CN103880419A - Application of zirconium dioxide ceramic in production of hot press sintering diamond saw - Google Patents

Application of zirconium dioxide ceramic in production of hot press sintering diamond saw Download PDF

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Publication number
CN103880419A
CN103880419A CN201410044746.2A CN201410044746A CN103880419A CN 103880419 A CN103880419 A CN 103880419A CN 201410044746 A CN201410044746 A CN 201410044746A CN 103880419 A CN103880419 A CN 103880419A
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diamond
mould
saw blade
ceramic
zirconia ceramic
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李坤
施玉芬
李政
周学琴
沈建民
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YANGZHOU DENUOHONG SUPERHARD MATERIALS EQUIPMENT Co Ltd
Changzhou University
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YANGZHOU DENUOHONG SUPERHARD MATERIALS EQUIPMENT Co Ltd
Changzhou University
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Abstract

The invention discloses a zirconium dioxide ceramic fabrication mold applied to hot press sintering production of a metal diamond saw. The ceramic comprises the following components: 94.5-95.5% of ZrO2 and 4.5-5.5% of Y2O3. The hot press sintering diamond composite saw produced by the ceramic mold has the process characteristics of being poor in wettability with iron, nickel and copper-based metal or alloy, poor in adhesion, small in adhesive power between the saw and the ceramic mold, and easy to demold. In addition, the composite diamond saw produced by using the zirconium dioxide ceramic mold disclosed by the invention is high in flatness, good in uniformity and good in compactness.

Description

The application of zirconia ceramic in thermal pressing sintering diamond sawing sheet is produced
Technical field
Technical field under this patent is diamond tool production field, specially for the mould in (1) thermal pressing sintering diamond composite tool process and the bonding problem of diamond saw blade; (2) planeness of composite diamond saw blade and thickness evenness problem.
Technical background
Diamond disc is the main tool of mechanically resistant material (as pottery, silicon crystal, silicate cement, Wimet, glass etc.) cutting, polishing, and whole world consumption is huge.The production method of diamond disc mainly contains at present: hot pressed sintering, composite plating, composite chemical plating, vacuum brazing.Wherein composite chemical depositing process uses compound and other chemical assistants of a large amount of hypophosphites or boron, and wastewater treatment is cumbersome, easily causes problem of environmental pollution.The plating solution that composite plating process uses can reuse, pollutes relatively little, but due to the larger stress of production between matrix in electroplating process and coating, coating should not be too thick, and the harm causing in order to reduce stress, electroplating velocity can not be too high, and production efficiency is lower.Vacuum brazing is a kind of diamond tool production technology of being developed by Korea S in recent years.This technique is that metal large to chromium, tungsten, titanium etc. and diamond sticking power is plated on to diamond particles surface, with low melting point alloy, diamond particles is being brazed in to matrix.The method not only can be arranged diamond particles on request, and has improved the adhesive power of diamond particles and metallic matrix.But because technique is loaded down with trivial details, equipment investment is large, production efficiency is not high, and production cost is higher.In addition, the temperature of this technique is higher (950-1050 ℃) generally, can cause the decline of diamond intensity.Therefore now widely used diamond disc production technique is hot pressed sintering.Wherein comprise again that integrated hot pressed sintering and hot pressed sintering composite block are brazed in two kinds of methods of metallic matrix.Hot pressed sintering is that diamond particles is mixed with low melting point alloy powder, passes through pressure forming, becomes product with mold stack, pressure sintering, integer.This explained hereafter efficiency is high, and therefore production cost is lower.The subject matter existing when hot-pressing sintering technique is prepared diamond saw blade is: (1) hot-pressing sintering technique generally carries out 850 ℃ of left and right, under high temperature, the diffusion of atoms metal and the formation of metallic carbide easily cause saw blade and mould adhesion, easily cause mould or the cracked damage of saw blade in the time that saw blade and mould are peeled off.(2) micro amount of oxygen in the not high or atmosphere of sintering oven vacuum tightness makes graphite jig material all make mould be difficult to guarantee surface finish in hot environment oxidation corrosion and surface second crystallization alligatoring.
Approximately 2700 ℃ of the fusing points of zirconium dioxide material, hardness 9; Use temperature, higher than 1700 ℃, is widely used in the burner hearth of retort furnace.The metals such as this material and iron, cobalt, nickel, copper, tin, lead, zinc, antimony melt body and do not infiltrate, and are therefore also widely used in the molten steel outlet of steel melting furnace.
Summary of the invention
Extraordinary zirconia ceramic mould heat pressure SINTERING PRODUCTION diamond disc for this patent.Utilize the metals such as zirconia ceramic and nickel, copper, tin, iron not invade mutually profit, the bonding trouble of mould and diamond saw blade while having avoided high temperature sintering, guarantees the yield rate of producing.The hardness of this stupalith under the following hot environment of 900 degree is high, and the coefficient of expansion is little, and deformation is very little, high with die surface its smooth precision after polished finish of its making, can guarantee the smooth precision of produced diamond saw blade.
The composition of zirconia ceramic is selected: containing ZrO 2quality 94.5-95.5%; Containing Y 2o 3quality 4.5-5.5%.Die design as shown in Figure 1, Figure 2, Fig. 3, Fig. 4.Mould is divided into: pressure head, die sleeve, upper and lower backing metal, assembling screw rod.The manufacture craft of zirconia ceramic mould is as follows: ceramic powder is dry-pressing formed, come unstuck 2 hours through 600 ℃, 950 ℃ of pre-burnings 1 hour; The ceramic body of pre-burning is lathed to the biscuit of desired shape with wolfram varbide cutter, because have a certain proportion of contraction when biscuit Low fire ceramic, therefore biscuit size should be amplified according to shrinking percentage.Method of calculation are: ceramic die size/shrinking percentage.Biscuit again lamination is embedded in zirconium white microballon (diameter 0.5mm), and 1450 ℃ of sintering of high temperature become zirconia ceramic mould base for 2 hours.Through diamond cutter, refine becomes zirconia ceramic mould with bistrique again.
Diamond saw blade production technique is: mould and diamond saw blade base substrate superposeed from down to up successively according to Fig. 4, and wherein pressure head and die sleeve stacked assembling repeatedly, middle filling saw blade base.With screw rod, the mould assembling is fixed again, and in lifting and sintering oven, according to required processing condition pressure sintering, once can be fired multiple saw blades.
Metal-powder formula requires: in metallic matrix formula, can not contain the pure metal powders such as chromium, titanium, tungsten, zirconium, tantalum, molybdenum, niobium; But can contain carbide, the nitride powder of these metals.The alloy of these metals or its formation easily causes the bonding of saw blade and zirconium dioxide mould.If one or more these metal evaporations, in diamond powder particle surface, then are mixed with saw bit matrix metal-powder, do not affect the adhesivity of diamond saw blade and ceramic die in sintering process.
Accompanying drawing explanation
Fig. 1 is pressure head part side-looking (section) figure of zirconia ceramic mould.R1 is the radius of mould; R2 is pressure head radius, considers that sintering gained saw blade also needs to put the first edge on a knife or a pair of scissors, therefore R2 will be less times greater than the design radial of diamond saw blade.R1-R2 is die sleeve width; Be generally: 10-20mm.T1 is pressure head thickness, and T2 is bench height.Zirconia ceramic is more crisp, and tensile strength is relatively little, and therefore, T1 is that pressure head thickness is 10-20mm, and T2 is bench height 5mm.R3 is protruding taper round platform radius, and corresponding to saw blade axis pore radius, round platform tapering is between 10-20 °.Be convenient to the demoulding, in assembling process, be easy to align up and down simultaneously.
Fig. 2 is the pressure head part front view of zirconia ceramic mould.Interstitial hole is that screw rod penetrates hole, and radius is 5mm.The surface of upper push-down head is through polishing, polishing.Because zirconia ceramic is more crisp, R2 size should not be too large, is generally 50-150, less times greater than the design radial of diamond saw blade.Design margin is 0.5mm.
Fig. 3 is coat part front view and side-looking (section) figure of zirconia ceramic mould.External diameter is identical with the radius R 1 of mould; Internal diameter is identical with pressure head platform radius R 2, and tolerance+100 micron, to prevent that pottery from collapsing limit.The thickness of die sleeve is 2x R2.Inwall and upper and lower surface are through grinding and buffing.
Fig. 4 is the saw blade production and assembly figure of zirconia ceramic mould.Be two high-temperature steel cushion blocks up and down, to prevent that mould from being crushed by screw rod in assembling and lifting.Screw rod and nut material are 316L stainless steel, composition range C≤0.03, Si≤1.00, Mn≤2.00, P≤0.035, S≤0.03, Ni:12.0-15.0, Cr:16.0-18.0, Mo:2.0-3.0.Because saw blade thickness in hot pressed sintering process is because of the attenuation of metal-powder partial melting, total thickness can reduce, and the therefore hot pressing graphite cushion block with holes at Jia Yikuai center, top makes the lax screw rod can free-extension.
embodiment
Alloy powder is mixed with bortz powder, add binding agent, dry-pressing formed.Then, saw blade blank and zirconium dioxide mould are successively assembled from the bottom up according to Fig. 4.Concrete steps are: first mould pressure head is accurately placed on backing metal, places saw blade blank, then place die sleeve; Several layers under connecing according to above-mentioned: the order of mould pressure head → saw blade blank → die sleeve is placed, and finally lays metal pressure head.Metal screw is passed to stacking die hole, and prefastened with nut.The mould assembling is placed in to retort furnace, and the hot pressing graphite cushion block with holes at Jia Yikuai center, top, applies the pressure of setting from upper end, takes out the oxygen in retort furnace with vacuum pump, or displaces air in retort furnace with reducing gas.Again in suitable temperature sintering certain hour.Due to the metal-base diamond saw blade of sintering touch swollen coefficient much larger than zirconia ceramic mould, therefore, cooling after, between die sleeve and saw blade outer rim, substantially depart from, die sleeve is easily dismantled.
Just because of the expansion coefficient difference of saw blade and mould, in the temperature-fall period after sintering completes, between saw blade and mould, can produce the frictional stress between contact surface.Therefore,, while starting to lower the temperature, first pressure is laid down.
Select diamond and the metal-powder of varying particle size, it is the diamond saw blade that 0.2-3mm, diameter are 50-150mm that this patent can be produced thickness.
Because zirconia ceramic is more crisp, and processing difficulties, consider die life (frangible when the pressurization of major diameter pressure head) and cost economic and practical (production cost of mould), this patent is not suitable for producing the larger saw blade of diameter.
Embodiment
Example 1
Pressure head size: R1 is 60mm; R2 is 50mm, and design margin is 0.5mm, and interstitial hole R4 is 5mm, and R3 is 7mm, and round platform tapering is at 20 °.T1 is 15mm, and T2 is 5mm.
Die sleeve: external diameter is that R1 is 60mm, internal diameter R2 is that 50+0.1mm thickness is 10mm.
Backing metal: exradius R1 is 60mm, thickness 20mm, centre hole and pit mate with screw rod and nut.
Hot pressing graphite block: exradius R1 is 60mm, thickness 100mm, centre hole radius 10mm.
The batching per-cent of saw blade base substrate: Fe:22%; Cu:55%; Sn:8%; Ni:7%; Zn:4%; Titanium-gold-plating hard rock (12kg level, particle diameter 50/60): 4%.
Metal-powder and diamond powder are mixed, according to rosin/always expect that quality is 2/100, under stirring, add the alcohol containing 5% rosin, air-dry.Mixed powder is made to diameter 100mm through dry pressuring forming process, thickness respectively approximately 0.21,0.55, the base substrate of 1.08mm.According to the assembling of operation described in patent working mode and hot pressing die, and in vacuum sintering funace sintering.16 tons of pressure (pressure 20MPa).Be warmed up to 600 ℃ with 3 ℃/min, be incubated 1 hour, then be warmed up to 800 ℃ with 2 ℃/min, be incubated 40 minutes, naturally cooling is laid down pressure in the time of 750 ℃ of furnace temperature.While being cooled to approach room temperature, from retort furnace, taking out and assemble and split out saw blade.Saw blade and mould are without bonding phenomenon.Mould is without embrittlement and collapse limit.Smooth and the good concentricity of saw blade, after putting the first edge on a knife or a pair of scissors with silicon carbide sintered compact, through 5000 revs/min of tests without breakage.To with thickness be 0.20mm, 0.50mm and 1.00mm diamond saw blade under different rotating speeds, cut just and kerf width as following table:
Table 1 different thickness diamond saw blade cuts the kerf width (diamond saw thickness: 0.20mm, 0.50mm and 1.00mm) of corundum under different rotating speeds
Figure BDA0000464087500000041
Note: (1) corundum sample is the corundum plate of thickness 5mm.
(2) feeding speed is 0.2-1.0mm/min; When cutting, spray with water.Accumulative total was cut after 96 hours, and blade wear amount is less than 0.050mm.
(3) size of kerf width and blade clamp, planeness, right alignment also have relation.
Example 2
Pressure head size: R1 is 60mm; R2 is 50mm, and design margin is 0.5mm, and interstitial hole R4 is 5mm, and R3 is 7mm, and round platform tapering is at 20 °.T1 is 15mm, and T2 is 5mm.
Die sleeve: external diameter is that R1 is 60mm, internal diameter R2 is that 50+0.1mm thickness is 10mm.
Backing metal: exradius R1 is 60mm, thickness 20mm, centre hole and pit mate with screw rod and nut.
Hot pressing graphite block: exradius R1 is 60mm, thickness 100mm, centre hole radius 10mm.
The batching per-cent of saw blade base substrate: Fe:35%; Cu:50%; Sn:5%; Zn:4%; WC:6%; ; Chromium plating diamond (12kg level, particle diameter 50/60, with the preparation of argon ion sputtering deposition): 4%.
Metal-powder and diamond powder are mixed, according to rosin/always expect that quality is 2/100, under stirring, add the alcohol containing 5% rosin, air-dry.Mixed powder is made to diameter 100mm through dry pressuring forming process, and thickness is respectively 0.55,1.08, the base substrate of 1.61mm.According to the assembling of operation described in patent working mode and hot pressing die, and in vacuum sintering funace sintering.16 tons of pressure (pressure 20MPa).Be warmed up to 600 ℃ with 3 ℃/min, be incubated 1 hour, then be warmed up to 820 ℃ with 2 ℃/min, be incubated 40 minutes, naturally cooling is laid down pressure in the time of 700 ℃ of furnace temperature.While being cooled to approach room temperature, from retort furnace, taking out and assemble and split out saw blade.Saw blade and mould are without bonding phenomenon.Mould is without embrittlement and collapse limit.Smooth and the good concentricity of saw blade, after putting the first edge on a knife or a pair of scissors with silicon carbide sintered compact, through 5000 revs/min of tests without breakage.
Table 2 different thickness diamond saw blade cuts the kerf width (diamond saw thickness: 0.50mm, 1.00mm and 1.50mm) of corundum under different rotating speeds
Figure BDA0000464087500000051
Note: condition is identical with example 1.

Claims (4)

1. zirconia ceramic being made to mould produces for the hot pressed sintering of metal-base diamond saw blade.Group of ceramics becomes containing ZrO 2quality 94.5-95.5%; Containing Y 2o 3quality 4.5-5.5%.
2. the manufacture craft of zirconia ceramic mould: ceramic powder is dry-pressing formed, come unstuck 2 hours through 500-600 ℃, 950 ℃ of pre-burnings 1 hour; The ceramic body of pre-burning is lathed to the biscuit of desired shape with wolfram varbide cutter.Biscuit again lamination is embedded in zirconium white microballon (diameter 0.5mm), and high temperature 1450-1550 ℃ sintering becomes zirconia ceramic mould base for 2 hours.Through diamond cutter, refine becomes zirconia ceramic mould with bistrique again.
3. zirconia ceramic being made to mould produces for the hot pressed sintering of metal-base diamond composite block.Hot pressed sintering temperature is at 850 ° below C.Unit surface pressure is less than 40MPa.
4. the batching percentage range of saw blade base substrate: Fe:18-26%; Cu:40-60%; Sn:5-10%; Ni:5-9%; Zn:3-6%; Titanium-gold-plating hard rock (10-14kg level, 200 microns of particle diameter 5 –, diamond particle diameter used be no more than saw blade thickness 1/20): 3-7%.
CN201410044746.2A 2014-02-07 2014-02-07 Application of zirconium dioxide ceramic in production of hot press sintering diamond saw Pending CN103880419A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106827261A (en) * 2017-03-21 2017-06-13 刘合融 The preparation method of eolith ware and eolith ware obtained by this method
CN108097960A (en) * 2018-01-30 2018-06-01 河南涵信金刚石工具有限公司 A kind of small dimension carves saw blade hot pressing die

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101036945A (en) * 2006-03-14 2007-09-19 中南大学 Method for preparing saw blades suitable for Asia red stone material
CN101798217A (en) * 2010-02-04 2010-08-11 山东轻工业学院 Composite rare earth-stabilized zirconia-based multielement nano/micro composite ceramic tool and die material and preparation method thereof
CN102151904A (en) * 2011-05-06 2011-08-17 福建万龙金刚石工具有限公司 Diamond saw blade tool bit and production process thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101036945A (en) * 2006-03-14 2007-09-19 中南大学 Method for preparing saw blades suitable for Asia red stone material
CN101798217A (en) * 2010-02-04 2010-08-11 山东轻工业学院 Composite rare earth-stabilized zirconia-based multielement nano/micro composite ceramic tool and die material and preparation method thereof
CN102151904A (en) * 2011-05-06 2011-08-17 福建万龙金刚石工具有限公司 Diamond saw blade tool bit and production process thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106827261A (en) * 2017-03-21 2017-06-13 刘合融 The preparation method of eolith ware and eolith ware obtained by this method
CN108097960A (en) * 2018-01-30 2018-06-01 河南涵信金刚石工具有限公司 A kind of small dimension carves saw blade hot pressing die

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Application publication date: 20140625