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CN104607110A - Manufacturing method for cubic boron nitride crystal - Google Patents

Manufacturing method for cubic boron nitride crystal Download PDF

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Publication number
CN104607110A
CN104607110A CN201510049045.2A CN201510049045A CN104607110A CN 104607110 A CN104607110 A CN 104607110A CN 201510049045 A CN201510049045 A CN 201510049045A CN 104607110 A CN104607110 A CN 104607110A
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boron nitride
cubic boron
nitride crystal
crude product
block
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CN104607110B (en
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马少彬
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Funik Ultrahard Material Co Ltd
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Funik Ultrahard Material Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0605Composition of the material to be processed
    • B01J2203/0645Boronitrides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/065Composition of the material produced
    • B01J2203/066Boronitrides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0675Structural or physico-chemical features of the materials processed

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a manufacturing method for a cubic boron nitride crystal. The manufacturing method comprises the following steps: uniformly mixing hexagonal boron nitride powder, catalyst powder and additives, and pressing the mixture into a synthesis stick, wherein the catalyst powder comprises lithium nitride and lithium hydride, and the additives comprise ammonium fluoride, titanium nitride and aluminium nitride; carrying out high-pressure high-temperature synthesis on the synthesis stick to obtain a cubic boron nitride crystal crude product; crushing the cubic boron nitride crystal crude product to obtain a massive cubic boron nitride crystal crude product; sequentially soaking the massive cubic boron nitride crystal crude product by water and acid-base to obtain a massive cubic boron nitride crystal finished product. The cubic boron nitride crystal obtained by the manufacturing method disclosed by the invention is an equiareal golden crystal, has the characteristics of high strength, high thermal stability, high wear resistance, high crack resistant capability, high thermal stability and the like, is suitable for long-life electroplated tools and ceramic bond systems, as well as is applied to processing hardened carbon tool steel, hard alloys, alloy steel, and nickel-based and cobalt-based high-temperature alloy materials.

Description

The manufacture method of cubic boron nitride crystal
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 70% ~ 85%, 7% ~ 14.5% lithium nitride, 2.5% ~ 5% lithium hydride, the ammonium fluoride of 1.5% ~ 4.5%, the titanium nitride of 2% ~ 3.5% and 2% ~ 2.5% aluminium nitride Homogeneous phase mixing, and be pressed into synthetic rod;
Step 2, under 1400 ~ 1600 degree, synthesis pressure 90 ~ 95 MPa is applied to described synthetic rod and carries out high pressure-temperature synthesis, obtain golden cubic boron nitride crystal crude product;
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 70% ~ 85%, 7% ~ 14.5% lithium nitride, 2.5% ~ 5% lithium hydride, the ammonium fluoride of 1.5% ~ 4.5%, the titanium nitride of 2% ~ 3.5% and 2% ~ 2.5% aluminium 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 raw materials is main synthesis material, and lithium nitride and lithium hydride are jointly as catalyst powder, and ammonium fluoride, titanium nitride and aluminium nitride 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, described step 2 comprises: loaded by described synthetic rod in high pressure chest, and be forced into 18 ~ 30 MPas, again the temperature in described high pressure chest is risen to 1400 ~ 1600 degree, then in 1 ~ 3 minute, the pressure in described high pressure chest is risen to described synthesis pressure 90 ~ 95 MPa, constant temperature and pressure 15 ~ 25 minutes again, release of finally lowering the temperature, obtains golden described cubic boron nitride crystal crude product.
Wherein, the pressure in described high pressure chest rose to synthesis pressure 90 ~ 95 MPa at 1 ~ 3 minute, 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 15 ~ 25 minutes is to make the cubic boron nitride crystal in described high pressure chest fully grow.Wherein, pressure when " constant temperature and pressure " in this step refers to that the pressure maintained in described high pressure chest reaches described synthesis pressure 90 ~ 95 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 described block cubic boron nitride crystal semi-finished product.
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 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 finished product.Wherein, the granularity of described block cubic boron nitride crystal finished product is 20 order ~ 60 orders, and as 20 orders, 30 orders, 40 orders, 50 orders, 60 orders, preferably, the granularity of described block cubic boron nitride crystal finished product is 30 order ~ 50 orders.
Following mixed material is synthesizing cubic boron nitride crystal under 1400 ~ 1600 degree and 90 ~ 95 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 the hexagonal boron nitride powder of 70% ~ 85% and 7% ~ 14.5% of composition catalyst powder lithium nitride and 2.5% ~ 5% lithium hydride time, the cubic boron nitride crystal that synthesis obtains is light yellow and size distribution is uneven, along with the increase of lithium hydride content, the color of cubic boron nitride crystal is progressively to orange and dark-brown transition; When hexagonal boron nitride powder, the lithium nitride of 7% ~ 14.5%, the lithium hydride of 2.5% ~ 5% that mixed material is 70% ~ 85%, during with the additive be made up of the ammonium fluoride of 1.5% ~ 4.5% and the aluminium nitride of 2% ~ 2.5%, synthesize the color of the cubic boron nitride crystal obtained in golden yellow or brownish red, its crystalline form mostly is tabular and class spherical surface body, and skewness; When using the mixed material of component provided by the invention and ratio thereof, the granularity of synthesizing the cubic boron nitride crystal obtained is comparatively large, crystalline form is regular, and pattern mostly is hexakisooctahedron bulk crystals, complete crystal form and being evenly distributed.Therefore, select hexagonal boron nitride powder, different lithium base as catalyzer contact agent, with additive as raw material, by the method synthesizing cubic boron nitride crystal of HTHP, the color of the cubic boron nitride crystal synthesized and pattern is made to have had different changes, proportionate relationship in adjustment raw material between a component, can reach the object controlling crystal color and crystalline form.
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.High-grade block cubic boron nitride crystal finished product can be produced by the manufacture method of cubic boron nitride crystal provided by the invention, and this golden block hexagonal boron nitride crystal finished product is excellent blocky crystal, there is high strength, high thermal stability, wearability is high, isostatic pressing strength Ti is 60 ~ 70, thermal toughness index TTi is 55 ~ 65, heat endurance is up to 1170 ~ 1270K, be applicable to long-life plating tool and vitrified bond system, be applied to hardened carbon tool steel, carbide alloy, steel alloy, the processing of Ni-based and cobalt base superalloy material, with long-life plating tool and vitrified bond system.The present invention adopts cubic hinge press can the golden block cubic boron nitride crystal particle of continuous seepage, 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 golden 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, according to mass percent, the purity of 70% is greater than the superfine hexagonal boron nitride powder of 99%, 7% lithium nitride, 2.5% lithium hydride, the ammonium fluoride of 1.5%, the titanium nitride of 2% and 2% aluminium nitride, above-mentioned raw materials 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, the diameter of this high pressure chest is 45 millimeters, the pressure in described high pressure chest is risen to 18 MPas, then the temperature in this high pressure chest is risen to 1400 degree; In 1 minute, the pressure in high pressure chest is risen to synthesis pressure 90 MPa, to control the nucleation quantity of cubic boron nitride crystal, and make the material in described high pressure chest enter generation cubic boron nitride crystal in the excellent crystalline region of high pressure, again under the state of this high pressure-temperature, keep within 15 minutes, making this cubic boron nitride crystal fully grow, then first the temperature in high pressure chest is dropped to room temperature, then release, obtain golden cubic boron nitride crystal crude product, 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, graphite produced in mechanical milling 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, use model selecting machine type selecting, stereomicroscope check processing, can obtain monolithic output reach 95 carats, productive rate be approximately 55% the golden cubic boron nitride crystal particle of granularity 50 object.
Adopt flying-spot microscope to analyze the block cubic boron nitride crystal particulate samples of described gold, as shown in Figure 2, the block cubic boron nitride crystal of described gold is excellent blocky crystal, and crystalline form mostly is octahedra or hexakisooctahedron, flawless.Employing national standard detects, its isostatic pressing strength Ti60 ~ 63, thermal toughness index TTi55 ~ 58, and heat endurance is up to 1170 ~ 1210K, and anti-crack ability is strong, and wearability is high, is applicable to long-life plating tool and vitrified bond system.
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, the purity of 78% is greater than the superfine hexagonal boron nitride powder of 99%, 11% lithium nitride, 3.8% lithium hydride, the ammonium fluoride of 3%, the titanium nitride of 2.8% and 2.3% aluminium 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, and be forced into 24 MPas, then temperature is risen to 1500 degree; Then in 2 minutes, the pressure in high pressure chest is risen to synthesis pressure 93 MPa, and under this HTHP, keep 20 minutes, release of finally lowering the temperature obtains golden described cubic boron nitride crystal crude product.
In the block cubic boron nitride crystal particle of the gold obtained by the present embodiment, granularity is that the monolithic output of the golden block cubic boron nitride crystal particle of 40 orders and 50 objects reaches 98 carats, and productive rate can reach 63%.
Adopt flying-spot microscope to analyze the block cubic boron nitride crystal particulate samples of gold that the present embodiment obtains, the block cubic boron nitride crystal of the gold that the present embodiment obtains is excellent blocky crystal, and crystalline form mostly is octahedra or hexakisooctahedron, flawless.Employing national standard detects, isostatic pressing strength Ti64 ~ 66 of the block cubic boron nitride crystal of the gold that the present embodiment obtains, thermal toughness index TTi59 ~ 61, heat endurance is up to 1200 ~ 1230K, anti-crack ability is strong, and wearability is high, is applicable to long-life plating tool and vitrified bond system.
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, the purity of 85% is greater than the superfine hexagonal boron nitride powder of 99%, 14.5% lithium nitride, the lithium hydride of 5%, ammonium fluoride, the titanium nitride of 3.5%, the aluminium nitride of 2.5% of 4.5%, in airtight three-dimensional material mixer, Homogeneous phase mixing 1 hour, makes raw material mix; In step 2, synthetic rod is loaded in the high pressure chest of cubic hinge press, after being forced into 30 MPas, temperature is risen to 1600 degree, and pressurization was continued in 3 minutes, the pressure in high pressure chest is made to rise to 95 MPas, then constant temperature and pressure 25 minutes, release of finally lowering the temperature obtains golden described cubic boron nitride crystal crude product.
In the block cubic boron nitride crystal particle of the gold obtained by the present embodiment, granularity is that the monolithic output of the golden block cubic boron nitride crystal particle of 50 objects reaches 102 carats, and productive rate can reach 78%.
Adopt flying-spot microscope to analyze the block cubic boron nitride crystal particulate samples of gold that the present embodiment obtains, the block cubic boron nitride crystal of the gold that the present embodiment obtains is excellent blocky crystal, and crystalline form mostly is octahedra or hexakisooctahedron, flawless.Employing national standard detects, isostatic pressing strength Ti67 ~ 70 of the block cubic boron nitride crystal of the gold that the present embodiment obtains, thermal toughness index TTi62 ~ 65, heat endurance is up to 1230 ~ 1270K, anti-crack ability is strong, and wearability is high, is applicable to long-life plating tool and vitrified bond system.
the performance verification test of golden block cubic boron nitride crystal
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 gold 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 gold 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 number 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 gold 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 gold 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 described gold 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 (5)

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 70% ~ 85%, 7% ~ 14.5% lithium nitride, 2.5% ~ 5% lithium hydride, the ammonium fluoride of 1.5% ~ 4.5%, the titanium nitride of 2% ~ 3.5% and 2% ~ 2.5% aluminium nitride Homogeneous phase mixing, and be pressed into synthetic rod;
Step 2, under 1400 ~ 1600 degree, synthesis pressure 90 ~ 95 MPa is applied to described synthetic rod and carries out high pressure-temperature synthesis, obtain golden cubic boron nitride crystal crude product;
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 70% ~ 85%, 7% ~ 14.5% lithium nitride, 2.5% ~ 5% lithium hydride, the ammonium fluoride of 1.5% ~ 4.5%, the titanium nitride of 2% ~ 3.5% and 2% ~ 2.5% aluminium nitride be placed in airtight three-dimensional material mixer, Homogeneous phase mixing 0.5 ~ 1 hour, obtains mixed material; 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 1 and 2, it is characterized in that, described step 2 comprises: loaded by described synthetic rod in high pressure chest, and be forced into 18 ~ 30 MPas, again the temperature in described high pressure chest is risen to 1400 ~ 1600 degree, then in 1 ~ 3 minute, the pressure in described high pressure chest is risen to described synthesis pressure 90 ~ 95 MPa, then constant temperature and pressure 15 ~ 25 minutes, finally to lower the temperature release, obtain golden described cubic boron nitride crystal crude product.
4. manufacture method according to claim 3, 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 described block cubic boron nitride crystal semi-finished product.
5. manufacture method according to claim 4, 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 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
CN109369192A (en) * 2018-11-29 2019-02-22 盐城师范学院 A kind of preparation method of cubic boron nitride
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
CN112456454A (en) * 2020-12-09 2021-03-09 长春阿尔玛斯科技有限公司 Cubic boron nitride powder and method for producing same
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

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CN106315525A (en) * 2016-08-30 2017-01-11 河南飞孟金刚石工业有限公司 Cubic boron nitride purification process
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
CN109369192A (en) * 2018-11-29 2019-02-22 盐城师范学院 A kind of preparation method of cubic boron nitride
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
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