CN100462331C - Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent - Google Patents
Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent Download PDFInfo
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- CN100462331C CN100462331C CNB2004100260861A CN200410026086A CN100462331C CN 100462331 C CN100462331 C CN 100462331C CN B2004100260861 A CNB2004100260861 A CN B2004100260861A CN 200410026086 A CN200410026086 A CN 200410026086A CN 100462331 C CN100462331 C CN 100462331C
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Abstract
The inventiono discloses a method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent, which comprises 11 steps including, mixing powdered silicon carbide, pulverized petroleum coke, graphite powder, activated charcoal powder by the weight parts of 0.30-0.90, 0.05-0.50, 0-0.20, 0-0.10, charging alcohol soluble, water-soluble formaldehyde-phenol resin, extrusion molding at normal temperature, and seasoning.
Description
Technical field
The invention belongs to the engineering ceramic material technical field, be specifically related to a kind of silicon carbide ceramics manufacturing process.
Background technology
The ceramics forming Technology is the key link of the various ceramic products of preparation, and its manufacturing process mainly comprises duse process and wet-formed two big classes.
Duse process comprises two kinds of die forming and hydrostatic pressings.Wherein mould pressing technology adopts already, but the shape of die forming product is subjected to bigger restriction; And product blank dimension that the hydrostatic pressing technology is shaped and form accuracy are difficult to guarantee, often need to adopt the method for post-treatment to reach required size and accuracy requirement, therefore have cost height, the problem that production efficiency is low.
Wet-formed plastic making and castable two classes of comprising.Plastic making helps realizing continuous production, and forming efficiency is higher, but the rheological characteristics of raw material is required height, and different material obtains plastic method also not exclusively equally simultaneously; The castable technology is applicable to the complicated or goods in irregular shape of shaping form, but the shaping required time is long, and it is big to take the work-yard, and efficient is lower, simultaneously ceramic material powder is had higher requirement, and the stable slip that obtains high solid loading is crucial.Extrusion molding is a kind of of plastic making, can continuous, high efficiency shaping tubulose, bar-shaped, tabular and porous column base substrate, be specially adapted to the shaping of uniform cross section, large length-diameter ratio ceramic product.Extrusion forming technology is widely used in oxide ceramics and is shaped, and generally makes the plasticity carrier with organic binder bond and water, often adds clay to improve the material consistency.
Silicon carbide ceramics has excellent mechanical property and physicals, is one of important engineering stupalith.The manufacturing process that the silicon carbide ceramics product is at present commonly used is die forming and hydrostatic pressing, and the colloidal state casting of casting and development in recent years etc., wherein casting is to produce the often main method of employing of silicon carbide structure spare institute.During the silicon carbide die forming at sic raw material and sinter additives to add resin as wedding agent (95100396.8), or clay is as wedding agent (94110569.5), perhaps clay+water glass is as wedding agent (94110570.9), or industrial paste and yellow starch gum are as wedding agent, raw material and wedding agent mix, then die forming or cold isostatic compaction.It is wedding agent that the extrusion molding of silicon carbide Heating element (globars) adopts pitch, it is main raw material that the silicon carbide of employing is also arranged, with polyvinyl alcohol as wedding agent (95100358.5), or polyvinyl alcohol+dextrin is as wedding agent (95100397.6) batch mixing at normal temperatures, through the technology of extrusion under vacuum.
Existing several silicon carbide ceramics forming techniques exist obvious deficiency at present, as:
Die forming is not suitable for the shaping of big L/D ratio product, and shape of product is restricted, if add clay etc. as binding agent then make the burnt product high-temperature behavior descend; Cold isostatic compaction equipment manufacturing cost height, production efficiency is low, and the size and dimension of product also is restricted.
The precondition of casting is the suspension that obtains the ideal high solid loading, raw material particle size, particle shape and feed particles surface property there is special requirement, and be difficult to obtain steady suspension for the bigger mixing raw material (as silicon carbide in the silicon carbide reaction-sintered raw material and carbon) of added ingredients in the raw material and main raw material physical difference, use this forming technique of product of macrobead sic raw material also to be difficult to adopt for requiring simultaneously.
Employing pitch commonly used is as the silicon carbide extrusion technique of wedding agent, and moulding process need adopt steam heating, equipment complexity, cost height; Pitch is yielding in heat-processed, coking temperature height, therefore the base substrate behind the extrusion molding need be placed in the fire proofed wood barrel of filling carbon granules under reductive condition 900～1000 ℃ and carries out biscuiting, pitch carbonization process volatile quantity is big simultaneously, green density does not reach requirement, often need double-steeping pitch, cause complex procedures, energy consumption is big, cost is high, uses pitch all very harmful to environment and health of operators in addition.
Use polyvinyl alcohol and polyvinyl alcohol+dextrin need adopt vacuum extrusion equipment, equipment manufacturing cost height, operation relative complex as the cold extrusion shaped technology of wedding agent.Behind the extrusion molding, need handle simultaneously, handle the back and in steam-heated pitch, flood 300～350 ℃ of oven dry.Exist complex procedures, energy consumption big, the problem of harm environment and HUMAN HEALTH.
Have not yet to see resol as wedding agent, the normal temperature extrusion molding is produced the document or the patent report of the method for silicon carbide ceramics.
Summary of the invention
At above-mentioned prior art situation, the objective of the invention is to set up a kind of wide to raw material particle size and size distribution requirement, that particle shape requires is low, be suitable for many components prescription, operation is simple, energy consumption is low, production efficiency is high, to the little resol of environment and human health damage as wedding agent, the normal temperature extrusion molding is produced the novel method of silicon carbide ceramics.
The inventive method should guarantee the blank strength height that is shaped, and is further indeformable during high temperature sintering; The material that is shaped has the controllable rheology characteristic, can extrusion molding under little squeeze, and it is indeformable to resist self gravitation after extruding; The defectives such as billet surface cracking, foaming, distortion or efflorescence of avoiding being shaped.
Resol of the present invention is characterized in that: may further comprise the steps as the silicon carbide ceramics normal temperature extrusion forming method of wedding agent:
Step 1: with massfraction is 0.30～0.95 sic powder, 0.05～0.50 petroleum coke powder, 0～0.20 Graphite Powder 99,0～0.10 activity charcoal powder, mixes on stirrer 0.2～1 hour;
Step 2: in the above-mentioned powder that mixes, add the pure dissolubility resol of massfraction 0.05～0.25 in addition, on wheel roller, rolled 0.5～1.5 hour;
Step 3: will roll material and be broken into bulk, normal temperature place or 50～80 ℃ of temperature under drying treatment;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 8～120 mesh sieve granulations, stand-by;
Step 5: with the water soluble phenol resin of stand-by raw material adding massfraction 0.01～0.20, mixed grind 10～45 minutes;
Step 6: the material sealing that mixed grind is good, placed 6～24 hours;
Step 7: raw material is the continuously extruded base substrate that goes out to be shaped on screw extrusion press or piston extrusion machine, and cutting obtains desired length;
Step 8: base substrate is in the room temperature standing and drying more than 24 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 150～200 ℃, is incubated 1～3 hour, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide shaping base substrate of sufficient intensity;
Step 10: base substrate such as cuts at the post-treatment operation, reaches the product length requirement;
Step 11: the blank after will cutting in vacuum atmosphere oven 1450～2300 ℃ carry out high temperature sintering, obtain silicon carbide reaction-sintered product or recrystallized silicon carbide product.
Description of drawings
Fig. 1: pressing materials apparent viscosity and shearing rate relation.
Shown in Figure 1 is the apparent viscosities il of embodiment material that obtains with capillary rheometer determining
aWith shearing rate
Relation curve, its rheology index n=0.35 (less than 1), apparent viscosity increases with shearing rate and reduces, and the feature of shear shinning is arranged, material flows easily during extruding, thereby realizes extrusion moulding under less pressure; Stop in case shearing, then material presents high apparent viscosity, the material of having extruded is inner, and evenly component is not yielding under the effect of viscous resistance, kept extrudate follow-up move put, geometric accuracy in the process such as oven dry.
Embodiment
Embodiment 1:
Step 1: with grain size number is 60 orders, and massfraction is that 0.70 sic powder, massfraction are that 0.20 petroleum coke powder, massfraction are that 0.05 Graphite Powder 99, massfraction are that 0.05 activity charcoal powder mixed on stirrer 0.5 hour;
Step 2: other interpolation massfraction is 0.12 pure dissolubility resol in the above-mentioned powder that mixes, and rolls on wheel roller 1 hour;
Step 3: will roll material and be broken into bulk, normal temperature is placed dry;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 8 mesh sieve granulations, stand-by;
Step 5: it is 0.10 water soluble phenol resin that stand-by raw material is added massfraction, mixed grind 15 minutes;
Step 6: the material sealing that mixed grind is good, placed 6 hours;
Step 7: raw material is at the continuously extruded base substrate that goes out to be shaped of screw extrusion press, and cutting obtains certain-length;
Step 8: base substrate was room temperature standing and drying 24 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 180 ℃, is incubated 2 hours, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide base substrate of sufficient intensity, blank density 1.85g/cm
3
Step 10: base substrate such as cuts at the post-treatment operation, reaches the product length requirement;
Step 11: the blank after will cutting obtains the silicon carbide reaction-sintered product, apparent density 2.9g/cm at 1650 ℃ of reaction sinterings
3, flexural strength 120MPa.
Embodiment 2:
Step 1: with grain size number is W14, and massfraction is that 0.80 sic powder, massfraction are that 0.15 petroleum coke powder, massfraction are that 0.05 activity charcoal powder mixed on stirrer 0.5 hour;
Step 2: other interpolation massfraction is 0.20 pure dissolubility resol in the above-mentioned powder that mixes, and rolls on wheel roller 1 hour;
Step 3: will roll material and be broken into bulk, normal temperature is placed dry;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 100 mesh sieve granulations, stand-by;
Step 5: it is 0.10 water soluble phenol resin that stand-by raw material is added mass percent, mixed grind 30 minutes;
Step 6: the material sealing that mixed grind is good, placed 12 hours;
Step 7: raw material is at the continuously extruded base substrate that goes out to be shaped of screw extrusion press, and cutting obtains desired length;
Step 8: base substrate was room temperature standing and drying 36 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 180 ℃, is incubated 2 hours, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide shaping base substrate of sufficient intensity, green density 2.1g/cm
3
Step 10: base substrate such as cuts at the post-treatment operation, reaches product requirement;
Step 11: the blank after will cutting obtains the silicon carbide reaction-sintered product, apparent density 3.1g/cm at 1650 ℃ of reaction sinterings
3, flexural strength 250MPa.
Embodiment 3:
Step 1: with grain size number is 120 orders, massfraction be 0.60 and grain size number be 180 orders, massfraction is that 0.25 sic powder, massfraction are that 0.10 petroleum coke powder, massfraction are that 0.05 activity charcoal powder mixed on stirrer 0.5 hour;
Step 2: in the above-mentioned powder that mixes, add the pure dissolubility resol of massfraction 0.10 in addition, on wheel roller, rolled 1 hour;
Step 3: will roll material and be broken into bulk, normal temperature is placed dry;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 40 mesh sieve granulations, stand-by;
Step 5: it is 0.08 water soluble phenol resin that stand-by raw material is added mass percent, mixed grind 30 minutes;
Step 6: the material sealing that mixed grind is good, placed 24 hours;
Step 7: raw material is at the continuously extruded base substrate that goes out to be shaped of screw extrusion press, and cutting obtains required length;
Step 8: base substrate was room temperature standing and drying 48 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 180 ℃, is incubated 2 hours, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide shaping base substrate of sufficient intensity, green density 2.0g/cm
3
Step 10: base substrate such as cuts at the post-treatment operation, reaches product requirement;
Step 11: the blank after will cutting obtains the silicon carbide reaction-sintered product, apparent density 3.1g/cm at 1650 ℃ of reaction sinterings
3, flexural strength 150MPa.
Adopt the beneficial effect of the inventive method:
(1) can squeeze out the elongated circle of external diameter≤150mm, random length or the different in nature cross section sky of corresponding size Core barrel (wall thickness 1 〉=mm) or bar-shaped silicon carbide products base substrate, other manufacturing process is difficult to realize at present;
(2) big to carborundum raw material accommodation, to granularity, the grain shape claimed range of sic raw material Wide, the maximum particle size that adds carborundum can reach 30 orders, and the carborundum content excursion is big. Have Be beneficial to adjustment and control to product mechanical property and physical property;
(3) but progressive forming goes out to have the long tube of different cross section, long rod, the production efficiency height, cost is low, is better than etc. The methods such as static pressure shaping, casting and colloidal state casting;
(4) the silicon carbide products blank density height that is shaped, solidification temperature is low, and dry rear green compact distortion is little, deflection Less than 0.5%, linearity reaches in 1%, and the intensity height can be processed after the curing. Need not the high temperature element Burn, also need not the materials such as impregnating pitch, energy savings is little to environmental and human health impacts harm.
Claims (2)
1. resol is characterized in that: may further comprise the steps as the silicon carbide ceramics normal temperature extrusion forming method of wedding agent:
Step 1: with massfraction is 0.30～0.95 sic powder, 0.05～0.50 petroleum coke powder, 0～0.20 Graphite Powder 99,0～0.10 activity charcoal powder, mixes on stirrer 0.2～1 hour;
Step 2: in the above-mentioned powder that mixes, add the pure dissolubility resol of massfraction 0.05～0.25 in addition, on wheel roller, rolled 0.5～1.5 hour;
Step 3: will roll material and be broken into bulk, normal temperature place or 50～80 ℃ of temperature under drying treatment;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 8～120 mesh sieve granulations, stand-by;
Step 5: stand-by raw material is added massfraction 0.01～0.20 water soluble phenol resin, mixed grind 10～45 minutes;
Step 6: the material sealing that mixed grind is good, placed 6～24 hours;
Step 7: raw material is the continuously extruded base substrate that goes out to be shaped on screw extrusion press or piston extrusion machine, and cutting obtains desired length;
Step 8: base substrate is in the room temperature standing and drying more than 24 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 150～200 ℃, is incubated 1～3 hour, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide shaping base substrate of sufficient intensity;
Step 10: base substrate cuts, and reaches the product length requirement;
Step 11: the blank after will cutting in vacuum atmosphere oven 1450～2300 ℃ carry out high temperature sintering, obtain silicon carbide reaction-sintered product or recrystallized silicon carbide product.
2. resol according to claim 1 is characterized in that: may further comprise the steps as the silicon carbide ceramics normal temperature extrusion forming method of wedding agent:
Step 1: with grain size number is 60 orders, and massfraction is that 0.70 sic powder, massfraction are that 0.20 petroleum coke powder, massfraction are that 0.05 Graphite Powder 99, massfraction are that 0.05 activity charcoal powder mixed on stirrer 0.5 hour;
Step 2: other interpolation massfraction is 0.12 pure dissolubility resol in the above-mentioned powder that mixes, and rolls on wheel roller 1 hour;
Step 3: will roll material and be broken into bulk, normal temperature is placed dry;
Step 4: the raw material of drying treatment is rolled fragmentation, cross 8 mesh sieve granulations, stand-by;
Step 5: it is 0.10 water soluble phenol resin that stand-by raw material is added massfraction, mixed grind 15 minutes;
Step 6: the material sealing that mixed grind is good, placed 6 hours;
Step 7: raw material is at the continuously extruded base substrate that goes out to be shaped of screw extrusion press, and cutting obtains certain-length;
Step 8: base substrate was room temperature standing and drying 24 hours;
Step 9: the shaping base substrate is put into the baking kiln and is heated to 180 ℃, is incubated 2 hours, cools to the room temperature kiln discharge with the furnace, obtains having the silicon carbide base substrate of sufficient intensity, blank density 1.85g/cm
3
Step 10: base substrate cuts, and reaches the product length requirement;
Step 11: the blank after will cutting obtains the silicon carbide reaction-sintered product, apparent density 2.9g/cm at 1650 ℃ of reaction sinterings
3, flexural strength 120MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100260861A CN100462331C (en) | 2004-04-29 | 2004-04-29 | Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100260861A CN100462331C (en) | 2004-04-29 | 2004-04-29 | Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent |
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| CN1569741A CN1569741A (en) | 2005-01-26 |
| CN100462331C true CN100462331C (en) | 2009-02-18 |
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| CNB2004100260861A Expired - Fee Related CN100462331C (en) | 2004-04-29 | 2004-04-29 | Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent |
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| CN101531527B (en) * | 2009-04-17 | 2012-06-27 | 奉化市中立密封件有限公司 | Producing method of sintering coarse granule silicon carbide products by one reaction |
| CN101560104B (en) * | 2009-05-12 | 2011-11-16 | 宁波欧翔精细陶瓷技术有限公司 | Preparation method for silicon carbide ceramic tube or rod |
| CN102358701B (en) * | 2011-08-25 | 2013-02-13 | 山东理工大学 | Preparation method of ceramic wiper plate |
| CN103449817A (en) * | 2012-05-30 | 2013-12-18 | 辽阳宏图碳化物有限公司 | Cold end of silicon carbide rod and production method thereof |
| CN105884366A (en) * | 2016-04-08 | 2016-08-24 | 三责（上海）新材料科技有限公司 | Light high-strength silicon carbide kiln furniture and manufacturing method thereof |
| CN110818425B (en) * | 2019-12-06 | 2021-08-24 | 江西拓普准晶新材料股份有限公司 | Method for processing silicon carbide recrystallization sintering high-purity ceramic abrasive by using powdered quartz |
| CN111348918A (en) * | 2020-03-11 | 2020-06-30 | 上海德宝密封件有限公司 | Boron nitride coating process for preventing graphite plate from being damaged |
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| US4987103A (en) * | 1986-04-09 | 1991-01-22 | Nippon Pillar Packing Co., Ltd. | Slider composed of a high-density silicon carbide sintered compact |
| CN1130163A (en) * | 1995-02-26 | 1996-09-04 | 薛天瑞 | Method for directly quick-sintered silicone-carbon stick |
| CN1144787A (en) * | 1995-02-16 | 1997-03-12 | 薛天瑞 | One-step burning method for silicon-carbon bar cold-extruded formed belt end |
| JP2000233977A (en) * | 1999-02-15 | 2000-08-29 | Harima Ceramic Co Ltd | Press-patching material for filling space within furnace wall of blast furnace |
| CN1269390A (en) * | 2000-04-21 | 2000-10-11 | 中南工业大学 | Adhesive for connecting carbon material |
| CN1364746A (en) * | 2001-04-28 | 2002-08-21 | 中国科学院长春光学精密机械与物理研究所 | Forming process for silicon carbide reflector blank and expansion and contraction mold |
-
2004
- 2004-04-29 CN CNB2004100260861A patent/CN100462331C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4987103A (en) * | 1986-04-09 | 1991-01-22 | Nippon Pillar Packing Co., Ltd. | Slider composed of a high-density silicon carbide sintered compact |
| CN1144787A (en) * | 1995-02-16 | 1997-03-12 | 薛天瑞 | One-step burning method for silicon-carbon bar cold-extruded formed belt end |
| CN1130163A (en) * | 1995-02-26 | 1996-09-04 | 薛天瑞 | Method for directly quick-sintered silicone-carbon stick |
| JP2000233977A (en) * | 1999-02-15 | 2000-08-29 | Harima Ceramic Co Ltd | Press-patching material for filling space within furnace wall of blast furnace |
| CN1269390A (en) * | 2000-04-21 | 2000-10-11 | 中南工业大学 | Adhesive for connecting carbon material |
| CN1364746A (en) * | 2001-04-28 | 2002-08-21 | 中国科学院长春光学精密机械与物理研究所 | Forming process for silicon carbide reflector blank and expansion and contraction mold |
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Assignee: Fengfeng New Oriental Science and Technology Development Co Ltd Assignor: Xi'an Jiaotong University Contract fulfillment period: 2009.9.11 to 2014.9.10 contract change Contract record no.: 2009130000251 Denomination of invention: Method for extrusion molding of thyrite at normal temperature with phenol-formaldehyde resin as binding agent Granted publication date: 20090218 License type: Exclusive license Record date: 20091111 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.9.11 TO 2014.9.10; CHANGE OF CONTRACT Name of requester: FENGFENG XINDONGFANG SCIENCE AND TECHNOLOGY DEVELO Effective date: 20091111 |
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