CN107935556A - A kind of preparation method of nano-grade ceramic binding agent - Google Patents

A kind of preparation method of nano-grade ceramic binding agent Download PDF

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CN107935556A
CN107935556A CN201711415293.XA CN201711415293A CN107935556A CN 107935556 A CN107935556 A CN 107935556A CN 201711415293 A CN201711415293 A CN 201711415293A CN 107935556 A CN107935556 A CN 107935556A
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preparation
vitrified bond
nano
grinding
nitride
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CN107935556B (en
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赵志伟
杨宝震
王顺
赵小苗
任瑛
陈利霞
毛淑芳
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Linying Decat New Material Co ltd
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Henan University of Technology
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/16Lean materials, e.g. grog, quartz
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/14Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/04Clay; Kaolin
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3886Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444Halide containing anions, e.g. bromide, iodate, chlorite
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    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The invention belongs to bonding agent preparation field, is related to a kind of preparation method of nano-grade ceramic binding agent.The preparation method comprises the following steps:A, 30~50% talcum, 10~20% kaolin, 15~20% boron glass, 8~10% fluorite and 20~25% silica flour is taken by mass percentage, 200~300 mesh sieves are crossed after grinding, and mixture is made;B, by mixture pressure, melting, water quenching made from step a.C, by after product drying made from step b, add nano vanadium nitride/chromium nitride modifying agent, be ground up, sieved, basis vitrified bond is made;D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace, the vitrified bond of the present invention is made.This method has the characteristics that reaction temperature is low, the reaction time is short, production cost is low, saves the energy, is easy to industrialized production.

Description

A kind of preparation method of nano-grade ceramic binding agent
Technical field
The invention belongs to bonding agent preparing technical field, specifically provides a kind of method for preparing nano-grade ceramic binding agent.
Background technology
CBN emery wheels have the chemical property of good appearance bits, heat dissipation, self-sharpening energy and stabilization, can meet difficulty well Rapidoprint is ground and the needs of high efficient grinding, application prospect are very wide.The quality of vitrified bond performance is directly related to Can CBN abrasive particles excellent performance be fully played, so as to eventually affect the ground effect of CBN emery wheels.So ceramics Bonding agent is one of key factor for studying vitrified bond CBN grinding tools.
The intensity of vitrified bond is to influence the key factor that CBN grinding tools use.The intensity of bonding agent mainly includes Both sides content:When the intensity of bonding agent in itself, second, the bonding streng between bonding agent and abrasive particle.The requirement of CBN grinding tools Vitrified bond used must be able to be formed very firm bonding agent bridge, and have good bonding streng to abrasive particle, otherwise The high rigidity of CBN abrasive materials just has no way of embodying.
The refractoriness of vitrified bond is one of main performance index of bonding agent, and the refractoriness such as bonding agent is too high, is burnt Into when sintering degree it is poor, it is bonded loosely with abrasive particle, makes grade of abrasive tool unstable;Opposite such as bonding agent refractoriness is too low, when burning till The viscosity of liquid phase is again small, will cause grinding tool deformation foaming.The principal element for influencing bonding agent refractoriness is chemical composition and raw material Granularity.Bonding agent granularity is thinner, and dispersion degree is bigger, and respond is stronger, can cause the reduction of refractoriness.
It is high that traditional normal pressure-sintered method prepares needed for vitrified bond sintering temperature, obtained vitrified bond intensity is low, Shock resistance, anti-fatigue performance are poor, and in order to improve its performance and avoid injury of the high temperature sintering to CBN abrasive materials, everybody is numerous and confused at present Low-temperature high-strength ceramic bond is studied, to realize the easy fired of grinding tool.Compared with normal pressure-sintered, microwave sintering energy Quick uniform Ground heating material is internally formed bonding agent uniform thin without causing bonding agent to crack or forming thermal stress in bonding agent Crystal structure, and then improve the performance of vitrified bond, strengthen the intensity of CBN grinding tools, improve use and the processing performance of grinding tool, reach To the preparation purpose of low-temperature high-strength CBN grinding tool vitrified bonds.In addition, sintering temperature can be reduced using microwave sintering, shorten Sintering time, and the ceramic structure prepared is uniform, fine and close.
Vanadium nitride has good thermal conductance, thermal-shock resistance, chemically and thermally electric conductivity, the characteristic such as stability, in machine Tool manufacture field is widely applied.Chromium nitride has high hardness and mechanical strength, excellent corrosion resistance and height Temperature stability energy.By by after the two compound and nanosizing, preparing nano vanadium nitride/chromium nitride composite powder.The composite powder End has the comprehensive performances such as high rigidity, high strength & high electric-conduction, corrosion resistance concurrently.Combination is added to as nano modifier In agent, the comprehensive performance of bonding agent is remarkably improved, most prominent is bending strength and the flowing that can greatly improve bonding agent Property.
Therefore, in order to preferably improve the comprehensive performance of Vitrified Bond CBN Tools, Low-temperature high-strength ceramic bond is obtained CBN grinding tools, it is necessary to explore a kind of achievable low temperature, quick prepare is added with nano vanadium nitride/chromium nitride composite modifier The method of vitrified bond.
The content of the invention
It is an object of the invention to provide a kind of the new of the excellent CBN grinding tool nano-grade ceramic binding agents of quick processability Method.Vitrified bond prepared by the method can more preferably meet the requirement of high-performance CBN grinding tools manufacture, make obtained low temperature high High speed that strong Vitrified Bond CBN Tools more easily reach, efficiently, the condition of high-precision grinding.This method has economic benefit High, the features such as clean energy-saving and technique are simple.
To achieve the above object, the technical solution adopted by the present invention is a kind of preparation method of nano-grade ceramic binding agent, institute Preparation method is stated to comprise the following steps:
A, take by mass percentage 30~50% talcum, 10~20% kaolin, 15~20% boron glass, 8~10% Fluorite and 20~25% silica flour, after grinding cross 200~300 mesh sieves, be made mixture;
B, mixture made from step a is subjected to melting, 0 DEG C~400 with after mould briquetting by programme-control heating mode DEG C when, the speed of heating is 5~10 DEG C/min, after reaching 400 DEG C, is warming up to 1200~1400 DEG C with 2~5 DEG C/min and keeps the temperature 4~8h, water quenching is carried out to the frit flow down after melting;
C, product made from step b is dried into 10~16h at 80~120 DEG C, adds the nanometer that mass fraction is 0.5~1.5% Vanadium nitride/chromium nitride composite powder, grinding, crosses 200~300 mesh sieves, and basis vitrified bond is made;
D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace, this is made The vitrified bond of invention.
Preferably, the mass ratio of vanadium nitride and chromium nitride is 1 in the nano vanadium nitride/chromium nitride composite powder:1.
Preferably, the microwave oven junction temperature be 550~700 DEG C, sintering time be 10min~1h.
The mixing, grinding are to be carried out in high energy ball mill, rotary mill and grinder in a kind of equipment.
It is any one equipment in air dry oven and vacuum drying chamber to be dried in the step c with equipment.
Preferably, the average grain diameter of the nano vanadium nitride/chromium nitride composite powder<100nm.
Nano vanadium nitride/chromium nitride composite powder used can use ordinary skill in the art method to synthesize in the present invention, Such as Chinese patent " a kind of method of CRN method synthesis nano vanadium nitride/chromium nitride composite powder "(The patent No. 201310672946.8), " a kind of preparation method of nano vanadium nitride/chromium nitride composite powder "(The patent No. 201310698867.4)Method is synthesized Deng disclosed in.
The present invention compares the existing method for preparing CBN grinding tool vitrified bonds, has the advantages that:
(1)Firing temperature is uniform, and microwave sintering method has the effect of inside and outside Synchronous Heating, and microwave sintering can quickly and evenly add Hot material is without causing bonding agent cracking or thermal stress being formed in bonding agent;
(2)Reaction temperature is low, and the reaction time is short, reduces the consumption of the energy, with respect to the side of conventional atmospheric sintering vitrified bond Reaction temperature can be greatly lowered in method, this preparation method, shorten the reaction time, effectively reduce energy consumption;
(3)Excellent performance, has a extensive future:The CBN grinding tool vitrified bonds of generation are reacted, bending strength is big, mobility It is good.In addition, ceramic bonding agent air hole made from the method is uniform, hold is big between abrasive particle, and obtained grinding tool grinding performance is good, should With having a extensive future.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will It will be appreciated that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the invention.Tool is not specified in embodiment Concrete conditions in the establishment of a specific crime person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer, For the conventional products that can be obtained by commercially available purchase.
Embodiment 1
A kind of preparation method of nano-grade ceramic binding agent, the preparation method comprise the following steps:
A, the silica flour of 44g talcums, 11g kaolin, 22g boron glasses, 8.8g fluorites and 24.2g are weighed respectively, and 200 are crossed after grinding Mesh sieve, is made mixture;
B, mixture made from step a is increased to 400 DEG C with after mould briquetting with the heating rate of 10 DEG C/min, then with 5 DEG C/heating rate of min is increased to 1400 DEG C, and keeps the temperature 8h, water quenching is carried out to the frit flow down after melting;
C, product made from step b is dried into 16h at 80 DEG C, adds 1.1g nano vanadium nitride/chromium nitride composite powders(Nitridation The mass ratio of vanadium and chromium nitride is 1:1), grinding, crosses 200 mesh sieves, and basis vitrified bond is made;
D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace(Sintering temperature Spend for 600 DEG C, sintering time 30min), vitrified bond of the invention is made.
The mobility and flexural strength of vitrified bond are measured respectively.The results show:The mobility of bonding agent is 210%, is resisted Folding intensity is 110MPa.
Embodiment 2
A kind of preparation method of nano-grade ceramic binding agent, the preparation method comprise the following steps:
A, the silica flour of 36.5g talcums, 18.5g kaolin, 15.4g boron glasses, 8.4g fluorites and 21.2g are weighed respectively, are ground 200 mesh sieves are crossed afterwards, and mixture is made;
B, by mixture made from step a with after mould briquetting, 400 DEG C are increased to the heating rate of 5 DEG C/min, then with 2 DEG C/ The heating rate of min is increased to 1200 DEG C, and keeps the temperature 4h, and water quenching is carried out to the frit flow down after melting;
C, product made from step b is dried into 10h at 120 DEG C, then adds 1.5g nano vanadium nitride/chromium nitride composite powders (The mass ratio of vanadium nitride and chromium nitride is 1:1), grinding, crosses 300 mesh sieves, and basis vitrified bond is made;
D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace(Sintering temperature Spend for 700 DEG C, sintering time 10min), vitrified bond of the invention is made.
The mobility and flexural strength of vitrified bond are measured respectively.The results show:The mobility of bonding agent is 160%, is resisted Folding intensity is 86MPa.
Embodiment 3
A kind of preparation method of nano-grade ceramic binding agent, the preparation method comprise the following steps:
A, the silica flour of 66.5g talcums, 26.25g kaolin, 29.75g boron glasses, 14g fluorites and 38.5g are weighed respectively, are ground 200 mesh sieves are crossed afterwards, and mixture is made;
B, by mixture made from step a with after mould briquetting, 400 DEG C are increased to the heating rate of 8 DEG C/min, then with 4 DEG C/ The heating rate of min is increased to 1350 DEG C, and keeps the temperature 6h, and water quenching is carried out to the frit flow down after melting;
C, product made from step b is dried into 12h at 100 DEG C, then adds 1.25g nano vanadium nitrides/chromium nitride composite powder End(The mass ratio of vanadium nitride and chromium nitride is 1:1), grinding, crosses 200 mesh sieves, and basis vitrified bond is made;
D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace(Sintering temperature Spend for 550 DEG C, sintering time 1h), vitrified bond of the invention is made.
The mobility and flexural strength of vitrified bond are measured respectively.The results show:The mobility of bonding agent is 182%, is resisted Folding intensity is 93MPa.
Embodiment 4
A kind of preparation method of nano-grade ceramic binding agent, the preparation method comprise the following steps:
A, the silica flour of 14g talcums, 4.2g kaolin, 6.3g boron glasses, 3.15g fluorites and 7.35g, mistake after grinding are weighed respectively 200 mesh sieves, are made mixture;
B, by mixture made from step a with after mould briquetting, 400 DEG C are increased to the heating rate of 6 DEG C/min, then with 3 DEG C/ The heating rate of min is increased to 1250 DEG C, and keeps the temperature 7h, and water quenching is carried out to the frit flow down after melting;
C, product made from step b is dried into 14h at 90 DEG C, adds 0.32g nano vanadium nitride/chromium nitride composite powders(Nitrogen The mass ratio for changing vanadium and chromium nitride is 1:1), grinding, crosses 300 mesh sieves, and basis vitrified bond is made;
D, basic vitrified bond made from step c is pressed into blank with press, is sintered with microwave agglomerating furnace(Sintering temperature Spend for 600 DEG C, sintering time 20min), vitrified bond of the invention is made.
The mobility and flexural strength of vitrified bond are measured respectively.The results show:The mobility of bonding agent is 202%, is resisted Folding intensity is 104MPa.
Comparative example 1:With embodiment 1 as a comparison, in the case of other conditions are constant, when nano vanadium nitride/nitrogen of addition It is 1 to change the mass ratio of vanadium nitride and chromium nitride in chromium composite powder:When 2, the mobility of bonding agent is 185%, and flexural strength is 96MPa。
Comparative example 2:With embodiment 1 as a comparison, in the case of other conditions are constant, when nano vanadium nitride/nitrogen of addition It is 2 to change the mass ratio of vanadium nitride and chromium nitride in chromium composite powder:When 1, the mobility of bonding agent is 172%, and flexural strength is 87MPa。
Comparative example 3:With embodiment 1 as a comparison, it is in the case of other conditions are constant, nano vanadium nitride/chromium nitride is multiple When conjunction powder is changed to nano vanadium nitride, the mobility of bonding agent is 157%, flexural strength 75MPa.
Comparative example 4:With embodiment 1 as a comparison, it is in the case of other conditions are constant, nano vanadium nitride/chromium nitride is multiple When conjunction powder is changed to nanometer chrome nitride, the mobility of bonding agent is 162%, flexural strength 79MPa.
By contrast we it can be found that being modified to bonding agent using nano vanadium nitride/chromium nitride composite powder Effect, hence it is evident that better than the modified effect that nano vanadium nitride or chromium nitride is used alone, and the matter of nano vanadium nitride and chromium nitride Amount is than being 1:When 1, modified effect is optimal.Illustrate all to show in terms of mobility, flexural strength according to product produced by the present invention It is excellent.
Although being illustrated and the invention has been described with specific embodiment, but will be appreciated that without departing substantially from the present invention's Many other change 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 (5)

  1. A kind of 1. preparation method of nano-grade ceramic binding agent, it is characterised in that:The preparation method comprises the following steps:
    A, take by mass percentage 30~50% talcum, 10~20% kaolin, 15~20% boron glass, 8~10% Fluorite and 20~25% silica flour, after grinding cross 200~300 mesh sieves, be made mixture;
    B, by mixture made from step a with after mould briquetting, 400 DEG C are increased to the heating rate for 5~10 DEG C/min, then 1200~1400 DEG C are warming up to 2~5 DEG C/min and keeps the temperature 4~8h, and water quenching is carried out to obtained frit;
    C, product made from step b is dried into 10~16h at 80~120 DEG C, adds the nanometer that mass fraction is 0.5~1.5% Vanadium nitride/chromium nitride composite powder, grinding, crosses 200~300 mesh sieves, and basis vitrified bond is made;
    D, basic vitrified bond made from step c is pressed into blank, is sintered with microwave agglomerating furnace, the nanometer is made Vitrified bond.
  2. 2. preparation method according to claim 1, it is characterised in that:The nano vanadium nitride/chromium nitride composite powder The mass ratio of middle vanadium nitride and chromium nitride is 1:1.
  3. 3. preparation method according to claim 1, it is characterised in that:The mixing, grinding are in high energy ball mill, roll Carried out in ball mill and grinder in a kind of equipment.
  4. 4. preparation method according to claim 1, it is characterised in that:The drying equipment is done for air dry oven and vacuum Any one equipment in dry case.
  5. 5. preparation method according to claim 1, it is characterised in that:The microwave oven junction temperature for 550~700 DEG C, Sintering time is 10min~1h.
CN201711415293.XA 2017-03-06 2017-12-25 Preparation method of nano ceramic binder Active CN107935556B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110640639A (en) * 2019-09-29 2020-01-03 河南工业大学 Preparation method of metal binding agent diamond product
CN112659000A (en) * 2020-12-23 2021-04-16 中国有色桂林矿产地质研究院有限公司 Cluster type inorganic bonding agent and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01240271A (en) * 1988-03-22 1989-09-25 Tokyo Daiyamondo Kogu Seisakusho:Kk Manufacture of vitrified bond for grinding wheel
CN103708429A (en) * 2013-12-19 2014-04-09 河南工业大学 Preparation method of nano vanadium nitride/chromium nitride composite powder
CN105130410A (en) * 2015-07-10 2015-12-09 河南工业大学 Preparation method of ceramic bonding agent used for quickly synthesizing CBN grinding tool

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01240271A (en) * 1988-03-22 1989-09-25 Tokyo Daiyamondo Kogu Seisakusho:Kk Manufacture of vitrified bond for grinding wheel
CN103708429A (en) * 2013-12-19 2014-04-09 河南工业大学 Preparation method of nano vanadium nitride/chromium nitride composite powder
CN105130410A (en) * 2015-07-10 2015-12-09 河南工业大学 Preparation method of ceramic bonding agent used for quickly synthesizing CBN grinding tool

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110640639A (en) * 2019-09-29 2020-01-03 河南工业大学 Preparation method of metal binding agent diamond product
CN112659000A (en) * 2020-12-23 2021-04-16 中国有色桂林矿产地质研究院有限公司 Cluster type inorganic bonding agent and preparation method thereof

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