CN111390182A - Diamond tool preparation process based on warm compaction - Google Patents
Diamond tool preparation process based on warm compaction Download PDFInfo
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B22—CASTING; POWDER METALLURGY
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B22F9/00—Making metallic powder or suspensions thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
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Abstract
The invention relates to the technical field of preparation of diamond tools, in particular to a preparation process of a diamond tool based on warm compaction forming. A preparation process of a diamond tool based on warm compaction forming comprises the following steps: step A, heating and kneading matrix alloy powder and a flowing warm-pressing water-based binder, and then granulating to prepare matrix alloy feed; step B, performing warm-pressing molding on the tire body alloy feed to obtain a tire body alloy blank; and step C, carrying out dipping degreasing and drying treatment on the matrix alloy blank. The invention aims to provide a diamond tool preparation process based on warm compaction, and the prepared diamond tool has the advantages of small sintered blank shrinkage, high dimensional precision, high density, improved bending strength and hardness, high yield and capability of manufacturing diamond tools with large sizes and complex shapes.
Description
Technical Field
The invention relates to the technical field of preparation of diamond tools, in particular to a preparation process of a diamond tool based on warm compaction forming.
Background
The traditional diamond tool manufacturing process mainly adopts a hot-pressing sintering forming process, firstly, matrix alloy powder is pre-pressed and formed into a matrix alloy blank in a cold press, then the matrix alloy blank is put into a graphite die to be heated and pressurized and sintered in a hot-pressing sintering furnace, the method can only produce the diamond tool with a simple section shape, and the sintering furnace usually needs repeated heating and cooling for many times, so that the energy consumption is large, the production efficiency is low, the loss of the graphite die is large, the environmental pollution is serious, the production cost is high, and the quality is unstable. At present, diamond tools are produced by adopting powder metallurgy injection molding and extrusion molding methods, and products with complex geometric shapes can be produced. However, powder metallurgy injection molding and extrusion molding require a large amount of binder to be added into matrix alloy powder to prepare matrix alloy feed, so that the fluidity of the matrix alloy feed can meet the requirements of injection molding and extrusion molding, and generally, the addition amount (mass percentage) of the binder in the matrix alloy feed is 9-15%, and the volume ratio (V) isBinder/VFeeding materials) 60-70%, because the addition of the binder is large, the difficulty of the subsequent degreasing process is increased, the degreasing time is long, the requirement on the temperature rise rate is high, the degreasing difficulty is high, bubbles and internal cracks are easily generated in the blank in the degreasing process, the blank can burst when the blank is serious, and the quality of the prepared diamond tool is greatly influenced.
Disclosure of Invention
The invention aims to provide a diamond tool preparation process based on warm compaction, and the prepared diamond tool has the advantages of small sintered blank shrinkage, high dimensional precision, high density, improved bending strength and hardness, high yield and capability of manufacturing diamond tools with large sizes and complex shapes.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of a diamond tool based on warm compaction forming comprises the following steps:
step A, heating and kneading matrix alloy powder and a flowing warm-pressing water-based binder, and then granulating to prepare matrix alloy feed;
step B, performing warm-pressing molding on the tire body alloy feed to obtain a tire body alloy blank;
step C, dipping, degreasing and drying the blank of the tire body alloy;
d, carrying out rapid heating vacuum thermal degreasing and hydrogen reduction pressure sintering on the matrix alloy blank treated in the step C to prepare a diamond tool based on warm compaction;
the raw material of the flowing warm-pressing water-based adhesive comprises a viscoelastic polymer.
Preferably, the raw materials of the flowing warm-pressing water-based binder comprise, by mass: 30-50% of water-soluble binder, 5-30% of rigid high polymer, 30-50% of viscoelastic polymer and 1-10% of assistant.
Preferably, the water-soluble binder is polyethylene glycol, and the polymerization degree of the polyethylene glycol is 1500-2500;
the rigid high molecular polymer is any one or a mixture of more of polyformaldehyde, polymethyl methacrylate and polybutyl methacrylate;
the viscoelastic polymer is any one or a mixture of more of vinyl acetate, polyvinyl butyral and random polypropylene;
the auxiliary agent is any one or a mixture of more of paraffin, stearic acid and dioctyl phthalate.
Preferably, the step a specifically includes:
step A1, adding 92-95% of matrix alloy powder and 5-8% of flowing warm-pressing water-based binder into a kneader according to mass percentage, heating and kneading for 1h at 140 ℃, and then cooling to prepare a kneaded feed;
and step A2, putting the kneaded feed into a crusher for crushing and granulating to prepare the matrix alloy feed.
Preferably, in the step B, the warm-pressing temperature of the warm-pressing forming is 50-200 ℃, the warm-pressing pressure is 1-3 tons/square centimeter, and the pressure maintaining time is 15-30 s.
Preferably, the matrix alloy powder comprises, by mass, 70-85% of metal pre-alloy powder, 5-10% of WC powder, 5-11% of Ni powder, 2-4% of Sn powder and 3-5% of diamond particles;
the components of the metal pre-alloy powder comprise 70% of Fe and 30% of Cu according to mass percentage, and the particle size of the metal pre-alloy powder is less than 2 mu m;
the grain diameters of the WC powder, the Ni powder and the Sn powder are respectively less than 5 mu m.
Preferably, the particle size of the diamond particles is 0.2-0.4 mm.
Preferably, in the step C, the dipping and degreasing is to soak the blank of the tire body alloy in a mixed solution of one or more of water, ethanol, aliphatic ketone or aromatic hydrocarbon at a constant temperature of 25 ℃ for 1-2 hours.
Preferably, in the step C, the drying treatment is to take out the dipped and degreased blank of the tire body alloy, dry the blank in the air for 20 to 30min, and then dry the blank in the vacuum for 20 to 30min at the temperature of 40 ℃ and the vacuum degree of 1000 Pa.
Preferably, the step D specifically includes:
step D1, placing the tire body alloy blank processed in the step C in a vacuum pressure sintering furnace, heating from room temperature to 450 ℃ at the heating rate of 150 ℃/h under the vacuum degree of 1Pa, preserving heat for 0.5h, and carrying out rapid heating vacuum thermal degreasing;
d2, heating the vacuum pressure sintering furnace from 450 ℃ to 550 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing hydrogen, controlling the pressure in the furnace to be 0.1035MPa, and performing hydrogen deoxidation and reduction;
step D3, heating the vacuum pressure sintering furnace from 550 ℃ to 950 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing argon gas, controlling the pressure in the furnace to be 9.6MPa, and carrying out vacuum pressure sintering;
and D4, naturally cooling the vacuum pressure sintering furnace to 100 ℃ under the condition that the pressure in the furnace is kept at 9.6MPa, opening the furnace door, and discharging to obtain the diamond tool based on warm compaction.
Compared with the prior art, the invention has the following beneficial effects:
the invention kneads the matrix alloy powder and the flowing warm-pressing water-based binder into the matrix alloy feed by heating, because the raw material of the flowing warm-pressing water-based binder comprises viscoelastic polymer, the creep temperature of the viscoelastic polymer is wide, the low-temperature creep fluidity and the plasticity are good, the using amount of the flowing warm-pressing water-based binder in the matrix alloy feed can be reduced by using the forming process of warm-pressing forming, the requirement of the warm-pressing forming on the fluidity of the matrix alloy feed can be met, the matrix alloy feed is subjected to warm-pressing forming to obtain the matrix alloy blank, the matrix alloy blank is subjected to dipping degreasing and drying treatment, and then is subjected to rapid temperature rise vacuum thermal degreasing and hydrogen reduction pressure sintering, thereby solving the problems that the traditional dry-pressing forming process has low efficiency and can not produce products with complex shapes, meanwhile, the problems that the feeding adhesive for injection molding and extrusion molding is large in addition amount, the degreasing process is complex, the degreasing time is long, and defects are easily generated in the tire body are solved, the sintered blank of the prepared diamond tool is small in shrinkage rate, high in size precision, high in density, high in hardness and breaking strength, high in yield and capable of being used for manufacturing diamond tools with large sizes and complex shapes.
Detailed Description
A preparation process of a diamond tool based on warm compaction forming comprises the following steps:
step A, heating and kneading matrix alloy powder and a flowing warm-pressing water-based binder, and then granulating to prepare matrix alloy feed;
step B, performing warm-pressing molding on the tire body alloy feed to obtain a tire body alloy blank;
step C, dipping, degreasing and drying the blank of the tire body alloy;
d, carrying out rapid heating vacuum thermal degreasing and hydrogen reduction pressure sintering on the matrix alloy blank treated in the step C to prepare a diamond tool based on warm compaction;
the raw material of the flowing warm-pressing water-based adhesive comprises a viscoelastic polymer.
The warm-pressing molding is a molding method between injection molding, extrusion molding and dry-pressing molding, in order to ensure the fluidity of the feed, a large amount of binder must be added in the feed, so that the degreasing of a blank with larger volume and thickness is very difficult, the yield is low, and waste products are easily generated due to long degreasing time. The dry pressing formed feed has poor flowability, uneven pressure inside the blank, poor density and strength of the sintered product, and the shape of the product is limited, so that only products with simple shapes can be manufactured. Heating and kneading the matrix alloy powder and the flowing warm-pressing water-based binder to form the matrix alloy feed, wherein the raw material of the flowing warm-pressing water-based binder comprises a viscoelastic polymer, the viscoelastic polymer has wide creep temperature and good low-temperature creep fluidity and plasticity, the use amount of the flowing warm-pressing water-based binder in the matrix alloy feed can be reduced by using a warm-pressing forming process, the requirement of warm-pressing forming on the fluidity of the matrix alloy feed can be met, the matrix alloy feed is subjected to warm-pressing forming to obtain a matrix alloy blank, the matrix alloy blank is subjected to dipping degreasing and drying treatment, and then subjected to rapid temperature rise vacuum thermal degreasing and hydrogen reduction pressure sintering, so that the problems that the traditional dry-pressing forming process has low efficiency and cannot produce products with complex shapes are solved, and the problems that the injection molding is used are solved, The feeding adhesive for extrusion molding has the problems of large addition amount, complex degreasing process, long degreasing time and easy generation of defects in the tire body, and the prepared diamond tool has the advantages of small shrinkage rate of a sintered blank, high dimensional precision, high density, improved hardness and breaking strength, high yield and capability of manufacturing the diamond tool with large size and complex shape.
Preferably, the raw materials of the flowing warm-pressing water-based binder comprise, by mass: 30-50% of water-soluble binder, 5-30% of rigid high polymer, 30-50% of viscoelastic polymer and 1-10% of assistant.
The flowing warm-pressing water-based binder has the main effects that the matrix alloy powder is completely coated, so that the binding effect between particles of the matrix alloy powder is realized, the particles of the matrix alloy powder are not easy to separate in the warm-pressing forming process, and the strength of a matrix alloy blank is improved;
the water-soluble binder can promote the flow of the matrix alloy feed in the warm-pressing forming process; the rigid high molecular polymer can play a skeleton role in the dipping and degreasing process, the tire body alloy blank is prevented from collapsing when the dipping and degreasing process is carried out, the tire body alloy blank formed by warm pressing is good in strength and not easy to deform when the tire body alloy blank is subjected to warm pressing and is subjected to mold stripping, and the content of the rigid high molecular polymer is low; the viscoelastic polymer can ensure that the tire body alloy feed has the characteristics of wide creep temperature, low-temperature creep fluidity and good plasticity, and the fluidity of the tire body alloy feed during warm-pressing molding is ensured; the auxiliary agent can effectively improve the feeding performance of the matrix alloy.
When the tire body alloy blank formed by warm pressing is subjected to dipping degreasing, binder components soluble in a dipping degreasing solvent in the tire body alloy blank are removed, binder components insoluble in the dipping degreasing solvent are reserved, the binding force among blank particles is ensured when the tire body alloy blank subjected to dipping degreasing is sintered, the strength of the tire body alloy blank is ensured, and the remaining binder components can be removed through the rapid heating vacuum thermal degreasing.
Preferably, the water-soluble binder is polyethylene glycol, and the polymerization degree of the polyethylene glycol is 1500-2500;
the rigid high molecular polymer is any one or a mixture of more of polyformaldehyde, polymethyl methacrylate and polybutyl methacrylate;
the viscoelastic polymer is any one or a mixture of more of vinyl acetate, polyvinyl butyral and random polypropylene;
the auxiliary agent is any one or a mixture of more of paraffin, stearic acid and dioctyl phthalate.
The water-soluble binder is polyethylene glycol (PEG), the polyethylene glycol can be dissolved in water or ethanol, can promote the flow of the matrix alloy feed in the warm-pressing forming process, and can be leached and degreased by using solvents such as a leaching water solution or an ethanol solution; when the polymerization degree of the polyethylene glycol is too small, the polyethylene glycol is in a liquid state, and cannot bond particles of the matrix alloy powder after being heated and kneaded in the step A, so that the hardness and the breaking strength of the prepared diamond tool are poor, when the polymerization degree of the polyethylene glycol is too large, the polyethylene glycol has low solubility in an aqueous solution, and is not easy to leach when the matrix alloy blank is leached and degreased, so that the degreasing efficiency and effect are influenced, and the polyethylene glycol is removed when the temperature is rapidly raised and the vacuum degreasing is carried out later, so that the prepared diamond tool is easy to generate bubbles, cracks and the like.
Polyoxymethylene (POM), polymethyl methacrylate (PMMA) or polybutyl methacrylate (PBMA) in the rigid high polymer can play a skeleton role in the dipping and degreasing process, so that the blank of the tire body alloy is prevented from collapsing during dipping and degreasing;
vinyl Acetate (EVA), polyvinyl butyral (PVB) or random polypropylene (APP) in the viscoelastic polymer can ensure the low-temperature creep fluidity and plasticity of the tire body alloy feed, wherein the polyvinyl butyral can play a strong bonding role in powder particles of the tire body alloy feed, and effectively enhances the molding strength of the tire body alloy blank obtained after warm-pressing molding;
paraffin (WAX) and Stearic Acid (SA) in the auxiliary agent are used as lubricants, so that the fluidity of the tire body alloy feed can be increased, the friction between the tire body alloy feed and a forming die is reduced, and dioctyl phthalate (DOP) in the auxiliary agent is used as a plasticizer, so that the plastic forming temperature and viscosity of a high polymer in the flowing warm-pressing water-based binder can be reduced.
Preferably, the step a specifically includes:
step A1, adding 92-95% of matrix alloy powder and 5-8% of flowing warm-pressing water-based binder into a kneader according to mass percentage, heating and kneading for 1h at 140 ℃, and then cooling to prepare a kneaded feed;
and step A2, putting the kneaded feed into a crusher for crushing and granulating to prepare the matrix alloy feed.
92-95% of matrix alloy powder and 5-8% of flowing warm-pressing water-based binder are heated and kneaded, the raw material of the flowing warm-pressing water-based binder comprises viscoelastic polymer, the creep temperature of the viscoelastic polymer is wide, the low-temperature creep fluidity and the plasticity of the viscoelastic polymer are good, the using amount of the flowing warm-pressing water-based binder in the matrix alloy feed can be reduced by using the warm-pressing forming process, the requirement of warm-pressing forming on the fluidity of the matrix alloy feed can be met, the fluidity of the matrix alloy feed during warm-pressing forming is ensured, the matrix alloy blank is obtained through warm-pressing forming, solvent degreasing, rapid thermal degreasing and hydrogen reduction pressure sintering are carried out, and the sintered blank of the prepared diamond tool is small in shrinkage and high in density. If the content of the flowing warm-pressing water-based binder is too small, the fluidity of the tire body alloy feed in the warm-pressing forming process is too poor, the forming is difficult, the shape of the obtained tire body alloy blank does not meet the requirement, the shape is easy to dent, the strength of the blank is poor, and the blank is easy to crush; if the content of the flowing warm-pressing water-based binder is too large, too much binder component of the flowing warm-pressing water-based binder remained in the tire body alloy blank after the dipping degreasing and drying treatment is insoluble in the dipping degreasing solvent, the rapid heating vacuum thermal degreasing is adopted, the excessive binder component of the flowing warm-pressing water-based binder insoluble in the dipping degreasing solvent is volatilized into gas, no channel is arranged in the tire body alloy blank in time to be removed, the structure of the tire body alloy blank is easy to damage, and the tire body alloy blank is easy to generate bubbles, cracks or crushing.
Preferably, in the step B, the warm-pressing temperature of the warm-pressing forming is 50-200 ℃, the warm-pressing pressure is 1-3 tons/square centimeter, and the pressure maintaining time is 15-30 s.
The matrix alloy feeding is put into a warm-pressing die with the temperature of 50-200 ℃ by adopting a warm-pressing forming process, under the pressing action of warm-pressing forming, the matrix alloy feeding obtains the temperature and pressure of plastic flow, the temperature and pressure are uniformly distributed in a warm-pressing die cavity of the warm-pressing forming to obtain a matrix alloy blank, if the warm-pressing temperature of the warm-pressing forming is too low and the warm-pressing pressure is too low, the shape of the obtained matrix alloy blank does not meet the requirements, shape depression is easy to occur, the strength of the blank is poor, the blank is easy to crush, if the warm-pressing temperature of the warm-pressing forming is too high, the components of the flowing warm-pressing water-based binder in the matrix alloy feeding are easy to decompose, the bonding of matrix alloy powder cannot be realized, the mechanical property of the prepared diamond tool is poor, and if the warm-pressing pressure of the warm-pressing forming is too high, the internal stress of the matrix alloy feed is easily generated in the pressing process, and the matrix alloy blank is easily cracked after being demoulded, so that the mechanical property of the prepared diamond tool is poor.
Preferably, the matrix alloy powder comprises, by mass, 70-85% of metal pre-alloy powder, 5-10% of WC powder, 5-11% of Ni powder, 2-4% of Sn powder and 3-5% of diamond particles;
the components of the metal pre-alloy powder comprise 70% of Fe and 30% of Cu according to mass percentage, and the particle size of the metal pre-alloy powder is less than 2 mu m;
the grain diameters of the WC powder, the Ni powder and the Sn powder are respectively less than 5 mu m.
The metal pre-alloy powder has high hardness and high impact strength, if the particle size of the metal pre-alloy powder is too large, the reactivity of the metal pre-alloy powder is reduced during sintering, the required sintering temperature is high, the density of a diamond tool obtained by sintering is reduced, the diamond tool is easy to burn at high temperature, and waste products are generated; the hardness of the prepared diamond tool can be enhanced by adding the WC powder, the Ni powder and the Sn powder, the smaller the particle size of the WC powder, the Ni powder and the Sn powder is, the better the uniformity of the metal particles of the prepared matrix alloy blank is, and the hardness and the bending strength of the sintered diamond tool are high.
Preferably, the particle size of the diamond particles is 0.2-0.4 mm.
If the particle size of the diamond particles is too large, the metal pre-alloy powder, WC powder, Ni powder and Sn powder cannot guarantee the holding force of the diamond particles, cannot guarantee that the diamond particles do not fall off, and the hardness and bending strength of the manufactured diamond tool are poor.
Preferably, in the step C, the dipping and degreasing is to soak the blank of the tire body alloy in a mixed solution of one or more of water, ethanol, aliphatic ketone or aromatic hydrocarbon at a constant temperature of 25 ℃ for 1-2 hours.
The dipping degreasing is to use a solvent capable of dissolving a certain component in the flowing warm-pressing water-based binder in the matrix alloy blank before sintering, and the component is dissolved out by soaking.
Preferably, in the step C, the drying treatment is to take out the dipped and degreased blank of the tire body alloy, dry the blank in the air for 20 to 30min, and then dry the blank in the vacuum for 20 to 30min at the temperature of 40 ℃ and the vacuum degree of 1000 Pa.
After dipping and degreasing, drying the tire body alloy blank in the air for 20-30 min to remove most of moisture of the tire body alloy blank, and then carrying out vacuum drying, so that the drying efficiency of the tire body alloy blank can be effectively improved, and the production efficiency of a diamond tool is improved.
Preferably, the step D specifically includes:
step D1, placing the tire body alloy blank processed in the step C in a vacuum pressure sintering furnace, heating from room temperature to 450 ℃ at the heating rate of 150 ℃/h under the vacuum degree of 1Pa, preserving heat for 0.5h, and carrying out rapid heating vacuum thermal degreasing;
d2, heating the vacuum pressure sintering furnace from 450 ℃ to 550 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing hydrogen, controlling the pressure in the furnace to be 0.1035MPa, and performing hydrogen deoxidation and reduction;
step D3, heating the vacuum pressure sintering furnace from 550 ℃ to 950 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing argon gas, controlling the pressure in the furnace to be 9.6MPa, and carrying out vacuum pressure sintering;
and D4, naturally cooling the vacuum pressure sintering furnace to 100 ℃ under the condition that the pressure in the furnace is kept at 9.6MPa, opening the furnace door, and discharging to obtain the diamond tool based on warm compaction.
And D, placing the tire body alloy blank in a vacuum pressure sintering furnace to complete the whole process of rapid heating vacuum thermal degreasing, hydrogen deoxidation and vacuum pressure sintering at one time, so that the production period and energy consumption are reduced, the production efficiency is improved, the labor intensity and the production cost are reduced, and the energy consumption and the environmental pollution are greatly reduced.
D1, binder components which are insoluble in the dipping degreasing solvent are remained in the tire body alloy blank degreased by the dipping soaking water and can be removed only by the thermal decomposition of the rapid heating vacuum thermal degreasing, the rapid heating vacuum thermal degreasing is carried out, the vapor pressure of the high polymer is improved by utilizing the vacuum action, the decomposition is promoted, the degreasing residues are reduced, the degreasing speed and efficiency are accelerated, in addition, the rapid heating vacuum thermal degreasing is realized by using the heating rate of 150 ℃/h, the degreasing speed is high, the production efficiency is high, and the diamond tool with large size can be prepared.
Because the metal component particles in the matrix alloy powder are inevitably polluted by water mist, air and the like in the processes of material mixing, warm-pressing forming and dipping degreasing, an oxide layer is generated on the surfaces of the metal component particles in the matrix alloy powder, the step D2 carries out hydrogen deoxidation and reduction, and metal oxide films formed on the surfaces of the metal component particles in the matrix alloy blank are reduced into alloy particles.
And D3, adding argon gas to carry out vacuum pressure sintering, so that the density and strength of the prepared diamond tool can be further improved, the compactness of a sintered body is improved, and pores and crack defects in the diamond tool are reduced.
The technical solution of the present invention is further explained by the following embodiments.
Examples 1 to 5
In examples 1 to 5, the raw materials are weighed according to table 1, and calculated according to mass percentage, wherein the metal prealloy powder in the matrix alloy powder consists of 70% of Fe and 30% of Cu, the particle size of the metal prealloy powder is 1 μm, and the particle sizes of WC powder, Ni powder and Sn powder are all 3 μm;
the grain diameter of diamond grains in the matrix alloy powder is 0.3 mm;
the polymerization degree of polyethylene glycol was 2000.
And examples 1-5 a diamond tool based on warm compaction was prepared according to the following procedure:
TABLE 1 Diamond tool feedstock composition
Step A, preparing a matrix alloy feed
Step A1, weighing matrix alloy powder and a flowing warm-pressing water-based binder according to the table 1, adding the mixture into a kneader, heating and kneading the mixture for 1 hour at the temperature of 140 ℃, and then cooling the mixture to prepare a kneaded feed;
and step A2, putting the prepared kneaded feed into a small jaw crusher for crushing and granulating to prepare the matrix alloy feed.
Step B, warm-pressing and molding the matrix alloy into a matrix alloy blank
Step B1, heating a warm pressing die of a warm pressing machine to 100 ℃ and keeping the temperature;
and step B2, adding the tire body alloy feed into a warm pressing die, pressurizing at the warm pressing pressure of 1.5 tons/square centimeter, maintaining the pressure for 15s, and then cooling and demolding to prepare the tire body alloy blank with the length, width and thickness of 24 x 15 x 16 mm.
Step C, dipping, degreasing and drying the blank of the matrix alloy
Step C1, placing the blank of the tire body alloy into a constant-temperature water tank at 25 ℃, and soaking the blank of the tire body alloy in water for 2 hours;
and step C2, taking the blank of the matrix alloy out of the constant-temperature water tank, drying the blank in the air for 30min, and then drying the blank in a vacuum drying box at the temperature of 40 ℃ and the vacuum degree of 1000Pa for 30min in vacuum.
Step D, rapid heating vacuum thermal degreasing and hydrogen reduction pressure sintering
Step D1, placing the tire body alloy blank processed in the step C in a vacuum pressure sintering furnace, heating from room temperature to 450 ℃ at the heating rate of 150 ℃/h under the vacuum degree of 1Pa, preserving heat for 0.5h, and carrying out rapid heating vacuum thermal degreasing;
d2, heating the vacuum pressure sintering furnace from 450 ℃ to 550 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing hydrogen, controlling the pressure in the furnace to be 0.1035MPa, and performing hydrogen deoxidation and reduction;
step D3, heating the vacuum pressure sintering furnace from 550 ℃ to 950 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing argon gas, controlling the pressure in the furnace to be 9.6MPa, and carrying out vacuum pressure sintering;
and D4, naturally cooling the vacuum pressure sintering furnace to 100 ℃ under the condition of keeping the pressure in the furnace at 9.6MPa, opening the furnace door, and discharging to obtain the diamond tool.
Comparative example 1
Example 1 was selected for comparison.
In this comparative example, the raw materials were identical to those of example 1, the step B of the preparation method was to injection mold the matrix alloy feedstock into a matrix alloy blank, the matrix alloy feedstock was injected into an injection molding machine mold with a working temperature of 180 ℃, the injection pressure was 15 tons, the dwell time was 30s, and a matrix alloy blank with a length, width and thickness of 24 x 15 x 16mm was prepared, and the remaining preparation method steps were identical to those of example 1, and a diamond tool was prepared.
Comparative example 2
Example 1 was selected for comparison.
In the comparative example, the flowing warm pressing water-based binder consists of the following raw materials in percentage by mass: 60% polyethylene glycol (PEG), 15% Polyoxymethylene (POM), 15% polymethyl methacrylate (PMMA), 5% Stearic Acid (SA), and 5% dioctyl phthalate (DOP), and the remaining raw material components were identical to those of example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 3
Example 1 was selected for comparison.
In the comparative example, the flowing warm pressing water-based binder consists of the following raw materials in percentage by mass: 50% polyethylene glycol (PEG), 15% Polyoxymethylene (POM), 10% polymethyl methacrylate (PMMA), 5% Ethylene Vinyl Acetate (EVA), 5% polyvinyl butyral (PVB), 5% atactic polypropylene (APP), 5% Stearic Acid (SA), and 5% dioctyl phthalate (DOP), and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 4
Example 1 was selected for comparison.
In this comparative example, the polymerization degree of polyethylene glycol (PEG) was 800, and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 5
Example 1 was selected for comparison.
In this comparative example, the polymerization degree of polyethylene glycol (PEG) was 2800, and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 6
Example 1 was selected for comparison.
In the comparative example, the matrix alloy feed consists of the following raw materials in percentage by mass: 97% of matrix alloy powder and 3% of a flowing warm-pressing water-based binder, and the remaining raw material components were the same as in example 1, and a diamond tool was produced according to the production method of example 1.
Comparative example 7
Example 1 was selected for comparison.
In the comparative example, the matrix alloy feed consists of the following raw materials in percentage by mass: 88% of matrix alloy powder and 12% of a flowing warm-pressing water-based binder, and the remaining raw material components were the same as in example 1, and a diamond tool was produced according to the production method of example 1.
Comparative example 8
Example 1 was selected for comparison.
In the comparative example, the raw materials are the same as those in example 1, and the step B of the preparation method, namely the warm-pressing of the carcass alloy feed into the carcass alloy blank, specifically comprises the following steps: step B1, heating a warm pressing die of a warm pressing machine to 40 ℃ and keeping the temperature; and step B2, adding the matrix alloy into a warm-pressing die, pressurizing to 0.5 ton/square centimeter under warm-pressing pressure, maintaining the pressure for 15 seconds, cooling and demolding to obtain a matrix alloy blank with the length, width and thickness of 24 x 15 x 16mm, and preparing the diamond tool according to the steps of the other preparation methods in the same way as the example 1.
Comparative example 9
Example 1 was selected for comparison.
In the comparative example, the raw materials are the same as those in example 1, and the step B of the preparation method, namely the warm-pressing of the carcass alloy feed into the carcass alloy blank, specifically comprises the following steps: step B1, heating a warm pressing die of a warm pressing machine to 250 ℃ and keeping the temperature constant; and step B2, adding the matrix alloy into a warm-pressing die, pressurizing at the warm-pressing pressure of 4 tons/square centimeter, maintaining the pressure for 15s, cooling and demolding to prepare a matrix alloy blank with the length, width and thickness of 24 x 15 x 16mm, and preparing the diamond tool by the steps of the other preparation methods consistent with the steps of the example 1.
Comparative example 10
Example 1 was selected for comparison.
In this comparative example, the particle size of the metal pre-alloy powder was 5 μm, and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 11
Example 1 was selected for comparison.
In this comparative example, the grain sizes of WC powder, Ni powder and Sn powder were 8 μm, respectively, and the remaining raw material components were the same as in example 1, and a diamond tool was produced in accordance with the production method of example 1.
Comparative example 12
Example 1 was selected for comparison.
In this comparative example, the diamond particles had a particle size of 0.6mm, and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
Comparative example 13
Example 1 was selected for comparison.
In this comparative example, the diamond particles had a particle size of 0.1mm, and the remaining raw material components were the same as in example 1, and a diamond tool was manufactured according to the manufacturing method of example 1.
The diamond tools prepared in examples 1 to 5 and comparative examples 1 to 13 were subjected to performance tests of bulk density (water drainage method), relative theoretical density (relative theoretical density ═ bulk density/theoretical density of standard substance), hardness (HRB steel ball indentation method), and flexural strength (three-point flexural method) by using the conventional metal material test method;
the theoretical density of the diamond tool (carcass) of each example and comparative example was calculated in the following manner: since the metal pre-alloyed powder consisted of 70% Fe and 30% Cu by mass, the density of Fe contained in the metal pre-alloyed powder was 7.86g/cm3The density of Cu is 8.9g/cm3And the metal prealloyed powder comprises Fe70g and Cu30g calculated as 100g of the metal prealloyed powder, and the density of the metal prealloyed powder is as follows: density ρ is mass M/volume V, then: the density ρ 1 of the metal prealloyed powder is:
ρ1=100/(70/7.86+30/8.9)=8.15g/cm3
taking example 1 as an example, since the matrix alloy powder of example 1 consists of 70% of metal pre-alloy powder, 10% of WC powder, 11% of Ni powder, 4% of Sn powder and 5% of diamond particles in percentage by mass, the density of the metal pre-alloy powder contained in the matrix alloy powder is 8.15g/cm3The density of WC powder is 15.63g/cm3The density of the Ni powder is 8.9g/cm3The density of Sn powder is 6.54g/cm3The density of the diamond particles was 3.52g/cm3And calculating by taking 100g of the matrix alloy powder, wherein the matrix alloy powder comprises 70g of metal prealloying powder, 10g of WC powder, 11g of Ni powder, 4g of Sn powder and 5g of diamond particles, and then: the theoretical density ρ 2 of the diamond tool (matrix) of example 1 is:
ρ2=100/(70/8.15+10/15.63+11/8.9+4/6.54+5/3.52)=8.00g/cm3the theoretical density of the diamond tool (matrix) of example 2 measured according to the above method was 8.05g/cm3The theoretical density of the diamond tool (matrix) of example 3 was 8.13g/cm3The theoretical density of the diamond tool (matrix) of example 4 was 8.04g/cm3The theoretical density of the diamond tool (matrix) of example 5 was 8.02g/cm3The theoretical densities of the diamond tools (tire casings) of comparative examples 1 to 13 were in accordance with example 1.
The following performance test results were obtained:
TABLE 2 Performance testing of examples and comparative examples
From the above test results, the diamond tools prepared in examples 1 to 5 have high density, hardness and flexural strength, and since the matrix alloy powder and the flowing warm-pressing water-based binder are heated and kneaded to form the matrix alloy feedstock during the preparation of the diamond tool, the raw materials of the flowing warm-pressing water-based binder include vinyl acetate (EVA), polyvinyl butyral (PVB) and atactic polypropylene (APP), and have the characteristics of wide creep temperature, good low-temperature creep fluidity and plasticity, and the usage amount of the flowing warm-pressing water-based binder is small by using the warm-pressing molding process, so that the requirement of warm-pressing molding on the fluidity of the matrix alloy feedstock can be met, the matrix alloy feedstock is subjected to warm-pressing molding to prepare the matrix alloy blank, then subjected to dipping degreasing and drying, subjected to rapid temperature rise, vacuum thermal degreasing and hydrogen reduction pressure sintering, the relative theoretical density of the diamond tool manufactured in the embodiment 1 can reach 99.8%, and the manufactured large-size diamond tool has high size precision, high density, high hardness and high breaking strength.
It can be known from example 1 and comparative example 1 that, when the matrix alloy feed is injection molded into the matrix alloy blank in step B of comparative example 1 by using the injection molding process, the fluidity of the matrix alloy feed cannot meet the injection molding requirement during injection molding due to the small content of the binder used, the molding is difficult, the prepared diamond tool has obvious cracks, the shape is not matched with the shape of a molding die, and the diamond tool is easy to crush under stress, while the matrix alloy blank is obtained by using the warm-pressing process to warm-press the matrix alloy feed by using the binder with the same content in example 1, and the prepared diamond tool has good density, hardness and breaking strength.
As can be seen from example 1, comparative example 2 and comparative example 3, when the viscoelastic polymer such as vinyl acetate (EVA), polyvinyl butyral (PVB) and atactic polypropylene (APP) is not added to the flowing warm-pressing water-based adhesive in comparative example 2, and the viscoelastic polymer such as vinyl acetate (EVA), polyvinyl butyral (PVB) and atactic polypropylene (APP) is added too small to the flowing warm-pressing water-based adhesive in comparative example 3, the low-temperature creep fluidity of the matrix alloy feed is poor, the plasticity is poor, the molding is difficult when the matrix alloy blank is prepared by performing warm-pressing, the diamond tool prepared in comparative example 2 has significant cracks, and the diamond tool prepared in comparative example 3 has significant cracks when crushed under stress.
As can be seen from example 1, comparative example 4 and comparative example 5, when the polymerization degree of the polyethylene glycol in comparative example 4 is too small, since the polyethylene glycol is in a liquid state at this time, after the flowing warm-pressing water-based binder is heated and kneaded with the matrix alloy powder in step a, the flowing warm-pressing water-based binder cannot bind the particles of the matrix alloy powder, and the hardness and the flexural strength of the diamond tool manufactured are significantly deteriorated, and the density is low; when the polymerization degree of the polyethylene glycol in the comparative example 5 is too large, the polyethylene glycol has low solubility in the aqueous solution, so that the tire body alloy blank is not easy to leach when subjected to leaching degreasing, the degreasing efficiency and effect are influenced, the polyethylene glycol is removed only when the tire body alloy blank is subjected to rapid temperature rise vacuum degreasing later, and the prepared diamond tool has the defect of bubbles due to the fact that no sufficient channel is arranged inside the tire body alloy blank to discharge, and the normal use of the diamond tool is influenced.
From example 1, comparative example 6 and comparative example 7, it can be seen that when the amount of the flowing warm-pressing water-based binder used in comparative example 6 is too small, the fluidity of the matrix alloy feedstock during warm-pressing molding is too poor, molding is difficult, the shape of the obtained matrix alloy blank does not meet the requirements, the obtained diamond tool has obvious cracks and is easy to crush; when the content of the flowing warm-pressing water-based binder in the comparative example 7 is too large, too much binder component is not dissolved in the dipping degreased aqueous solution in the flowing warm-pressing water-based binder remaining in the carcass alloy blank after the dipping degreasing and drying treatment, and then rapid heating vacuum thermal degreasing is performed, the binder component in which the excessive flowing warm-pressing water-based binder is not dissolved in the dipping degreased solvent is volatilized into gas, no channel is formed in the carcass alloy blank to be removed in time, the structure of the carcass alloy blank is damaged, and cracks of the manufactured diamond tool are obvious.
As can be seen from example 1, comparative example 8 and comparative example 9, when the temperature of the warm compaction mold in the warm compaction molding of comparative example 8 is too low and the warm compaction pressure is too low, the prepared diamond tool is easy to crush due to poor flowability of the matrix alloy feed at the too low warm compaction temperature and too low compaction pressure; when the temperature of the warm-pressing die in warm-pressing molding is too high and the warm-pressing pressure is too high in comparative example 9, the components of the flowing warm-pressing water-based binder in the matrix alloy feed are easily decomposed at the too high warm-pressing temperature, so that the matrix alloy powder cannot be bonded, the matrix alloy feed is easily subjected to internal stress in the pressing process due to the too high warm-pressing pressure, the matrix alloy blank is easily cracked after being demoulded, and the prepared diamond tool is poor in mechanical property and obvious in crack.
From example 1 and comparative example 10, it is clear that since the particle size of the metal pre-alloy powder in comparative example 10 is too large, the reactivity of the metal pre-alloy powder is reduced during sintering, the required sintering temperature is high, the densification of the sintered diamond tool is reduced, and the hardness and breaking strength are also significantly reduced.
As can be seen from example 1 and comparative example 11, the diamond tool manufactured in comparative example 11 has lower density, hardness and flexural strength than those of example 1, and since the particle diameters of WC powder, Ni powder and Sn powder in comparative example 11 are too large, the uniformity of metal particles in the matrix alloy blank is poor, and the density, hardness and flexural strength of the diamond tool manufactured after sintering are poor.
As is apparent from example 1, comparative example 12 and comparative example 13, when the particle size of the diamond particles in comparative example 12 is too large, since the holding force of the metal pre-alloy powder, WC powder, Ni powder and Sn powder cannot be secured to the diamond particles, while the particle size of the diamond particles in comparative example 13 is too small, the diamond particles are easily dropped, and the hardness and bending strength of the diamond tool manufactured are poor, the density is poor, and the service life of the diamond tool is affected.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. A preparation process of a diamond tool based on warm compaction is characterized by comprising the following steps:
step A, heating and kneading matrix alloy powder and a flowing warm-pressing water-based binder, and then granulating to prepare matrix alloy feed;
step B, performing warm-pressing molding on the tire body alloy feed to obtain a tire body alloy blank;
step C, dipping, degreasing and drying the blank of the tire body alloy;
d, carrying out rapid heating vacuum thermal degreasing and hydrogen reduction pressure sintering on the matrix alloy blank treated in the step C to prepare a diamond tool based on warm compaction;
the raw material of the flowing warm-pressing water-based adhesive comprises a viscoelastic polymer.
2. The process for preparing a diamond tool based on warm compaction forming according to claim 1, wherein the raw materials of the flowing warm compaction water-based binder comprise the following components in percentage by mass: 30-50% of water-soluble binder, 5-30% of rigid high polymer, 30-50% of viscoelastic polymer and 1-10% of assistant.
3. The preparation process of the diamond tool based on warm compaction molding according to claim 2, wherein the water-soluble binder is polyethylene glycol, and the polymerization degree of the polyethylene glycol is 1500-2500;
the rigid high molecular polymer is any one or a mixture of more of polyformaldehyde, polymethyl methacrylate and polybutyl methacrylate;
the viscoelastic polymer is any one or a mixture of more of vinyl acetate, polyvinyl butyral and random polypropylene;
the auxiliary agent is any one or a mixture of more of paraffin, stearic acid and dioctyl phthalate.
4. The process for preparing a diamond tool based on warm compaction as claimed in claim 1, wherein the step A specifically comprises:
step A1, adding 92-95% of matrix alloy powder and 5-8% of flowing warm-pressing water-based binder into a kneader according to mass percentage, heating and kneading for 1h at 140 ℃, and then cooling to prepare a kneaded feed;
and step A2, putting the kneaded feed into a crusher for crushing and granulating to prepare the matrix alloy feed.
5. The process for preparing a diamond tool based on warm compaction is characterized in that in the step B, the warm compaction temperature is 50-200 ℃, the warm compaction pressure is 1-3 tons/square centimeter, and the pressure maintaining time is 15-30 s.
6. The preparation process of a diamond tool based on warm compaction, according to claim 1, characterized in that the matrix alloy powder comprises, by mass, 70-85% of metal pre-alloy powder, 5-10% of WC powder, 5-11% of Ni powder, 2-4% of Sn powder and 3-5% of diamond particles;
the components of the metal pre-alloy powder comprise 70% of Fe and 30% of Cu according to mass percentage, and the particle size of the metal pre-alloy powder is less than 2 mu m;
the grain diameters of the WC powder, the Ni powder and the Sn powder are respectively less than 5 mu m.
7. The manufacturing process of the diamond tool based on warm compaction forming as claimed in claim 6, wherein the diameter of the diamond particles is 0.2-0.4 mm.
8. The process for preparing a diamond tool based on warm compaction as claimed in claim 1, wherein in the step C, the dipping and degreasing is to put the blank of the matrix alloy into a mixture of one or more of water, ethanol, aliphatic ketone or aromatic hydrocarbon, and soak the blank at a constant temperature of 25 ℃ for 1-2 h.
9. The process for preparing a diamond tool based on warm compaction as claimed in claim 1, wherein in the step C, the drying treatment is to take out the matrix alloy blank after the dipping and degreasing, dry the matrix alloy blank in air for 20-30 min, and then dry the matrix alloy blank in vacuum for 20-30 min at 40 ℃ and 1000 Pa.
10. The process for preparing a diamond tool based on warm compaction as claimed in claim 1, wherein the step D specifically comprises:
step D1, placing the tire body alloy blank processed in the step C in a vacuum pressure sintering furnace, heating from room temperature to 450 ℃ at the heating rate of 150 ℃/h under the vacuum degree of 1Pa, preserving heat for 0.5h, and carrying out rapid heating vacuum thermal degreasing;
d2, heating the vacuum pressure sintering furnace from 450 ℃ to 550 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing hydrogen, controlling the pressure in the furnace to be 0.1035MPa, and performing hydrogen deoxidation and reduction;
step D3, heating the vacuum pressure sintering furnace from 550 ℃ to 950 ℃ at the heating rate of 250 ℃/h, preserving the heat for 1h, introducing argon gas, controlling the pressure in the furnace to be 9.6MPa, and carrying out vacuum pressure sintering;
and D4, naturally cooling the vacuum pressure sintering furnace to 100 ℃ under the condition that the pressure in the furnace is kept at 9.6MPa, opening the furnace door, and discharging to obtain the diamond tool based on warm compaction.
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