CN104128897B - Method for preparing ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering - Google Patents
Method for preparing ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering Download PDFInfo
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Abstract
The invention belongs to the technical field of super-hard material preparation, and particularly relates to a method for preparing a ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering. The method includes the steps that an aluminum, silicon and zirconium composite sol solution is prepared, a gel mixture is prepared by adding cBN abrasive material, diamond abrasive material, sintering additives, short carbon fiber, short glass fiber and dewatered sludge after sol curing is conducted, compression molding forming is conducted after pre-heating is conducted so that a cBN abrasive disc prefabricated block can be obtained, and then the ceramic cBN abrasive disc is obtained through microwave sintering. Compared with a high-temperature sintering method where traditional dry method mixed material compression molding forming is adopted, uniformity of raw material mixing can be obviously improved, stable pre-forming can be easily achieved, production programs are simple, production cost is reduced, and the method for preparing the cBN ceramic abrasive disc is capable of saving energy and efficient and can bring remarkable economic benefits and social benefits.
Description
Technical field
The invention belongs to superhard material preparing technical field, and in particular to a kind of to adopt wet chemical method molding microwave sintering
The method for preparing ceramics cBN emery wheels.
Background technology
Diamond is hitherto known material most hard in the world, and the hardness of cubic boron nitride is only second to diamond,
Diamond and cubic boron nitride are referred to as superhard material.Superhard material is widely used in abrasive material, grinding tool and cutter material, diamond
High temperature is easily aoxidized, particularly good with iron family element affinity, is not suitable for the processing of iron family element ferrous metal.Cube nitridation
Boron（cBN）There is exclusive, such as high thermal stability compared with diamond, with iron family element chemical inertness.Cubic boron nitride
Main performance is as follows：The microhardness of cBN is only second to diamond；The heat stability of cBN is better than diamond, in high temperature
Under remain to keep sufficiently high mechanical property and hardness, with good red hardness；CBN Stability Analysis of Structures, with high antioxidation
Ability, chemical stability are good, and compared with diamond, its particularly pertinent part is cBN in up to 1100～1300 DEG C of temperature
Under also not with iron family element chemically reactive, therefore cBN be particularly suitable for process ferrous metal；The thermal conductivity ratio Buddha's warrior attendant of cBN
Stone is little, but higher than hard alloy, with good heat conductivity；Bending strength is high；It is as grinding tool material, long service life, wear-resisting
Property is good.
So far, oarse-grained cBN single crystal preparations technology is still without breakthrough.Short grained cBN monocrystalline is mainly used as grinding tool material
Material.CBN grinding tools are that cBN abrasive particles are bonded to the product with certain geometrical shape by means of the effect of bonding agent, and cBN grinding tools are made
For a kind of superhard material grinding tool, the processing of iron can be used for, can be used for the processing of nonmetallic materials, range of application ratio
Diamond abrasive tool is wider, is the super-hard abrasive tool that a class has many uses, and for High speed Pyrometer and Honing process, imitates can grinding
Rate is greatly improved, and its grinding accuracy is high, and wheel life is long, and grinding performance is good, has been saved emery wheel and has been changed finishing, setting for machine and work
Many non-cutting times such as part detection.
The principal item of cBN grinding tools is emery wheel, and the preparation method of general cBN vitrified abrasives is dry-press process, first pottery
Porcelain bonding agent mix homogeneously with cBN abrasive materials after cold moudling, the demoulding, high-temperature firing, machining and shaping remove excess surface part,
Obtain final product vitrified abrasive.A lot, such as the Chinese patent about the patent documentation of cBN vitrified abrasives（CN101602188B,
CN101353258B, CN102009391B）.Chinese publication（CN103537993A）, it is indicated that due to cold moudling, ceramic junction
Mixture is not to fix very much with abrasive material, and the demoulding easily causes emery wheel deformation or fracture damage, and yield rate is low.Chinese patent
（CN102009393B）A kind of high-speed grinding cBN grinding wheel preparation methods are disclosed, after needing the mixing of various raw materials, Jing high temperature burns
Knot, sub-cooled, broken, drying, ball milling such as sieve at the operation, and manufacturing process is complicated, repeat Jing high temperature meltings sintering, and energy consumption is big,
High cost, properties of product are unstable.Generally, cBN vitrified abrasives are prepared using conventional dry molding, with following deficiency
Place, such as：High energy consumption, operating process is more, complex procedures, and yield rate is low, and manufacturing cost is high.
The content of the invention
It is an object of the invention to provide a kind of employing wet chemical method molding microwave sintering prepares the side of ceramics cBN emery wheels
Method, can overcome the defects such as high energy consumption existing for current dry-press process, complex procedures.
To solve above-mentioned technical problem, the technical solution used in the present invention is as follows：
A kind of method that employing wet chemical method molding microwave sintering prepares ceramics cBN emery wheels, first prepares sial zirconium and is combined
Thing sol solution, adds abrasive material, sintering aid, reinforcing material, sintering pore former to prepare gel compound, pre-add after colloidal sol ripening
Compression molding after heat treatment obtains cBN emery wheel prefabricated sections, and microwave sintering obtains ceramics cBN emery wheels afterwards.
When preparing sial zirconium composite sol solution, by by aluminum source compound, silicon-containing compound, zirconium-containing compound and urging
Agent reacts acquisition in aqueous medium, and reaction temperature is 50～80 DEG C.
Source of aluminium compound is selected from the mixed of one or more in aluminium powder, aluminum isopropylate., aluminum nitrate and aluminum chloride
Compound, silicon-containing compound are tetraethyl orthosilicate, and the zirconium-containing compound is basic zirconium chloride, and catalyst is hydrochloric acid or acetic acid.
In aluminum source compound, silicon-containing compound, the quality summation of zirconium-containing compound three, aluminum source compound accounts for 50～60%,
Tetraethyl orthosilicate accounts for 35～40%, balance of basic zirconium chloride；The consumption of catalyst is regulation pH value to 2～3.
Described sintering pore former is preferably dewatered sludge of the moisture content less than 40%.
Described abrasive material is preferably cBN and diamond, and sintering aid is Graphene, and reinforcing material is chopped carbon fiber and short
Cut glass fibre.
Following material total amount according to 100 parts count, the mass parts being separately added into be 60～80 parts of cBN abrasive materials, Buddha's warrior attendant stone grinder
5～16 parts of material, 1～3 part of Graphene, 3～6 parts of chopped carbon fiber, 5～12 parts of short glass fiber, balance of dehydration are dirty
Mud.
Wherein, the length of chopped carbon fiber is 5～30mm, and short glass fiber length is 5～30mm.
The condition of pre-add heat treatment be 350～450 DEG C of temperature, 2～5 hours time.
800～1200 DEG C of microwave sintering temperature, 20～40min of sintered heat insulating time.
Microwave power 20KW, 915 ± 50MHz of microwave frequency.
The inventive method is comprised the following steps that：
1）Aluminum source compound, silicon-containing compound, zirconium-containing compound and catalyst are reacted in aqueous medium and obtains transparent
Sial zirconium composite colloidal sol；
2）Step 1）The colloidal sol ripening for obtaining, adds cBN abrasive materials, diamond abrasive, Graphene, chopped carbon fiber, short
Glass fibre, dewatered sludge are cut, through being thoroughly mixed, is evaporated, obtain gel compound, pre-add heat treatment, molding compacting
Molding obtains cBN emery wheel prefabricated sections；
3）Step 2）Emery wheel prefabricated section, heat-agglomerating is carried out using microwave, after microwave sintering, using natural cooling,
Shaped processed obtains cBN vitrified abrasives.
For the various deficiencies for overcoming dry-press process to exist, the invention provides a kind of method of wet chemistry molding, is
In sol-gel chemistries course of reaction, the good microwave sintering auxiliary agent Graphene of addition cBN abrasive materials, chopped carbon fiber, heat conductivity,
The dewatered sludge of pretreatment is added, after collosol and gel, preheated process, compression molding, then using Microwave Sintering Techniques, finally
Light weight, hardness height, the cBN emery wheel sintered bodies that heat conductivity is good, intensity is high and wearability is good are obtained, emery wheel product is processed in shaping.
Wherein, vitrified abrasive bonding agent is synthesized using wet chemical method, sol-gal process prepares colloidal sol, collosol stability,
Good fluidity, it is easy to infiltrate abrasive material and various fillers, it is strong to the hold of abrasive material after abrasive wheel forming, it is suitable for regrinding application.
In sol-gal process chemical reaction process, dewatered sludge is additionally added as high temperature sintering pore former.As dehydrated sludge contains
Have substantial amounts of Organic substance, high temperature sintering pore-creating character is good, and after these Organic substances are burnt, remaining inorganic matters main component be also with
The mixture of aluminium oxide and silicon oxide based on silicon dioxide, the exactly main component of cBN vitrified abrasives bonding agent.Colloidal sol Jing is micro-
When aluminium oxide, silicon oxide, zirconia blend, exactly dry-press process emery wheel pre-embossed molding are formed after ripple high temperature sintering, Jing often makes
The main component of bonding agent.Additionally, colloidal sol Jing after high temperature sintering, during dry method batch mixing, chopped strand is difficult uniform mixing, wet method
Molding batch mixing then evenly, particularly with the addition of enhancing chopped carbon fiber and glass fibre be easier to be evenly distributed in emery wheel,
Reinforced effects are obvious.Meanwhile, using microwave sintering, replacing conventional heating by electric cooker, sintering time is short, little to the hot injury of abrasive material.
Coupled with the basic structure of material-to-be-heated object using microwave special wave band and produce heat, be molecule microwave energy
Kinetic energy and heat energy, the dielectric loss of material make material integrally heat, thus have homogeneous heating, and programming rate is fast, the efficiency of heating surface
Height, temperature retention time are short, and energy consumption is low, simple to operate, the low many advantages of cost.
The present invention compared with prior art, has the advantage that：
The present invention can significantly improve the equal of raw material mixing compared with using conventional dry batch mixing compression molding high-temperature sintering process
Even property, it is easy to which stable preforming, production routine are simple, reduce production cost, are a kind of preparation cBN ceramic sands of efficient energy-saving
The method of wheel, can bring significant economic benefit and social benefit.
Specific embodiment
Below with specific embodiment illustrating technical scheme, but protection scope of the present invention not limited to this：
Embodiment 1
Metering weighs 3 moles of aluminum nitrate, and 3 moles of aluminum isopropylate., 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN 60%, diadust
10%, Graphene 2%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 16%.Through being thoroughly mixed, steam
Send out, obtain gel compound, 4 hours are preheated at 350 ± 5 DEG C, compressing cBN emery wheel prefabricated sections are molded.It is pressed into
The prefabricated section of type is by carrying out heat-agglomerating, microwave power 20KW using microwave；915 ± 50MHz of microwave frequency；Far infrared is surveyed
Temperature, 1050 ± 20 DEG C of microwave sintering temperature；Sintered heat insulating time 36min.It is after microwave sintering, using natural cooling, shaped to add
Work process obtains cBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV3500, and impact flexibility is 456 times, and three-point bending method test bending resistance is strong
Spend for 787 ± 56 MPa, standard JB/T3235-1999 wear tested ratio is adopted for 76220 ± 180.
Embodiment 2
Metering weighs 3 moles of aluminum nitrate, and 2 moles of basic zirconium chloride, 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN 61.5%, diadust
13%, Graphene 2.5%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 11%, through being thoroughly mixed,
Evaporation, obtains gel compound, preheats 4 hours, is molded compressing cBN emery wheel prefabricated sections at 350 ± 5 DEG C.Compacting
The prefabricated section of molding is by carrying out heat-agglomerating, microwave power 20KW using microwave；915 ± 50MHz of microwave frequency；Far infrared is surveyed
Temperature, 1000 ± 20 DEG C of microwave sintering temperature；Sintered heat insulating time 40min.It is after microwave sintering, using natural cooling, shaped to add
Work process obtains cBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV3429, and impact flexibility is 490 times, and three-point bending method test bending resistance is strong
Spend for 881 ± 71 MPa, standard JB/T3235-1999 wear tested ratio is adopted for 66205 ± 210.
Embodiment 3
Metering weighs 3 moles of aluminum nitrate, and 2 moles of basic zirconium chloride, 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN66%, diadust 14%,
Graphene 2%, chopped carbon fiber 4%, short glass fiber 8%, dewatered sludge 6%.Through being thoroughly mixed, evaporation is obtained
To gel compound, 3 hours are preheated at 4200 ± 5 DEG C, compressing cBN emery wheel prefabricated sections are molded.Compressing
Prefabricated section is by carrying out heat-agglomerating, microwave power 20KW using microwave；915 ± 50MHz of microwave frequency；Far infrared temperature measurement, it is micro-
1000 ± 20 DEG C of ripple sintering temperature；Sintered heat insulating time 40min.After microwave sintering, using natural cooling, shaped processed
Obtain cBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV4150, and impact flexibility is 437 times, and three-point bending method test bending resistance is strong
Spend for 723 ± 50 MPa, standard JB/T3235-1999 wear tested ratio is adopted for 77210 ± 190.
Embodiment 4
Metering weighs 3 moles of aluminum nitrate, and 2 moles of basic zirconium chloride, 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN 70%, diadust 15%,
Graphene 1%, chopped carbon fiber 4%, short glass fiber 9%, dewatered sludge 1%, through being thoroughly mixed, evaporate, obtain
Gel compound, preheats 4 hours at 380 ± 5 DEG C, is molded compressing cBN emery wheel prefabricated sections.Compressing is pre-
Clamp dog is by carrying out heat-agglomerating, microwave power 20KW using microwave；915 ± 50MHz of microwave frequency；Far infrared temperature measurement, microwave
1000 ± 20 DEG C of sintering temperature；Sintered heat insulating time 40min.After microwave sintering, using natural cooling, shaped processed is obtained
To cBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV3890, and impact flexibility is 651 times, and three-point bending method test bending resistance is strong
Spend for 812 ± 54 MPa, standard JB/T3235-1999 wear tested ratio is adopted for 71110 ± 185.
Embodiment 5
Metering weighs 3 moles of aluminum nitrate, and 2 moles of basic zirconium chloride, 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN 75%, diadust 8%,
Graphene 2%, chopped carbon fiber 5%, short glass fiber 5%, dewatered sludge 5%, through being thoroughly mixed, evaporate, obtain
Gel compound, preheats 4 hours at 390 ± 5 DEG C, is molded compressing cBN emery wheel prefabricated sections.Compressing is prefabricated
Block is by carrying out heat-agglomerating, microwave power 20KW using microwave；915 ± 50MHz of microwave frequency；Far infrared temperature measurement, microwave burn
1100 ± 20 DEG C of junction temperature；Sintered heat insulating time 30min.After microwave sintering, using natural cooling, shaped processed is obtained
CBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV3188, and impact flexibility is 651 times, and three-point bending method test bending resistance is strong
Spend for 682 ± 51MPa, standard JB/T3235-1999 wear tested ratio is adopted for 67227 ± 189.
Comparative example 1
Metering weighs 3 moles of aluminum nitrate, and 2 moles of basic zirconium chloride, 2 moles of tetraethyl orthosilicate add 124 moles of water, add
Hydrochloric adjustment pH value is 2.8,65 ± 2oReact under the temperature conditionss of C, polymerization obtains transparent colloidal sol；Colloidal sol Jing
Ageing concentration, is subsequently adding the following material after purified treatment：According to mass percent meter, cBN 70%, diadust
10%, Graphene 2%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 6%, through being thoroughly mixed, steam
Send out, obtain gel compound, 4 hours are preheated at 350 ± 5 DEG C, compressing cBN emery wheel prefabricated sections are molded.It is pressed into
The prefabricated section of type carries out heat-agglomerating, 1000 ± 20 DEG C of sintering temperature using Muffle furnace；Sintered heat insulating time 120min.High temperature burns
After knot, using natural cooling, shaped processed obtains cBN vitrified abrasives.
Jing is tested, and emery wheel sample microhardness is HV3266, and impact flexibility is 451 times, and three-point bending method test bending resistance is strong
Spend for 667 ± 53 MPa, standard JB/T3235-1999 wear tested ratio is adopted for 42206 ± 220.
Claims (4)
1. a kind of method that employing wet chemical method molding microwave sintering prepares ceramics cBN emery wheels, it is characterised in that first prepare
Sial zirconium composite sol solution, adds cBN abrasive materials and diamond abrasive, Graphene, chopped carbon fiber and short after colloidal sol ripening
Cut the dewatered sludge of glass fibre, moisture content less than 40% and prepare gel compound, the molded acquisition cBN of pre-add heat treatment rear mold
Emery wheel prefabricated section, the microwave sintering at 800～1200 DEG C afterwards, 20～40min of sintered heat insulating time, microwave sintering obtain ceramics
CBN emery wheels；Wherein above-mentioned each material total amount according to 100 parts count, the mass parts being separately added into be 60～80 parts of cBN abrasive materials, Buddha's warrior attendant
5～16 parts of stone grinder material, 1～3 part of Graphene, 3～6 parts of chopped carbon fiber, 5～12 parts of short glass fiber are balance of de-
Sewage sludge；When preparing sial zirconium composite sol solution, by by aluminum source compound, silicon-containing compound, zirconium-containing compound and urging
Agent reacts acquisition in aqueous medium, and reaction temperature is 50～80 DEG C, and source of aluminium compound is selected from aluminium powder, aluminum isopropylate., nitre
One or more mixture in sour aluminum and aluminum chloride, silicon-containing compound is tetraethyl orthosilicate, the zirconium-containing compound
For basic zirconium chloride, catalyst is hydrochloric acid or acetic acid；Aluminum source compound, silicon-containing compound, the quality summation of zirconium-containing compound three
In, aluminum source compound accounts for 50～60%, and tetraethyl orthosilicate accounts for 35～40%, balance of basic zirconium chloride；The consumption of catalyst is regulation
PH value is to 2～3.
2. the method for ceramics cBN emery wheels being prepared using wet chemical method molding microwave sintering as claimed in claim 1, its feature
It is that the length of chopped carbon fiber is 5～30mm, and short glass fiber length is 5～30mm.
3. the method for ceramics cBN emery wheels being prepared using wet chemical method molding microwave sintering as claimed in claim 1, its feature
It is that the condition of pre-add heat treatment is 350～450 DEG C of temperature, 2～5 hours time.
4. the method for ceramics cBN emery wheels being prepared using wet chemical method molding microwave sintering as claimed in claim 1, its feature
It is, microwave power 20KW, 915 ± 50MHz of microwave frequency.
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| CN106994652A (en) * | 2016-01-25 | 2017-08-01 | 江苏华东砂轮有限公司 | Fibre reinforced high porosity ceramic bonding agent CBN grinding wheel preparation methods |
| CN105583742A (en) * | 2016-02-03 | 2016-05-18 | 浙江工业大学 | Production method of fixed abrasive particle grinding disc |
| CN106425897B (en) * | 2016-08-30 | 2018-10-26 | 湖北东方玉扬电子科技有限公司 | Brake block grinding machine grinding disc and preparation method thereof |
| CN108321260B (en) * | 2017-12-30 | 2020-02-14 | 苏州赛尔科技有限公司 | LED epitaxial wafer grinding wheel and preparation method thereof |
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| US4311489A (en) * | 1978-08-04 | 1982-01-19 | Norton Company | Coated abrasive having brittle agglomerates of abrasive grain |
| JPH0499871A (en) * | 1990-08-17 | 1992-03-31 | Olympus Optical Co Ltd | Synthetic method for cubic carbon nitride |
| CN101573424A (en) * | 2006-12-22 | 2009-11-04 | 3M创新有限公司 | Abrasive articles with nanoparticulate fillers and method for making and using them |
| CN100532318C (en) * | 2007-03-26 | 2009-08-26 | 长春理工大学 | Laser transparent ceramic and method for producing the same |
| CN101219530B (en) * | 2008-02-03 | 2010-09-01 | 北京国瑞升科技有限公司 | Granulation type pouncing paper, preparation method and application thereof |
| JP2010274383A (en) * | 2009-05-29 | 2010-12-09 | Nisshin Seisakusho:Kk | Method and device for manufacturing metal bonded grinding wheel |
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