CN103551080B - 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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- CN103551080B CN103551080B CN201310536406.7A CN201310536406A CN103551080B CN 103551080 B CN103551080 B CN 103551080B CN 201310536406 A CN201310536406 A CN 201310536406A CN 103551080 B CN103551080 B CN 103551080B
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- nitride
- boron nitride
- cubic boron
- titanium
- graphite
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 61
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 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
- 239000000463 material Substances 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005554 pickling Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910000831 Steel Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010959 steel Substances 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 22
- 239000010949 copper Substances 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 22
- 239000010459 dolomite Substances 0.000 claims description 17
- 229910000514 dolomite Inorganic materials 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 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
- 239000010936 titanium Substances 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 6
- 239000010419 fine particle Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 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
- 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
- 238000003860 storage Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 239000000203 mixture Substances 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
- 238000011049 filling Methods 0.000 claims description 2
- 239000012065 filter cake 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
- 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
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 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
- 239000007788 liquid Substances 0.000 description 8
- 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
- 230000015572 biosynthetic process 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
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- 238000003786 synthesis reaction 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, is that other removing materials are incomparable in field of machining; Cubic boron nitride also has that energy gap is large, optical index is little, oxidizing temperature high, obtains application in automobile, space flight and aviation, microelectronic component, optics field.
Cubic boron nitride monocrystal HTHP, have catalyst existent condition under synthesize, in building-up process, due to the difference of raw material, condition, catalyst kind, additive, the color of the cubic boron nitride of synthesis, component ratio, performance also have difference; In order to improve the wearability of cubic boron nitride in grinding, electric conductivity and non-oxidizability, usually 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 have impact on the grinding performance of cubic boron nitride greatly.
Titanium is a kind of excellent enhancing jointing material, and titanium nitride is a kind of excellent additive especially, if doing plating agent processing cubic boron nitride with titanium nitride is urgency problem to be studied.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology, lithium nitride is adopted to be the catalyst of synthesizing cubic boron nitride, titanium valve is that additive does coating, cubic boron nitride carries out coating, rete is formed on cubic boron nitride surface, 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, and it is as follows that its combination prepares consumption: with gram, millimeter, milliliter for 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 × 0.5 mm × 12 mm
Graphite flake: C Φ 12 mm × 0.3 mm × 12 mm
Copper sheet: Cu Φ 12 mm × 0.1 mm
Conductive steel cap: 2 Φ 12 mm × 5 mm × 4 mm
Pyrophyllite block: Al
2[Si
4o
10] (OH)
226 mm × 24, mm × 26 mm
Dolomite sleeve pipe: CaMg [CO
3]
2Φ 16 mm × 1 mm × 14 mm
Pyrophillite ring: Al
2[Si
4o
10] (OH)
22 Φ 16 mm × 1 mm × 3 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 × 200 mm × 0.3 mm
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry 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 tubular shape 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 liquid concentration 98 %
Nitric acid: liquid liquid concentration 68 %
Alcohol: liquid liquid 99.9 %
Deionized water: liquid liquid 99.9 %
Sand paper: solid-state paper-like
(2) solid powder ground material, sieve
1. by hexagonal boron nitride 100 g ± 0.1 g agate mortar, pestle grinding, then sieve with 400 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.037 mm;
2. by lithium nitride 10 g ± 0.1 g agate mortar, pestle grinding, then sieve with 200 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.074 mm;
3. by titanium valve 4 g ± 0.1 g agate mortar, pestle grinding, then sieve with 200 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.074 mm;
(3) mixing fine powders is prepared
Grinding, hexagonal boron nitride 100 g ± 0.1 g, lithium nitride 10 g ± 0.1 g that sieve, titanium valve 4 g ± 0.1 g are added in quartz container, then be placed in batch mixer to mix, batch mixer rotating speed is 100 r/min, and incorporation time is 300 min, becomes batch mixing fine powder after mixing;
(4) roasting pyrophyllite block, pyrophillite ring, dolomite sleeve pipe
Pyrophyllite block, pyrophillite ring, dolomite sleeve pipe are placed in 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, removing steel cap each position oxide layer;
(6) processing graphite pipe, graphite flake
1. by the sand papering of graphite-pipe two ends, surfacing, bright and clean is made;
2. the sand papering of graphite flake positive and negative, makes any surface finish;
(7) the batch mixing fine powder of pyrophyllite block and inside thereof is assembled
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. conductive steel cap, pyrophillite ring under putting bottom pyrophyllite block;
3. circular copper sheet is put on conductive steel cap top;
4. graphite flake, dolomite sleeve pipe, graphite-pipe is put on circular copper sheet top;
5. in graphite-pipe, put the batch mixing fine powder of preparation;
6. graphite flake is put on graphite-pipe top;
7. circular copper sheet is put on graphite flake top;
8. pyrophillite ring, conductive steel cap is put on circular copper sheet top;
(8) cubic boron nitride particle titanium-nitride carries out in the hyperbaric chamber of cubic hinge press, is in pyrophyllite block, completes under pressurization, heating, constant temperature keeping warm mode;
1. by between the top hammer of the parallel bottom moved in the hyperbaric chamber of cubic hinge press of batch mixing fine powder of the pyrophyllite block of assembling and inside, rear portion and left part;
2. other three top hammers of cubic hinge press are opened near pyrophyllite block, form six squeezed states;
3. open compression system, six of cubic hinge press top hammers are extruded pyrophyllite block, produce pressure and make pyrophillite internal pressure rise to 5.2 GPa gradually, 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. the batch mixing fine powder in pyrophyllite block is constant temperature and pressure 10 min in hyperbaric chamber;
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 terminates, stop heating, stop exerting pressure, make the pyrophyllite block in hyperbaric chamber and batch mixing fine powder 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, ethanol wash
1. preparating acid dilution
Measure sulfuric acid 100 mL ± 5 mL, nitric acid 300 mL ± 5 mL is placed in beaker, be uniformly mixed, become acid solution;
2. be placed on electric heater by the beaker filling acid solution, add in beaker by crystal grain product, heating stirring and pickling, heating-up temperature is 400
oc, pickling time 15 min;
3. the crystal grain after pickling is placed in another beaker, adds deionized water 1000 mL, agitator treating 10 min;
4. the crystal grain after deionized water being washed is placed in another beaker, adds alcohol 400 mL, agitator treating 10 min, becomes mixed solution;
(10) suction filtration
Mixed liquor after ethanol wash is placed in the Buchner funnel of bottle,suction, carries out suction filtration with miillpore filter, remaining product filter cake on filter membrane, cleaning solution is evacuated in filter flask;
(11) vacuum drying
Product cake is placed in quartz container, and be then placed in vacuum drying chamber dry, baking temperature is 200
oc, vacuum is 10 Pa, drying time 15 min, dried product exhibited is the cubic boron nitride monocrystal body of 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;
Crystal material phase analysis is carried out with powder x-ray diffraction;
Crystal morphology analysis is carried out by SEM;
Conclusion: the cubic boron nitride monocrystal body of titanium-nitride is brown bulk crystals graininess, and 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 storage
To the cubic boron nitride monocrystal body particle size of titanium-nitride of preparation in the glass container of amber transparent, airtight lucifuge stores, and storage temperature is 20
oc, relative humidity≤10 %.
Beneficial effect
The present invention has obvious advance compared with background technology, 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 raw mill, batch mixing, assembling, prepare through HP-HT synthesize, through plated film, pickling, washing, suction filtration, dry, the cubic boron nitride particle of obtained titanium-nitride, achieve cubic boron nitride monocrystal growth to carry 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 morphology 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.
Detailed description of the invention
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 wants correct, and proportioning is assembled, pushed up pressure according to the order of sequence according to quantity.
The value of the chemical substance needed for preparation determines by the scope pre-set, with milligram, millimeter, milliliter for measurement unit.
Pyrophyllite block is cuboid, the second conductive steel cap 6 is placed at pyrophyllite block 1 inner bottom part, be the second copper sheet 12 on the top of the second conductive steel cap 6, second copper sheet 12 top is the second graphite flake 10, dolomite sleeve pipe 2, it is graphite-pipe 3 in dolomite sleeve pipe 2, be the first graphite flake 9, first graphite flake 9 top on graphite-pipe 3 top being the first copper sheet 11, is the first pyrophillite ring 7, first conductive steel cap 5 on the first copper sheet 11, dolomite sleeve pipe 2 top; Be batch mixing fine powder 4 in graphite-pipe 3.
Shown in Fig. 3, be cubic boron nitride titanium-nitride product morphology figure, visible in figure, product is granular crystals, and single crystal grain is many prismatic.
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, in irregular stacking.
Shown in Fig. 5, for the cubic boron nitride monocrystal diffracted intensity collection of illustrative plates of 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 (111), (200), (220) peak position of (111), (200) of titanium nitride, (220) peak position and cubic boron nitride from left to right respectively.
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 its combination prepares consumption: with gram, millimeter, milliliter for measurement unit
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity, concentration control:
(2) solid powder ground material, sieve
1. by hexagonal boron nitride 100g ± 0.1g agate mortar, pestle grinding, then sieve with 400 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.037mm;
2. by lithium nitride 10g ± 0.1g agate mortar, pestle grinding, then sieve with 200 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.074mm;
3. by titanium valve 4g ± 0.1g agate mortar, pestle grinding, then sieve with 200 eye mesh screens, grind, sieving repeats, become fine powder, fine particle diameter≤0.074mm;
(3) mixing fine powders is prepared
Add in quartz container by grinding, the hexagonal boron nitride 100g ± 0.1g, the lithium nitride 10g ± 0.1g that sieve, titanium valve 4g ± 0.1g, be then placed in batch mixer and mix, batch mixer rotating speed is 100r/min, and incorporation time is 300min, becomes batch mixing fine powder after mixing;
(4) roasting pyrophyllite block, pyrophillite ring, dolomite sleeve pipe
Pyrophyllite block, pyrophillite ring, dolomite sleeve pipe are placed in baking oven roasting, sintering temperature 200 DEG C ± 5 DEG C, roasting time 26h, to remove moisture;
(5) polishing conductive steel cap
Two conductive steel caps are polished with sand paper respectively, removing steel cap each position oxide layer;
(6) processing graphite pipe, graphite flake
1. by the sand papering of graphite-pipe two ends, surfacing, bright and clean is made;
2. the sand papering of graphite flake positive and negative, makes any surface finish;
(7) the batch mixing fine powder of pyrophyllite block and inside thereof is assembled
1. rectangle pyrophyllite block is vertically placed on mechanical flat board;
2. conductive steel cap, pyrophillite ring under putting bottom pyrophyllite block;
3. circular copper sheet is put on conductive steel cap top;
4. graphite flake, dolomite sleeve pipe, graphite-pipe is put on circular copper sheet top;
5. in graphite-pipe, put the batch mixing fine powder of preparation;
6. graphite flake is put on graphite-pipe top;
7. circular copper sheet is put on graphite flake top;
8. pyrophillite ring, conductive steel cap is put on circular copper sheet top;
(8) cubic boron nitride particle titanium-nitride carries out in the hyperbaric chamber of cubic hinge press, is at leaf
In cured stone, complete under pressurization, heating, constant temperature keeping warm mode;
1. by between the top hammer of the parallel bottom moved in the hyperbaric chamber of cubic hinge press of batch mixing fine powder of the pyrophyllite block of assembling and inside, rear portion and left part;
2. other three top hammers of cubic hinge press are opened near pyrophyllite block, form six squeezed states;
3. open compression system, six of cubic hinge press top hammers are extruded pyrophyllite block, produce pressure and make pyrophillite internal pressure rise to 5.2GPa gradually, rate of rise 520MPa/min;
4. open the heating system of cubic hinge press, the batch mixing fine powder in heating pyrophyllite block, heating-up temperature is 1600 DEG C ± 5 DEG C, firing rate 320 DEG C/min;
5. the constant temperature and pressure 10min 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 terminates, stop heating, stop exerting pressure, make the pyrophyllite block in hyperbaric chamber and batch mixing fine powder be cooled to 25 DEG C, be down to normal pressure;
7. open hyperbaric chamber, take out the crystal grain product in pyrophyllite block;
(9) pickling, washing, ethanol wash
1. preparating acid dilution
Measure sulfuric acid 100mL ± 5mL, nitric acid 300mL ± 5mL is placed in beaker, be uniformly mixed, become acid solution;
2. be placed on electric heater by the beaker filling acid solution, add in beaker by crystal grain product, heating stirring and pickling, heating-up temperature is 400 DEG C, pickling time 15min;
3. the crystal grain after pickling is placed in another beaker, adds deionized water 1000mL, agitator treating 10min;
4. the crystal grain after deionized water being washed is placed in another beaker, adds alcohol 400mL, agitator treating 10min, becomes mixed solution;
(10) suction filtration
Mixed liquor after ethanol wash is placed in the Buchner funnel of bottle,suction, carries out suction filtration with miillpore filter, remaining product filter cake on filter membrane, cleaning solution is evacuated in filter flask;
(11) vacuum drying
Product cake is placed in quartz container, and be then placed in vacuum drying chamber dry, baking temperature is 200 DEG C, and vacuum is 10Pa, drying time 15min, dried product exhibited is the cubic boron nitride monocrystal body of 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;
Crystal material phase analysis is carried out with powder x-ray diffraction;
Crystal morphology analysis is carried out by SEM;
Conclusion: the cubic boron nitride monocrystal body of titanium-nitride is brown bulk crystals graininess, and crystal grain size≤0.4mm, titanium nitride film layer thickness≤500nm, crystal has Emission in Cubic structure, and product purity reaches 98%, and surperficial Vickers hardness reaches H
v4200;
(13) product storage
The cubic boron nitride monocrystal body particle size of the titanium-nitride of preparation is in the glass container of amber transparent, and airtight lucifuge stores, and storage temperature is 20 DEG C, 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, the second conductive steel cap (6) is placed at pyrophyllite block (1) inner bottom part, be the second copper sheet (12) on the top of the second conductive steel cap (6), second copper sheet (12) top is the second graphite flake (10), dolomite sleeve pipe (2), be graphite-pipe (3) in dolomite sleeve pipe (2), be the first graphite flake (9) on graphite-pipe (3) top, 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), first conductive steel cap (5), be batch mixing fine powder (4) in graphite-pipe (3).
Priority Applications (1)
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