CN103553637B - Cubic boron nitride glomerocryst composite with surface coating structure and preparation method thereof - Google Patents
Cubic boron nitride glomerocryst composite with surface coating structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of material machining, and particularly relates to a cubic boron nitride glomerocryst composite with a surface coating structure and a preparation method thereof. The composite is prepared by the following steps of firstly preparing mullite precursor sol; after aging and concentrating the sol, adding the sol into cubic boron nitride powder for in situ solation and gelation; drying and obtaining cubic boron nitride with a surface coating; mixing the cubic boron nitride with a binder, then pressing into test blocks, assembling the test blocks and transmission mediums into compound blocks, then sintering so as to obtain the cubic boron nitride glomerocryst composite with the surface coating structure. According to the preparation method for the cubic boron nitride glomerocryst composite with the surface coating structure, a layer of mullite chemical substance is coated on the surface of the cubic boron nitride, so that the chemical structure and composition of the surface of the cubic boron nitride are improved, and the impact toughness and cutting efficiency of the sintered glomerocryst cubic boron nitride composite are improved.
Description
Technical field
The invention belongs to machining field of material technology, particularly a kind of polycrystalline cubic boron nitride compound material with full-package structure and preparation method thereof.
Background technology
The bonding agent preparation that single crystal particle small for cubic boron nitride (cBN) can be bondd at high temperature under high pressure is utilized to become the PcBN(polycrystalline cubic boron nitride of block), there is due to polycrystalline cubic boron nitride the advantages such as the high-temperature behavior of high rigidity, high-wearing feature, high heat transfer efficiency and excellence, therefore, polycrystalline CBN cutting tool can be used to the cutter material making the difficult-to-machine metals such as quenched steel, cold hard cast-iron, superstrength iron group alloy, titanium alloy.
For improving cutting wear and working (machining) efficiency, employing polycrystalline CBN cutting tool substitutes inserted tool and sintex is the trend that ultra-hard cutting tool develops.Along with the progress of Materials science, the requirement of the hardness of cutter material, wear resistance, toughness and intensity is had higher requirement, desirable cutter material should both have high hardness, wear resistance, be conducive to improving stock-removing efficiency, extend tool life, the toughness simultaneously had again, makes it can bear large cutting force.If poor toughness, easily there is " collapsing cutter " phenomenon in use procedure, not only destroy workpiece to be machined, even occur the injury accident of infringement to equipment or operator, must the course of processing be stopped, the blade more renewed, cause production cost obviously to increase.
In order to overcome this deficiency, people start the toughness improving polycrystalline CBN cutting tool material.Patent WO2004040029 disclosed in Element Six company of Britain, the core adopting the mixture of various carbide and nitride to form a kind of complexity is scattered in matrix, superhard material cubic boron nitride and diamond is surrounded by matrix, and bonding agent, there is through high pressure-temperature synthesis a kind of polycrystalline cubic boron nitride of polynuclear plane, there is excellent intensity and fracture toughness property.Chinese patent CN201010542237.4 discloses a kind of plating nickel on surface Si
3n
4the preparation method of crystal whisker toughened polycrystalline cubic boron nitride compound sheets, adopts Si
3n
4the Si of whisker and coating surface nano nickel
3n
4the introducing of whisker increases the toughness of polycrystalline cubic boron nitride compound sheets, improves the impact resistance of cutter, thus realizes its turning continuously for a long time, improves the production efficiency of cutting-tool's used life and enterprise.Chinese patent 201010615047.0 also discloses a kind of powdery binder of polycrystalline cubic boron nitride compound sheets, includes TiN, AlN, Si
3n4, Co and SiO
2, the shock resistance of composite sheet can be strengthened.Chinese patent 201110325539.0 is by utilizing the high tenacity of body material W-Co kind Wimet, sexually revise the powder content of high tenacity W-Co kind hard alloy substrate in the glomerocryst layer chemical gradient of polycrystalline cubic boron nitride, and adopt the crystal whisker reinforced and toughened overall flexibility improving sintered polycrystalline cubic boron nitride composite piece of inorganic non-metallic.
Summary of the invention
The object of this invention is to provide a kind of new thinking, undertaken coated by cubic boron nitride, thus polycrystalline cubic boron nitride matrix material that a kind of high tenacity is provided and preparation method thereof.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of polycrystalline cubic boron nitride compound material with full-package structure, obtained by laxative remedy: first prepare mullite precursor colloidal sol, add in cubic boron nitride powder after colloidal sol ageing is concentrated and carry out original position solation and gelation, obtain after dry and there is surface coated cubic boron nitride; Suppress test block after it being mixed with binding agent, then be assembled into Synthetic block with transmission medium, sintering obtains the polycrystalline cubic boron nitride compound material with full-package structure afterwards.
The method preparing mullite precursor colloidal sol is as follows: aluminum contained compound, silicon-containing compound and catalyzer and water mixed and carry out polyreaction, obtains described mullite precursor colloidal sol.
Aluminum contained compound and silicon-containing compound are according to mullite chemical composition 3Al
2o
32SiO
2stoichiometric equation sets the proportioning added, the amount of substance that water adds is aluminum contained compound, the 5-16 of both silicon-containing compounds amount of substance summation doubly, the amount that catalyzer adds with adjusted to ph for 2 ~ 3.
Aluminum contained compound is selected from one or more the mixture in aluminium powder, aluminum isopropylate, aluminum chloride and aluminum nitrate; Described silicon-containing compound is tetraethoxy; The preferred hydrochloric acid of described catalyzer or acetic acid.
Wherein, aluminum contained compound is aluminium source, and silicon-containing compound is silicon source.The condition of polyreaction is as follows: time 2-72h, temperature of reaction 30 ~ 60 DEG C.
Mullite precursor colloidal sol is 50 ~ 60
othe ageing that C carries out 10 ~ 24 hours concentrates, and when adding in cubic boron nitride powder, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40 ~ 60:60-40.
When colloidal sol ageing concentrates, temperature can have upper and lower 1 DEG C floating.
Original position solation process temperature is 60 ~ 65 DEG C, and time controling was at 2 ~ 8 hours; Gelling temperature is 65 ~ 120 DEG C, and time controling was at 4 ~ 12 hours.Solation and gelling temperature can have upper and lower 1-2 DEG C floating.
Described cubic boron nitride powder is made up of the cubic boron nitride micro mist of the size distribution of following mass percent: 1-4 μm accounts for 42 ~ 45%, 7-10 μm and account for 35 ~ 50%, 12-15 μm and account for 5 ~ 20%.
Have surface coated cubic boron nitride when mixing with binding agent, both mass fractions are as follows: have surface coated cubic boron nitride 25-90 part, binding agent 2-25 part; Preferably there is surface coated cubic boron nitride 75-83 part, binding agent 17-25 part.
Described binding agent is one or more the mixture in metal cobalt powder, metal nickel powder, titanium nitride, aluminium nitride, titanium carbide, wolfram varbide.
The mixture of binding agent preferable alloy cobalt powder and titanium nitride.Both are preferably 6-12 part at ratio: 7-14 part.
The best purity of binding agent is all greater than 99%, and particle diameter is not more than 10 μm.
The test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then puts the salt pipe installed into graphite jig, and finally load agalmatolite cavity, end socket, is assembled into Synthetic block.
Matrix material adopts cubic pressure machine equipment to synthesize, and pressure is 4.6 ~ 7.0 GPa, temperature 1300 ~ 1600 DEG C, generated time 6 ~ 35 minutes.
Concrete, step prepared by material of the present invention is as follows:
1) will the aluminum contained compound in aluminium source be provided, provide the silicon-containing compound in silicon source and catalyzer to mix in water medium according to the proportioning of reaction setting, to join in polymerization reaction kettle and at 30-60 DEG C reactive polymeric 2 ~ 72 hours, obtain transparent mullite precursor colloidal sol.
2) the mullite precursor colloidal sol in step 1) is carried out ageing at 50 ~ 60 DEG C to concentrate, then the cubic boron nitride powder after purifying treatment is added, again through original position solation process and gelation, dry the cubic boron nitride obtaining Surface coating one deck mullite chemical composition.
3) by step 2) in the cubic boron nitride that obtains and binding agent mix according to different massfraction ratios respectively, be pressed into test block.
4) test block of step 3) compression moulding and transmission medium are assembled into Synthetic block, obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.
The present invention adopts sol-gel method technique, sol-gel method in-situ polymerization can make cubic boron nitride powder dispersed and mixing in the liquid phase, the effective coated one deck mullite Chemical Composition in surface can be made at low temperatures, improve surface chemical structure and the composition of cubic boron nitride, improve toughness and the stock-removing efficiency of the PcBN of preparation, extend work-ing life.
The cutter be processed into is for processing following material: the workpiece material of main more than workhardness HRC45, as, high rigidity such as various graphitic cast iron, quenched steel, superalloy, high-cobalt hart metal, surface spraying material, black powder sintering metal, titanium alloy, pure nickel, pure tungsten, wear-resisting etc. are difficult to carry out with universal cutter the workpiece material processed.
Compared with prior art, tool has the following advantages in the present invention:
The preparation method that the present invention has a polycrystalline cubic boron nitride compound material of full-package structure makes the material of cubic boron nitride Surface coating one deck mullite chemical composition, improve surface chemical structure and the composition of cubic boron nitride, improve toughness and the stock-removing efficiency of the polycrystalline cubic boron nitride matrix material of sintering.
Embodiment
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited thereto:
Embodiment 1
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) aluminum nitrate 0.30 mole taken containing 9 crystal water is measured, aluminum isopropylate 0.30 mole, tetraethoxy 0.2 mole, add 12.4 moles, water, adding hydrochloric adjusted to ph is 2, react under the temperature condition of 60 ± 1 DEG C, be polymerized 22 hours, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 10 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 42% to 4 micrometer ranges, 7 microns account for 45% to 10 micrometer ranges, and 12 microns account for 13% to 15 micrometer ranges.Above-mentioned cubic boron nitride powder after purifying treatment is joined in precursor sol, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40/60, again through original position solation process and gelation, the insulation of original position solation process is at 60 ± 1 DEG C, time controling was at 5 hours, gelling temperature is at 95 ± 2 DEG C, and time controling, at 8 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 83%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 10% and 7%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.6 GPa, temperature 1450 DEG C, generated time 6 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7410, and impelling strength is 722 times, and three-point bending method test bending strength is 781MPa.
Embodiment 2
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) measure the aluminum nitrate 0.30 mole taken containing 9 crystal water, aluminum isopropylate 0.30 mole, tetraethoxy 0.2 mole, adds 12.4 moles, water, and adding hydrochloric adjusted to ph is 2.5,60 ± 1
oreact under the temperature condition of C, be polymerized 25 hours, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 10 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 45% to 4 micrometer ranges, 7 microns account for 40% to 10 micrometer ranges, and 12 microns account for 15% to 15 micrometer ranges.Above-mentioned cubic boron nitride powder after purifying treatment is joined in precursor sol, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40/60, again through original position solation process and gelation, the insulation of original position solation process is at 60 ± 1 DEG C, time controling was at 5 hours, gelling temperature is at 90 ± 2 DEG C, and time controling, at 10 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 83%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 6% and 11%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.3 GPa, temperature 1500 DEG C, generated time 8 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7230, and impelling strength is 732 times, and three-point bending method test bending strength is 805MPa.
Embodiment 3
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) aluminum nitrate 0.30 mole taken containing 9 crystal water is measured, aluminum isopropylate 0.30 mole, tetraethoxy 0.2 mole, add 12.4 moles, water, adding hydrochloric adjusted to ph is 2, react under the temperature condition of 60 ± 1 DEG C, be polymerized 22 hours, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 10 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 42% to 4 micrometer ranges, 7 microns account for 45% to 10 micrometer ranges, and 12 microns account for 13% to 15 micrometer ranges.Join in precursor sol by the above-mentioned cubic boron nitride powder after purifying treatment, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 50/50, then through original position solation process and gelation, the insulation of original position solation process is 65 ± 1
oc, time controling was at 5 hours, and gelling temperature is 90 ± 2
oc, time controling, at 10 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 75%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 11% and 14%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.3 GPa, temperature 1500 DEG C, generated time 8 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7160, and impelling strength is 783 times, and three-point bending method test bending strength is 825MPa.
Embodiment 4
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) metering takes aluminium powder 0.30 mole, containing the aluminum nitrate 0.08 mole of 9 crystal water, tetraethoxy 0.076 mole, add 5.5 moles, water, adding hydrochloric adjusted to ph is 2, react under the temperature condition of 55 ± 1 DEG C, polyase 13 0 hour, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 15 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 45% to 4 micrometer ranges, 7 microns account for 48% to 10 micrometer ranges, and 12 microns account for 7% to 15 micrometer ranges.Join in precursor sol by the cubic boron nitride powder after purifying treatment, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40/60, then through original position solation process and gelation, the above-mentioned solation process insulation of original position is 65 ± 1
oc, time controling was at 5 hours, and gelling temperature is 100 ± 2
oc, time controling, at 8 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 83%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 6% and 11%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.3 GPa, temperature 1500 DEG C, generated time 8 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7580, and impelling strength is 764 times, and three-point bending method test bending strength is 891MPa.
Embodiment 5
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) metering takes aluminium powder 0.38 mole, and containing 0.10 mole, the aluminum chloride of 6 crystal water, tetraethoxy 0.056 mole, adds 5.5 moles, water, and adding hydrochloric adjusted to ph is 2.5,50 ± 1
oreact under the temperature condition of C, polyase 13 5 hours, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 15 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 42% to 4 micrometer ranges, 7 microns account for 45% to 10 micrometer ranges, and 12 microns account for 13% to 15 micrometer ranges.Join in precursor sol by the above-mentioned cubic boron nitride powder after purifying treatment, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 50/50, then through original position solation process and gelation, the insulation of original position solation process is 60 ± 1
oc, time controling was at 5 hours, and gelling temperature is 100 ± 2
oc, time controling, at 8 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 83%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 10% and 7%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.3 GPa, temperature 1500 DEG C, generated time 6 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7260, and impelling strength is 747 times, and three-point bending method test bending strength is 832MPa.
Embodiment 6
There is a polycrystalline cubic boron nitride compound material for full-package structure, obtained by laxative remedy:
(1) metering takes aluminium powder 0.38 mole, and containing 0.10 mole, the aluminum chloride of 6 crystal water, tetraethoxy 0.056 mole, adds 5.5 moles, water, and adding hydrochloric adjusted to ph is 2,55 ± 1
oreact under the temperature condition of C, polyase 13 0 hour, obtain transparent mullite precursor colloidal sol;
(2) by the mullite precursor colloidal sol in step (1), warp is 60 ± 1
othe ageing that C carries out 10 hours concentrates.Select the admixed finepowder of three kinds of particle diameter cubic boron nitrides, massfraction ratio in each comfortable admixed finepowder of cubic boron nitride of different-grain diameter is: 1 micron accounts for 42% to 4 micrometer ranges, 7 microns account for 40% to 10 micrometer ranges, and 12 microns account for 18% to 15 micrometer ranges.Join in precursor sol by the above-mentioned cubic boron nitride powder after purifying treatment, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40/60, then through original position solation process and gelation, the insulation of original position solation process is 65 ± 1
oc, time controling was at 6 hours, and gelling temperature is 90 ± 2
oc, time controling, at 10 hours, obtains the cubic boron nitride of Surface coating one deck mullite chemical composition after oven dry.
(3) cubic boron nitride micro mist accounts for the massfraction ratio of raw material micro mist is 75%, and the massfraction ratio that cementing metal cobalt powder and titanium nitride account for raw material micro mist is respectively 12% and 13%.Above-mentioned raw materials micro mist is mixed in setting ratio, and is pressed into test block.
(4) test block of compression moulding is put in the molybdenum cup of salt tube shield layer isolation, then put the salt pipe installed into graphite jig, finally load agalmatolite cavity, end socket, be assembled into Synthetic block, dry in baking oven, then obtain polycrystalline cubic boron nitride by high pressure high temperature sintering.The actual conditions of sintering adopts cubic pressure machine equipment to synthesize, and pressure is 5.6 GPa, temperature 1450 DEG C, generated time 6 minutes.
The polycrystalline cubic boron nitride matrix material microhardness that aforesaid method prepares is HV7060, and impelling strength is 689 times, and three-point bending method test bending strength is 843MPa.
Claims (9)
1. one kind has the polycrystalline cubic boron nitride compound material of full-package structure, it is characterized in that, obtained by laxative remedy: first prepare mullite precursor colloidal sol, add in cubic boron nitride powder after colloidal sol ageing is concentrated and carry out original position solation and gelation, obtain after dry and there is surface coated cubic boron nitride; Suppress test block after it being mixed with binding agent, then be assembled into Synthetic block with transmission medium, sintering obtains the polycrystalline cubic boron nitride compound material with full-package structure afterwards;
The method preparing mullite precursor colloidal sol is as follows: be incorporated in 30-60 DEG C of polyreaction 2-72h obtain described mullite precursor colloidal sol by mixed to aluminum contained compound, silicon-containing compound and catalyzer and water; The amount of substance that water adds is aluminum contained compound, the 5-16 of both silicon-containing compounds amount of substance summation times;
When adding in cubic boron nitride powder, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40 ~ 60:60-40.
2. one kind has the preparation method of the polycrystalline cubic boron nitride compound material of full-package structure, it is characterized in that, first prepare mullite precursor colloidal sol, add in cubic boron nitride powder after colloidal sol ageing is concentrated and carry out original position solation and gelation, obtain after dry and there is surface coated cubic boron nitride; Suppress test block after it being mixed with binding agent, then be assembled into Synthetic block with transmission medium, sintering obtains the polycrystalline cubic boron nitride compound material with full-package structure afterwards;
The method preparing mullite precursor colloidal sol is as follows: be incorporated in 30-60 DEG C of polyreaction 2-72h obtain described mullite precursor colloidal sol by mixed to aluminum contained compound, silicon-containing compound and catalyzer and water; The amount of substance that water adds is aluminum contained compound, the 5-16 of both silicon-containing compounds amount of substance summation times;
When adding in cubic boron nitride powder, in cubic boron nitride powder and colloidal sol, the mass ratio of solid matter is 40 ~ 60:60-40.
3. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 2, it is characterized in that, aluminum contained compound is selected from one or more the mixture in aluminum isopropylate, aluminum chloride and aluminum nitrate; Described silicon-containing compound is tetraethoxy; Described catalyzer is hydrochloric acid or acetic acid.
4. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 2, it is characterized in that, mullite precursor colloidal sol concentrates 10-24h 50 ~ 60 DEG C of ageings.
5. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 4, it is characterized in that, original position solation process temperature is 60 ~ 65 DEG C, and time controling was at 2 ~ 8 hours, gelling temperature is 65 ~ 120 DEG C, and time controling was at 4 ~ 12 hours.
6. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 4, it is characterized in that, described cubic boron nitride powder is made up of the cubic boron nitride micro mist of the size distribution of following mass percent: 1-4 μm accounts for 42 ~ 45%, 7-10 μm accounts for 35 ~ 50%, 12-15 μm and accounts for 5 ~ 20%.
7. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 2, it is characterized in that, there is surface coated cubic boron nitride when mixing with binding agent, both mass fractions are as follows: have surface coated cubic boron nitride 25-90 part, binding agent 2-25 part.
8. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 7, it is characterized in that, described binding agent is one or more the mixture in metal cobalt powder, metal nickel powder, titanium nitride, aluminium nitride, titanium carbide, wolfram varbide.
9. a kind of preparation method with the polycrystalline cubic boron nitride compound material of full-package structure as claimed in claim 2, it is characterized in that, matrix material adopts cubic pressure machine equipment to synthesize, and pressure is 4.6 ~ 7.0 GPa, temperature 1300 ~ 1600 DEG C, generated time 6 ~ 35 minutes.
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| CN102505090A (en) * | 2011-10-21 | 2012-06-20 | 中原工学院 | Preparation method of high-toughness polycrystalline cubic boron nitride compound sheets |
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| US4353714A (en) * | 1981-10-26 | 1982-10-12 | General Electric Company | Polycrystalline silicon-bonded cubic boron nitride body and method |
| US5320988A (en) * | 1988-11-10 | 1994-06-14 | General Electric Company | Process for preparing polycrystalline CBN ceramic masses and resulting product |
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| CN102505090A (en) * | 2011-10-21 | 2012-06-20 | 中原工学院 | Preparation method of high-toughness polycrystalline cubic boron nitride compound sheets |
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