CN108675776A - Preparation method with laminated structure Ceramic corundum abrasive - Google Patents
Preparation method with laminated structure Ceramic corundum abrasive Download PDFInfo
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- CN108675776A CN108675776A CN201810549245.8A CN201810549245A CN108675776A CN 108675776 A CN108675776 A CN 108675776A CN 201810549245 A CN201810549245 A CN 201810549245A CN 108675776 A CN108675776 A CN 108675776A
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C09K3/14—Anti-slip materials; Abrasives
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Abstract
Present invention relates particularly to a kind of preparation methods with laminated structure Ceramic corundum abrasive, it is characterised in that steps are as follows:1) filter cake is dried in an oven;2) colloid is prepared:The aqueous solution of modifying agent is added, blocky-shaped particle absorbs water, fierce heat release and water quenching occurs, is broken into 1 millimeter of fine particle below strongly, then forms uniform suspension with colloid mill is broken;It imports in vacuum kneader, starts kneader, nitric acid is added, starts and vacuumizes, become gel;3) colloid is dried:Gel is put into baking oven and is dried;4) it is crushed, calcines;5) it is sintered.The preparation method of the present invention has that low energy consumption, and production stage simplifies, it is easy to accomplish the advantages of the serialization and automation of technique.Contain laminated structure using abrasive material produced by the present invention, has the advantages that grinding efficiency is high, durability is high.
Description
Technical field
Present invention relates particularly to a kind of preparation methods with laminated structure Ceramic corundum abrasive.
Background technology
Ceramic corundum abrasive is a kind of novel corundum class abrasive material, is a kind of common corundum being substantially better than fusion method manufacture
The corundum kind of abrasive material, bonded abrasive tool, coated abrasive tool and the various abrasive articles prepared with Ceramic corundum abrasive have
The feature that grinding efficiency is high, service life is long, grinding heat is low, and it is largely used to the grinding of difficult grind material.In recent years, ceramic
Corundum abrasive product obtains tremendous development.
Ceramic corundum abrasive is invented by the Minnesota Mining and Manufacturing Co. (3M companies) in the U.S. earliest, the 3M of early stage
The patent 4314827 (U.S. Patent number) of company is raw material using a water aluminium oxide, forms colloidal sol after nitric acid is added, adds nitre
As gel is formed after modifying agent, then drying, broken, screening, calcining, sintering has been prepared ceramic rigid for sour magnesium or acetic acid zirconium
Beautiful abrasive material;The method by the way that alumina seed is added has been invented again by later Norton Co, reduces sintering temperature, makes crystal
The technology of preparing (United States Patent (USP) 4623364) of the Ceramic corundum abrasive become smaller in size.United States Patent (USP) (patent No. 5164348)
Modifying agent being introduced using infusion process again and being prepared for new varieties Ceramic corundum abrasive, manufacturing step is to prepare collosol and gel, then
Drying is crushed, and the particle of needs is sifted out, after these particles are calcined at a certain temperature, with the aqueous solution of modifying agent to it
It is impregnated, since the particle after calcining contains a large amount of micro- stomata, dipping solution is easily entered inside particle, then carried out
Drying, calcining, sintering, become the extraordinary Ceramic corundum abrasive of performance.Later, the patent of a series of Ceramic corundum abrasive is not
It is disconnected to emerge.The country also has the patent of Ceramic corundum abrasive to occur, such as present inventor Zhai Han after 2000
The patent of invention《A kind of α-alumina-based abrasive and preparation method thereof》(patent No. ZL 201110283203.2) and《One kind contains
α-alumina-based abrasive of laminated structure and preparation method thereof》(patent No. ZL 201110283236.7) utilizes domestic production
Thin nurse stone semi-finished product have produced two kinds of Ceramic corundum abrasive products as raw material using sol-gel technique.
《A kind of α-alumina-based abrasive and preparation method thereof containing laminated structure》(patent No. ZL201110283236.7)
The preparation process of middle Ceramic corundum abrasive is prepared by following procedures using thin nurse stone semi-finished product as raw material:
1) colloid is prepared:A small amount of pure water and a certain amount of peptizing agent is added in thin nurse stone semi-finished product, and (peptizing agent is usually
Monoacid, most preferably nitric acid) colloidal sol is formed after mixing, colloidal sol gradually becomes gel, which contains Al2O3·nH2O
(wherein n approximations are 1.8) is generally in 25% or so (Al2O3·nH2The content of O is commonly referred to as solid content), it is other to be nearly all
Water, if solid content height is a bit, viscosity is too big, and producing colloidal sol can more difficult operation in technique.
2) colloid is dried:Gel is dried in an oven, gel becomes about ten millimeters or so of block, this block
Very crisp, intensity very little, these blocks also contain about 25% or so the crystallization water.
3) it is crushed, calcines:It is broken into certain granularity with crusher, the granularity of needs is sifted out with sieve;At 700 DEG C
These particles are calcined at a high temperature of left and right, to the crystallization water of removal 25% or so.
4) it impregnates:Burnt particle is impregnated with the dipping solution containing modifying agent, to introduce the various improvement of needs
Agent.The introducing of modifying agent can also together be added when preparing colloidal sol in the patent, but in this case, in the drying course of colloid
In, the migration of modifying agent intermediate ion can be caused, keeps the component distributing of modifying agent uneven, causes the decline of product quality.By reality
It applies in example 3, by calculating, the solid content (Al of colloid2O3·nH2O (wherein n approximations are 1.8)) it is 36%, due to water content
Greatly, during the drying process, the ion in modifying agent will produce migration, and surface concentration is caused to be more than concentration inside, make the pottery come
Porcelain corundum abrasive uneven components will be obvious that from color and.
5) it dries again:Then the moisture in maceration extract is dried in an oven;
6) it is sintered:It is sintered at a high temperature of 1450 DEG C or so, has just prepared Ceramic corundum abrasive, this kind of ceramic corundum mill
Material is a kind of Ceramic corundum abrasive containing laminated structure.
Boehmite semi-finished product described in foregoing invention refer to when producing industrial products boehmite (being called boehmite),
Sodium aluminate solution is produced with aluminum ore or other raw materials that can manufacture sodium metaaluminate or sodium aluminate, is then acidified, is pure
After the series of processes such as change, the suspension produced, then after most of water is removed in press filtration or other means, the filter cake of formation,
As boehmite semi-finished product, (wherein attached water about 65% or so) containing total Water 70%~80%, thin nurse stone semi-finished product profit
After being dried with flash process, broken, sieving is industrial products boehmite or is thin nurse stone.Thin nurse stone is a kind of containing big
The aqueous alumina of about 1.8 crystallizations water, some data are just Al2O3·H2O.It is that raw material makes ceramic corundum with thin nurse masonry
Abrasive material needs that colloidal sol is made, this step needs that a large amount of pure water is added, and uses thin nurse stone semi-finished product as raw material, is exactly utilized
Containing about 65% or so attached water in thin nurse stone semi-finished product.Thin nurse stone semi-finished product do not remove contained large quantity of moisture, production cost
Naturally it just reduces, price is also relatively low.Thin nurse stone semi-finished product using temperature when flash process moisture removal be it is relatively high, in this way
High temperature can change certain performances of thin nurse stone, be unfavorable to production ceramic abrasive.Using thin nurse stone semi-finished product as original
The advantages of material produces Ceramic corundum abrasive is the raw material that can obtain low cost, saves when colloidal sol is produced in part and needs the water being added
Point, due to the high temperature without flash evaporation drying, thus the extraordinary colloidal sol of quality and gel can be made.The disadvantage is that with thin nurse stone
Semi-finished product are as waste colloidal sol, and the moisture in colloidal sol is very big, and general moisture is up to 70%-80%, the viscosity of colloidal sol
Also very big, the solid content in colloidal sol is relatively low, and the collosol and gel drying difficulty of low-solid content is more difficult than the drying of thin nurse stone semi-finished product
It spends much larger.Thin nurse stone semi-finished product drying uses flash process, and quickly, efficiency is very high for drying rate.The drying of collosol and gel is not
Flash process can be used, requirement that must be in large grained or bulk after collosol and gel drying, the bulky grain after drying or block
Shape object is fine and close as possible, not generate stomata, so that the process below carries out the broken granularity for reaching needs, flash process dries
Material is loose powder-material after dry, and back can not just make the particle of needs.Therefore the drying of collosol and gel can only use drying box
Equal similar devices, making colloid, drying is to obtain large grained or bulk under static situation, since the property of colloid itself is dried
It starts working extremely difficult, drying rate is very slow, and energy consumption is very high.Water content fluctuation is very big between thin nurse stone semi-finished product different batches,
That is solid content fluctuation is very big, when preparing colloidal sol, the peptizing agent and modifying agent of addition can not accurate quantitative analysis, cause product quality
Fluctuation.
Invention content
Present invention aim to address the prior art sol-gel technique system is utilized as raw material using thin nurse stone semi-finished product
Standby Ceramic corundum abrasive is big in the presence of drying difficulty, speed is slow, high energy consumption, and the big defect of quality fluctuation, providing one kind having sheet
The preparation method of structural ceramics corundum abrasive, energy consumption substantially reduce, and production stage is simplified, it is easy to accomplish technique it is continuous
Change and automates.
The present invention is achieved through the following technical solutions:
I.e. a kind of preparation method with laminated structure Ceramic corundum abrasive, it is characterised in that steps are as follows:
1) filter cake is dried:The thin nurse stone semi-finished product of filter cake shape are fitted into stainless steel disc, are put into 140 ± 40 DEG C of baking oven
Drying, the thin nurse stone after drying is at 1-10 millimeters of blocky-shaped particles;
Moisture in thin nurse stone semi-finished product is very high, but due to being attached water, and drying gets up to be easier, and drying rate is very
Soon, for the thin nurse stone after drying at about 1-10 millimeters of blocky-shaped particle, these blocky-shaped particles contain many crackles, very crisp, can with hand
Easily to crumb, molecular formula Al2O3·nH2O (wherein n approximations are 1.8)) its alumina content about 75%, contain the crystallization water
About 25%.Other certain more economical drying sides and completely can with.
2) colloid is prepared:The aqueous solution of modifying agent is added in the blocky-shaped particle for taking constant weight, which contains nitric acid
Neodymium, lanthanum nitrate, yttrium nitrate, magnesium nitrate and cobalt nitrate, after five kinds of nitrate are converted into oxide, using aluminium oxide therein as base
Number contains neodymia 0.7%-1.5%, lanthana 0.7%-1.5%, yttrium oxide 0.7%-1.5%, magnesia 0.7%- respectively
1.5%, cobalt oxide 0.06%-0.09%, blocky-shaped particle accounts for the 45%-60% of gross mass;After the aqueous solution of modifying agent is added, by
Blocky-shaped particle after these drying absorbs water strongly, it may occur that fierce heat release and water quenching, bulky grain be broken into one after another 1 millimeter with
Under fine particle, then added the solidliquid mixture of modifying agent is broken to form uniform suspension these with colloid mill;So
These suspension are imported in vacuum kneader afterwards, kneader is started, blocky-shaped particle weight is slowly added into these suspension
8% nitric acid, nitric acid used are that 65% concentration nitric acid is started and vacuumized after nitric acid is added, and suspension gradually becomes very viscous
Thick gel, these gels do not have mobility, in big blocky;
The effect of modifying agent is to increase its toughness and hardness, while reducing sintering temperature to improve the density of sintered body,
Obtain smaller crystallite dimension.In addition to this, the combination of these types of modifying agent can form a kind of mineral of magnetoplumbite type, this
Kind of mineral are a kind of laminated structures, are very suitable for doing abrasive material, and very high grinding efficiency and durable can be obtained in grinding process
Degree.
As a preferred solution of the present invention:Blocky-shaped particle accounts for the 50%-55% of gross mass, i.e. solid content is 50%-
55%.
Ratio of the blocky-shaped particle (i.e. solid content) of the present invention in gross mass is extremely important, and blocky-shaped particle accounting is high,
It can be too viscous in colloid mill grinding below, it is not easy to operate;Blocky-shaped particle accounting is few, and moisture is just high, is easy to make
It is uneven at product composition.Colloid is made in drying, since large quantity of moisture gradually volatilizees from surface, part modifying agent ion
From internal migration to surface, the improvement agent content on surface is caused to be more than the content of internal improvement agent, Ion transfer can be from addition
Cobalt nitrate color discrimination, cobalt nitrate is pink, and the place of pink weight illustrates that the concentration of cobalt nitrate is high, and pink is shallow
The concentration of local cobalt nitrate is low.It is demonstrated experimentally that solid content is at least more than 45%, and best 50% or more, in the lower drying of temperature
At a temperature of and moisture migration path it is short as possible under conditions of, can just obtain relatively uniform component content.
3) colloid is dried:Gel is taken out, cut with knife or with extruder be extruded into thickness be less than 5mm sheet, or with extrusion
Machine is extruded into the strip of 1-5 millimeters of diameter, and then sheet or strip gel are fitted into stainless steel disc, is put into baking oven and dries, and dries
The temperature of case is set between 50 DEG C -90 DEG C.
Drying temperature is extremely important, and temperature is too low, and drying rate is slow, and temperature is high, will also result in Ion transfer.Experiment card
Bright, under the solid content index that we set, and after being cut into the sheet of 1-5mm, drying temperature compares between being set in 50 DEG C -90 DEG C
It is appropriate, at this point, the material color after drying is relatively uniform.
Preferred embodiment as the present invention:It is dried 2 hours at 50 DEG C of scenario earthquake, improves to 60 DEG C and dry 1 hour,
It is improved again to 70 DEG C and is dried 1 hour, 80 DEG C dry 1 hour, and last 90 DEG C dry 1 hour.Since these gel water content compare
It is small, and these shape table areas are big, and it is relatively high to dry efficiency.
The transport phenomena of ion enhances with the raising of drying temperature, weakens with the raising of solid content, setting drying temperature
It writes music line, the material uniformity that can have not only obtained, but also drying rate can be accelerated.
The moisture of colloid be all from surface formed vapor be separated from colloid, the moisture inside colloid must gradually migrate to
Surface is volatilized into steam, and colloid just gradually becomes drying.It is cut into thickness and is less than 5mm sheets, or be extruded into the strip of diameter 1-5mm,
It is the distance in order to reduce moisture from colloid internal migration to surface, migration distance of the moisture from inside to surface is shorter, ion
Migration with regard to smaller, can be more preferable by the way that colloid is cut into sheet of the thickness less than 5mm or is extruded into the strip of a diameter of 1-5mm
Decrease ion migration.
4) it is crushed, calcines:Gel after drying is at large grained, with crusher in crushing at the granularity of needs, such as 16
Granularity between 120 mesh of mesh -, is fitted into saggar, and the moisture also contained is removed in 550 DEG C of -800 DEG C of calcinings,
The present invention is preferably calcined with rotary calcining kiln, and rotary calcining kiln can be with continuous calcining, and production capacity is big, and compares
Compared with the saving energy;
5) it is sintered:Material after calcining needs further sintering, could form hard Ceramic corundum abrasive.Sintering is preferred
With swinging sintering furnace, pivoting part recrystallized silicon carbide pipe, sintering time 5-30 minutes, sintering temperature control is 1440
℃。
The present invention preparation method have low energy consumption, production stage simplify, it is easy to accomplish the serialization and automation of technique
The advantages of.Contain laminated structure using abrasive material produced by the present invention, has the advantages that grinding efficiency is high, durability is high.
Description of the drawings
Fig. 1 is the stereoscan photograph on Ceramic corundum abrasive surface produced by the present invention;
Fig. 2 is the stereoscan photograph of Ceramic corundum abrasive section produced by the present invention.
Specific implementation mode
Embodiment 1
It takes and contains Al2O3·nH233% or so thin nurse stone semi-finished product 10kg of O, are placed in an a height of 650mm*450mm* of length and width
It in the stainless steel disc of 50mm, puts in box drying box, temperature is set as 140 DEG C, becomes size about 10mm or so after several hours
Blocky-shaped particle, blocky-shaped particle after drying salic generally 75% is total about containing the crystallization water and a small amount of attached water
25%.
64 grams of magnesium nitrate hexahydrate, six 26 grams of water neodymium nitrates, lanthanum nitrate hexahydrate 26.6 are added in one 5 liters of rustless steel container
Gram, 33.9 grams of yttrium nitrate hexahydrate, 2.7 grams of cobalt nitrate hexahydrate, 1050 grams of pure water adds after all nitrate all dissolving
Block-like thin 1333 grams of the nurse stone semi-finished granules for entering drying, can hear the fragmentation sound of crack in Pi, this is thin nurse after adding
The sound of stone water quenching, quickly, these bulky grains are broken into 1mm or so little particles.These mixtures are poured into a colloid mill, wink
Between these little particles the suspension that can be flowed is worn by colloid mill.
Suspension is transferred in a kneader with vacuum extractor, 65% 106 grams of nitric acid is gradually added into, starts
Vacuum extractor, in the kneading process of kneader, material becomes very sticky, and after mediating uniformly, takes out, thickness is cut into stainless steel knife
The piece for spending about 5mm or so, is put into baking oven, is dried at a temperature of 80 DEG C, becomes the fritter of 1-10mm or so after drying.
It is broken into thinner particle with a disk crusher, under sieve takes 16 mesh to sieve, the particle on 120 mesh sieve is mounted in porcelain
In crucible, in 750 DEG C of temperature lower calcinations 30 minutes, it is then transferred into platinum crucible, is put into 1440 DEG C of Muffle furnace and is sintered
10 minutes.Sintered material is Ceramic corundum abrasive, these Ceramic corundum abrasive colors are blue, that is to say cobalt member therein
The color for the cobalt blue that element is formed with aluminium oxide, color uniformity are not different with the color for being introduced modifying agent using infusion process.
Test these Ceramic corundum abrasives, 3.895 grams/cm of density3, microhardness 21GPa, stereoscan photograph is shown in Fig. 1, Fig. 2.
Embodiment 2
With embodiment 1, except that after block-like gel is made in kneader, it is put into an extruder and is extruded into diameter
It for the strip of 3mm, is fitted into stainless steel disc, is put into drying box, scenario earthquake:50 DEG C dry 2 hours, and 60 DEG C of drying 1 are small
When, 70 DEG C dry 1 hour, and 80 DEG C dry 1 hour, and 90 DEG C dry 1 hour (in fact, the drying time under each drying temperature
Should be according to the size of baking oven, the number and the humidity in baking oven of the material being fitted into baking oven are adjusted, because baking oven is big
Small, material number and the humidity of baking oven can all significantly affect drying rate.This example is a special case).Other same embodiments
1.The Ceramic corundum abrasive shape that the present embodiment is made is more sharp, and color uniformity, density is 3.902, and microhardness is
20.5GPa。
Embodiment 3
With embodiment 1, it is only added 44.9 grams of magnesium nitrate hexahydrate, six 18.2 grams of water neodymium nitrates, 18.6 grams of lanthanum nitrate hexahydrate,
23.7 grams of yttrium nitrate hexahydrate, 3.5 grams of cobalt nitrate hexahydrate, its color of the Ceramic corundum abrasive made is than embodiment 1 and embodiment 2
Color is more blue, and color uniformity, density is 3.885, and microhardness is 20.3GPa.
It is clear that industry technical staff can refer to the Ceramic corundum abrasive that the present invention prepares other kinds completely.
Claims (3)
1. a kind of preparation method with laminated structure Ceramic corundum abrasive, it is characterised in that steps are as follows:
1) filter cake is dried:The thin nurse stone semi-finished product of filter cake shape are fitted into stainless steel disc, is put into 140 ± 40 DEG C of baking oven and dries
Dry, the thin nurse stone after drying is at 1-10 millimeters of blocky-shaped particles;
2) colloid is prepared:The aqueous solution of modifying agent is added in the blocky-shaped particle for taking constant weight, and the blocky-shaped particle after drying is inhaled strongly
Fierce heat release and water quenching occur for water, and bulky grain is broken into 1 millimeter of fine particle below one after another, then use colloid mill this
It is a little to have added the solidliquid mixture of modifying agent is broken to form uniform suspension;These suspension are imported in vacuum kneader, are opened
Dynamic kneader is slowly added into 65% concentration nitric acid of blocky-shaped particle weight 8% into these suspension and is opened after nitric acid is added
Dynamic to vacuumize, suspension gradually becomes very sticky gel, these gels do not have mobility, in big blocky;The water of modifying agent
Solution contains neodymium nitrate, lanthanum nitrate, yttrium nitrate, magnesium nitrate and cobalt nitrate, after five kinds of nitrate are converted into oxide, with therein
Aluminium oxide is radix, contains neodymia 0.7%-1.5%, lanthana 0.7%-1.5%, yttrium oxide 0.7%-1.5%, oxygen respectively
Change magnesium 0.7%-1.5%, cobalt oxide 0.06%-0.09%, blocky-shaped particle accounts for the 45%-60% of gross mass;
3) colloid is dried:Gel is taken out, cut with knife or is extruded into the sheet that thickness is less than 5mm with extruder, or is squeezed with extruder
At 1-5 millimeters of strip of diameter, then sheet or strip gel are fitted into stainless steel disc, is put into baking oven and dries, baking oven
Temperature is set in 50 DEG C -90 DEG C;
4) it is crushed, calcines:Gel after drying is fitted into crusher in crushing at the granularity of needs in saggar at large grained,
The moisture that 550 DEG C of -800 DEG C of calcining removals also contain;
5) it is sintered:Sintering time 5-30 minutes, sintering temperature are 1440 DEG C.
2. the preparation method according to claim 1 with laminated structure Ceramic corundum abrasive, it is characterised in that step 3)
In, temperature curve is to be dried 2 hours at 50 DEG C, improves to 60 DEG C and dries 1 hour, then improves to 70 DEG C and dry 1 hour, 80 DEG C of bakings
1 hour dry, last 90 DEG C dry 1 hour.
3. the preparation method according to claim 1 with laminated structure Ceramic corundum abrasive, it is characterised in that step 2)
In, blocky-shaped particle accounts for the 50%-55% of gross mass.
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CN111019605A (en) * | 2019-12-05 | 2020-04-17 | 青岛瑞克尔新材料科技有限公司 | Ceramic microcrystalline abrasive material with low bulk density and preparation method of abrasive tool product thereof |
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CN110104974B (en) * | 2019-03-11 | 2021-06-08 | 山东天汇研磨耐磨技术开发有限公司 | Special anti-collision and modified microcrystalline ceramic abrasive for machine tool industry and manufacturing method thereof |
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CN112939587A (en) * | 2021-02-09 | 2021-06-11 | 洛阳润宝研磨材料有限公司 | Preparation method of high-density nano ceramic grinding material |
CN112939587B (en) * | 2021-02-09 | 2023-03-03 | 洛阳润宝研磨材料有限公司 | Preparation method of high-density nano ceramic grinding material |
CN113214790A (en) * | 2021-04-06 | 2021-08-06 | 白鸽磨料磨具有限公司 | Hollow alumina ball-based composite abrasive, preparation method thereof and grinding tool |
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