CN104667826A - Manufacturing method for cubic boron nitride crystals - Google Patents
Manufacturing method for cubic boron nitride crystals Download PDFInfo
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- CN104667826A CN104667826A CN201510049012.8A CN201510049012A CN104667826A CN 104667826 A CN104667826 A CN 104667826A CN 201510049012 A CN201510049012 A CN 201510049012A CN 104667826 A CN104667826 A CN 104667826A
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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Abstract
The invention provides a manufacturing method for cubic boron nitride crystals. The manufacturing method comprises the following steps: uniformly mixing hexagonal boron nitride powder, catalytic agent powder and an additive, and pressing a synthesized stick, wherein the catalytic agent powder comprises lithium nitride and lithium hydride, and the additive comprises calcium boride, boron carbide and titanium nitride; performing high-pressure and high-temperature synthesis on the synthesized stick to obtain coarse cubic boron nitride crystals; breaking the coarse cubic boron nitride crystals to obtain coarse cubic boron nitride crystal blocks; immersing the coarse cubic boron nitride crystal blocks by water, acid and alkali to obtain blocked semi-finished cubic boron nitride crystals. The black blocked cubic boron nitride crystals are provided with high-intensity abrasive materials with specific crystal surfaces; the granularity peak value is more intensive, the static pressure strength Ti is 65-70, and the thermal impact toughness TTi is 60-65; the manufacturing method can be applied to processing of specific high-speed steel, surface hardening steel, hard alloy, alloy steel, nickel-base and cobalt-base high-temperature alloy materials.
Description
Technical field
The present invention relates to a kind of manufacture method of superhard material, particularly relate to a kind of manufacture method of cubic boron nitride crystal.
Background technology
Cubic boron nitride, molecular formula is BN, is first developed in nineteen fifty-seven by the R.H. Wen Tuofu of the U.S., its crystal structure class dimantine.Cubic boron nitride is synthesized at high temperature under high pressure by hexagonal boron nitride and catalyst usually.Cubic boron nitride has very high hardness, heat endurance and chemical inertness, and the excellent properties such as good saturating infrared shape and wider energy gap, the hardness of cubic boron nitride crystal is only second to diamond, but heat endurance is far above diamond, to Ferrious material, unit have larger chemical stability, is commonly used for abrasive material and cutter material.The grinding performance of CBN is very excellent, can not only be competent at the processing of difficult grind material, boost productivity, and effectively can also improve the grinding quality of workpiece.The use of cubic boron nitride crystal is contributed greatly one of intermetallic composite coating, causes grinding generation revolutionary variation, is the second leap of grinding technique.Cubic boron nitride is applied widely as the manufacture field acquisition of super hard abrasive in different industries, becomes now the indispensable important materials such as automobile, space flight and aviation, mechano-electronic, microelectronics especially, thus obtains the very big attention of each industrially developed country.
But, existing conventional cubic boron nitride crystal as its intensity of abrasive material and anti-wear performance limited, be not suitable for processing plating tool and vitrified bonding system, the service life of plating tool and vitrified bonding system can be made shorter.
Summary of the invention
By Given this, the necessary manufacture method providing a kind of cubic boron nitride crystal of bulk, to overcome the problems referred to above.
A manufacture method for cubic boron nitride crystal, it comprises the following steps:
Step one, according to mass percent, by the hexagonal boron nitride powder of 75% ~ 85%, 2.5% ~ 5% lithium nitride, 4% ~ 6% lithium hydride, the calcium boride of 2% ~ 4%, the boron carbide of 3.5% ~ 5.5% and 3% ~ 4.5% titanium nitride Homogeneous phase mixing, and be pressed into synthetic rod;
Step 2, under 1500 ~ 1650 degree, synthesis pressure 90 ~ 97 MPa is applied to described synthetic rod and carries out high pressure-temperature synthesis, obtain the cubic boron nitride crystal crude product of black;
Step 3, broken described cubic boron nitride crystal crude product, obtain block cubic boron nitride crystal crude product; Adopt block cubic boron nitride crystal crude product described in water soaking, soda acid process successively, obtain block cubic boron nitride crystal semi-finished product;
Step 4, type selecting process is carried out to described block cubic boron nitride crystal semi-finished product, obtain block cubic boron nitride crystal finished product.
Based on above-mentioned manufacture method, described step one comprises: according to mass percent, by the hexagonal boron nitride powder of 75% ~ 85%, 2.5% ~ 5% lithium nitride, 4% ~ 6% lithium hydride, the calcium boride of 2% ~ 4%, the boron carbide of 3.5% ~ 5.5% and 3% ~ 4.5% titanium nitride be placed in airtight three-dimensional material mixer, Homogeneous phase mixing obtains mixed material in 0.5 ~ 1 hour; Adopt four column press and described mixed material is pressed into predetermined shape by the pressure applying 10 ~ 15 MPas, and load in graphite-pipe and make described synthetic rod.Wherein, the hexagonal boron nitride powder in above-mentioned mixed material is main synthesis material, and lithium nitride and lithium hydride are jointly as catalyst powder, and boron carbide, titanium nitride and calcium boride are jointly as additive.
Particularly, described mixed material is placed on described four column press, and applies 10 ~ 15 MPa and repeatedly make power, increase the density of mixed material, make it easily shaping, and be pressed into cylinder according to pre-provisioning request and load in graphite heating pipe and make described synthetic rod.Wherein, the shape of described synthetic rod is not limited to cylindric, and it can be determined according to needs, and e.g., it can be prism-shaped.
Based on above-mentioned manufacture method, comprise taking a step forward of described step one: in vacuum drying oven, adopt nitrogen to carry out purified treatment hexagonal boron nitride powder raw material.
Based on above-mentioned manufacture method, described step step 2 comprises: loaded in high pressure chest by described synthetic rod, and be forced into 30 ~ 45 MPas; In 2 ~ 4 minutes, the temperature in described high pressure chest is risen to 1500 ~ 1650 degree; Continue boosting and the pressure in described high pressure chest is risen to synthesis pressure 90 ~ 97 MPa; Constant temperature and pressure is lowered the temperature after 25 ~ 35 minutes release, obtains the described cubic boron nitride crystal crude product of black.
Wherein, the pressure in described high pressure chest rose to synthesis pressure 90 ~ 97 MPa at 2 ~ 4 minutes, was the nucleation quantity for controlling cubic boron nitride crystal, and made the material in high pressure chest enter in the excellent crystalline region of high pressure, to obtain the perfect cubic boron nitride crystal of crystalline form; In this step 2, constant temperature and pressure 25 ~ 35 minutes is to make the cubic boron nitride crystal in described high pressure chest fully grow at high temperature under high pressure.Wherein, " constant temperature and pressure " in this step refers to and maintains pressure when pressure in described high pressure chest reaches described synthesis pressure 90 ~ 97 MPa and temperature, the cubic boron nitride nucleus synthesized to make above-mentioned synthetic rod fully grows, and obtains the cubic boron nitride crystal meeting demand.
Based on above-mentioned manufacture method, described step 3 comprises: cubic boron nitride crystal crude product described in fragmentation, ball milling successively, obtains block cubic boron nitride crystal crude product; Adopt block cubic boron nitride crystal crude product described in water soaking, obtain block elementary cubic boron nitride crystal crude product; According to the mixed acid that the volume ratio modulation concentration of 3 ︰ 1 is the sulfuric acid of 95% ~ 98% and the nitric acid of concentration 63% ~ 65%, elementary for described bulk cubic boron nitride crystal crude product is placed in described mixed acid, be heated to 150 ~ 180 degree and boil 4 ~ 6 hours, obtaining block intermediate cubic boron nitride crystal crude product; Intermediate for described bulk cubic boron nitride crystal crude product is placed in the industry alkali alive that concentration is 95% ~ 98%, is heated to 250 ~ 350 degree and boils 4 ~ 5 hours, obtaining block senior cubic boron nitride crystal crude product; Rinse successively, dry the senior cubic boron nitride crystal crude product of described bulk, obtain the described block cubic boron nitride crystal semi-finished product of black.
Wherein, in this step 3, being soaked in water is to remove unconverted hexagonal boron nitride powder; Soaking with described mixed acid is to remove the impurity such as metal dust, graphite produced in mechanical milling process; Soaking with industry alkali alive is to remove the impurity such as remaining pyrophillite, graphite.
Based on above-mentioned manufacture method, described step step 3 comprises further: carry out grading, type selecting, stereomicroscope check processing successively to described block cubic boron nitride crystal semi-finished product, obtains varigrained described block cubic boron nitride crystal semi-finished product.Wherein, the granularity of the block cubic boron nitride crystal finished product of described black is 20 order ~ 60 orders, and as 20 orders, 30 orders, 40 orders, 50 orders, 60 orders, preferably, the granularity of the block cubic boron nitride crystal finished product of described black is 30 order ~ 50 orders.
Following mixed material is synthesizing cubic boron nitride crystal under 1500 ~ 1650 degree and 90 ~ 97 MPas.Under the condition that synthesis temperature is identical with synthesis pressure, along with the component of mixed material and the difference of ratio thereof, the cubic boron nitride crystal obtained is also different.Particularly, when mixed material be 75% ~ 85% hexagonal boron nitride powder and as catalyzer contact agent 2.5% ~ 5% lithium nitride and 4% ~ 6% lithium hydride time, synthesizing the cubic boron nitride crystal obtained is black, crystalline form is in the majority with class sphere, granular size is uneven, and has a small amount of translucent yellow crystals to exist; When mixed material be 75% ~ 85% hexagonal boron nitride powder, the lithium nitride of 2.5% ~ 5%, the lithium hydride of 4% ~ 6% and as additive 2% ~ 4% calcium boride time, the color of the cubic boron nitride crystal after synthesis is bright black, fine grained still has a small amount of transparent crystal, and the output of black cubic boron nitride crystal declines to some extent with the increase of calcium boride; When mixed material be 75% ~ 85% hexagonal boron nitride powder, the lithium nitride of 2.5% ~ 5%, the lithium hydride of 4% ~ 6% and be made up of the calcium boride of 2% ~ 4% and the titanium nitride of 3% ~ 4.5% additive time, the granularity of synthesizing the cubic boron nitride crystal obtained increases, crystalline form rule, in the majority with hexakisooctahedron, bright black, and with a small amount of yellow head.When using the mixed material of component provided by the invention and ratio thereof, synthesize the complete crystal form of the cubic boron nitride crystal obtained, color and luster is glossy, and granularity peak value is concentrated, and along with the increase of boron carbide, defect reduces, and crystalline form is fuller.Along with the continuous increase of boron element in building-up process, the color of cubic boron nitride crystal is transitioned into black non transparent state from yellow transparent gradually, the ratio of adjustment additive can change the growing environment of cubic boron nitride crystal, improves the ability of its impurities removal, reduces defect and increases its compression strength.
Therefore, the present invention realizes mainly through the content of the boron element in control raw material and nitrogen element the color controlling gained cubic boron nitride crystal, and reaches the object of the crystalline form controlling the final cubic boron nitride crystal synthesized by the component and ratio thereof controlling additive.Can produce high-grade block cubic boron nitride crystal semi-finished product by the manufacture method of cubic boron nitride crystal provided by the invention, the block cubic boron nitride crystal of this black is the high strength abrasive material with particular crystal plane; And the granularity peakedness ratio of the block cubic boron nitride crystal of this black is more concentrated, wherein there is the granularity of the product of 45% at 40 ~ 50 orders, surveying its isostatic pressing strength Ti is 65 ~ 70, thermal toughness index TTi is 60 ~ 65, so these block cubic boron nitride crystal semi-finished product can be applied to the processing of certain high-speed steel and case-hardened steel, carbide alloy, steel alloy, Ni-based and cobalt base superalloy material.The present invention adopts cubic hinge press can the block cubic boron nitride crystal particle of continuous seepage black, can enter suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is pressure-temperature in the synthesis technique that provides of the embodiment of the present invention 1 and the graph of a relation of time.
Fig. 2 is the electron scanning electromicroscopic photograph figure of the black cubic boron nitride crystal provided by the embodiment of the present invention 1.
Detailed description of the invention
Below by detailed description of the invention, technical scheme of the present invention is described in further detail.
Embodiment 1
The embodiment of the present invention 1 provides a kind of manufacture method of cubic boron nitride crystal, and it comprises the following steps:
Step one, by purity be 99% superfine hexagonal boron nitride powder in vacuum drying oven, carry out 100 DEG C of nitrogen treatment 4 hours, to remove the gas foreign material of moisture and adsorption, obtain pure hexagonal boron nitride powder; According to mass percent, the purity of 75% is greater than the pure hexagonal boron nitride powder of 99%, 2.5% lithium nitride, 4% lithium hydride, the calcium boride of 2%, the boron carbide of 3.5% and 3% titanium nitride to be placed in airtight three-dimensional material mixer Homogeneous phase mixing 0.5 hour, obtain mixed material, then described mixed material is placed on four column press, and the pressure applying 10 MPas repeatedly makes power, increase the density of described mixed material, make it easily shaping, and be pressed into cylinder and load in graphite-pipe and make synthetic rod;
Step 2, described synthetic rod loaded in the high pressure chest of cubic hinge press, wherein, the diameter of this high pressure chest is 45mm, after being forced into 30 MPas, then in 2 minutes, the temperature in high pressure chest is risen to 1500 degree, and is controlled to nuclear volume; Then continue boosting and the pressure in high pressure chest is risen to synthesis pressure 90 MPa, material in described high pressure chest is entered in the excellent crystalline region of high pressure and generates cubic boron nitride crystal, keep 25 minutes under this high pressure-temperature again, this cubic boron nitride crystal is fully grown, finally first the temperature in high pressure chest is dropped to room temperature, release again, obtains the described cubic boron nitride crystal crude product of black, specifically as shown in Figure 1;
Step 3, successively cubic boron nitride crystal crude product described in fragmentation, ball milling, obtain block cubic boron nitride crystal crude product; Block cubic boron nitride crystal crude product described in water soaking is adopted to remove unconverted hexagonal boron nitride powder, to obtain block elementary cubic boron nitride crystal crude product; According to the mixed acid that the volume ratio modulation concentration of 3 ︰ 1 is the sulfuric acid of 95% ~ 98% and the nitric acid of concentration 63% ~ 65%, elementary for described bulk cubic boron nitride crystal crude product is placed in described mixed acid, be heated to 150 ~ 180 degree and boil remove the impurity such as metal dust, graphite produced in ball milling reforming process in 4 ~ 6 hours, obtain block intermediate cubic boron nitride crystal crude product; Adopt and intermediate for described bulk cubic boron nitride crystal crude product is placed in the industry alkali alive that concentration is 95% ~ 98%, be heated to 250 ~ 350 degree and boil 4 ~ 5 hours, obtaining block senior cubic boron nitride crystal crude product; Rinse successively, dry the senior cubic boron nitride crystal crude product of described bulk, obtain granularity for block cubic boron nitride crystal semi-finished product described in 20 order ~ 60 objects;
Step 4, grading that block cubic boron nitride crystal semi-finished product described in 20 order ~ 60 objects are carried out successively, adopt model selecting machine type selecting, stereomicroscope check processing, monolithic output can be obtained and reach 90 carats, granularity 40 order ~ 50 object black cubic boron nitride crystal particle, as shown in Figure 2, this granularity is the productive rate of 40 order ~ 50 object cubic boron nitride crystal particles is 36%;
Flying-spot microscope is adopted to analyze the block cubic boron nitride crystal particulate samples of described black, as shown in Figure 2, the block cubic boron nitride crystal of described black is excellent blocky crystal, crystalline form mostly is hexakisooctahedron, flawless, isostatic pressing strength Ti65 ~ 67, thermal toughness index TTi60 ~ 62, can be applied to the processing of certain high-speed steel and case-hardened steel, carbide alloy, steel alloy, Ni-based and cobalt base superalloy material.
Embodiment 2
The embodiment of the present invention 2 is substantially identical with the manufacture method of the cubic boron nitride crystal that embodiment 1 provides, difference is: in step one, according to mass percent, by the pure hexagonal boron nitride powder of 80%, 3.8% lithium nitride, 5% lithium hydride, the calcium boride of 3%, the boron carbide of 4.5% and 4% titanium nitride be placed in airtight three-dimensional material mixer, full and uniform mixing 0.8 hour, obtains mixed material; In step 2, synthetic rod is loaded in the high pressure chest of cubic hinge press, after being forced into 40 MPas, then in 3 minutes, temperature is risen to 1600 degree; Then continue boosting and the pressure in high pressure chest is risen to synthesis pressure 93.5 MPa, then keep 30 minutes under this HTHP, release of then lowering the temperature, obtains described cubic boron nitride crystal crude product.
In the block cubic boron nitride crystal particle of the black obtained by the present embodiment, granularity is that the monolithic output of the block cubic boron nitride crystal particle of 40 orders and 50 object black reaches 95 carats, and productive rate can reach 39%.
Flying-spot microscope is adopted to analyze the block cubic boron nitride crystal particulate samples of described black, the block cubic boron nitride crystal of described black is excellent blocky crystal, crystalline form mostly is hexakisooctahedron, flawless, isostatic pressing strength Ti is 67 ~ 69, thermal toughness index TTi is 62 ~ 64, can be applied to the processing of certain high-speed steel and case-hardened steel, carbide alloy, steel alloy, Ni-based and cobalt base superalloy material.
Embodiment 3
The embodiment of the present invention 3 is substantially identical with the manufacture method of the cubic boron nitride crystal that embodiment 1 provides, difference is: in step one, according to mass percent, by the pure hexagonal boron nitride powder of 85%, 5% lithium nitride, 6% lithium hydride, the calcium boride of 4%, the boron carbide of 5.5% and 4.5% titanium nitride be placed in airtight three-dimensional material mixer Homogeneous phase mixing 1 hour, raw material is mixed; In step 2, synthetic rod is loaded in the high pressure chest of cubic hinge press, after being forced into 45 MPas, in 4 minutes, temperature is risen to 1600 degree again, then continue the pressure be forced in described high pressure chest and reach synthesis pressure 95 MPa, keep 35 minutes again, release of finally lowering the temperature, obtain the described cubic boron nitride crystal crude product of black.
In the block cubic boron nitride crystal particle of the black obtained by the present embodiment, granularity is that the monolithic output of the block cubic boron nitride crystal particle of 30 orders and 40 object black reaches 90 carats, and productive rate can reach 30%.
Flying-spot microscope is adopted to analyze the block cubic boron nitride crystal particulate samples of described black, the block cubic boron nitride crystal particle of described black is excellent blocky crystal, crystalline form mostly is hexakisooctahedron, flawless, isostatic pressing strength Ti is 69 ~ 70, thermal toughness index TTi is 63 ~ 65, can be applied to the processing of certain high-speed steel and case-hardened steel, carbide alloy, steel alloy, Ni-based and cobalt base superalloy material.
the performance verification test of the block cubic boron nitride crystal of black
The quantity of 45 Hardened Steel Workpiece that described performance test mainly can be made by the described vitrified bonded grinding wheel of same thickness of wearing and tearing represents the intensity of the block cubic boron nitride crystal of described black and the common cubic boron nitride monocrystal manufactured by above-described embodiment 1 to 3.Specific as follows:
Adopt the block cubic boron nitride crystal sample of the black prepared by the embodiment of the present invention 1 to 3 of same particle sizes respectively and commercially available common cubic boron nitride monocrystal sample making hardness reaches P level, external diameter is 400 millimeters and the vitrified bonded grinding wheel of ring width 10 millimeters, and use corresponding emery wheel making 45 Hardened Steel Workpiece.Wherein, the relevant parameter condition of this performance test is: the granularity of described crystal prototype is 40 orders or 50 orders; Abrasive concentration in described vitrified bonded grinding wheel is 125%, and the linear velocity of this vitrified bonded grinding wheel is 60 meter per seconds, and feed speed is 10 micro-meter per seconds, and adopts the grinding method determining amount of feeding cylindrical incision mill to make described 45 Hardened Steel Workpiece; The rotating speed of described 45 Hardened Steel Workpiece is 100 revs/min; External diameter is 120 millimeters, and thickness is 10 millimeters.The performance test results of above-mentioned two kinds of cubic boron nitride crystals is as shown in the table:
Performance comparison test's tables of data of different cubic boron nitride crystal
As can be seen from the above table: after the above-mentioned four kinds of crystal preparation of employing become described vitrified bonded grinding wheel, when the vitrified bonded grinding wheel consuming condition of equivalent thickness makes 45 Hardened Steel Workpiece, many obviously than 45 Hardened Steel Workpiece using common cubic boron nitride crystal to process of the quantity of 45 Hardened Steel Workpiece that the block cubic boron nitride crystal of the black adopting the method that provided by the embodiment of the present invention 1 to 3 to prepare processes, and the described vitrified bonded grinding wheel to be prepared by the block cubic boron nitride crystal of described black is with the consumption of its stock removal, the proportional rising of quantity of its processing work, its service life and efficiency are all better than the emery wheel prepared by common cubic boron nitride crystal, so, the wearability of the block cubic boron nitride crystal of the described black manufactured by the embodiment of the present invention 1 to 3, intensity and heat endurance well more a lot of than common cubic boron nitride crystal.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (6)
1. a manufacture method for cubic boron nitride crystal, comprises the following steps:
Step one, according to mass percent, by the hexagonal boron nitride powder of 75% ~ 85%, 2.5% ~ 5% lithium nitride, 4% ~ 6% lithium hydride, the calcium boride of 2% ~ 4%, the boron carbide of 3.5% ~ 5.5% and 3% ~ 4.5% titanium nitride Homogeneous phase mixing, and be pressed into synthetic rod;
Step 2, under 1500 ~ 1650 degree, synthesis pressure 90 ~ 97 MPa is applied to described synthetic rod and carries out high pressure-temperature synthesis, obtain the cubic boron nitride crystal crude product of black;
Step 3, broken described cubic boron nitride crystal crude product, obtain block cubic boron nitride crystal crude product; Adopt block cubic boron nitride crystal crude product described in water soaking, soda acid process successively, obtain block cubic boron nitride crystal semi-finished product;
Step 4, type selecting process is carried out to described block cubic boron nitride crystal semi-finished product, obtain block cubic boron nitride crystal finished product.
2. manufacture method according to claim 1, it is characterized in that, described step one comprises: according to mass percent, by the hexagonal boron nitride powder of 75% ~ 85%, 2.5% ~ 5% lithium nitride, 4% ~ 6% lithium hydride, the calcium boride of 2% ~ 4%, the boron carbide of 3.5% ~ 5.5% and 3% ~ 4.5% titanium nitride be placed in airtight three-dimensional material mixer, Homogeneous phase mixing obtains mixed material in 0.5 ~ 1 hour; Adopt four column press and described mixed material is pressed into predetermined shape by the pressure applying 10 ~ 15 MPas, and load in graphite-pipe and make described synthetic rod.
3. manufacture method according to claim 2, is characterized in that, comprises taking a step forward of described step one: in vacuum drying oven, adopt nitrogen to carry out purified treatment hexagonal boron nitride powder raw material.
4. the manufacture method according to any one of claims 1 to 3, is characterized in that, described step 2 comprises: loaded in high pressure chest by described synthetic rod, and be forced into 30 ~ 45 MPas; In 2 ~ 4 minutes, the temperature in described high pressure chest is risen to 1500 ~ 1650 degree again; Then continue boosting and the pressure in described high pressure chest is risen to synthesis pressure 90 ~ 97 MPa; Constant temperature and pressure 25 ~ 35 minutes again, release of finally lowering the temperature, obtains the described cubic boron nitride crystal crude product of black.
5. manufacture method according to claim 1, is characterized in that, described step 3 comprises: cubic boron nitride crystal crude product described in fragmentation, ball milling successively, obtains block cubic boron nitride crystal crude product; Adopt block cubic boron nitride crystal crude product described in water soaking, obtain block elementary cubic boron nitride crystal crude product; According to the mixed acid that the volume ratio modulation concentration of 3 ︰ 1 is the sulfuric acid of 95% ~ 98% and the nitric acid of concentration 63% ~ 65%, elementary for described bulk cubic boron nitride crystal crude product is placed in described mixed acid, be heated to 150 ~ 180 degree and boil 4 ~ 6 hours, obtaining block intermediate cubic boron nitride crystal crude product; Intermediate for described bulk cubic boron nitride crystal crude product is placed in the industry alkali alive that concentration is 95% ~ 98%, is heated to 250 ~ 350 degree and boils 4 ~ 5 hours, obtaining block senior cubic boron nitride crystal crude product; Rinse successively, dry the senior cubic boron nitride crystal crude product of described bulk, obtain the described block cubic boron nitride crystal semi-finished product of black.
6. manufacture method according to claim 5, it is characterized in that, described step 4 comprises: carry out grading, type selecting, stereomicroscope check processing successively to described block cubic boron nitride crystal semi-finished product, obtains varigrained described block cubic boron nitride crystal semi-finished product.
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| CN107805489A (en) * | 2017-10-12 | 2018-03-16 | 信阳市德隆超硬材料有限公司 | A kind of micro/nano level cubic boron nitride abrasive materials and preparation method thereof |
| CN109825880A (en) * | 2019-03-07 | 2019-05-31 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN109825880B (en) * | 2019-03-07 | 2021-08-24 | 信阳市德隆超硬材料有限公司 | Cubic boron nitride single crystal and preparation method thereof |
| CN113444490A (en) * | 2021-06-25 | 2021-09-28 | 郑州益奇超硬材料有限公司 | Polycrystalline cubic boron nitride abrasive and preparation method thereof |
| CN113444490B (en) * | 2021-06-25 | 2022-08-26 | 郑州益奇超硬材料有限公司 | Polycrystalline cubic boron nitride abrasive and preparation method thereof |
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