CN103691363A - Synthesis method of cubic boron nitride polycrystalline particles - Google Patents
Synthesis method of cubic boron nitride polycrystalline particles Download PDFInfo
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- CN103691363A CN103691363A CN201310665344.XA CN201310665344A CN103691363A CN 103691363 A CN103691363 A CN 103691363A CN 201310665344 A CN201310665344 A CN 201310665344A CN 103691363 A CN103691363 A CN 103691363A
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Abstract
The invention relates to a synthesis method of cubic boron nitride polycrystalline particles. Specific to the conditions that the surface of cubic boron nitride resists abrasion and is easy to dissociate, by adopting hexagonal boron nitride as a raw material, lithium nitride as a synthesis catalytic agent and magnesium and aluminum alloy powder as an additive, steps of raw material grinding, mixing, assembling, synthesis at high temperature and high pressure, particle growth, ball milling, acid pickling, washing, suction-filtering, drying and screening are carried out to prepare the cubic boron nitride polycrystalline particles, thus the direct growth of the cubic boron nitride polycrystalline particles is realized. According to the preparation method, the process is advanced, and data is complete and accurate. The cubic boron nitride polycrystalline particles are polycrystalline particles, and are high in purity reaching 98 percent, and are firmly bound. A single crystal forming the polycrystalline particles is less than 10 micrometers, and thus the synthesis method is an ideal synthesis method of the cubic boron nitride polycrystalline particles.
Description
Technical field
The present invention relates to a kind of synthetic method of polycrystalline cubic boron nitride particle, belong to the technical field of cubic boron nitride particle growth and high pressure synthesis method.
Background technology
Cubic boron nitride is a kind of nonmetallic materials of high rigidity, has high hardness and good thermal conduction characteristic, not with iron family element and alloy reaction thereof, in field of machining, is good removing material; Cubic boron nitride is divided into monocrystalline, glomerocryst and complex from application form, and multi-form cubic boron nitride has different purposes industrial; Polycrystalline cubic boron nitride particle be by fine grain cubic boron nitride monocrystal at high temperature, high pressure, have under the condition that binding agent exists synthetic, in building-up process, due to the difference of monocrystalline size, synthesis condition, binding agent kind, additive, the particle size of synthetic polycrystalline cubic boron nitride, component ratio, performance also have difference; In order to improve wearability, the non-oxidizability of cubic boron nitride in grinding, conventionally polycrystalline cubic boron nitride particle is to consist of many little monocrystal, makes the polycrystalline cubic boron nitride particle face that do not dissociate, and each little crystal is the face that independently dissociates; In metal processing, can effectively improve working (machining) efficiency and machining accuracy.
Patent CN101891481A discloses a kind of method for producing polycrystal cubic boron nitride abrasive materials, the metallic bond that the method is prepared by utilization carries out sintering, pulverizing, soda acid to be processed and has obtained the good polycrystal of sintering, it is raw material that this method adopts the cubic boron nitride micro mist of 10 microns, expensive, binding agent kind is many, preparation is complicated, and needed high-temperature and high-pressure conditions is harsh, the soda acid processing time in later stage is long, is therefore difficult to apply.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology, employing hexagonal boron nitride is that raw material, lithium nitride are synthesizing cubic boron nitride catalyst, magnesium aluminum-alloy powder is additive, promote cubic boron nitride nucleation, synthesizing cubic boron nitride glomerocryst particle, to increase substantially the surface oxidation-resistant performance of cubic boron nitride, expand the scope of application of cubic boron nitride.
Technical scheme
The chemical substance material that the present invention uses is: hexagonal boron nitride, lithium nitride, magnesium aluminum-alloy powder, graphite-pipe, graphite flake, copper sheet, conductive steel cap, pyrophyllite block, dolomite sleeve pipe, pyrophillite ring, sulfuric acid, nitric acid, alcohol, deionized water, sand paper, it is as follows that consumption is prepared in its combination: take gram, millimeter, milliliter as measurement unit
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carries out quality purity, content, concentration control:
(2) solid powder material grinds, sieves
1. the agate mortar of hexagonal boron nitride 100g ± for 0.1g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037mm;
2. the agate mortar of lithium nitride 15g ± for 0.1g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074mm;
3. the agate mortar of magnesium aluminum-alloy powder 8g ± for 0.1g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037mm;
(3) preparation mixing fine powders
Hexagonal boron nitride 100g ± 0.1g, the lithium nitride 15g ± 0.1g, the magnesium aluminum-alloy powder 8g ± 0.1g that grind, sieve are added in quartz container, then being placed in batch mixer mixes, batch mixer rotating speed is 100r/min, and incorporation time is 180min, after mixing, becomes batch mixing fine powder;
(4) roasting pyrophyllite block, pyrophillite ring, dolomite sleeve pipe
Pyrophyllite block, pyrophillite ring, dolomite sleeve pipe are placed in to heating kiln roasting, 200 ℃ of sintering temperatures, roasting time 26h, to remove moisture;
(5) polishing conductive steel cap
Two conductive steel caps are polished with sand paper respectively, remove each position oxide layer of steel cap;
(6) assembling pyrophyllite block and inner batch mixing fine powder thereof
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. in pyrophyllite block bottom, put conductive steel cap, pyrophillite ring;
3. on conductive steel cap top, put circular copper sheet;
4. on circular copper sheet top, put graphite flake, dolomite sleeve pipe, graphite-pipe;
5. in graphite-pipe, put batch mixing fine powder;
6. on graphite-pipe top, put graphite flake;
7. on graphite flake top, put circular copper sheet;
8. on circular copper sheet top, put pyrophillite ring, conductive steel cap;
(7) prepare polycrystalline cubic boron nitride particle
Polycrystalline cubic boron nitride particle is to carry out in the hyperbaric chamber of cubic hinge press, is in pyrophyllite block, under pressurization, heating, constant temperature keeping warm mode, completes;
1. by the pyrophyllite block of assembling and inner batch mixing fine powder capable of parallel moving to the bottom top hammer in the hyperbaric chamber of cubic hinge press;
2. three top hammers in cubic hinge press are opened near pyrophyllite block, form six squeezed states;
3. open compression system, six top hammers of cubic hinge press are pushed pyrophyllite block, produce pressure and make pyrophillite internal pressure rise to gradually 5.4GPa, rate of rise 520MPa/min;
4. open cubic hinge press heating system, the batch mixing fine powder in heating pyrophyllite block, heating-up temperature is 1650 ℃ ± 5 ℃, 320 ℃/min of firing rate;
5. the constant temperature and pressure 20min in hyperbaric chamber of the batch mixing fine powder in pyrophyllite block;
Batch mixing fine powder generates polycrystalline cubic boron nitride particle in high temperature, hyperbaric environment, particle surface growth, and blending is integrated mutually;
6. after synthetic reaction finishes, stop heating, stop exerting pressure, make pyrophyllite block and batch mixing fine powder in hyperbaric chamber be cooled to 25 ℃, Pressure Drop is to 0.1MPa;
7. open hyperbaric chamber, take out the crystal block product in pyrophyllite block;
(8) synthetic crystal block product is put into ball mill and carry out ball milling, Ball-milling Time 180min, is polycrystalline cubic boron nitride particle after ball milling;
(9) washing
1. preparating acid dilution
Measure sulfuric acid 100mL ± 5mL, nitric acid 300mL ± 5mL is placed in beaker, is uniformly mixed, and becomes acid solution;
2. the beaker that fills acid solution is placed on electric heater, polycrystalline cubic boron nitride particle is added in beaker, heating stirring and pickling, heating-up temperature is 400 ℃, pickling time 30min;
3. the glomerocryst particle after pickling is placed in to another beaker, adds deionized water 1000mL, agitator treating 10min;
4. the glomerocryst particle after deionized water washing is placed in to another beaker, adds alcohol 400mL, agitator treating 10min, becomes mixed solution;
(10) suction filtration
The Buchner funnel that mixed liquor after alcohol washing is placed in to bottle,suction, carries out suction filtration with three layers of middling speed qualitative filter paper, retains product filter cake on filter paper, and cleaning solution is evacuated in filter flask;
(11) vacuum drying
Product filter cake is placed in to quartz container, is then placed in vacuum drying chamber dry, baking temperature is 200 ℃, and vacuum is 10Pa, and drying time, 15min, was polycrystalline cubic boron nitride particle after being dried;
(12) particle screen selecting
Utilize 40 eye mesh screen cubic boron nitride glomerocryst particles to screen, obtain the polycrystalline cubic boron nitride particle of homogeneous grain diameter, particle diameter≤0.425mm;
(13) detect, analyze, characterize
The pattern of cubic boron nitride glomerocryst particle, color and luster, composition, Chemical Physics performance detect, analyze, characterize;
With powder x-ray diffraction, carry out the facies analysis of glomerocryst particle;
By SEM, carry out the analysis of glomerocryst granule-morphology;
Conclusion: polycrystalline cubic boron nitride particle is black particle shape, glomerocryst particle diameter≤0.425mm, the monocrystal≤10 μ m of formation glomerocryst particle, crystal has Emission in Cubic structure, and product purity reaches 98%;
(14) product stores
Polycrystalline cubic boron nitride particle to preparation is stored in brown transparent glass container, and airtight lucifuge stores, and storage temperature is 20 ℃, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has obvious advance, be for cubic boron nitride surface abrasion resistance and surperficial legibility from situation, employing hexagonal boron nitride is raw material, lithium nitride is synthetic catalyst, magnesium aluminum-alloy powder is additive, through former abrasive lapping, batch mixing, assembling, synthetic through HTHP, germination, ball milling, pickling, washing, suction filtration, dry, screening, make polycrystalline cubic boron nitride particle, realized the direct growth of polycrystalline cubic boron nitride particle, this preparation method's technique is advanced, informative data is accurate, product is glomerocryst crystal, purity is high, reach 98%, particle is in conjunction with firm, the glomerocryst particle monocrystal≤10 μ m forming, it is the synthetic method of very good polycrystalline cubic boron nitride particle.
Accompanying drawing explanation
The jack unit figure of Fig. 1 cubic hinge press
Fig. 2 pyrophyllite block and batch mixing fine powder assembled state figure
Fig. 3 polycrystalline cubic boron nitride granule-morphology figure
Fig. 4 polycrystalline cubic boron nitride particle packing shape appearance figure
Fig. 5 polycrystalline cubic boron nitride particle diffracted intensity collection of illustrative plates
Shown in figure, list of numerals is as follows:
1, pyrophyllite block, 2, dolomite sleeve pipe, 3, graphite-pipe, 4, batch mixing fine powder, 5, the first conductive steel cap, the 6, second conductive steel cap, the 7, first pyrophillite ring, the 8, second pyrophillite ring, 9, the first graphite flake, the 10, second graphite flake, the 11, first copper sheet, the 12, second copper sheet.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the jack unit figure of cubic hinge press, jack unit is six symmetric designs, cubic pressure uniform stressed.
Shown in Fig. 2, be pyrophyllite block and batch mixing fine powder assembled state figure, each position, annexation want correct, and proportioning is assembled according to quantity, press on top according to the order of sequence.
The value of preparing required chemical substance is to determine by the scope setting in advance, and take gram, millimeter, milliliter as measurement unit.
Pyrophyllite block is cuboid, at pyrophyllite block 1 inner bottom part, place the second conductive steel cap 6, the second pyrophillite ring 8, on the second conductive steel cap 6 tops, it is the second copper sheet 12, the second copper sheet 12 tops are the second graphite flake 10, on the second pyrophillite ring 8 tops, it is dolomite sleeve pipe 2, it in dolomite sleeve pipe 2, is graphite-pipe 3, on graphite-pipe 3 tops, it is the first graphite flake 9, the first graphite flake 9 tops are the first copper sheet 11, are the first pyrophillite ring 7, the first conductive steel cap 5 on the first copper sheet 11, dolomite sleeve pipe 2 tops; In graphite-pipe 3, it is batch mixing fine powder 4.
Shown in Fig. 3, for polycrystalline cubic boron nitride granule-morphology figure, visible in figure, product is glomerocryst graininess, and glomerocryst particle is cone angle shape.
Shown in Fig. 4, for polycrystalline cubic boron nitride particle packing shape appearance figure, visible in figure, glomerocryst particle has many little germinations to form, and is irregular stacking.
Shown in Fig. 5, for polycrystalline cubic boron nitride particle diffracted intensity collection of illustrative plates, visible in figure, ordinate is diffracted intensity, and abscissa is the angle of diffraction 2 θ, and in figure, three highest peaks represent respectively (111), (200), (220) peak position of cubic boron nitride from left to right.
Claims (2)
1. the synthetic method of a polycrystalline cubic boron nitride particle, it is characterized in that: the chemical substance material of use is: hexagonal boron nitride, lithium nitride, magnesium aluminum-alloy powder, graphite-pipe, graphite flake, copper sheet, conductive steel cap, pyrophyllite block, dolomite sleeve pipe, pyrophillite ring, sulfuric acid, nitric acid, alcohol, deionized water, sand paper, it is as follows that consumption is prepared in its combination: take gram, millimeter, milliliter as measurement unit
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carries out quality purity, content, concentration control:
(2) solid powder material grinds, sieves
1. the agate mortar of hexagonal boron nitride 100g ± for 0.1g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037mm;
2. the agate mortar of lithium nitride 15g ± for 0.1g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074mm;
3. the agate mortar of magnesium aluminum-alloy powder 8g ± for 0.1g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037mm;
(3) preparation mixing fine powders
Hexagonal boron nitride 100g ± 0.1g, the lithium nitride 15g ± 0.1g, the magnesium aluminum-alloy powder 8g ± 0.1g that grind, sieve are added in quartz container, then being placed in batch mixer mixes, batch mixer rotating speed is 100r/min, and incorporation time is 180min, after mixing, becomes batch mixing fine powder;
(4) roasting pyrophyllite block, pyrophillite ring, dolomite sleeve pipe
Pyrophyllite block, pyrophillite ring, dolomite sleeve pipe are placed in to heating kiln roasting, 200 ℃ of sintering temperatures, roasting time 26h, to remove moisture;
(5) polishing conductive steel cap
Two conductive steel caps are polished with sand paper respectively, remove each position oxide layer of steel cap;
(6) assembling pyrophyllite block and inner batch mixing fine powder thereof
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. in pyrophyllite block bottom, put conductive steel cap, pyrophillite ring;
3. on conductive steel cap top, put circular copper sheet;
4. on circular copper sheet top, put graphite flake, dolomite sleeve pipe, graphite-pipe;
5. in graphite-pipe, put batch mixing fine powder;
6. on graphite-pipe top, put graphite flake;
7. on graphite flake top, put circular copper sheet;
8. on circular copper sheet top, put pyrophillite ring, conductive steel cap;
(7) prepare polycrystalline cubic boron nitride particle
Polycrystalline cubic boron nitride particle is to carry out in the hyperbaric chamber of cubic hinge press, is in pyrophyllite block, under pressurization, heating, constant temperature keeping warm mode, completes;
1. by the pyrophyllite block of assembling and inner batch mixing fine powder capable of parallel moving to the bottom top hammer in the hyperbaric chamber of cubic hinge press;
2. three top hammers in cubic hinge press are opened near pyrophyllite block, form six squeezed states;
3. open compression system, six top hammers of cubic hinge press are pushed pyrophyllite block, produce pressure and make pyrophillite internal pressure rise to gradually 5.4GPa, rate of rise 520MPa/min;
4. open cubic hinge press heating system, the batch mixing fine powder in heating pyrophyllite block, heating-up temperature is 1650 ℃ ± 5 ℃, 320 ℃/min of firing rate;
5. the constant temperature and pressure 20min in hyperbaric chamber of the batch mixing fine powder in pyrophyllite block;
Batch mixing fine powder generates polycrystalline cubic boron nitride particle in high temperature, hyperbaric environment, particle surface growth, and blending is integrated mutually;
6. after synthetic reaction finishes, stop heating, stop exerting pressure, make pyrophyllite block and batch mixing fine powder in hyperbaric chamber be cooled to 25 ℃, Pressure Drop is to 0.1MPa;
7. open hyperbaric chamber, take out the crystal block product in pyrophyllite block;
(8) synthetic crystal block product is put into ball mill and carry out ball milling, Ball-milling Time 180min, is polycrystalline cubic boron nitride particle after ball milling;
(9) washing
1. preparating acid dilution
Measure sulfuric acid 100mL ± 5mL, nitric acid 300mL ± 5mL is placed in beaker, is uniformly mixed, and becomes acid solution;
2. the beaker that fills acid solution is placed on electric heater, polycrystalline cubic boron nitride particle is added in beaker, heating stirring and pickling, heating-up temperature is 400 ℃, pickling time 30min;
3. the glomerocryst particle after pickling is placed in to another beaker, adds deionized water 1000mL, agitator treating 10min;
4. the glomerocryst particle after deionized water washing is placed in to another beaker, adds alcohol 400mL, agitator treating 10min, becomes mixed solution;
(10) suction filtration
The Buchner funnel that mixed liquor after alcohol washing is placed in to bottle,suction, carries out suction filtration with three layers of middling speed qualitative filter paper, retains product filter cake on filter paper, and cleaning solution is evacuated in filter flask;
(11) vacuum drying
Product filter cake is placed in to quartz container, is then placed in vacuum drying chamber dry, baking temperature is 200 ℃, and vacuum is 10Pa, and drying time, 15min, was polycrystalline cubic boron nitride particle after being dried;
(12) particle screen selecting
Utilize 40 eye mesh screen cubic boron nitride glomerocryst particles to screen, obtain the polycrystalline cubic boron nitride particle of homogeneous grain diameter, particle diameter≤0.425mm;
(13) detect, analyze, characterize
The pattern of cubic boron nitride glomerocryst particle, color and luster, composition, Chemical Physics performance detect, analyze, characterize;
With powder x-ray diffraction, carry out the facies analysis of glomerocryst particle;
By SEM, carry out the analysis of glomerocryst granule-morphology;
Conclusion: polycrystalline cubic boron nitride particle is black particle shape, glomerocryst particle diameter≤0.425mm, the monocrystal≤10 μ m of formation glomerocryst particle, crystal has Emission in Cubic structure, and product purity reaches 98%;
(14) product stores
Polycrystalline cubic boron nitride particle to preparation is stored in brown transparent glass container, and airtight lucifuge stores, and storage temperature is 20 ℃, relative humidity≤10%.
2. according to the synthetic method of a kind of polycrystalline cubic boron nitride particle described in right 1, be characterised in that: described polycrystalline cubic boron nitride particle is cone angle shape, glomerocryst particle is formed by granule growth, is irregular stacking.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170029A (en) * | 2015-07-16 | 2015-12-23 | 河南飞孟金刚石工业有限公司 | Synthetic method of granularity-centralized cubic boron nitride |
| CN105386118A (en) * | 2014-08-26 | 2016-03-09 | 信阳市德隆超硬材料有限公司 | Method for synthesizing coarse particle size cubic boron nitride single crystal through magnesium-based catalyst |
| CN107311663A (en) * | 2017-04-01 | 2017-11-03 | 四川大学 | A kind of new tantalum nitride hard alloy and preparation method thereof |
| CN107523875A (en) * | 2017-10-12 | 2017-12-29 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN108176329A (en) * | 2017-12-22 | 2018-06-19 | 郑州中南杰特超硬材料有限公司 | A kind of synthetic method of cubic boron nitride |
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2013
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386118A (en) * | 2014-08-26 | 2016-03-09 | 信阳市德隆超硬材料有限公司 | Method for synthesizing coarse particle size cubic boron nitride single crystal through magnesium-based catalyst |
| CN105170029A (en) * | 2015-07-16 | 2015-12-23 | 河南飞孟金刚石工业有限公司 | Synthetic method of granularity-centralized cubic boron nitride |
| CN107311663A (en) * | 2017-04-01 | 2017-11-03 | 四川大学 | A kind of new tantalum nitride hard alloy and preparation method thereof |
| CN107523875A (en) * | 2017-10-12 | 2017-12-29 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN108176329A (en) * | 2017-12-22 | 2018-06-19 | 郑州中南杰特超硬材料有限公司 | A kind of synthetic method of cubic boron nitride |
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