CN106242584A - A kind of preparation method of composite ceramic die material - Google Patents

A kind of preparation method of composite ceramic die material Download PDF

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CN106242584A
CN106242584A CN201610640856.4A CN201610640856A CN106242584A CN 106242584 A CN106242584 A CN 106242584A CN 201610640856 A CN201610640856 A CN 201610640856A CN 106242584 A CN106242584 A CN 106242584A
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composite ceramic
ceramic die
die material
collect
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雷春生
宋奇
陆娜
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Abstract

The invention discloses the preparation method of a kind of composite ceramic die material, belong to mold materials technical field.The present invention is with dimethyldichlorosilane, Oleum Verniciae fordii and barium chloride pre-hot mixing under gaseous mixture is protected, high temperature is released as reflection condition again using magnesium rod instancy of combustion, reflect, the most chilled process, with sodium tungstate, the mixing such as graphite carries out high-temperature calcination, through acidleach remove impurity, then with the mixing of the adjuvant such as zirconium oxide, sieve and put into graphite jig, calcine to obtain composite ceramic die material, the present invention prepares composite ceramic die material with homemade composite ceramic die material base material, improve its hardness, bending resistance, add that toughness is strong and corrosion resistance, the bending strength that compensate for traditional ceramics mold materials is the highest, and in use it is susceptible to the phenomenon of brittle fracture, there is wide application prospect.

Description

A kind of preparation method of composite ceramic die material
Technical field
The invention discloses the preparation method of a kind of composite ceramic die material, belong to mold materials technical field.
Background technology
Heat stability and the wearability of ceramic material are splendid, are the ideal materials manufacturing shaping dies, before having development very much Scape, but its toughness is very poor, is not used widely in terms of mould industry.Ceramic material expensive, and Also lack experience for producing, but along with development, the improvement of manufacturing process and the increase of consumption of science and technology, cost is inherently Declining, application also will be the most extensive.In the long term, should set about carrying out the research and development of advanced ceramics mold materials.From The research of some ceramic dies is it can be seen that the premium properties such as the high hardness of ceramic material, thermostability, wearability are poor strong because of it Toughness and played far away, be only used for not having or seldom have on the mould of shock loading and tension, former is many For the static load equipment such as extruder or hydraulic press, and mold shape is the most relatively simple, and material is only limitted to ZTA, TZP, Sialon Pottery etc..The most at present from the point of view of the general status of research and application, the kind of ceramic die material, performance and range of application all need In expanding further and improving.
Mould is indispensable important equipment in modern industry, but mold work condition is extremely severe, during such as cold extrusion Extrusion pressure is up to more than 2000MPa, simultaneously because metal is at mold flow and die surface severe friction, makes mould temperature rise Height, thus it occur frequently that the phenomenon such as mould sticking to mould, oxidation, even seam, unstable wear and make reduce die life.And at hot extrusion During pressure, higher extrusion temperature can make mold materials soften, and wearability is decreased obviously, and service life reduces, and produces Product surface quality is poor, becomes the key factor that restriction produces.Therefore, the important channel improving die life selects height exactly Hardness, the mold materials of high-wearing feature.Bending strength and the fracture toughness of traditional ceramic die material are the best, cause it to combine Close that less than optimal performance is good occurs in that use limitation.
Summary of the invention
The technical problem that present invention mainly solves: the highest for current traditional moulds material bending strength, and it is tough to rupture Property is the best, causes the defect that the combination property of mould is the most excellent, it is provided that the preparation method of a kind of composite ceramic die material.This Invent with dimethyldichlorosilane, Oleum Verniciae fordii and barium chloride pre-hot mixing under gaseous mixture is protected, then put with magnesium rod instancy of combustion Go out high temperature as reflection condition, reflect, more chilled process, mix with sodium tungstate, graphite etc. and carry out high-temperature calcination, through acid Leaching is miscellaneous, then with the mixing of the adjuvant such as zirconium oxide, sieves and puts into graphite jig, calcine to obtain composite ceramic die material, the present invention Prepare composite ceramic die material with homemade composite ceramic die material base material, improve its hardness, bending resistance, add Toughness is strong and corrosion resistance, and the bending strength that compensate for traditional ceramics mold materials is the highest, and the most easily sends out The phenomenon of raw brittle fracture, has wide application prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) count by weight, take 30～36 parts of dimethyldichlorosilanes, 23～26 parts of Oleum Verniciae fordii and 12～16 parts of Barium monoxides, put Enter in autoclave, use gaseous mixture to be discharged by air in reactor, and boost to 2～3MPa, design temperature 300～400 DEG C, with 200r/min stirring preheating 50～70min, described gaseous mixture is 4:2:1 by volume, by nitrogen, carbon monoxide and first Silane mixture forms；
(2) after above-mentioned preheating terminates, it is depressurized to normal atmosphere, takes above-mentioned dimethyldichlorosilane quality 13～the magnesium of 16% Bar, lights magnesium rod and puts in reactor, after temperature of reaction kettle is stable, is cooled to 75～85 DEG C with 5 DEG C/min speed, goes out while hot Material, collects discharging thing, and puts in liquid nitrogen freezers, design temperature-20～-10 DEG C, freezing processing 20～30min；
(3) after above-mentioned freezing processing terminates, warm naturally to room temperature, filter, collect filtering residue, count by weight, take 42～45 parts of filtering residues, 14～16 parts of sodium tungstates, 11～13 parts of graphite and 4～5 parts of aluminium oxidies, stir, put in calcining furnace, Calcine 30～40min at 1100～1200 DEG C, cool to room temperature with the furnace, collect calcined material, and be soaked in the quality such as calcined material Mass fraction is 15% hydrochloric acid solution, stirs 48～52min with 200r/min, filters subsequently, uses distilled water wash filtering residue extremely Neutrality, and put in air-dry machine air-dried, obtain composite ceramic die material base material；
(4) count by weight, take 48～52 parts of above-mentioned composite ceramic die material base materials, 13～16 parts of zirconium oxides, 3～6 parts Tantalum oxide and 1～2 part of nickelous carbonate, put in ball mill, by ratio of grinding media to material 12:1, adds alloying pellet, uses nitrogen protection, ball milling 18 ～22h, to cross 150 mesh sieves subsequently, collect the granule that sieves, and put in graphite jig, place in hot pressing furnace, design temperature is 1500～1600 DEG C, pressure is 28～32MPa, is incubated 24～32min, then with stove after being cooled to 700～750 DEG C with 12 DEG C/min Be cooled to room temperature, composite ceramic die material.
The physical property of the present invention is: the composite ceramic die material die cavity hardness that the present invention prepares is HRC80～85, quenches Fire hardness is HRC85～95,1200～1300 DEG C of long-term works, does not aoxidizes, good stability of the dimension, deformation rate be 0.03～ 0.05%, there is enough quenching degree.
The invention has the beneficial effects as follows:
(1) compared with existing ceramic die material, this composite ceramic die material has good comprehensive mechanical property and wear-resisting Performance, can be used for making extrusion die, drawing die etc. and cutter, wear-and corrosion-resistant parts etc.；
(2) this mould ageing resistance and anti-wear by force, there is good comprehensive mechanical property and excellent properties of antifriction and wear resistance；
(3) to have intensity high for the composite ceramic die material that the present invention prepares, and thermal coefficient of expansion is low, service life the advantage such as length, Can improve production efficiency and product quality.
Detailed description of the invention
Count the most by weight, take 30～36 parts of dimethyldichlorosilanes, 23～26 parts of Oleum Verniciae fordii and 12～16 parts of oxidations Barium, puts in autoclave, uses gaseous mixture to be discharged by air in reactor, and boosts to 2～3MPa, design temperature 300 ～400 DEG C, with 200r/min stirring preheating 50～70min, described gaseous mixture is 4:2:1 by volume, by nitrogen, carbon monoxide Mix with monosilane；After above-mentioned preheating terminates, it is depressurized to normal atmosphere, takes above-mentioned dimethyldichlorosilane quality 13 ～the magnesium rod of 16%, light magnesium rod and put in reactor, after temperature of reaction kettle is stable, with 5 DEG C/min speed be cooled to 75～ 85 DEG C, discharging while hot, collect discharging thing, and put in liquid nitrogen freezers, design temperature-20～-10 DEG C, freezing processing 20～ 30min；After above-mentioned freezing processing terminates, warm naturally to room temperature, filter, collect filtering residue, count by weight, take 42 ～45 parts of filtering residues, 14～16 parts of sodium tungstates, 11～13 parts of graphite and 4～5 parts of aluminium oxidies, stir, put in calcining furnace, 1100～1200 DEG C of calcinings 30～40min, cool to room temperature with the furnace, collect calcined material, and are soaked in the matter of the quality such as calcined material Amount mark is 15% hydrochloric acid solution, stirs 48～52min with 200r/min, filters subsequently, in using distilled water wash filtering residue extremely Property, and put in air-dry machine air-dried, obtain composite ceramic die material base material；Count by weight, take 48～52 parts above-mentioned compound Ceramic die material base material, 13～16 parts of zirconium oxides, 3～6 parts of tantalum oxide and 1～2 part of nickelous carbonate, put in ball mill, by ball Material ratio 12:1, adds alloying pellet, uses nitrogen protection, ball milling 18～22h, crosses 150 mesh sieves subsequently, collect the granule that sieves, and put Entering in graphite jig, place in hot pressing furnace, design temperature is 1500～1600 DEG C, and pressure is 28～32MPa, insulation 24～ 32min, then cool to room temperature with the furnace after being cooled to 700～750 DEG C with 12 DEG C/min, composite ceramic die material.
Example 1
Count the most by weight, take 30 parts of dimethyldichlorosilanes, 23 parts of Oleum Verniciae fordii and 12 parts of Barium monoxides, put into autoclave In, using gaseous mixture to be discharged by air in reactor, and boost to 2MPa, design temperature 300 DEG C, with 200r/min stirring preheating 50min, described gaseous mixture is 4:2:1 by volume, nitrogen, carbon monoxide and monosilane is mixed；At above-mentioned pre-accumulation of heat Shu Hou, is depressurized to normal atmosphere, takes the magnesium rod of above-mentioned dimethyldichlorosilane quality 13%, lights magnesium rod and put into reactor In, after temperature of reaction kettle is stable, it is cooled to 75 DEG C with 5 DEG C/min speed, discharging while hot, collect discharging thing, and put into liquid nitrogen In fridge, design temperature-20 DEG C, freezing processing 20min；After above-mentioned freezing processing terminates, warm naturally to room temperature, carry out Filtering, collect filtering residue, count by weight, take 42 parts of filtering residues, 14 parts of sodium tungstates, 11 parts of graphite and 4 parts of aluminium oxidies, stirring is all Even, put in calcining furnace, calcine 30min at 1100 DEG C, cool to room temperature with the furnace, collect calcined material, and be soaked in calcined material etc. The mass fraction of quality is 15% hydrochloric acid solution, stirs 48min with 200r/min, filters subsequently, uses distilled water wash filtering residue To neutral, and put in air-dry machine air-dried, obtain composite ceramic die material base material；Count by weight, take 48 parts above-mentioned compound Ceramic die material base material, 13 parts of zirconium oxides, 3 parts of tantalum oxide and 1 part of nickelous carbonate, put in ball mill, by ratio of grinding media to material 12:1, add Enter alloying pellet, use nitrogen protection, ball milling 18h, cross 150 mesh sieves subsequently, collect the granule that sieves, and put in graphite jig, then Putting in hot pressing furnace, design temperature is 1500 DEG C, and pressure is 28MPa, is incubated 24min, then after being cooled to 700 DEG C with 12 DEG C/min Cool to room temperature with the furnace, composite ceramic die material.
The composite ceramic die material die cavity hardness that the present invention prepares is HRC80, and quenching hardness is HRC85, at 1200 DEG C Long-term work, does not aoxidizes, good stability of the dimension, and deformation rate is 0.03%, has enough quenching degree.Example 2
Count the most by weight, take 33 parts of dimethyldichlorosilanes, 24 parts of Oleum Verniciae fordii and 14 parts of Barium monoxides, put into autoclave In, use gaseous mixture to be discharged by air in reactor, and boost to 2.5MPa, design temperature 350 DEG C, pre-with 200r/min stirring Hot 60min, described gaseous mixture is 4:2:1 by volume, nitrogen, carbon monoxide and monosilane is mixed；In above-mentioned preheating After end, it is depressurized to normal atmosphere, takes the magnesium rod of above-mentioned dimethyldichlorosilane quality 15%, light magnesium rod and put into reactor In, after temperature of reaction kettle is stable, it is cooled to 80 DEG C with 5 DEG C/min speed, discharging while hot, collect discharging thing, and put into liquid nitrogen In fridge, design temperature-15 DEG C, freezing processing 25min；After above-mentioned freezing processing terminates, warm naturally to room temperature, carry out Filtering, collect filtering residue, count by weight, take 44 parts of filtering residues, 15 parts of sodium tungstates, 12 parts of graphite and 4.5 parts of aluminium oxidies, stirring is all Even, put in calcining furnace, calcine 35min at 1150 DEG C, cool to room temperature with the furnace, collect calcined material, and be soaked in calcined material etc. The mass fraction of quality is 15% hydrochloric acid solution, stirs 50min with 200r/min, filters subsequently, uses distilled water wash filtering residue To neutral, and put in air-dry machine air-dried, obtain composite ceramic die material base material；Count by weight, take 50 parts above-mentioned compound Ceramic die material base material, 15 parts of zirconium oxides, 5 parts of tantalum oxide and 1.5 parts of nickelous carbonates, put in ball mill, by ratio of grinding media to material 12:1, Add alloying pellet, use nitrogen protection, ball milling 20h, cross 150 mesh sieves subsequently, collect the granule that sieves, and put in graphite jig, Placing in hot pressing furnace, design temperature is 1550 DEG C, and pressure is 30MPa, is incubated 28min, then is cooled to 730 DEG C with 12 DEG C/min After cool to room temperature with the furnace, composite ceramic die material.
The composite ceramic die material die cavity hardness that the present invention prepares is HRC85, and quenching hardness is HRC95, at 1300 DEG C Long-term work, does not aoxidizes, good stability of the dimension, and deformation rate is 0.05%, has enough quenching degree.Example 3
Count the most by weight, take 36 parts of dimethyldichlorosilanes, 26 parts of Oleum Verniciae fordii and 16 parts of Barium monoxides, put into autoclave In, using gaseous mixture to be discharged by air in reactor, and boost to 3MPa, design temperature 400 DEG C, with 200r/min stirring preheating 70min, described gaseous mixture is 4:2:1 by volume, nitrogen, carbon monoxide and monosilane is mixed；At above-mentioned pre-accumulation of heat Shu Hou, is depressurized to normal atmosphere, takes the magnesium rod of above-mentioned dimethyldichlorosilane quality 16%, lights magnesium rod and put into reactor In, after temperature of reaction kettle is stable, it is cooled to 85 DEG C with 5 DEG C/min speed, discharging while hot, collect discharging thing, and put into liquid nitrogen In fridge, design temperature-10 DEG C, freezing processing 30min；After above-mentioned freezing processing terminates, warm naturally to room temperature, carry out Filtering, collect filtering residue, count by weight, take 45 parts of filtering residues, 16 parts of sodium tungstates, 13 parts of graphite and 5 parts of aluminium oxidies, stirring is all Even, put in calcining furnace, calcine 40min at 1200 DEG C, cool to room temperature with the furnace, collect calcined material, and be soaked in calcined material etc. The mass fraction of quality is 15% hydrochloric acid solution, stirs 52min with 200r/min, filters subsequently, uses distilled water wash filtering residue To neutral, and put in air-dry machine air-dried, obtain composite ceramic die material base material；Count by weight, take 52 parts above-mentioned compound Ceramic die material base material, 16 parts of zirconium oxides, 6 parts of tantalum oxide and 2 parts of nickelous carbonates, put in ball mill, by ratio of grinding media to material 12:1, add Enter alloying pellet, use nitrogen protection, ball milling 22h, cross 150 mesh sieves subsequently, collect the granule that sieves, and put in graphite jig, then Putting in hot pressing furnace, design temperature is 1600 DEG C, and pressure is 32MPa, is incubated 32min, then after being cooled to 750 DEG C with 12 DEG C/min Cool to room temperature with the furnace, composite ceramic die material.
The composite ceramic die material die cavity hardness that the present invention prepares is HRC82, and quenching hardness is HRC90, at 1250 DEG C Long-term work, does not aoxidizes, good stability of the dimension, and deformation rate is 0.04%, has enough quenching degree.

Claims (1)

1. the preparation method of a composite ceramic die material, it is characterised in that concrete preparation process is:
(1) count by weight, take 30～36 parts of dimethyldichlorosilanes, 23～26 parts of Oleum Verniciae fordii and 12～16 parts of Barium monoxides, put Enter in autoclave, use gaseous mixture to be discharged by air in reactor, and boost to 2～3MPa, design temperature 300～400 DEG C, with 200r/min stirring preheating 50～70min, described gaseous mixture is 4:2:1 by volume, by nitrogen, carbon monoxide and first Silane mixture forms；
(2) after above-mentioned preheating terminates, it is depressurized to normal atmosphere, takes above-mentioned dimethyldichlorosilane quality 13～the magnesium of 16% Bar, lights magnesium rod and puts in reactor, after temperature of reaction kettle is stable, is cooled to 75～85 DEG C with 5 DEG C/min speed, goes out while hot Material, collects discharging thing, and puts in liquid nitrogen freezers, design temperature-20～-10 DEG C, freezing processing 20～30min；
(3) after above-mentioned freezing processing terminates, warm naturally to room temperature, filter, collect filtering residue, count by weight, take 42～45 parts of filtering residues, 14～16 parts of sodium tungstates, 11～13 parts of graphite and 4～5 parts of aluminium oxidies, stir, put in calcining furnace, Calcine 30～40min at 1100～1200 DEG C, cool to room temperature with the furnace, collect calcined material, and be soaked in the quality such as calcined material Mass fraction is 15% hydrochloric acid solution, stirs 48～52min with 200r/min, filters subsequently, uses distilled water wash filtering residue extremely Neutrality, and put in air-dry machine air-dried, obtain composite ceramic die material base material；
(4) count by weight, take 48～52 parts of above-mentioned composite ceramic die material base materials, 13～16 parts of zirconium oxides, 3～6 parts Tantalum oxide and 1～2 part of nickelous carbonate, put in ball mill, by ratio of grinding media to material 12:1, adds alloying pellet, uses nitrogen protection, ball milling 18 ～22h, to cross 150 mesh sieves subsequently, collect the granule that sieves, and put in graphite jig, place in hot pressing furnace, design temperature is 1500～1600 DEG C, pressure is 28～32MPa, is incubated 24～32min, then with stove after being cooled to 700～750 DEG C with 12 DEG C/min Be cooled to room temperature, composite ceramic die material.
CN201610640856.4A 2016-08-08 2016-08-08 A kind of preparation method of composite ceramic die material Pending CN106242584A (en)

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Application publication date: 20161221