CN1317230C - Method for producing cubic boron nitride abrasive grains - Google Patents

Method for producing cubic boron nitride abrasive grains Download PDF

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CN1317230C
CN1317230C CNB02810207XA CN02810207A CN1317230C CN 1317230 C CN1317230 C CN 1317230C CN B02810207X A CNB02810207X A CN B02810207XA CN 02810207 A CN02810207 A CN 02810207A CN 1317230 C CN1317230 C CN 1317230C
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boron nitride
abrasive grain
cubic boron
abrasive
abrasive grains
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CN1703383A (en
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大坪裕彦
井原荣治
大久保卓也
笠原真
饭塚诚
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Resonac Holdings Corp
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Showa Denko KK
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    • C09K3/14Anti-slip materials; Abrasives
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Abstract

The present invention relates to a method for producing cubic boron nitride abrasive grains used for producing a grinding wheel, etc., and to cubic boron nitride abrasive grains. The method comprises maintaining a mixture containing hexagonal boron nitride and seed crystals of cubic boron nitride under pressure and temperature conditions where cubic boron nitride remains thermodynamically stable, characterized in that the seed crystals contain cubic boron nitride twin crystals.

Description

The production method of cubic boron nitride abrasive grains
The application number that the application submits on May claimed calendar year 2001 31 is 60/294222 U.S. Provisional Application No..
Technical field
The present invention relates to a kind of production method and cubic boron nitride abrasive grains that is used to prepare the cubic boron nitride abrasive grains of emery wheel etc.
Background technology
Cubic boron nitride is second in hardness to diamond and its chemical stability is higher than diamond.Therefore, cubic boron nitride is used as the abrasive grain of producing abrasive substance, polishing material or cutting material day by day.
The various method that is used to prepare cubic boron nitride has been proposed.Wherein, a kind of method the most known and that be used to industrial circle widely is, for example remaining on hexagonal boron nitride, the such material of solvent (being also referred to as catalyzer) exists and can make cubic boron nitride keep Thermodynamically stable (about 4-6GPa, about 1400-1600 ℃) condition under, make hexagonal boron nitride directly change into cubic boron nitride (for example, Japanese patent gazette (bulletin) Nos.59-39362,3-14495,3-47132, and 3-15488 is disclosed).
The cubic boron nitride abrasive grains that obtains by any method in these methods all has above-mentioned high rigidity and chemical stability, and is used to electroplating abrasion wheel, melts combine emery wheel etc.
The cubic boron nitride abrasive grains that obtains by any aforesaid method nearly all is spheric (being block abrasive grain).Therefore, these abrasive grains are not suitable for the grinding that requirement has the vitrified bonded grinding wheel of low abrasive power.
Japanese Patent Application Publication (disclosing) No.9-169971 discloses the low abrasive power that uses the cubic boron nitride abrasive grains emery wheel in order to strengthen, " use has the cubic boron nitride abrasive grains of sharp shape and low defect level " causes " persistent low abrasive power ".Reached the improvement abrasive power although use the emery wheel of the cubic boron nitride abrasive grains that makes by aforesaid method to compare, at the industrial still emery wheel of the low abrasive power of demand always with the conventional emery wheel that uses block abrasive grain.
To be used for the wedding agent fusing of vitrified bonded grinding wheel lapped face,, and after by cooled and solidified, provide strong bonding strength so that when heating, make the space of intergranule bonding.In order to reach the good abrasive power of the porous wheel as vitrified bonded grinding wheel, must increase the porosity of emery wheel.
Yet so that porosity when increasing, the confining force of abrasive grain weakens when the amount that reduces wedding agent, because the load when grinding makes the quantity increase that abrasive grain comes off.Therefore, the surfaceness of processing materials worsens, and makes that the interval between the trimming operation is shortened, and can not reach satisfied grinding ratio.When reducing the per-cent of abrasive grain, the level of bridge construction reduces in the abrasive grain, thus, even the confining force of abrasive grain is enough, also can reduce the hardness of emery wheel.Therefore, the abrasive grain number that can not stand institute's load application when grinding increases, and the quantity that causes abrasive grain to come off increases and can not reach satisfied grinding ratio.
In order to address these problems, a kind of method has also been proposed, this method is to add a kind of loss with compensation abrasive grain or wedding agent.Yet when adding granule, the porosity of emery wheel reduces, and thus, has hindered the raising of low abrasive power.
Summary of the invention
In order to address the above problem, the inventor has carried out extensive studies, found that, in a kind of method that is used for preparing cubic boron nitride abrasive grains, in particularly a kind of ultra-high voltage method, can obtain having the cubic boron nitride abrasive grains (" abrasive grain " also can abbreviate " particle " as) of the shape that is suitable for preparing vitrified bonded grinding wheel as the seed crystal of cubic boron nitride by using the stratiform twin.According to this discovery, thereby finished the present invention.
Therefore, scheme provided by the invention is as follows:
(1) a kind of production method of cubic boron nitride abrasive grains, this method comprises a kind of mixture that contains hexagonal boron nitride and cubic boron nitride seed crystal is remained under the condition that can make cubic boron nitride maintenance heat mechanics pressure stable and temperature, it is characterized in that this seed crystal contains the cubic boron nitride twin.
(2) a kind of production method of cubic boron nitride abrasive materials is characterized in that, this method comprises the cubic boron nitride abrasive grains fragmentation that the production method by cubic boron nitride abrasive grains as described in (1) is made.
(3) production method of the cubic boron nitride abrasive grains described in (2), wherein, by roller crusher with the cubic boron nitride abrasive grains fragmentation.
(4) a kind of production method of cubic boron nitride abrasive grains, it is characterized in that, this method comprises by by removing L/T in the cubic boron nitride abrasive grains that each described method makes in (1)-(3) than being 1.5 or littler cubic boron nitride abrasive grains, and L represents the major diameter (μ m) of defined in cubic boron nitride abrasive grains three axle systems and T represents the thickness (μ m) of defined herein.
(5) a kind of cubic boron nitride abrasive grains, wherein, this abrasive grain is that the production method by each described cubic boron nitride abrasive grains in (1)-(4) makes.
(6) a kind of cubic boron nitride abrasive grains is characterized in that, described abrasive grain is by the tap density (unit: g/cm with cubic boron nitride 3) divided by its true density (3.48g/cm 3) packing ratio that calculates is in the following scope:
During the JIS B4130 abrasive grain level 40/50 of abrasive grain is 0.482-0.282;
During the JIS B4130 abrasive grain level 50/60 of abrasive grain is 0.480-0.280;
During the JIS B4130 abrasive grain level 60/80 of abrasive grain is 0.478-0.278;
During the JIS B4130 abrasive grain level 80/100 of abrasive grain is 0.474-0.274;
During the JIS B4130 abrasive grain level 100/120 of abrasive grain is 0.469-0.269;
During the JIS B4130 abrasive grain level 120/140 of abrasive grain is 0.464-0.264;
During the JIS B4130 abrasive grain level 140/170 of abrasive grain is 0.459-0.259;
During the JIS B4130 abrasive grain level 170/200 of abrasive grain is 0.453-0.253;
During the JIS B4130 abrasive grain level 200/230 of abrasive grain is 0.446-0.246;
During the JIS B4130 abrasive grain level 230/270 of abrasive grain is 0.440-0.240;
During the JIS B4130 abrasive grain level 270/325 of abrasive grain is 0.433-0.233; And
During the JIS B4130 abrasive grain level 325/400 of abrasive grain is 0.426-0.226.
(7) the cubes norbide abrasive grain described in (6), wherein said abrasive grain is made up of single crystal particle basically.
(8) a kind of emery wheel that makes by each described cubic boron nitride abrasive grains and wedding agent in (5)-(7).
(9) emery wheel described in (8), wherein said wedding agent is a ceramic bond.
(10) emery wheel described in (9), wherein said ceramic bond is incorporated in the emery wheel according to the amount that is in the 10-30 volume % scope.
(11) as each described emery wheel in (8)-(10), this emery wheel has and is in the abrasive grain per-cent of ((cubic boron nitride abrasive grains packing ratio-0.1) * 100) volume % to ((cubic boron nitride abrasive grains packing ratio+0.05) * 100%) (volume) scope;
(12) as each described emery wheel in (8)-(10), this emery wheel has and is in the abrasive grain per-cent of ((cubic boron nitride abrasive grains packing ratio-0.05) * 100) volume % to ((cubic boron nitride abrasive grains packing ratio+0.05) * 100%) (volume) scope;
(13) a kind of coated abrasives, this abrasive material makes by using tackiness agent that each described cubic boron nitride abrasive grains in (5)-(7) is fixed on cotton fabric or the textile-like.
Description of drawings
Fig. 1
(A) view of cubic boron nitride twin, arrow has been pointed out the direction of preferred growth.
(B) view of cubic boron nitride stratiform twin, arrow has been pointed out the direction of preferred growth.
The detailed description of better embodiment
Cubic boron nitride abrasive grains of the present invention is by the tap density (unit: g/cm with cubic boron nitride 3) divided by its true density (3.48g/m 3) packing ratio that calculates is in the following scope:
During the JIS B4130 abrasive grain level 40/50 of abrasive grain is 0.482-0.282;
During the JIS B4130 abrasive grain level 50/60 of abrasive grain is 0.480-0.280;
During the JIS B4130 abrasive grain level 60/80 of abrasive grain is 0.478-0.278;
During the JIS B4130 abrasive grain level 80/100 of abrasive grain is 0.474-0.274;
During the JIS B4130 abrasive grain level 100/120 of abrasive grain is 0.469-0.269;
During the JIS B4130 abrasive grain level 120/140 of abrasive grain is 0.464-0.264;
During the JIS B4130 abrasive grain level 140/170 of abrasive grain is 0.459-0.259;
During the JIS B4130 abrasive grain level 170/200 of abrasive grain is 0.453-0.253;
During the JIS B4130 abrasive grain level 200/230 of abrasive grain is 0.446-0.246;
During the JIS B4130 abrasive grain level 230/270 of abrasive grain is 0.440-0.240;
During the JIS B4130 abrasive grain level 270/325 of abrasive grain is 0.433-0.233; And
During the JIS B4130 abrasive grain level 325/400 of abrasive grain is 0.426-0.226.
The packing ratio of the conventional cubic boron nitride abrasive grains that uses is higher than the packing ratio of cubic boron nitride abrasive grains of the present invention.In order to improve the abrasive grain confining force in the emery wheel that uses conventional cubic boron nitride abrasive grains, must fully strengthen the level of bridge construction in the abrasive grain.This requirement causes reducing the per-cent of abrasive grain in the emery wheel inevitably when keeping grinding ratio.
Determine that the cubic boron nitride abrasive grains of the present invention by use has above-mentioned packing ratio even reduce the per-cent of abrasive grain, also can reach the bridge construction of enough levels in the abrasive grain.Even in reducing emery wheel during the per-cent of abrasive grain, the confining force of abrasive grain can not reduce yet in the emery wheel, thereby can prevent coming off of abrasive material therefore; And strengthen grinding ratio significantly.In addition, improve the porosity of emery wheel, can improve abrasive power significantly.
By the tap density of cubic boron nitride can be obtained the packing ratio of cubic boron nitride abrasive grains of the present invention divided by its true density.Tap density can be measured by " the manufactured abrasive tap density test method " of JIS-R6126 defined.
To specifically describe measuring method below.Clog the outlet of funnel with stopper, and the sample to be determined of weight 20.0 ± 0.1g is placed in the funnel.With a cylinder (capacity: 8.0 ± 0.1ml) be placed on hopper outlet under, and being adjusted to 95.0 ± 1.0mm by hopper outlet to the distance of fall at cylinder top.When removing unstopper, all sample falls into cylinder.Remove that part of sample outstanding with tinsel, the sample of retaining in the cylinder is carried out quality determination from the cylinder top.With the quality that records volume, obtain the tap density of sample thus divided by cylinder.
Be to measuring the brief description of tap density above.In order to measure tap density more accurately, before mensuration, must use dilute hydrochloric acid or chloroazotic acid washing abrasive grain, remove acid wherein then, and after drying, with avoid for example precipitating or material that stain is such to influence that abrasive grain was caused.
When abrasive grain was specific JIS-B4130 abrasive grain level, cubic boron nitride abrasive grains of the present invention had the packing ratio that is in the above-mentioned scope.The abrasive grain that belongs to different abrasive grain levels can be mixed.Can the cubic boron nitride abrasive grains of the present invention classification again of specific packing ratio will be had according to another kind of abrasive grain level or the another kind of standard different with JIS-B4130.
Synthetic method to the used abrasive grain that is made of cubic boron nitride of the present invention limits without any special.Yet, consider productivity, preferably cubic boron nitride is kept under the thermodynamically stable condition, when having solvent to exist, keep hexagonal boron nitride, make lonsdaleite boron change into cubic boron nitride thus.
But the commodity in use hexagonal boron nitride powder is as raw material.Yet, preferably use the hexagonal boron nitride of low oxygen content because come autoxidisable substance for example the oxygen impurities of boron oxide form often hinder hexagonal boron nitride and change into cubic boron nitride.Excessive particle diameter the granular size of hexagonal boron nitride without any special qualification, but generally is preferably 150 orders or littler by the particle diameter of JIS-R6001 regulation, because may reduce the reactive behavior of hexagonal boron nitride and vehicle substance.
To being used for hexagonal boron nitride is changed into solvent that the cubic boron nitride method uses without any special qualification, can use any known solvent.The example of suitable solvents comprises basic metal (for example Li); Its nitride (Li for example 3N), its nitrogen boride (Li for example 3BN 2); Alkaline-earth metal (for example Ca, Mg, Sr. and Ba), its nitride (Ca for example 3N 2, Mg 3N 2, Sr 3N 2And Ba 3N 2), its nitrogen boride (Ca for example 3B 2N 4, Mg 3B 2N 4, Sr 3B 2N 4And Ba 3B 2N 4) and the compound nitrogen boride (LiCaBN for example that contains basic metal and alkaline-earth metal 2And LiBaBN 2).Particle diameter to solvent is provided with any special qualification, but preferred particle diameter is 150 orders, because excessive particle diameter may reduce the reactive behavior of hexagonal boron nitride and vehicle substance.
The vehicle substance that preferably in the hexagonal boron nitride of 100 mass parts, adds the 5-50 mass parts.
In order to reach the coexistence of solvent and hexagonal boron nitride, vehicle substance powder and hexagonal boron nitride powder are mixed.Randomly, can with the hexagonal boron nitride layer and vehicle substance is alternately laminated be placed in the reactor.
Specifically, in a preferred version, with hexagonal boron nitride and vehicle substance, or the about 1-2t/cm of its mixture 2The press working moulding, and the briquet that obtains packed in the reactor.By utilizing this method, improve the operability of raw material powder and reduced the raw material contraction that in reactor, produces, improved the productivity of cubic boron nitride abrasive grains thus.
In another preferred version of the present invention, in advance the cubic boron nitride seed crystal is added contain the above-mentioned briquet of solvent and hexagonal boron nitride or contain solvent and the stack product of hexagonal boron nitride in, promoted to become the process of cubic boron nitride thus by seeded growth as nucleus.In this occasion, seed crystal useable solvents material applies.
Containing catalyst substance, hexagonal boron nitride, and the above-mentioned briquet of another kind of material or similar material are packed in the reactor, and this reactor is placed in the known high temp/high pressure producer, at this place briquet remained on cubic boron nitride is kept under the condition of thermodynamically stable temperature/pressure.O.Fukunaga is at Diamond Relat.Mater, and 9, (2000) disclose thermodynamically stable condition among the 7-12, and this condition is usually in the about 1600 ℃ scope of the about 6GPa of about 4-and about 1400-.Briquet kept about 1 second-Yue 6 hours at this place usually.
By briquet is kept, can make hexagonal boron nitride change into cubic boron nitride in that cubic boron nitride is kept under the thermodynamically stable above-mentioned condition.Usually, produce and contain hexagonal boron nitride, cubic boron nitride, and the synthetic ingot bar of solvent.With the synthetic ingot bar fragmentation of such output to separate and the purification cubic boron nitride.
Can use disclosed separation and method of purification among Japanese patent gazette (bulletin) No.49-27757.In one approach, the synthetic ingot bar of output is broken into is of a size of 5mm or littler particle, and sodium hydroxide and less water are added in the particle.About 300 ℃ with this mixture heating up, optionally dissolve hexagonal boron nitride thus.With the mixture cooling, also pass through filtering separation with acid and water washing insolubles successively, obtain cubic boron nitride abrasive grains thus.
In the boron nitride abrasive grains that obtains like this, be applicable to that those abrasive grains of the present invention are basically by the monocrystal abrasive granulometric composition.Although this cubic boron nitride abrasive grains except that its monocrystalline, also contains just like polycrystalline particle and the such cubic boron nitride abrasive grains of microcrystal grain, the preferred monocrystalline that uses among the present invention.Thereby polycrystalline or micro-crystal cubic boron nitride abrasive grain have the anti-finishing of higher crystal grain intensity.When using this abrasive grain in the emery wheel, the cut edge of abrasive grain is tending towards taking place abrasion and wearing and tearing.Thereby polycrystalline or crystallite abrasive grain are not suitable as cubic boron nitride abrasive grains of the present invention.
In the present invention, the cubic boron nitride abrasive grains of being made up of single crystal particle basically is defined as contains 90 volume % or higher, be preferably 95 volume % or higher, be more preferred from 99 volume % or higher above-mentioned monocrystal abrasive particulate cubic boron nitride abrasive grains.More than Gui Ding per-cent only is provided with according to cubic boron nitride and considers other impurity.
The cubic boron nitride abrasive grains classification that will obtain by aforesaid method according to the abrasive material grade of defined among the JIS-B4130.By use the shape selector or similarly device with blocky abrasive grain by separating in each grade, obtain having the cubic boron nitride abrasive grains of packing ratio within the scope of the present invention thus.
Term " block abrasive material " is meant normally spheric crystal grain, more precisely, has L/T than those crystal grain that are about 1, and wherein L represents the major diameter (μ m) of defined in three axle systems of crystal grain, and T represents the thickness (μ m) of defined.Funtai Kogaku Binran (the 1st edition, the 1st printing (1986), by The Society of Powder Technology, Japan, publish) page 1 the above, by converting corresponding cuboid to, can utilize three axle systems described herein to carry out quantitatively to having erose grain shape with irregularly shaped.
In brief, provide two parallel lines, it is clipped under quiescent conditions, place the particle projection figure that selects on the plane in office.When these two line contact projection figure, measure the distance between two lines.The longest distance is as the major diameter L (μ m) of crystal grain, perpendicular to along the direction of longest distance line and the distance between the two other line that contacts with sciagraph as the minor axis B (μ m) of crystal grain.By the height at the plane of under quiescent conditions, placing crystal grain thereon to crystal grain top as thickness T (μ m).In the present invention, the thickness of three axle systems (μ m) is the smaller value that is selected from minor axis B (μ m) and the thickness T (μ m).
According to the present invention, by shape selector or allied equipment by reduction have L/T than be 1.5 or the per-cent of littler abrasive grain can obtain having the cubic boron nitride abrasive grains that is in packing ratio in the scope of the invention.Words and phrases in preparation method of the present invention " remove have L/T than be 1.5 or littler cubic boron nitride abrasive grains " be meant " and reduction have L/T than be 1.5 or littler cubic boron nitride abrasive grains per-cent " step.
As the shape selector, as long as this device can achieve the above object, any device all can use.Particularly, can use by vibration and remove and have the method for low L/T than abrasive grain.
The structure of a particular instance of used shape selector in the aforesaid method will be described now.An oscillating plate is equilateral triangle (drift angle A, B and C) state, is provided with the limit wall that prevents that abrasive grain from falling everywhere at AB and AC limit.Oscillating plate forms skewed so that drift angle B upwards is provided with respect to the AC limit as tilting axis.Pitch angle with respect to the horizontal plane is preferably 1-45 °.This oscillating plate is inclined in addition and makes drift angle A tilt to drift angle C.Preferably pitch angle with respect to the horizontal plane, AC limit is 1-30 °.
When vibration plate vibrates, abrasive grain is fed to drift angle A and by BC limit discharge.The abrasive grain that infeeds drops to the BC limit by vibration by drift angle A.In the process of this step, have the block abrasive grain of spheric usually and be tending towards dropping to than lower part and along the AC limit and move.On the contrary, erose abrasive grain (being non-block abrasive grain) by vibration rise to higher part and by on the BC limit near the part discharge of drift angle B.By utilizing the outlet on the BC limit to separate, can obtain by the abrasive grain of wherein having removed block (normally spherical) abrasive grain.
" particle size of diamond and cubic boron nitride " (JIS-B4130) among the abrasive grain level of defined, those grades related to the present invention are summarised in the table 1.By using motor-vibro screen to obtain size distribution in the table 1.
In order to improve the productive rate with cubic boron nitride abrasive grains of packing ratio in the scope of the invention, the step that preferably is used to prepare cubic boron nitride abrasive grains comprises a step with the cubic boron nitride abrasive grains fragmentation.The special breaking method that preferably destroys cubic boron nitride abrasive materials by compressive load.Be more preferably by roller crusher and carry out fragmentation.
In the breaking method by the formula of rolling crusher, abrasive grain is extruded between two rollers and is broken.This method is based on carrying out fragmentation by abrasive grain being applied compression and shear-stress, and these abrasive grains can be applied in the short time cycle powerful measure fragmentation.Thereby abrasive grain can not improve the productive rate with cubic boron nitride abrasive grains of packing ratio in the scope of the invention by overcrushing to surpassing required degree and can not forming circular block abrasive grain usually usually thus.
The another kind of method that is used to prepare the cubic boron nitride abrasive grains of the packing ratio with scope of the invention will be described now.In the method, under the Pressure/Temperature condition of superelevation, keep hexagonal boron nitride when having solvent to exist, make hexagonal boron nitride change into cubic boron nitride thus, can directly obtain having the abrasive grain of packing ratio in the scope of the invention.More particularly, in preparing the method for cubic boron nitride abrasive grains, this method comprises that the mixture that will contain hexagonal boron nitride and cubic boron nitride seed crystal remains on can be made under cubic boron nitride maintenance heat mechanics pressure stable/temperature condition, use twin and stratiform twin seed crystal, the cubic boron nitride abrasive grains that can obtain having packing ratio in the scope of the invention thus as cubic boron nitride.
Term " twin " is meant to have the crystal of symmetric two parts mutually.Fig. 1 shows a kind of synoptic diagram of crystalline structure of specific twin.By using twin can obtain having the reasons are as follows of cubic boron nitride abrasive grains of packing ratio in the scope of the invention as seed crystal.At the dished portion of twin, uniaxially promptly by specific crystalline orientation, produces nucleus.Therefore, compare, in these direction generation crystal growths, and increased the anisotropic growth of crystal grain with significantly different speed with other crystalline orientations.Thereby erose abrasive grain is tending towards growth, causes being easy to produce the cubic boron nitride abrasive grains with packing ratio in the scope of the invention.
For example, in the twin shown in Fig. 1 (A), carrying out crystal growth by three orientation preferentiallies shown in the arrow.When using the stratiform twin that has two or more twinpistons shown in Fig. 1 (B) during as seed crystal, the number of planes with dished portion increases.Thereby, compare with the occasion of using seed crystal shown in Fig. 1 (A), being easier to grow has the cubic boron nitride abrasive grains of packing ratio in the scope of the invention.
When using cubic boron nitride abrasive grains of the present invention to prepare emery wheel, can reach high grinding ratio and low abrasive power.Particularly, in the occasion significantly generation effect of porous ceramics in conjunction with emery wheel.
The abrasive grain per-cent of vitrified bonded grinding wheel preferably at ((packing ratio of cubic boron nitride abrasive grains-0.1) * 100) volume % to the scope of ((packing ratio of cubic boron nitride abrasive grains+0.05) * 100) volume %, particularly preferably in ((packing ratio of cubic boron nitride abrasive grains-0.05) * 100) volume % to the scope of ((packing ratio of cubic boron nitride abrasive grains+0.05) * 100) volume %.When the per-cent of abrasive grain during less than ((packing ratio of cubic boron nitride abrasive grains-0.1) * 100) volume %, can not reach bridge construction enough in the abrasive grain and enough abrasive grain confining forces, cause grinding ratio to reduce thus, and when abrasive grain per-cent surpasses ((packing ratio of cubic boron nitride abrasive grains+0.05) * 100) volume %, can reach bridge construction enough in the abrasive grain, but because the pressure of abrasive grain filling when forming emery wheel, abrasive grain edges broken or abrasive grain itself destroyed, cause that these abrasive grains cracked or damage come off and grinding ratio is reduced when grinding.
The per-cent of abrasive grain is meant with the emery wheel volume to be the percent by volume of the abrasive grain of basic calculation.
In order to prepare vitrified bonded grinding wheel,, can use any wedding agent that is generally used in conjunction with cubic boron nitride abrasive grains according to application target.The example of this wedding agent comprises and contains SiO 2-Al 2O 3It is main wedding agent.The amount of mixing wedding agent in emery wheel is preferably in the scope of 10-30 volume %.When it measured less than 10 volume %, the confining force of abrasive grain reduces also made the abrasive grain that comes off increase, and causes being unsuitable for the low grinding ratio of abrasive tool.When its amount surpassed 30 volume %, the porosity of emery wheel reduced, and causes the deterioration of abrasion wheel grinding power, and was tending towards taking place volume increase (foaming) when the heating of preparation emery wheel, and these effects are disadvantageous.
Also can use the additive (for example agglomerate and adhesion promotor) or the similar substance that when preparing emery wheel, use usually with cubic boron nitride abrasive grains.
Cubic boron nitride abrasive grains of the present invention is suitable in the emery wheel of preparations such as other types wedding agent, coated abrasives and uses in above-mentioned vitrified bonded grinding wheel.Term " coated abrasives " is meant that a class contains the abrasive substance that is fixed on the abrasive grain on the fabric by tackiness agent.Particularly, for example gelatin, gelatin or synthetic resins are fixed on the grinding fabric that cotton fabric or textile-like are made above with abrasive grain by using tackiness agent.
Embodiment
To the present invention be described by embodiment below, but can not think that these embodiment are limitation of the invention.
(embodiment 1)
Will be as the LiCaBN of cBN synthetic 2(15 mass parts) and contain as shown in Figure 1, (median size: cubic boron nitride abrasive grains 30 μ) (0.5 mass parts) adds hBN (UHP-1, the product of Showa Denko k.k. as a large amount of twins of seed crystal; Median size: 8-10 μ; Purity: 98%) in (100 mass parts), obtain a kind of mixture thus.Is 1.92g/cm with this mixture in mold pressing density 2Condition under mold pressing, obtain a briquet thus.With this briquet reactor of packing into, and this reactor is placed in the high temp/high pressure producer, under 5GPa and 1500 ℃, carries out 15 minutes synthetic therein.Behind end of synthesis, be broken into the 5mm or the particle of small particle size more by the synthetic briquet that take out to generate in the reactor and with it, and sodium hydroxide and less water are added in these particles.About 300 ℃ with mixture heating up, optionally dissolve hexagonal boron nitride thus.With mixture cooling, successively with sour and water washing insolubles and by filtering separation to carry out purifying, obtain the yellow transparent cubic boron nitride abrasive grains thus.
It is 99% or higher that the cubic boron nitride abrasive grains that obtains like this contains the single crystal particle amount.
(embodiment 2)
Repeat the step among the embodiment 1, different is not add any cubic boron nitride seed crystal, obtains a kind of mixture thus, and the synthesizing cubic boron nitride abrasive grain separates and these abrasive grains of purifying.
The amount that the cubic boron nitride abrasive grains that obtains like this contains single crystal particle is 99% or higher.
(embodiment 3)
Resulting cubic boron nitride abrasive grains among the embodiment 1 is classified into the abrasive grain level of defined among the JIS-B4130.Wash the abrasive grain that belongs to 100/200 abrasive material degree level with dilute hydrochloric acid, remove acid wherein then, and be dried.Measure the tap density of dry abrasive grain, measure its packing ratio in view of the above.
Measure tap density with the following method.Clog the outlet of funnel with stopper, the cubic boron nitride abrasive grains that 20.0 ± 0.1g is to be measured is placed in the funnel.With a cylinder (volume: 8.0 ± 0.1ml) be placed on hopper outlet under, and being adjusted to 95.0 ± 1.0mm by hopper outlet to the dropping distance at cylinder top.When removing stopper, cause whole cubic boron nitride abrasive grains to fall into cylinder.Remove that part of cubic boron nitride abrasive grains outstanding with tinsel, the cubic boron nitride abrasive grains of retaining in the cylinder is carried out quality determination from the cylinder top.The quality that records divided by the cylinder volume, is therefore obtained tap density.
The abrasive grain packing ratio that belongs to 100/120 abrasive grain level is shown in Table 2.
(embodiment 4)
The cubic boron nitride abrasive grains that obtains among the embodiment 2 is classified into the abrasive grain level of stipulating among the JIS-B4130.Be subordinated to by above-mentioned shape selector in the abrasive grain of 100/120 abrasive grain level and remove block abrasive grain.
Use a kind of shape selector of using each edge lengths for the equilateral triangle oscillating plate of about 1m.Make this oscillating plate (drift angle A, B and C) form 13 ° inclination, make drift angle B upwards be provided with respect to AC limit as tilting axis.This oscillating plate further is tilted 7 °, makes drift angle A tilt to drift angle C.
By using the shape selector, reduced and containedly in the cubic boron nitride abrasive grains had L/T than being 1.5 or littler abrasive grain per-cent.Subsequently, with the cubic boron nitride abrasive grains that the dilute hydrochloric acid washing was handled like this, remove acid wherein then, and be dried.Measure the tap density of dry abrasive grain with the method among the embodiment 3 of being similar to, measure its packing ratio in view of the above.
The abrasive grain packing ratio of 100/120 abrasive grain level is shown in Table 2.
(embodiment 5)
By roller crusher with resulting cubic boron nitride abrasive grains fragmentation among the embodiment 2.
Use a kind of roller crusher (Yoshida Seisaku-shi product).Each used roller diameter is 140mm in roller crusher, and length is 140mm and is made by high carbon steel.Pair roller applies the load of 50kgf (490N), with 20g/ minute speed cubic boron nitride abrasive grains is infeeded in two rollers by the 100rpm rotation, thus with the abrasive grain fragmentation simultaneously.
The cubic boron nitride abrasive grains of such fragmentation is classified into the abrasive grain level of defined among the JIS-B4130.Wash the abrasive grain of 100/120 abrasive grain level with dilute hydrochloric acid, remove then wherein acid and be dried.According to embodiment 3 in similarly method measure the tap density of dry abrasive grain, measure its packing ratio in view of the above.
The abrasive grain packing ratio of 100/120 abrasive grain level is shown in Table 2.
(embodiment 6)
Under condition similar to Example 5 with resulting cubic boron nitride abrasive materials fragmentation among the embodiment 2.
The cubic boron nitride abrasive grains of such fragmentation is classified into the abrasive grain level of stipulating among the JIS-B4130.According to method similar to Example 4, reducing in the 100/120 abrasive grain level the contained L/T of having by the shape selector is 1.5 or littler abrasive grain per-cent, and with the abrasive grain that dilute hydrochloric acid washing was handled like this, remove acid wherein then and be dried.According to method similar to Example 3, measure the tap density of dry abrasive grain, measure its packing ratio in view of the above.
The abrasive grain packing ratio that belongs to 100/120 abrasive grain level is shown in Table 2.
(Comparative Examples 1)
Resulting cubic boron nitride abrasive grains among the embodiment 2 is classified into the abrasive grain level of stipulating among the JIS-B4130.Belong to the abrasive grain of 100/120 abrasive grain level with dilute hydrochloric acid washing, remove acid wherein then and be dried.According to method similar to Example 3, measure the tap density of dry abrasive grain, measure basic packing ratio in view of the above.
The abrasive grain packing ratio of 100/120 abrasive grain level is shown in table 2.
(embodiment 7 and 8 and Comparative Examples 2-6)
Prepare various grinding wheels by resulting those abrasive grains in resulting among the use embodiment 3 or the Comparative Examples 1.Specifically, preparation a kind ofly contain abrasive grain, as the borosilicate glass wedding agent of tackiness agent and the mixture of a kind of tackiness agent (resol); At 150 ℃ with this mixture press molding; The briquet that sintering is obtained under 1000 ℃ (in atmosphere).When sintering prepared grinding wheel, used tackiness agent was burnt, thereby formed hole.Used abrasive grain type, its ratio, the porosity of sintered product abrasive grain and the bond strength of per-cent and various grinding wheels is shown in Table 3 when forming various grinding wheel.
(embodiment 9 and 10 and Comparative Examples 7-11)
With embodiment 7 and 8 and Comparative Examples 2-6 in the various grinding wheels that make combine with aluminum alloy wheel, form emery wheel thus, emery wheel is stood grinding test under the following conditions.The results are shown in the table 4.
Emery wheel: 1A1 type, 150D * 10U * 3X * 76.2H
Shredder: transverse axis surface grinding machine (grinding wheel spindle motor: 3.7kw)
Work material: SKH-51 (HRc=62-64)
The surface-area of work material: 200mm * 100mm
Ginding process: wet type surface transverse grinding
Grinding condition:
Circumference of emery wheel speed: 1800m/min
Table top speed: 15m/min
Traverse rod feeding rate: 5mm/pass
Grinding depth: 25 μ m
Lapping liquid: FIS W2, only to cBN (diluting 50 times)
Table 1
First sieve Second sieve The 3rd sieve The 4th sieve
A B C D E
μm μm μm μm
40/50 600 * 455 8 302 90 8 213
50/60 455 322 8 255 90 8 181
60/80 384 271 8 181 90 8 127
80/100 271 197 10 151 87 10 107
100/120 227 165 10 127 87 10 90
120/140 197 139 10 107 87 10 75
140/170 165 116 11 90 85 11 65
170/200 139 97 11 75 85 11 57
200/230 116 85 11 65 85 11 49
230/270 97 75 11 57 85 11 41
270/325 85 65 15 49 80 15 -
325/400 75 57 15 41 80 15 -
The sieve that the A:99.97% particle must pass through
B: predetermined amount or more particles retention sieve in the above can not be arranged, and this predetermined amount
C: predetermined amount particle retention sieve in the above must be arranged, and this predetermined amount
D: can be by the particulate maximum of this sieve
E: have at least 2% particle intransitablely to sieve
*: do not use motor-vibro screen
Table 2
Used cubic boron nitride abrasive grains The abrasive grain packing ratio of 100/120 abrasive grain level
Embodiment 3 Embodiment 1 0.43
Embodiment 4 Embodiment 2 0.45
Embodiment 5 Embodiment 2 0.48
Embodiment 6 Embodiment 2 0.44
Comparative Examples 1 Embodiment 2 0.53
Table 3
Used cubic boron nitride abrasive grains Abrasive grain-wedding agent-tackiness agent ratio (volume %) Emery wheel (behind the sintering) Bending strength (kg/mm 2)
Porosity (volume %) Crystal particle volume per-cent (volume %)
Embodiment 7 Embodiment 3 45-20-10 35 45 5.53
Embodiment 8 Embodiment 3 35-20-10 45 35 5.38
Comparative Examples 2 Embodiment 3 50-20-10 30 50 4.92
Comparative Examples 3 Embodiment 3 30-20-10 50 30 2.61
Comparative Examples 4 Comparative Examples 1 50-8-10 42 50 3.84
Comparative Examples 5 Comparative Examples 1 50-20-10 30 50 5.31
Comparative Examples 6 Comparative Examples 1 40-20-10 40 40 4.07
Table 4
Used emery wheel Grinding ratio Research power (W)
Embodiment 9 Embodiment 7 1,683 920
Embodiment 10 Embodiment 8 1,622 940
Comparative Examples 7 Comparative Examples 2 1,229 1,190
Comparative Examples 8 Comparative Examples 3 627 970
Comparative Examples 9 Comparative Examples 4 878 1,260
Comparative Examples 10 Comparative Examples 5 1,582 1,780
Comparative Examples 11 Comparative Examples 6 1,060 1,430
Industrial applicibility
Cubic boron nitride abrasive grains of the present invention has the packing ratio lower than conventional cubic boron nitride abrasive grains. Thereby, although abrasive grain percentage reduces, can in abrasive grain, keep high-caliber bridge construction. So even the emery wheel of use cubic boron nitride abrasive grains of the present invention when porosity improves, also can reach high rigidity, high-flexural strength and high abrasive grain confining force. In addition, the cubic boron nitride abrasive grains of the application of the invention can make the emery wheel with good abrasive power, and does not reduce the grinding ratio of emery wheel.
Particularly, cubic boron nitride abrasive grains of the present invention is applicable to vitrified bonded grinding wheel. Use the vitrified bonded grinding wheel of hexagonal boron nitride abrasive grain of the present invention can play the effect of porous wheel and can bring into play good nonferromagnetic substance.

Claims (12)

1. cubic boron nitride abrasive grains, wherein, the packing ratio that described abrasive grain calculates divided by its true density by the tap density with cubic boron nitride is in the following scope:
During the JIS B4130 abrasive grain level 40/50 of abrasive grain is 0.482-0.282;
During the JIS B4130 abrasive grain level 50/60 of abrasive grain is 0.480-0.280;
During the JIS B4130 abrasive grain level 60/80 of abrasive grain is 0.478-0.278;
During the JIS B4130 abrasive grain level 80/100 of abrasive grain is 0.474-0.274;
During the JIS B4130 abrasive grain level 100/120 of abrasive grain is 0.469-0.269;
During the JIS B4130 abrasive grain level 120/140 of abrasive grain is 0.464-0.264;
During the JIS B4130 abrasive grain level 140/170 of abrasive grain is 0.459-0.259;
During the JIS B4130 abrasive grain level 170/200 of abrasive grain is 0.453-0.253;
During the JIS B4130 abrasive grain level 200/230 of abrasive grain is 0.446-0.246;
During the JIS B4130 abrasive grain level 230/270 of abrasive grain is 0.440-0.240;
During the JIS B4130 abrasive grain level 270/325 of abrasive grain is 0.433-0.233; And
During the JIS B4130 abrasive grain level 325/400 of abrasive grain is 0.426-0.226.
2. cubic boron nitride abrasive grains as claimed in claim 1, wherein said abrasive grain is made up of single crystal particle basically.
3. the production method of a cubic boron nitride abrasive grain as claimed in claim 1, this method comprises the steps:
A kind of mixture that contains hexagonal boron nitride and cubic boron nitride seed crystal is remained under the condition that can make cubic boron nitride maintenance heat mechanics pressure stable and temperature; Described seed crystal contains the cubic boron nitride twin.
4. the production method of cubic boron nitride abrasive grains as claimed in claim 3, wherein, this method also comprises a step with said cubic boron nitride abrasive grains fragmentation.
5. the production method of cubic boron nitride abrasive grains as claimed in claim 4, wherein, by roller crusher with the cubic boron nitride abrasive grains fragmentation.
6. as the production method of each described cubic boron nitride abrasive grains among the claim 3-5, this method comprises that also one is used for removing L/T than being 1.5 or the step of littler cubic boron nitride abrasive grains from cubic boron nitride abrasive grains,
L herein represents the major diameter (μ m) of defined in cubic boron nitride abrasive grains three axle systems, and T represents the thickness (μ m) of defined.
7. emery wheel that makes by claim 1 or 2 described cubic boron nitride abrasive grains and wedding agent.
8. emery wheel as claimed in claim 7, wherein said wedding agent is a ceramic bond.
9. emery wheel as claimed in claim 8, wherein said ceramic bond is incorporated in the emery wheel according to the amount that is in the 10-30 volume % scope.
10. as each described emery wheel among the claim 7-9, wherein said emery wheel has and is in the abrasive grain per-cent of ((packing ratio of cubic boron nitride abrasive grains-0.1) * 100 volumes) % to ((packing ratio of cubic boron nitride abrasive grains+0.05) * 100) volume % scope.
11. as each described emery wheel among the claim 7-9, wherein said emery wheel has and is in the abrasive grain per-cent of ((packing ratio of cubic boron nitride abrasive grains-0.05) * 100) volume % to ((packing ratio of cubic boron nitride abrasive grains+0.05) * 100) volume % scope.
12. a coated abrasives, described abrasive material makes by using tackiness agent that claim 1 or 2 described cubic boron nitride abrasive grains are fixed on the fabric.
CNB02810207XA 2001-05-21 2002-05-21 Method for producing cubic boron nitride abrasive grains Expired - Lifetime CN1317230C (en)

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JPH09169971A (en) * 1995-12-18 1997-06-30 Showa Denko Kk Cubic boron nitride abrasive grain and its production
CN1269273A (en) * 1999-04-07 2000-10-11 桑德维克公司 Materials based on porous cubic crystal series boron nitride for post production of cutting tools and preparation method thereof

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CN1269273A (en) * 1999-04-07 2000-10-11 桑德维克公司 Materials based on porous cubic crystal series boron nitride for post production of cutting tools and preparation method thereof

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