CN103551080A - Method for plating titanium nitride on surface of cubic boron nitride particle - Google Patents
Method for plating titanium nitride on surface of cubic boron nitride particle Download PDFInfo
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- CN103551080A CN103551080A CN201310536406.7A CN201310536406A CN103551080A CN 103551080 A CN103551080 A CN 103551080A CN 201310536406 A CN201310536406 A CN 201310536406A CN 103551080 A CN103551080 A CN 103551080A
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- nitride
- boron nitride
- graphite
- titanium
- cubic boron
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 63
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 63
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000007747 plating Methods 0.000 title abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005554 pickling Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 229910000831 Steel Inorganic materials 0.000 claims description 26
- 239000010439 graphite Substances 0.000 claims description 26
- 229910002804 graphite Inorganic materials 0.000 claims description 26
- 239000010959 steel Substances 0.000 claims description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 24
- 229910052802 copper Inorganic materials 0.000 claims description 24
- 239000010459 dolomite Substances 0.000 claims description 19
- 229910000514 dolomite Inorganic materials 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 244000137852 Petrea volubilis Species 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000010419 fine particle Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 235000011868 grain product Nutrition 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000006835 compression Effects 0.000 claims description 2
- 238000007906 compression Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000000227 grinding Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- -1 condition Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The invention relates to a method for plating titanium nitride on a surface of a cubic boron nitride particle, which aims at solving the problems that the surface abrasive resistance of the cubic boron nitride is poor and the coating film is easy to fall off. According to the method, hexagonal boron nitride is taken as the raw material, lithium nitride is taken as the contact agent, titanium powder is taken as the coating material, the cubic boron nitride particle plated with titanium nitride is prepared from the raw materials through steps of grinding, mixing, assembling, synthesizing at high temperature under high pressure, plating film, acid pickling, washing, leaching and drying, so that the cubic boron nitride is plated with film while the single crystal grows. The method is advanced, data is full and accurate, single crystal is the product, the size of the crystal is less than or equal to 0.4mm, the thickness of the titanium nitride film is less than or equal to 500nm, the crystal has a cubic phase structure, the purity of the product reaches 98%, the surface Vickers hardness reaches Hv 4200, so that the method for plating titanium nitride on the surface of the cubic boron nitride particle is ideal.
Description
Technical field
The present invention relates to a kind of method of cubic boron nitride particle plated surface titanium nitride, belong to the technical field of cubic boron nitride particle surface treatment and synthetic method.
Background technology
Cubic boron nitride is a kind of nonmetallic materials of extreme hardness, has high hardness and good thermal conduction characteristic, not with iron family element and alloy reaction thereof, in field of machining, is that other removing materials are incomparable; Cubic boron nitride also has that energy gap is large, optical index is little, oxidizing temperature high, in automobile, space flight and aviation, microelectronic component, optics field, has obtained application.
Cubic boron nitride monocrystal is at HTHP, has under the condition that catalyst exists syntheticly, and in building-up process, due to the difference of raw material, condition, catalyst kind, additive, the color of synthetic cubic boron nitride, component ratio, performance also have difference; In order to improve wearability, electric conductivity and the non-oxidizability of cubic boron nitride in grinding, conventionally at METAL ALLOY BOND nickel, chromium or titanium; Film plating process mainly contains electrostatic spray spraying process, chemical vapor infiltration, vapour deposition process, utilizes chemical reaction to form one deck plated film on cubic boron nitride surface; But thickness, the uneven components of the cubic boron nitride coating that these methods obtain, the adhesion on plated film and cubic boron nitride crystal surface is little, and in grinding process, plated film easily comes off, and has affected greatly the grinding performance of cubic boron nitride.
Titanium is a kind of good enhancing jointing material, and titanium nitride is a kind of good additive especially, if do plating agent processing cubic boron nitride with titanium nitride, is a problem that urgency is to be studied.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology, adopt the catalyst that lithium nitride is synthesizing cubic boron nitride, titanium valve is that additive is done coating, cubic boron nitride is carried out coating, on cubic boron nitride surface, form rete, to increase substantially the surface mechanical properties 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, titanium valve, 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
Hexagonal boron nitride: 100 g ± 0.1 g
Lithium nitride: Li
3n 10 g ± 0.1 g
Titanium valve: Ti 4 g ± 0.1 g
Graphite-pipe: C Φ 12 mm * 12, mm * 0.5 mm
Graphite flake: C Φ 12 mm * 12, mm * 0.3 mm
Copper sheet: Cu Φ 12 mm * 0.1 mm
Conductive steel cap: 2 Φ 12 mm * 4, mm * 5 mm
Pyrophyllite block: Al
2[Si
4o
10] (OH)
226 mm * 24, mm * 26 mm
Dolomite sleeve pipe: CaMg[CO
3]
2Φ 16 mm * 14, mm * 1 mm
Pyrophillite ring: Al
2[Si
4o
10] (OH)
22 Φ 16 mm * 3, mm * 1 mm
Sulfuric acid: H
2sO
4100 mL ± 5 mL
Nitric acid: HNO
3300 mL ± 5 mL
Alcohol: C
2h
5oH 400 mL ± 5 mL
Deionized water: H
2o 1000 mL ± 5 mL
Sand paper: SiC 200 mm * 0.3, mm * 200 mm
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, concentration control:
Hexagonal boron nitride: solid powder 98 %
Lithium nitride: solid powder 96 %
Titanium valve: solid powder 99.9 %
Graphite-pipe: solid-state tubular 99 %
Graphite flake: solid-state disc-shaped 99 %
Copper sheet: solid-state disc-shaped 99 %
Conductive steel cap: solid cylindrical 99 %
Pyrophyllite block: solid block 95%
Dolomite sleeve pipe: solid-state tubulose 98 %
Pyrophillite ring: solid-state ring-type 95 %
Sulfuric acid: liquid strength of fluid 98 %
Nitric acid: liquid strength of fluid 68 %
Alcohol: liquid liquid 99.9 %
Deionized water: liquid liquid 99.9 %
Sand paper: solid-state paper shape
(2) solid powder material grinds, sieves
1. hexagonal boron nitride 100 g ± 0.1 agate mortar for g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037 mm;
2. lithium nitride 10 g ± 0.1 agate mortar for g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074 mm;
3. titanium valve 4 g ± 0.1 agate mortar for g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074 mm;
(3) preparation mixing fine powders
Hexagonal boron nitride 100 g ± 0.1 g, lithium nitride 10 g ± 0.1 g, titanium valve 4 g ± 0.1 g that grind, sieve are added in quartz container, then being placed in batch mixer mixes, batch mixer rotating speed is 100 r/min, and incorporation time is 300 min, 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 baking oven roasting, sintering temperature 200
oc ± 5
oc, roasting time 26 h, 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) processing graphite pipe, graphite flake
1. by the sand papering of graphite-pipe two ends, make surfacing, bright and clean;
2. the sand papering of graphite flake positive and negative, makes any surface finish;
(7) assembling pyrophyllite block and inner batch mixing fine powder thereof
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. conductive steel cap, pyrophillite ring under putting in pyrophyllite block bottom;
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 the batch mixing fine powder of preparation;
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;
(8) cubic boron nitride particle titanium-nitride 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 between the top hammer of bottom, rear portion and left part in the hyperbaric chamber of cubic hinge press;
2. other three top hammers of 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 5.2 GPa, the rate of rise 520 MPa/min;
4. open the heating system of cubic hinge press, the batch mixing fine powder in heating pyrophyllite block, heating-up temperature is 1600
oc ± 5
oc, firing rate 320
oc/min;
5. constant temperature and pressure 10 min in hyperbaric chamber of the batch mixing fine powder in pyrophyllite block;
Batch mixing fine powder generates cubic boron nitride monocrystal in high temperature, hyperbaric environment, and at cubic boron nitride crystal particle surface titanium-nitride;
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
oc, is down to normal pressure;
7. open hyperbaric chamber, take out the crystal grain product in pyrophyllite block;
(9) pickling, washing, alcohol washing
1. preparating acid dilution
Measure sulfuric acid 100 mL ± 5 mL, nitric acid 300 mL ± 5 mL are placed in beaker, are uniformly mixed, and become acid solution;
2. the beaker that fills acid solution is placed on electric heater, crystal grain product is added in beaker, heating stirring and pickling, heating-up temperature is 400
oc, pickling time 15 min;
3. the crystal grain after pickling is placed in to another beaker, adds deionized water 1000 mL, agitator treating 10 min;
4. the crystal grain after deionized water washing is placed in to another beaker, adds alcohol 400 mL, agitator treating 10 min, become 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 miillpore filter, retains product filter cake on filter membrane, 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
oc, vacuum is 10 Pa, drying times 15 min, the cubic boron nitride monocrystal body that dried product exhibited is titanium-nitride;
(12) detect, analyze, characterize
The pattern of the cubic boron nitride monocrystal body of titanium-nitride, color and luster, composition, Chemical Physics performance are detected, analyze, characterized;
With powder x-ray diffraction, carry out crystal material phase analysis;
By SEM, carry out crystal morphology analysis;
Conclusion: the cubic boron nitride monocrystal body of titanium-nitride is brown bulk crystals graininess, crystal grain size≤0.4 mm, titanium nitride film layer thickness≤500 nm, crystal has Emission in Cubic structure, and product purity reaches 98 %, and surperficial Vickers hardness reaches H
v4200;
(13) product stores
Cubic boron nitride monocrystal body particle to the titanium-nitride of preparation is stored in brown transparent glass container, and airtight lucifuge stores, and storage temperature is 20
oc, relative humidity≤10 %.
Beneficial effect
The present invention compares with background technology has obvious advance, for cubic boron nitride surface abrasion resistance and the caducous situation of plated film, employing hexagonal boron nitride is raw material, lithium nitride is synthetic catalyst, titanium valve is Coating Materials, through former abrasive lapping, batch mixing, assembling, through the synthetic preparation of HTHP, through plated film, pickling, washing, suction filtration, dry, make the cubic boron nitride particle of titanium-nitride, realized cubic boron nitride monocrystal growth carries out with plated film simultaneously, this preparation method's technique is advanced, informative data is accurate, product is monocrystalline, purity is high, reach 98 %, coating is firm, thickness of coating≤500 nm, case hardness is high, Vickers hardness reaches H
v4200, be the method for very good cubic boron nitride particle plated surface titanium nitride.
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 cubic boron nitride titanium-nitride product shape appearance figure
The cubic boron nitride crystal granule-morphology figure of Fig. 4 titanium-nitride
The cubic boron nitride monocrystal diffracted intensity collection of illustrative plates of Fig. 5 titanium-nitride
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, it is correct that each position annexation is wanted, 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, take milligram, millimeter, milliliter be measurement unit.
Pyrophyllite block is cuboid, at pyrophyllite block 1 inner bottom part, place the second conductive steel cap 6, on the top of the second conductive steel cap 6, it is the second copper sheet 12, the second copper sheet 12 tops are the second graphite flake 10, dolomite sleeve pipe 2, it in dolomite sleeve pipe 2, is graphite-pipe 3, on graphite-pipe 3 tops, being that the first graphite flake 9, the first graphite flake 9 tops are the first copper sheet 11, is 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 cubic boron nitride titanium-nitride product shape appearance figure, visible in figure, product is graininess crystal, and single crystal grain is many ribs shape.
Shown in Fig. 4, be the cubic boron nitride crystal granule-morphology figure of titanium-nitride, visible in figure, each crystal is irregular particle shape, is irregular stacking.
Shown in Fig. 5, cubic boron nitride monocrystal diffracted intensity collection of illustrative plates for titanium-nitride, visible in figure, ordinate is diffracted intensity, abscissa is the angle of diffraction 2 θ, and in figure, square and circles mark represent respectively (111), (200), (220) peak position of (111), (200), (220) peak position and the cubic boron nitride of titanium nitride from left to right.
Claims (2)
1. the method for a cubic boron nitride particle plated surface titanium nitride, it is characterized in that: the chemical substance material of use is: hexagonal boron nitride, lithium nitride, titanium valve, 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
Hexagonal boron nitride: 100 g ± 0.1 g
Lithium nitride: Li
3n 10 g ± 0.1 g
Titanium valve: Ti 4 g ± 0.1 g
Graphite-pipe: C Φ 12 mm * 12, mm * 0.5 mm
Graphite flake: C Φ 12 mm * 12, mm * 0.3 mm
Copper sheet: Cu Φ 12 mm * 0.1 mm
Conductive steel cap: 2 Φ 12 mm * 4, mm * 5 mm
Pyrophyllite block: Al
2[Si
4o
10] (OH)
226 mm * 24, mm * 26 mm
Dolomite sleeve pipe: CaMg[CO
3]
2Φ 16 mm * 14, mm * 1 mm
Pyrophillite ring: Al
2[Si
4o
10] (OH)
22 Φ 16 mm * 3, mm * 1 mm
Sulfuric acid: H
2sO
4100 mL ± 5 mL
Nitric acid: HNO
3300 mL ± 5 mL
Alcohol: C
2h
5oH 400 mL ± 5 mL
Deionized water: H
2o 1000 mL ± 5 mL
Sand paper: SiC 200 mm * 0.3, mm * 200 mm
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, concentration control:
Hexagonal boron nitride: solid powder 98 %
Lithium nitride: solid powder 96 %
Titanium valve: solid powder 99.9 %
Graphite-pipe: solid-state tubular 99 %
Graphite flake: solid-state disc-shaped 99 %
Copper sheet: solid-state disc-shaped 99 %
Conductive steel cap: solid cylindrical 99 %
Pyrophyllite block: solid block 95%
Dolomite sleeve pipe: solid-state tubulose 98 %
Pyrophillite ring: solid-state ring-type 95 %
Sulfuric acid: liquid strength of fluid 98 %
Nitric acid: liquid strength of fluid 68 %
Alcohol: liquid liquid 99.9 %
Deionized water: liquid liquid 99.9 %
Sand paper: solid-state paper shape
(2) solid powder material grinds, sieves
1. hexagonal boron nitride 100 g ± 0.1 agate mortar for g, pestle are ground, then with 400 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.037 mm;
2. lithium nitride 10 g ± 0.1 agate mortar for g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074 mm;
3. titanium valve 4 g ± 0.1 agate mortar for g, pestle are ground, then with 200 eye mesh screens, sieve, grind, sieving repeats, one-tenth fine powder, fine particle diameter≤0.074 mm;
(3) preparation mixing fine powders
Hexagonal boron nitride 100 g ± 0.1 g, lithium nitride 10 g ± 0.1 g, titanium valve 4 g ± 0.1 g that grind, sieve are added in quartz container, then being placed in batch mixer mixes, batch mixer rotating speed is 100 r/min, and incorporation time is 300 min, 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 baking oven roasting, sintering temperature 200
oc ± 5
oc, roasting time 26 h, 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) processing graphite pipe, graphite flake
1. by the sand papering of graphite-pipe two ends, make surfacing, bright and clean;
2. the sand papering of graphite flake positive and negative, makes any surface finish;
(7) assembling pyrophyllite block and inner batch mixing fine powder thereof
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. conductive steel cap, pyrophillite ring under putting in pyrophyllite block bottom;
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 the batch mixing fine powder of preparation;
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;
(8) cubic boron nitride particle titanium-nitride 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 between the top hammer of bottom, rear portion and left part in the hyperbaric chamber of cubic hinge press;
2. other three top hammers of 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 5.2 GPa, the rate of rise 520 MPa/min;
4. open the heating system of cubic hinge press, the batch mixing fine powder in heating pyrophyllite block, heating-up temperature is 1600
oc ± 5
oc, firing rate 320
oC/ min;
5. constant temperature and pressure 10 min in hyperbaric chamber of the batch mixing fine powder in pyrophyllite block;
Batch mixing fine powder generates cubic boron nitride monocrystal in high temperature, hyperbaric environment, and at cubic boron nitride crystal particle surface titanium-nitride;
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
oc, is down to normal pressure;
7. open hyperbaric chamber, take out the crystal grain product in pyrophyllite block;
(9) pickling, washing, alcohol washing
1. preparating acid dilution
Measure sulfuric acid 100 mL ± 5 mL, nitric acid 300 mL ± 5 mL are placed in beaker, are uniformly mixed, and become acid solution;
2. the beaker that fills acid solution is placed on electric heater, crystal grain product is added in beaker, heating stirring and pickling, heating-up temperature is 400
oc, pickling time 15 min;
3. the crystal grain after pickling is placed in to another beaker, adds deionized water 1000 mL, agitator treating 10 min;
4. the crystal grain after deionized water washing is placed in to another beaker, adds alcohol 400 mL, agitator treating 10 min, become 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 miillpore filter, retains product filter cake on filter membrane, 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
oc, vacuum is 10 Pa, drying times 15 min, the cubic boron nitride monocrystal body that dried product exhibited is titanium-nitride;
(12) detect, analyze, characterize
The pattern of the cubic boron nitride monocrystal body of titanium-nitride, color and luster, composition, Chemical Physics performance are detected, analyze, characterized;
With powder x-ray diffraction, carry out crystal material phase analysis;
By SEM, carry out crystal morphology analysis;
Conclusion: the cubic boron nitride monocrystal body of titanium-nitride is brown bulk crystals graininess, crystal grain size≤0.4 mm, titanium nitride film layer thickness≤500 nm, crystal has Emission in Cubic structure, and product purity reaches 98 %, and surperficial Vickers hardness reaches H
v4200;
(13) product stores
Cubic boron nitride monocrystal body particle to the titanium-nitride of preparation is stored in brown transparent glass container, and airtight lucifuge stores, and storage temperature is 20
oc, relative humidity≤10 %.
2. the method for a kind of cubic boron nitride particle plated surface titanium nitride according to claim 1, it is characterized in that: pyrophyllite block is cuboid, at pyrophyllite block (1) inner bottom part, place the second conductive steel cap (6), on the top of the second conductive steel cap (6), be the second copper sheet (12), the second copper sheet (12) top is the second graphite flake (10), dolomite sleeve pipe (2), in dolomite sleeve pipe (2), be graphite-pipe (3), on graphite-pipe (3) top, be the first graphite flake (9), the first graphite flake (9) top is the first copper sheet (11), in the first copper sheet (11), dolomite sleeve pipe (2) top is the first pyrophillite ring (7), the first conductive steel cap (5), in graphite-pipe (3), be batch mixing fine powder (4).
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