CN101596745A - The preparation method of skive vitrified bond and skive - Google Patents

The preparation method of skive vitrified bond and skive Download PDF

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CN101596745A
CN101596745A CNA2009103043811A CN200910304381A CN101596745A CN 101596745 A CN101596745 A CN 101596745A CN A2009103043811 A CNA2009103043811 A CN A2009103043811A CN 200910304381 A CN200910304381 A CN 200910304381A CN 101596745 A CN101596745 A CN 101596745A
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skive
vitrified bond
colloidal sol
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CN101596745B (en
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万隆
胡伟达
刘小磐
汪洋
张洪磊
张国威
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Hunan University
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Abstract

The invention discloses the preparation method of a kind of skive vitrified bond and skive, earlier with technical grade SiO 2Colloidal sol and NaNO 3, KNO 3, LiNO 3, H 3BO 3Mix Deng the solution mechanical agitation, adjusting mixed solution pH is 4～6, adds technical grade Al again 2O 3Colloidal sol; The mixed sols of gained is crossed the 100-120 eye mesh screen in 500 ℃ ~ 550 ℃ oven dry, the broken back of grinding, promptly make the skive vitrified bond.Prepare skive on the basis of vitrified bond again making.This vitrified bond has material component and mixes, and the bond particle diameter can reach the nanoscale scope, and rupture strength is 101.8-105.3MPa after the sinter molding; Vitrified bond is complete to the diamond abrasive coating behind the sintering, and the porosity is 20%-28%, and operating speed can reach 80-100m/s.

Description

The preparation method of skive vitrified bond and skive
Technical field
The invention belongs to the material engineering field, relate to the preparation method of a kind of skive vitrified bond and skive, be used for to prepare low melting point, high strength, ultra micro granularity vitrified bond and emery wheel.
Background technology
The super-hard abrasive tool emery wheel mainly contains two kinds with the preparation method of vitrified bond at present: a kind of is to mix according to a certain percentage after natural silicate material is pulverized to obtain, as: systems such as clay feldspar talcum, clay feldspar quartz; Another kind is according to the bond prescription various chemical substances at high temperature to be smelted into glass or pottery, and then melting thing Mechanical Crushing is obtained the bond powder.From the process conditions analysis, the granularity of vitrified bond is determined by Mechanical Crushing that mainly the gained vitrified bond minimizes granularity can only be in micron order (1.0 microns-50.0 microns) scope.Along with development of science and technology, industrial more and more higher to the surface of the work required precision, use vitrified bonded grinding tool to add man-hour in some field, not only require the granularity of abrasive material to reach in the micron order (0.1 micron), more require the granularity of bond to reach nanoscale (0.1nm-100nm) scope, otherwise in grinding process, bond can scratch surface of the work.Therefore adopt traditional vitrified bond method to be difficult to prepare the required vitrified bond of high manufacturing accuracy emery wheel.
Summary of the invention:
The technical problem to be solved in the present invention is that the preparation method of a kind of skive vitrified bond and skive is provided
Technical solution of the present invention is as follows:
A kind of preparation method of skive vitrified bond is characterized in that, may further comprise the steps:
Earlier with technical grade SiO 2Colloidal sol (SiO 2Solid phase percentage composition 30.45%, particle diameter 12.39nm) and analyze pure level NaNO 3, KNO 3, LiNO 3, H 3BO 3Deng solution according to SiO 2: NaNO 3: KNO 3: LiNO 3: H 3BO 3Mass ratio is (40 ~ 50): (18 ~ 21.93): (12.22 ~ 15.04): (40 ~ 46): the ratio mechanical agitation of (30 ~ 35.52) is mixed, wherein NaNO 3, KNO 3, LiNO 3, H 3BO 3The solution concentration scope is 10%-60%; Adjusting mixed sols PH is 4 ~ 6 o'clock, according to SiO 2: Al 2O 3Mass ratio is (40 ~ 50): the ratio of (10 ~ 15) adds technical grade Al 2O 3Colloidal sol; With the colloidal sol of the mixing of gained 500 ℃ ~ 550 ℃ oven dry, grind broken back and cross 100 ~ 120 eye mesh screens, promptly make the skive vitrified bond.
As preferably, H 3BO 3Solution concentration is 10%, NaNO 3, KNO 3, LiNO 3The concentration of solution is 50%.
A kind of preparation method of skive is characterized in that, may further comprise the steps: earlier with technical grade SiO 2Colloidal sol (SiO 2Solid phase percentage composition 30.45%, particle diameter 12.39nm) and analyze pure level NaNO 3, KNO 3, LiNO 3, H 3BO 3Solution is according to SiO 2: NaNO 3: KNO 3: LiNO 3: H 3BO 3Mass ratio is (40 ~ 50): (18 ~ 21.93): (12.22 ~ 15.04): (40 ~ 46): (30 ~ 35.52) ratio ratio mechanical agitation is mixed, wherein NaNO 3, KNO 3, LiNO 3, H 3BO 3The solution concentration scope is 10%-60%; Adjusting mixed sols PH is 4 ~ 6 o'clock, according to SiO 2: Al 2O 3Mass ratio is (40 ~ 50): the ratio of (10 ~ 15) adds technical grade Al 2O 3Colloidal sol (Al 2O 3Percentage composition 28.12%, particle diameter 10nm-20nm); In mixed sols viscosity reaches the 20mpa.s-40mpa.s scope, under the mechanical agitation condition, add diamond abrasive, diamond abrasive and bond siccative proportion are 1 ~ 2; The quality of diamond abrasive will account for 60% ~ 70% of last emery wheel gross mass, after mixing, the mixed slurry of gained is crossed the 100-120 eye mesh screen in 500 ℃-550 ℃ oven dry, the broken back of grinding, cold moudling then, and in room temperature to 750 ℃ temperature range, sintering skive into.
Described sintering process is, heating rate is 3～5 ℃/min, reach 500 ℃ after, insulation 40～60min; Speed with 2～3 ℃/min is warming up to 600 ℃, and insulation 30min rises to 750 ℃ with 2～3 ℃/min then, and insulation 120min naturally cools to normal temperature at last.
Vitrified bond preparation at present mainly is the mode of Mechanical Crushing after employing solid block and the powder glassization, and the present invention breaks through the preparation method of traditional grinding wheel bond, earlier with technical grade SiO 2Colloidal sol (SiO 2Solid phase percentage composition 30.45%, particle diameter 12.39nm) and analyze pure level (material purity 〉=99.5%) NaNO 3, KNO 3, LiNO 3, H 3BO 3Mix Deng the solution mechanical agitation, wherein NaNO 3, KNO 3, LiNO 3, H 3BO 3The solution concentration scope is 10%-60%, H 3BO 3Preferred value is 10%, and all the other solution are preferred value with 50%.Adjusting mixed sols PH is 4 o'clock adding technical grade Al 2O 3Colloidal sol (Al 2O 3Percentage composition 28.12% is at technical grade Al 2O 3Aluminium chlorine is 1.1 than Al/Cl in the sol system, particle diameter 10nm-20nm), as with 100g Li 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Vitrified bond is an example, and above-mentioned each quality of material ratio range is: SiO 2Colloidal sol 130g-165g, Al 2O 3Colloidal sol 35g-55g, H 3BO 330g-35g, LiNO 340g-48g, NaNO 318g-20g, KNO 312g-16g.In mixed sols viscosity reaches the 20mpa.s-40mpa.s scope, under the mechanical agitation condition, add diamond abrasive, (quality of diamond abrasive will account for last emery wheel gross mass 60% ~ 70%), after evenly mixing, slurry is dried, grinds broken back cross the 100-120 eye mesh screen 500 ℃-550 ℃ (preferred value is 500 ℃), 20MPa cold moudling then, and in 720 ℃ of-750 ℃ of temperature ranges, sinter emery wheel into.
Thinking of the present invention is: utilize the following characteristics of colloidal sol, be applied to Li 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2The production of wheel ceramic bond.Colloidal sol is a kind of non-setting colloid of solid matter that keeps in dispersion, and the decentralized medium here mainly is a liquid, and the solids size in the colloidal sol is a nanoscale.Compare with the traditional preparation process method with the powder particle that colloidal sol is prepared, it has the dopant variation, and goods are even, the purity height, and firing temperature is low, and grain graininess more can reach advantages such as nanoscale.In recent years, at ceramic fibre, the preparation aspect of materials such as glass-ceramic has obtained extensive use, as using Al 2O 3Colloidal sol, SiO 2Colloidal sol is produced MgO-Al 2O 3-SiO 2Microcrystalline glass in series, this devitrified glass have the preparation that low dielectric constant, low thermal coefficient of expansion, high mechanical strength etc. are widely used in special glass.
Advantage of the present invention and effect:
The present invention adopts the technical grade SiO of ceramic-like component 2Colloidal sol, Al 2O 3Colloidal sol and the pure level of analysis NaNO 3, KNO 3, LiNO 3, H 3BO 3The method that the solution liquid phase is mixed is prepared low melting point, high strength, ultra micro granularity vitrified bond and emery wheel.Specifically comprise following characteristics:
(1) adopt the colloidal sol of ceramic-like component and solution liquid phase to mix, because the colloidal sol particle diameter is the nanoscale scope, all the other multi-component materials are to exist with ionic compound solution form, after the liquid phase substance oven dry, the mixture homogeneity height of resulting product, particle diameter distributes can reach nanoscale; As the made Li of inventive method for this reason of white agglomerated particle (1nm-100nm) in (Fig. 1) 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2It is the vitrified bond particulate.
(2) made bond is by colloidal sol or solution combination, and because of good uniformity, particle is tiny, and specific area is big, the surface can be high, has high sintering activity, so in sintering process, each material reaction between crystals energy barrier is low, sintering temperature is low, and frit reaction is abundant, and high temperature solution is evenly distributed.With the prepared bond refractoriness scope of the method at 720 ℃-750 ℃; Thermal coefficient of expansion 5.06*10 after 500 ℃ of oven dry of bond -6-5.68*10 -6/ ℃ between; Rupture strength is 101.8-105.3MPa behind 720 ℃ of-750 ℃ of sintering of bond.As with identical material ratio, adopt the Li of vitreous mechanical crushing method preparation 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Be vitrified bond refractoriness scope at 760-780 ℃, thermal coefficient of expansion is 5.32*10 -6/ ℃, rupture strength is 87.6MPa behind 720 ℃ of-750 ℃ of sintering, and 760-780 ℃ of rupture strength is 100.2-104.4MPa, and its material property is inferior to the performance of the vitrified bond that the present invention makes.
(3) the present invention can also simplify mixing of abrasive material and bond, and being blended in the liquid system of abrasive material and bond carried out, and the slurry oven dry is ground, and can obtain the molding mass (Fig. 1) that abrasive material and bond mix after sieving; Bond is good to the diamond abrasive wetability in the sintering process, coat complete, emery wheel uniform microstructure (Fig. 2).
Vitrified bond consists of (percentage meter (%) by weight): SiO 240-45, Al 2O 310-15, B 2O 318-20, Li 2O9-10, Na 2O7-8, K 2O 7-6, sintering temperature 720-750 ℃, rupture strength is 101.8-105.3MPa after the sinter molding; Adopt the method to prepare vitrified bond and can also simplify and the diamond abrasive hybrid technique, vitrified bond is complete to the diamond abrasive coating behind the sintering, and wheel face hardness is 99.2 ~ 110.1HRB, and the porosity is 20%-28%, and operating speed can reach 80-100m/s.
Description of drawings:
Fig. 1 vitrified bond is pulverized and to be expected microstructure scanning electron figure behind 120 mesh sieves;
Fig. 2 emery wheel sintering rear surface microstructure scanning electron figure;
The process chart of Fig. 3 emery wheel preparation.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Patent of the present invention prepares Li 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2The raw material that vitrified bond adopts has: technical grade SiO 2Colloidal sol (solid concentration 30.45%) and Al 2O 3Colloidal sol (solid concentration 28.12%) is analyzed pure lithium nitrate, sodium nitrate, potassium nitrate, boric acid etc., and adopt concentration be 30% nitric acid for regulating pH value, the parameter in following examples of the present invention is to prepare 100 gram Li 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Vitrified bond is a normative reference.
Specific embodiment 1:
Component SiO 2Colloidal sol Al 2O 3Colloidal sol H 3BO 3 LiNO 3 NaNO 3 KNO 3
Quality (g) 131.36 53.34 35.52 46 21.93 15.04
According to filling a prescription at first with H shown in the last table 3BO 3, LiNO 3, NaNO 3, KNO 3Four kinds of materials are provided as mixed solution, wherein H 3BO 3Solution concentration is 10%, LiNO 3, NaNO 3, KNO 3Solution concentration is 50%; Take by weighing technical grade SiO 2Colloidal sol slowly adds above-mentioned mixed solution at stirring condition, uses 30%HNO 3It is 4 o'clock that solution is adjusted mixed sols PH, adds technical grade Al 2O 3Colloidal sol stirs, and with 500 ℃ of oven dry of this mixed sols, grinds, and crosses 120 eye mesh screens, the Li that obtains 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Vitrified bond chemical composition (wt%) scope is as shown in the table:
Component SiO 2 Al 2O 3 B 2O 3 Li 2O Na 2O K 2O
Quality (g) 40 15 20 10 8 7
wt％ 40％ 15％ 20％ 10％ 8％ 7％
This bond refractoriness is 720 ℃, and rupture strength is 101.8MPa, and thermal coefficient of expansion is 5.68*10 -6/ ℃.
For simplifying the batch mixing program of bond and diamond abrasive, the present invention adds diamond abrasive (particle diameter w3.5) with bond at the mixed sols liquid phase state.In mixed sols viscosity reaches the 20mpa.s-40mpa.s scope, under the mechanical agitation condition, add diamond abrasive (quality of diamond abrasive will account for last emery wheel gross mass 60% ~ 70%).After evenly mixing, 120 eye mesh screens are crossed in 500 ℃ of oven dry of slurry, the broken back of grinding, adding the 1g methylated cellulose aqueous solution with the 100g siccative is the emery wheel wetting agent, 20MPa cold moudling then.The emery wheel sintering process is, heating rate is 3～5 ℃/min, reach 500 ℃ after, insulation 40～60min; Speed with 2～3 ℃/min is warming up to 600 ℃, and insulation 30min rises to 730 ℃ with 2～3 ℃/min then, and insulation 120min naturally cools to normal temperature at last.The made emery wheel porosity is 20% ~ 26%, and grinding speed can reach 80 ~ 100m/s.
Specific embodiment 2:
Figure A20091030438100071
According to filling a prescription at first with H shown in the last table 3BO 3, LiNO 3, NaNO 3, KNO 3Four kinds of materials are provided as mixed solution, wherein H 3BO 3Solution concentration is 10%, LiNO 3, NaNO 3, KNO 3Solution concentration is 50%; Take by weighing technical grade SiO 2Colloidal sol dropwise adds above-mentioned mixed solution at stirring condition, uses 30%HNO 3It is 4 o'clock that solution is adjusted mixed sols PH, adds technical grade Al 2O 3Colloidal sol stirs, and with 500 ℃ of oven dry of this mixed sols, grinds, and crosses 120 eye mesh screens, the Li that obtains 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Vitrified bond chemical composition (wt%) scope is as shown in the table:
Component SiO 2 Al 2O 3 B 2O 3 Li 2O Na 2O K 2O
Quality (g) 45 15 18 9 7 6
wt％ 45％ 15％ 18％ 9％ 7％ 6％
This bond refractoriness is 740 ℃, and rupture strength is 103.2MPa, and thermal coefficient of expansion is 5.31*10 -6/ ℃.
Prepared skive under the experiment condition similarly to Example 1, emery wheel sintering process be, heating rate is 3～5 ℃/min, reach 500 ℃ after, insulation 40～60min; Speed with 2～3 ℃/min is warming up to 600 ℃, and insulation 30min rises to 740 ℃ with 2～3 ℃/min then, and insulation 120min naturally cools to normal temperature at last.The porosity is 23% ~ 25%, and grinding speed can reach 80 ~ 100m/s.
Specific embodiment 3:
Component SiO 2Colloidal sol Al 2O 3Colloidal sol H 3BO 3 LiNO 3 NaNO 3 KNO 3
Quality (g) 164.2 35.56 31.97 41.4 19.19 12.89
According to filling a prescription at first with H shown in the last table 3BO 3, LiNO3, NaNO 3, KNO 3Four kinds of materials are provided as mixed solution, wherein H 3BO 3Solution concentration is 10%, LiNO 3, NaNO 3, KNO 3Solution concentration is 50%; Take by weighing technical grade SiO 2Colloidal sol dropwise adds above-mentioned mixed solution at stirring condition, uses 30%HNO 3It is 4 o'clock that solution is adjusted mixed sols PH, adds technical grade Al 2O 3Colloidal sol stirs, and with 500 ℃ of oven dry of this mixed sols, grinds the back and crosses 120 eye mesh screens, the Li that obtains 2O-Na 2O-K 2O-Al 2O 3-B 2O 3-SiO 2Vitrified bond chemical composition (wt%) scope is as shown in the table:
Component SiO 2 Al 2O 3 B 2O 3 Li 2O Na 2O K 2O
Quality (g) 50 10 18 9 7 6
wt％ 50％ 10％ 18％ 9％ 7％ 6％
This bond refractoriness is 750 ℃, and rupture strength is 105.3MPa, and thermal coefficient of expansion is 5.06*10 -6/ ℃.
Prepared skive under the experiment condition similarly to Example 1, emery wheel sintering process be, heating rate is 3～5 ℃/min, reach 500 ℃ after, insulation 40～60min; Speed with 2～3 ℃/min is warming up to 600 ℃, and insulation 30min rises to 750 ℃ with 2～3 ℃/min then, and insulation 120min naturally cools to normal temperature at last.The porosity is 24% ~ 28%, and grinding speed can reach 80 ~ 100m/s.

Claims (4)

1. the preparation method of a skive vitrified bond is characterized in that, may further comprise the steps:
Earlier with technical grade SiO2 colloidal sol and the pure level of analysis NaNO3, KNO3, LiNO3, H3BO3 solution is according to SiO2: NaNO3: KNO3: LiNO3: the H3BO3 quality is (40 ~ 50): (18 ~ 21.93): (12.22 ~ 15.04): (40 ~ 46): the ratio mechanical agitation of (30 ~ 35.52) is mixed, NaNO3 wherein, KNO3, LiNO3, H3BO3 solution concentration scope is 10%-60%; Adjusting mixed solution PH is 4 ~ 6, and again in SiO2: the Al2O3 mass ratio is (40 ~ 50): the ratio of (10 ~ 15) adds technical grade Al2O3 colloidal sol; The gained mixed sols is crossed the 100-120 eye mesh screen in 500 ℃ ~ 550 ℃ oven dry, the broken back of grinding, promptly make the skive vitrified bond.
2. the preparation method of skive vitrified bond according to claim 1 is characterized in that, the method preparation that vitrified bond adopts colloidal sol and solution to mix through liquid phase, the H3BO3 solution concentration is 10%, NaNO3, KNO3, the concentration of LiNO3 solution is 50%.
3. the preparation method of a skive, it is characterized in that, may further comprise the steps: earlier with technical grade SiO2 colloidal sol and the pure level of analysis NaNO3, KNO3, LiNO3, H3BO3 solution are according to SiO2: NaNO3: KNO3: LiNO3: the H3BO3 quality is (40 ~ 50): (18 ~ 21.93): (12.22 ~ 15.04): (40 ~ 46): (30 ~ 35.52) ratio mechanical agitation is mixed, NaNO3 wherein, KNO3, LiNO3, H3BO3 solution concentration scope is 10% ~ 60%; Adjusting mixed sols PH is 4 ~ 6, and by SiO2: the Al2O3 mass ratio is (40 ~ 50): the ratio adding technical grade Al2O3 colloidal sol of (10 ~ 15); In mixed sols viscosity reaches the 20mpa.s-40mpa.s scope, under the mechanical agitation condition, add diamond abrasive, the quality of diamond abrasive accounts for 60% ~ 70% of forming grinding wheel gross mass; , after mixing, the mixed slurry of gained is crossed the 100-120 eye mesh screen in 500 ℃-550 ℃ oven dry, the broken back of grinding, cold moudling then, and in room temperature to 750 ℃ temperature range, sinter skive into.
4. the preparation method of skive according to claim 3 is characterized in that, described sintering process is, heating rate is 3～5 ℃/min, reach 500 ℃ ~ 550 ℃ from room temperature after, insulation 40～60min; Speed with 2～3 ℃/min is warming up to 600 ℃ ~ 650 ℃, and insulation 30min ~ 40min rises to 720 ℃ ~ 750 ℃ with 2～3 ℃/min then, and insulation 100min ~ 120min naturally cools to normal temperature at last.
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