CN106518026A - Method for preparing ceramic drawing die material - Google Patents

Method for preparing ceramic drawing die material Download PDF

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Publication number
CN106518026A
CN106518026A CN201610876178.1A CN201610876178A CN106518026A CN 106518026 A CN106518026 A CN 106518026A CN 201610876178 A CN201610876178 A CN 201610876178A CN 106518026 A CN106518026 A CN 106518026A
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safety glass
glass powder
drawing die
ball milling
under
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吴蓉蓉
蒋玉芳
陆娜
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TRUSYN CHEM-TECH Co Ltd
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TRUSYN CHEM-TECH Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/405—Iron group metals
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time

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  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a method for preparing a ceramic drawing die material, which belongs to the technical field of the drawing die material. According to the invention, the toughened glass powder after ball milling is spread at the bottom of a stainless steel die, then the toughened glass powder is compacted, a layer of mixed powder after ball milling of alumina and titanium carbide is spread and compacted, then a layer of toughened glass powder is continuously spread and compacted, and then placed in the die for insulation fusion, demoulding and ball milling to obtain the ceramic drawing die material. The toughened glass powder is taken as a base material for bedding, and has the advantages of high toughened glass intensity and good heat stability; compared with the traditional glass, the high cold-resistance heat-resistance property is increased by 3-5 times, the example proves that during a wire drawing process, the drawing die material and the metal wire are not adhered, the high temperature resistance can reach 500-800 DEG C, mechanical properties and hardness of the drawing die are increased, amount of machining is less, the drawing die is suitable for batch production, and has wide economic prospect.

Description

A kind of preparation method of ceramic bull block material
Technical field
The invention discloses a kind of preparation method of ceramic bull block material, belongs to wire drawing die field of material technology.
Background technology
After 20 beginning of the century ceramic materials step into industrial application, the present age three is listed as with metal material, macromolecular material Big solid material.Ceramic material has the advantages that many other materials do not possess, such as unique high rigidity, wear-resistant, anticorrosive And the good characteristic such as high temperature resistant, therefore it is widely used in many fields.The research of ceramic material is throughout various Oxide, nitride, carbide and boride ceramics, and larger progress is achieved in some fields.External metallic article Industry increasingly payes attention to the improvement of the quality and manufacturing process of wire drawing die, from the raising wire drawing die longevity for improving manufacturing competitive capabilities Life is started with, and material, structure, manufacturing process, manufacturing equipment and detecting instrument to wire drawing die etc. have carried out systematic research, open New section design method of composite die, wire drawing die new material, face coat new technique, wire drawing die etc. is sent, generation has been promoted The development of boundary's wire drawing production.Wire drawing die, as the critical component in metal wire rod wire drawing forming technology, is a kind of typical easily consumption Damage part.Made using cemented carbide powder or ceramic powders sintering more than usual metal wire rod wire drawing die, its production technology For：Powder body mixing forming of green body high temperature sintering grinding.Due to the extremely difficult processing of material after sintering, therefore, finally The grinding used time it is many, cutter consumes big so that the cost of high-quality wire drawing die remains high.Additionally, shaping in wire drawing In journey, die bearing temperature is raised quickly, while Service Environment is severe, therefore wire drawing die wear out failure quickly, it has to stop life Produce, the wire drawing die for more renewing, this also causes die cost proportion in the metal wire rod product that wire drawing shapes to remain high； Simultaneously because frequent more mold exchange, reduces production efficiency.Traditional wire drawing mold materialss generally adopt sintered carbide wire drawing die, due to Easily cause adhesive attraction in drawing process with tinsel, affect wire surface performance, especially draw coloured hard silk Material such as W, during Mo silks, operates under high-temperature situation, then affect more very.
The content of the invention
Present invention mainly solves technical problem：Exist in drawing process for current wire drawing mold materialss and draw with tinsel Adhesive attraction is played, causes surface property wiry and performance to reduce, the defect for causing its hardness and anti-wear performance poor, The present invention takes the safety glass powder after ball milling and is layed in stainless steel mold bottom and is suppressed, and re-lays one layer of aluminium oxide, carbon Change the mixed-powder compacting after the ball millings such as titanium, after continuing one layer of safety glass powder compacting of laying, be placed in insulation melting in mould, Ceramic bull block material is obtained final product after the demoulding, ball milling, and the present invention is using safety glass powder as base material shop fixtures, safety glass intensity Height, and heat stability is preferably, raising of the resistance to thermal shocks matter than 3～5 times of traditional glass, by safety glass coating ceramic Material, effectively prevents which from occurring to adhere to metal, and Jing examples prove that wire drawing mold materialss are not glued with tinsel in drawing process It is attached, can 500～800 DEG C of high temperature resistant, and wire drawing die mechanical property and hardness improves, and amount of machining is few, is adapted to batch production, has Wide economic outlook.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Discarded safety glass is collected, is dried after being cleaned naturally, is subsequently broken up to the safety glass fragment of a diameter of 1cm, 10～12h of ball milling under 250～300r/min, crosses 200 mesh sieves, collects to obtain safety glass powder, standby；
（2）Count by weight, weigh respectively 45～50 parts of aluminium oxidies, 45～50 parts of titanium carbides, 5～10 parts of magnesium oxide, 3～5 Part yittrium oxide and 5～8 parts of metallic nickels are placed in ball grinder, 20～24h of ball milling under 650～700r/min, 200 mesh of subsequent mistake Sieve, is prepared into mixed-powder；
（3）By step（1）The safety glass powder of preparation is laid to the stainless steel mould bottom of 10cm × 10cm × 10cm, control Laying depth be 1.5～2.0cm, under 5～10MPa suppress 5～8s after, then on safety glass powder bed lay one layer 3～ The mixed-powder of 4cm thick above-mentioned preparation, and 5～8s is suppressed under 5～10MPa, it is 2～3cm to continue thereafter with laying thick layer Safety glass powder, subsequently under 15～20MPa suppresses 10～15s, mould is placed in 1～2h of preheating at 450～500 DEG C；
（4）After the completion of waiting to preheat, 1650～1750 DEG C are warming up to by 10 DEG C/min, after insulation melting 1～2, stand and subsequently cool down To room temperature, hybrid ceramic is collected to obtain in the demoulding, is crushed and is placed in ball grinder, 3～5h of ball milling under 750～800r/min, Cross 110～120 mesh sieves, you can be prepared into a kind of ceramic bull block material.
The present invention application process be：Ceramic bull block material obtained in the present invention is placed in flat-crushing type belt sander, gold Metal work-pieces are sent at the mobile briquetting in abrasive band by transmission belt, adjust wire drawing die aperture be 4.0～4.5mm, drawing speed For 300～380m/min, terminating to use by taking-up is cooled to room temperature to wire drawing, wire drawing die Tensile strength is 1.8～ 2.8GPa, comprcssive strength be 6.4～8.8GPa, bending strength be 1.1～1.9GPa, hardness be 89～98HRA, wire drawing mold materialss Working life improve 10～12 times.
The invention has the beneficial effects as follows：
（1）The inventive method is simply easily operated, and with safety glass powder as raw material, not only raw material access approaches are simple, and Operating process is simple, and operating condition is easily controllable；
（2）The wire drawing die high mechanical properties, amount of machining are few, are adapted to batch production, are adapted to large-scale production and application.
Specific embodiment
Discarded safety glass is collected first, dries naturally, subsequently break up to the safety glass of a diameter of 1cm after being cleaned Fragment, 10～12h of ball milling under 250～300r/min are crossed 200 mesh sieves, collect to obtain safety glass powder, standby；By weight Number meter, weighs 45～50 parts of aluminium oxidies, 45～50 parts of titanium carbides, 5～10 parts of magnesium oxide, 3～5 parts of yittrium oxide and 5～8 parts respectively Metallic nickel is placed in ball grinder, 20～24h of ball milling under 650～700r/min, and 200 mesh sieve of subsequent mistake is prepared into mixed-powder； The safety glass powder of preparation is laid to the stainless steel mould bottom of 10cm × 10cm × 10cm, laying depth is controlled for 1.5 ～2.0cm, after suppressing 5～8s, then lays the thick above-mentioned systems of one layer of 3～4cm on safety glass powder bed under 5～10MPa Standby mixed-powder, and 5～8s is suppressed under 5～10MPa, it is 2～3cm safety glass powder to continue thereafter with laying thick layer, Subsequently 10～15s is suppressed under 15～20MPa, mould is placed in into 1～2h of preheating at 450～500 DEG C；After the completion of waiting to preheat, press 10 DEG C/min is warming up to 1650～1750 DEG C, and after insulation melting 1～2, standing is then cooled to room temperature, and the demoulding is collected and must mix pottery Porcelain, is crushed and is placed in ball grinder, 3～5h of ball milling under 750～800r/min, crosses 110～120 mesh sieves, you can prepared Obtain a kind of ceramic bull block material.
Example 1
Discarded safety glass is collected first, dries naturally, subsequently break up broken to the safety glass of a diameter of 1cm after being cleaned Block, the ball milling 10h under 250r/min are crossed 200 mesh sieves, collect to obtain safety glass powder, standby；Count by weight, claim respectively Amount 45 parts of aluminium oxidies, 45 parts of titanium carbides, 5 parts of magnesium oxide, 3 parts of yittrium oxide and 5 parts of metallic nickels are placed in ball grinder, in 650r/min Lower ball milling 20h, 200 mesh sieve of subsequent mistake, is prepared into mixed-powder；By the safety glass powder of preparation lay to 10cm × 10cm × The stainless steel mould bottom of 10cm, it is 1.5cm to control laying depth, after suppressing 5s under 5MPa, then in safety glass powder bed The mixed-powder of upper one layer of 3cm of laying thick above-mentioned preparation, and 5s is suppressed under 5MPa, it is 2cm to continue thereafter with laying thick layer Safety glass powder, subsequently suppresses 10s under 15MPa, mould is placed at 450 DEG C and preheats 1h；After the completion of waiting to preheat, by 10 DEG C/min is warming up to 1650 DEG C, after insulation melting 1, standing is then cooled to room temperature, and the demoulding is collected to obtain hybrid ceramic, crushed It is placed in ball grinder, the ball milling 3h under 750r/min, crosses 110 mesh sieves, you can be prepared into a kind of ceramic bull block material.
The present invention application process be：Ceramic bull block material obtained in the present invention is placed in flat-crushing type belt sander, gold Metal work-pieces are sent at the mobile briquetting in abrasive band by transmission belt, and the aperture for adjusting wire drawing die is 4.0mm, and drawing speed is 300m/min, terminates to use by taking-up is cooled to room temperature to wire drawing, and wire drawing mold materialss compression ratio is 28%, and tensile strength is 1.8GPa, comprcssive strength is 6.4GPa, and bending strength is 1.1GPa, and hardness is 89HRA, and the working life of wire drawing mold materialss is improved 10 times.
Example 2
Discarded safety glass is collected first, dries naturally, subsequently break up broken to the safety glass of a diameter of 1cm after being cleaned Block, the ball milling 12h under 300r/min are crossed 200 mesh sieves, collect to obtain safety glass powder, standby；Count by weight, claim respectively Amount 50 parts of aluminium oxidies, 50 parts of titanium carbides, 10 parts of magnesium oxide, 5 parts of yittrium oxide and 8 parts of metallic nickels are placed in ball grinder, in 700r/ Ball milling 24h under min, 200 mesh sieve of subsequent mistake, is prepared into mixed-powder；By the safety glass powder of preparation lay to 10cm × The stainless steel mould bottom of 10cm × 10cm, it is 2.0cm to control laying depth, after suppressing 8s under 10MPa, then in safety glass The mixed-powder of the thick above-mentioned preparations of one layer of 4cm is laid on powder bed, and suppresses 8s under 10MPa, continue thereafter with one layer of laying Thick is 3cm safety glass powder, subsequently suppresses 15s under 20MPa, mould is placed at 500 DEG C and preheats 2h；Treat that preheating is completed Afterwards, 1750 DEG C are warming up to by 10 DEG C/min, after insulation melting 2, standing is then cooled to room temperature, and hybrid ceramic is collected to obtain in the demoulding, Crushed and be placed in ball grinder, the ball milling 5h under 800r/min is crossed 120 mesh sieves, you can be prepared into a kind of ceramic bull block Material.
The present invention application process be：Ceramic bull block material obtained in the present invention is placed in flat-crushing type belt sander, gold Metal work-pieces are sent at the mobile briquetting in abrasive band by transmission belt, and the aperture for adjusting wire drawing die is 4.5mm, and drawing speed is 380m/min, terminates to use by taking-up is cooled to room temperature to wire drawing, and wire drawing mold materialss compression ratio is 30%, and tensile strength is 2.8GPa, comprcssive strength is 8.8GPa, and bending strength is 1.9GPa, and hardness is 98HRA, and the working life of wire drawing mold materialss is improved 12 times.
Example 3
Discarded safety glass is collected first, dries naturally, subsequently break up broken to the safety glass of a diameter of 1cm after being cleaned Block, the ball milling 11h under 270r/min are crossed 200 mesh sieves, collect to obtain safety glass powder, standby；Count by weight, claim respectively Amount 47 parts of aluminium oxidies, 47 parts of titanium carbides, 7 parts of magnesium oxide, 4 parts of yittrium oxide and 7 parts of metallic nickels are placed in ball grinder, in 670r/min Lower ball milling 22h, 200 mesh sieve of subsequent mistake, is prepared into mixed-powder；By the safety glass powder of preparation lay to 10cm × 10cm × The stainless steel mould bottom of 10cm, it is 1.7cm to control laying depth, after suppressing 7s under 7MPa, then in safety glass powder bed The mixed-powder of upper one layer of 3.5cm of laying thick above-mentioned preparation, and 7s is suppressed under 7MPa, continuing thereafter with laying thick layer is 2.5cm safety glass powder, subsequently suppresses 13s under 17MPa, mould is placed at 470 DEG C and preheats 1.5h；Treat that preheating is completed Afterwards, 1700 DEG C are warming up to by 10 DEG C/min, after insulation melting 1.5, standing is then cooled to room temperature, and the demoulding is collected and must mix pottery Porcelain, is crushed and is placed in ball grinder, the ball milling 4h under 770r/min, crosses 115 mesh sieves, you can be prepared into a kind of ceramic wire drawing Mold materialss.
The present invention application process be：Ceramic bull block material obtained in the present invention is placed in flat-crushing type belt sander, gold Metal work-pieces are sent at the mobile briquetting in abrasive band by transmission belt, and the aperture for adjusting wire drawing die is 4.3mm, and drawing speed is 340m/min, terminates to use by taking-up is cooled to room temperature to wire drawing, and wire drawing mold materialss compression ratio is 29%, and tensile strength is 2.4GPa, comprcssive strength is 7.4GPa, and bending strength is 1.5GPa, and hardness is 93HRA, and the working life of wire drawing mold materialss is improved 11 times.

Claims (1)

1. a kind of preparation method of ceramic bull block material, it is characterised in that concrete preparation process is：
（1）Discarded safety glass is collected, is dried after being cleaned naturally, is subsequently broken up to the safety glass fragment of a diameter of 1cm, 10～12h of ball milling under 250～300r/min, crosses 200 mesh sieves, collects to obtain safety glass powder, standby；
（2）Count by weight, weigh respectively 45～50 parts of aluminium oxidies, 45～50 parts of titanium carbides, 5～10 parts of magnesium oxide, 3～5 Part yittrium oxide and 5～8 parts of metallic nickels are placed in ball grinder, 20～24h of ball milling under 650～700r/min, 200 mesh of subsequent mistake Sieve, is prepared into mixed-powder；
（3）By step（1）The safety glass powder of preparation is laid to the stainless steel mould bottom of 10cm × 10cm × 10cm, control Laying depth be 1.5～2.0cm, under 5～10MPa suppress 5～8s after, then on safety glass powder bed lay one layer 3～ The mixed-powder of 4cm thick above-mentioned preparation, and 5～8s is suppressed under 5～10MPa, it is 2～3cm to continue thereafter with laying thick layer Safety glass powder, subsequently under 15～20MPa suppresses 10～15s, mould is placed in 1～2h of preheating at 450～500 DEG C；
（4）After the completion of waiting to preheat, 1650～1750 DEG C are warming up to by 10 DEG C/min, after insulation melting 1～2, stand and subsequently cool down To room temperature, hybrid ceramic is collected to obtain in the demoulding, is crushed and is placed in ball grinder, 3～5h of ball milling under 750～800r/min, Cross 110～120 mesh sieves, you can be prepared into a kind of ceramic bull block material.
CN201610876178.1A 2016-10-08 2016-10-08 Method for preparing ceramic drawing die material Pending CN106518026A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1063476A (en) * 1991-01-24 1992-08-12 合肥工业大学 Ceramic drawing die with precise structure and manufacture method thereof
CN102936137A (en) * 2012-10-18 2013-02-20 济南大学 Al2O3-TiC/Al2O3-TiC-CaF2 self-lubricating lamination ceramic drawing mold material
CN103586296A (en) * 2013-10-23 2014-02-19 大连理工大学 Mosaic ceramic drawing die and making method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1063476A (en) * 1991-01-24 1992-08-12 合肥工业大学 Ceramic drawing die with precise structure and manufacture method thereof
CN102936137A (en) * 2012-10-18 2013-02-20 济南大学 Al2O3-TiC/Al2O3-TiC-CaF2 self-lubricating lamination ceramic drawing mold material
CN103586296A (en) * 2013-10-23 2014-02-19 大连理工大学 Mosaic ceramic drawing die and making method thereof

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Application publication date: 20170322