskers, zirconium oxide, titanium oxide and zinc oxide are added in absolute ethyl alcohol, ultrasound It is scattered, dispersant polyethylene glycol is added, stirring, pH to 3.5-4.0 is adjusted, obtains suspension B；
    Step 3, suspending liquid A and suspension B are mixed, adds molybdenum, magnesia, nickel, ultrasonic disperse, adjust pH to 3.5-4.0, obtain To mixing suspension；
    Step 4, mixing suspension is poured into ball grinder, using sintered carbide ball mechanical ball mill 50h, mixing suspension and hard The mass ratio of alloying pellet is 1：10, obtain lapping liquid；
    Step 5, lapping liquid is dried and is placed under the conditions of 100 DEG C and is dried in vacuo, through hot pressed sintering after the sieving of gained composite powder, i.e., .
  7. 7. the preparation method of alumina-based nano composite ceramic die material according to claim 6, it is characterised in that：Institute It is PEG2000 to state dispersant polyethylene glycol.
  8. 8. the preparation method of alumina-based nano composite ceramic die material according to claim 6, it is characterised in that：Step Rapid 1, NH is used in step 2, step 34OH adjusts pH.
CN201710799333.9A 2017-09-07 2017-09-07 A kind of alumina-based nano composite ceramic die material and preparation method thereof Pending CN107445636A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108017389A (en) * 2017-12-11 2018-05-11 苏州浩焱精密模具有限公司 A kind of mould ceramic material
CN110483022A (en) * 2019-09-17 2019-11-22 东莞理工学院 A kind of environment-friendly, high-intensity porous ceramic film support and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101164963A (en) * 2007-09-26 2008-04-23 山东轻工业学院 Micro-nano composite ceramic die material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101164963A (en) * 2007-09-26 2008-04-23 山东轻工业学院 Micro-nano composite ceramic die material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108017389A (en) * 2017-12-11 2018-05-11 苏州浩焱精密模具有限公司 A kind of mould ceramic material
CN110483022A (en) * 2019-09-17 2019-11-22 东莞理工学院 A kind of environment-friendly, high-intensity porous ceramic film support and preparation method thereof

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