CN109265176A - A method of high-performance honeycomb ceramic is prepared using Si crystal-cut tailing - Google Patents

A method of high-performance honeycomb ceramic is prepared using Si crystal-cut tailing Download PDF

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CN109265176A
CN109265176A CN201811000952.8A CN201811000952A CN109265176A CN 109265176 A CN109265176 A CN 109265176A CN 201811000952 A CN201811000952 A CN 201811000952A CN 109265176 A CN109265176 A CN 109265176A
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tailing
temperature
hours
powder
crystal
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黄宏贵
黄达
史忠旗
李延军
金志浩
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Jining Quanda Industrial Co Ltd
Xian Jiaotong University
Xian University of Architecture and Technology
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Jining Quanda Industrial Co Ltd
Xian Jiaotong University
Xian University of Architecture and Technology
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Priority to CN201811000952.8A priority Critical patent/CN109265176A/en
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Abstract

The present invention relates to a kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing, steps are as follows: the metal impurities first in removing Si crystal-cut tailing, then heating removes the high molecular material impurity in tailing；Graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, be uniformly mixed, obtain powder；Mixing after phenolic resin and tung oil is added into powder, ageing is sealed after filter mud-pugging；Extrusion molding obtains green body；Green body is air-dried and obtains green compact；By green compact under protective atmosphere high temperature firing, it is cooling after up to ceramic honey comb finished product.The present invention realizes the resource utilization of industrial solid castoff, avoids caused environmental pollution during the processing and storage of tailing；And ceramic honey comb mechanical property that the present invention obtains is good, good thermal shock, thermal conductivity are high, has biggish specific heat capacity, and good corrosion resistance.

Description

A method of high-performance honeycomb ceramic is prepared using Si crystal-cut tailing
Technical field
The present invention relates to a kind of methods for preparing high-performance honeycomb ceramic using Si crystal-cut tailing, and in particular to utilizes The method that the tailing that electroplated diamond cutting Si crystal obtains prepares high-performance honeycomb ceramic, belongs to the technology of preparing of ceramic honey comb Field.
Background technique
Ceramic honey comb is a kind of Multifunctional environment material, since its specific surface area is high, chemical property is stable, corrosion resistance It is good, it is constantly subjected to the favor of people.Silicon carbide ceramic honey comb has excellent chemical stability, high thermal conductivity, tolerance temperature The features such as spending height, good mechanical property, wide firing temperature, so that silicon carbide is expected to that cordierite is replaced more preferably to manufacture as one kind The material of ceramic honey comb.
Si crystal (including single crystalline Si and polycrystalline Si) has obtained extensively in every field such as electronic information, new energy, military projects Application, led the development of epoch new and high technology.The production of large scale Si crystal and cutting technique also reflect certain height New technology is horizontal.Pile up like a mountain with annual tens of thousands of tons for Si crystal-cut tailing (as trade waste), causes dirt to environment Dye.Conventional cutting method is adopted using high-strength wear-resistant alloy silk (Mo) and SiC abrasive material in recent years in order to improve cutting efficiency With the plating of diamond powder in the alloy wire of high-strength wearable, due to cutting method difference, cuts and sent out in the chemical component of tailing Significant change is given birth to.The former is based on the mixing tailing of SiC slurry and the simple substance Si micro mist cut；The latter is with simple substance Si micro mist Based on, and it is mixed with various metals and nonmetallic and oxide and high molecular material.With tailing storage environment and time difference, tail The chemical component of material also changes therewith, it is difficult to use directly as the raw material of high-performance SiC ceramic honey comb.
Summary of the invention
The purpose of the present invention is to provide a kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing, tools Body relates to the use of the method that the tailing that electroplated diamond Mo cutting Si crystal obtain prepares high-performance honeycomb ceramic.The present invention adopts It is that raw material prepares high performance silicon carbide ceramic honey comb with industrial solid castoff crystal silicon cutting tailing, realizes that industrial solid is useless The resource utilization of gurry, the problems such as avoiding the storage and generated environmental pollution of tailing；Tailing is taken full advantage of simultaneously In high-purity Si powder be ceramic material high-grade raw material, advantageously reduce the production cost of ceramic honey comb, improve product quality.This The technical solution of invention is as follows:
A method of high-performance honeycomb ceramic is prepared using Si crystal-cut tailing, the specific steps are as follows:
(1) pickling is carried out to Si crystal-cut tailing using the dilute hydrochloric acid that mass concentration is 10-20% and removes metal impurities, It cleans 2~3 times through pure water, then the tailing after pickling is heated under the conditions of 200-500 DEG C, remove the height in tailing Molecular material impurity obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, the mass ratio of graphite powder and tailing is 12: 28；Y2O3+Al2O3Additional amount be 3~10% (datum quantity for wherein, matching calculating is graphite powder, cutting tailing and compound burning Tie auxiliary agent Y2O3+Al2O3Total amount), Y2O3And Al2O3With the mixing of any mass ratio；It is uniformly mixed, obtains through ball mill or vibration mill Powder is obtained, is 8~24 hours according to ball mill incorporation time, is 30 minutes~2 hours according to vibration mill incorporation time.
(3) phenolic resin 5~15%, tung oil 3~10%, through batch mixer mixing 2~6 hours, through filtering are added into powder Mud machine, vacuum deairing machine filter mud-pugging 1~3 time, the sealing ageing of gained pug, Aging Temperature is 20~25 DEG C, and digestion time is 1~3 day；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtained Sectional dimension is 40~300mm*40~300mm, and thickness of honeycomb wall is 0.1~1.5mm, and pore size is 0.4~2mm*0.4~2mm Ceramic honey comb green body, extruder vacuum degree be 200-500Pa；
(5) green body that step (4) obtain is being divulged information, is being protected from light, air-dried 2~3 days at constant temperature, then be placed in thermostatic drying chamber 60 It is 1~3 day dry under the conditions of~180 DEG C, obtain green compact；
(6) green compact that step (5) obtain are placed in air furnace and are buried under carbocyclic ring border, or be placed in argon gas in high-temperature atmosphere furnace Under atmosphere protection environment, 3~10 hours are kept the temperature in 400~800 DEG C, then heating rate is that 3~10 DEG C/min is warming up to 1300- 1600 DEG C, room temperature is cooled to the furnace to get ceramic honey comb finished product after keeping the temperature 3-12 hour.
Further, in the step (1) using the dilute hydrochloric acid that mass concentration is 10-20% to Si crystal-cut tailing into Row pickling removes metal impurities, cleans 3 times through pure water, then heats, remove under the conditions of 400 DEG C to the tailing after pickling The high molecular material impurity in tailing is removed, obtains micro mist tailing after cooling.
Graphite powder, Y are added into micro mist tailing for the step (2)2O3+Al2O3Mixture； Y2O3+Al2O3Additional amount It is 5%, wherein Y2O3And Al2O3Mass ratio 2:3；It is uniformly mixed through ball mill or vibration mill, powder is obtained, according to ball Grinding machine incorporation time is 15 hours, is 1 hour according to vibration mill incorporation time.
Phenolic resin 10%, tung oil 7%, through batch mixer mixing 4 hours, through filter mud are added into powder for the step (3) Machine, vacuum deairing machine filter mud-pugging 2 times, the sealing ageing of gained pug, Aging Temperature is 25 DEG C, and digestion time is 2 days.
It is squeezed through step (3) treated pug using hydraulic piston type or spiral vacuum-extruder in the step (4) It forms out, acquisition sectional dimension is 120mm*120mm, and thickness of honeycomb wall 1mm, pore size is the ceramic honey comb of 1.2mm*1.2mm Green body, extruder vacuum degree are 300Pa.
The green body that step (4) obtain is being divulged information, is being protected from light, air-dried 3 days at constant temperature in the step (5), then is being placed in constant temperature It is 2 days dry under the conditions of 100 DEG C of drying box, obtain green compact.
The green compact that step (5) obtain are placed in air furnace in the step (6) and are buried under carbocyclic ring border or in high-temperature atmosphere furnace Argon atmosphere protection keeps the temperature 5 hours in 600 DEG C, and then heating rate is that 6 DEG C/min is warming up to 1500 DEG C, after keeping the temperature 8 hours Room temperature is cooled to the furnace to get ceramic honey comb finished product.
The invention also includes the high-performance honeycomb ceramics prepared by the above method.
Compared with the prior art, the present invention has the following advantages:
The present invention realizes the recycling of industrial solid castoff using industrial solid castoff crystal silicon cutting tailing as raw material The problem of utilizing, comprehensively utilize resource, avoiding environmental pollution caused by the processing and storage in the process of tailing；Make full use of tail High-purity silicon powder in material can effectively improve the performance of prepared ceramic material as the raw material of ceramic honey comb.
Detailed description of the invention
To be illustrated more clearly that background technique or technical solution of the present invention, below to the prior art or specific embodiment The attached drawing of middle combined use is briefly described；It should be evident that below in conjunction with the attached drawing side of being only for of specific embodiment Just understand the embodiment of the present invention, for those of ordinary skill in the art, without creative efforts, may be used also To obtain other drawings based on these drawings；
Fig. 1 is the X-ray map of high-performance honeycomb ceramic of the present invention；
Fig. 2 is the SEM micrograph of high-performance honeycomb ceramic of the present invention.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and It is apparent.But examples are merely exemplary, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art answer It should be appreciated that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form repair Change or replace, but these modifications and replacement are fallen within the protection scope of the present invention.
A kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing of embodiment 1
Specific step is as follows:
(1) pickling is carried out to Si crystal-cut tailing using the dilute hydrochloric acid that mass concentration is 10-20% and removes metal impurities, It cleans 3 times through pure water, then the tailing after pickling is heated under the conditions of 400 DEG C, remove the macromolecule material in tailing Expect impurity, obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture；The mass ratio of graphite powder and tailing is 12: 28；Y2O3+Al2O3Additional amount be 5%, wherein Y2O3And Al2O3Mass ratio 2:3；It is equal that mixing in 15 hours is mixed through ball mill It is even, obtain powder；
(3) phenolic resin 10% is added into powder, tung oil 7% was practiced through batch mixer mixing 4 hours through mud press, vacuum Mud machine filter mud-pugging 2 times, the sealing ageing of gained pug, Aging Temperature is 25 DEG C, and digestion time is 2 days；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtained Acquisition sectional dimension is 120mm*120mm, and thickness of honeycomb wall 1mm, pore size is the ceramic honey comb green body of 1.2mm*1.2mm, is squeezed Machine vacuum degree is 300Pa out；
(5) green body that step (4) obtain is being divulged information, is being protected from light, air-dried 3 days at constant temperature, then be placed in 100 DEG C of thermostatic drying chamber Under the conditions of dry 2 days, obtain green compact；
(6) green compact that step (5) obtain are placed in air furnace and are buried under carbocyclic ring border, kept the temperature 5 hours in 600 DEG C, then rise Warm speed is that 6 DEG C/min is warming up to 1500 DEG C, cools to room temperature after keeping the temperature 8 hours with the furnace to get ceramic honey comb finished product.
A kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing of embodiment 2
Specific step is as follows:
(1) dilute hydrochloric acid for being 10% using mass concentration carries out pickling to Si crystal-cut tailing and removes metal impurities, warp Pure water cleans 2 times, then heats under the conditions of 200 DEG C to the tailing after pickling, removes the high molecular material in tailing Impurity obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, the mass ratio of graphite powder and tailing is 12: 28；Y2O3+Al2O3Additional amount be 3%, wherein Y2O3And Al2O3Mass ratio 1:2；It is equal through mixing in ball mill ball milling 12 hours It is even；
(3) phenolic resin 5% is added into powder, tung oil 8% was practiced through batch mixer mixing 3 hours through mud press, vacuum Mud machine filter mud-pugging 1 time, the sealing ageing of gained pug, Aging Temperature is 20 DEG C, and digestion time is 1 day；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtained Sectional dimension is 40mm*40mm, and thickness of honeycomb wall 0.1mm, pore size is the ceramic honey comb green body of 0.4mm*0.4mm, extruder Vacuum degree is 200Pa；
(5) green body that step (4) obtain is being divulged information, is being protected from light, air-dried 1 day at constant temperature, then be placed in 60 DEG C of thermostatic drying chamber Under the conditions of dry 1 day, obtain green compact；
(6) green compact that step (5) obtain are placed under the protection of atmosphere furnace argon atmosphere, keep the temperature 3 hours in 400 DEG C, then Heating rate is that 10 DEG C/min is warming up to 1300 DEG C, cools to room temperature after keeping the temperature 3 hours with the furnace to get ceramic honey comb finished product.
A kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing of embodiment 3
Specific step is as follows:
(1) dilute hydrochloric acid for being 20% using mass concentration carries out pickling to Si crystal-cut tailing and removes metal impurities, warp Pure water cleans 2 times, then heats under the conditions of 300 DEG C to the tailing after pickling, removes the high molecular material in tailing Impurity obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, the mass ratio of graphite powder and tailing is 12: 28；Y2O3+Al2O3Additional amount be 5%, wherein Y2O3And Al2O3Mass ratio 2:3；It is mixed for 70min through vibration mill incorporation time It closes uniformly, obtains powder；
(3) phenolic resin 8% is added into powder, tung oil 5% was practiced through batch mixer mixing 5 hours through mud press, vacuum Mud machine filter mud-pugging 3 times, the sealing ageing of gained pug, Aging Temperature is 25 DEG C, and digestion time is 2 days；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtained Sectional dimension is 150mm*100mm, and thickness of honeycomb wall 0.15mm, pore size is the ceramic honey comb green body of 2mm*2mm, extruder Vacuum degree is 400Pa；
(5) green body that step (4) obtain is being divulged information, is being protected from light, air-dried 2 days at constant temperature, then be placed in 60 DEG C of thermostatic drying chamber Under the conditions of dry 1 day, obtain green compact；
(6) green compact that step (5) obtain are placed in air furnace and are buried under carbocyclic ring border, kept the temperature 5 hours in 600 DEG C, then rise Warm speed is that 8 DEG C/min is warming up to 1500 DEG C, cools to room temperature after keeping the temperature 8 hours with the furnace to get ceramic honey comb finished product.
A kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing of embodiment 4
Specific step is as follows:
(1) dilute hydrochloric acid for being 15% using mass concentration carries out pickling to Si crystal-cut tailing and removes metal impurities, warp Pure water cleans 3 times, then heats under the conditions of 500 DEG C to the tailing after pickling, removes the high molecular material in tailing Impurity obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, the mass ratio of graphite powder and tailing is 12: 28；Y2O3+Al2O3Additional amount be 10%, wherein Y2O3And Al2O3Mass ratio 7:3；It is 1 hour through vibration mill incorporation time It is uniformly mixed, obtains powder；
(3) phenolic resin 15% is added into powder, tung oil 3% was practiced through batch mixer mixing 4 hours through mud press, vacuum Mud machine filter mud-pugging 2 times, the sealing ageing of gained pug, Aging Temperature is 25 DEG C, and digestion time is 3 days；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtained Sectional dimension is 200mm*200mm, and thickness of honeycomb wall 1.2mm, pore size is the ceramic honey comb green body of 4.8mm*4.8mm, is squeezed out Machine vacuum degree is 300Pa；
(5) green body that step (4) obtain is being divulged information, is being protected from light, air-dried 3 days at constant temperature, then be placed in 60 DEG C of thermostatic drying chamber Under the conditions of dry 1 day, obtain green compact；
(6) green compact that step (5) obtain are placed in atmosphere furnace under argon atmosphere protection, keep the temperature 10 hours in 800 DEG C, so Afterwards heating rate be 3 DEG C/min be warming up to 1600 DEG C, cooled to the furnace after keeping the temperature 12 hours room temperature to get ceramic honey comb at Product.
The performance detection for the high-performance honeycomb ceramic that 1 present invention of test example obtains
The sample for taking 1-4 of the embodiment of the present invention to obtain carries out mechanical property, corrosion resistance, thermal shock resistance and thermal conductivity Test, experimental result is as shown in table 1.Experiment finds that good sample mechanical property of the present invention, good thermal shock, thermal conductivity are high, has Biggish specific heat capacity, and good corrosion resistance.There is preferable tolerance to other inorganic acids in addition to hydrofluoric acid.
1 ceramic honey comb property list of table
Test example 2
The sample for taking the embodiment of the present invention 1 to obtain, sample X-ray diffraction analysis figure spectrum is as shown in Figure 1, produce after material sintering Product principal crystalline phase is β-SiC, and no other apparent miscellaneous phases occur, SEM micrograph as shown in Fig. 2, granular size of the present invention and It is evenly distributed；And ceramic honey comb of the present invention is detected for thermal conductivity, it thermally expands, compression strength has facilitation.

Claims (8)

1. a kind of method for preparing high-performance honeycomb ceramic using Si crystal-cut tailing, which is characterized in that specific step is as follows:
(1) pickling is carried out to Si crystal-cut tailing using the dilute hydrochloric acid that mass concentration is 10-20% and removes metal impurities, through pure Water purification is cleaned 2~3 times, is then heated under the conditions of 200-500 DEG C to the tailing after pickling, and the macromolecule in tailing is removed Impurities of materials obtains micro mist tailing after cooling；
(2) graphite powder, Y are added into micro mist tailing2O3+Al2O3Mixture, the mass ratio of graphite powder and tailing is 12:28； Y2O3+Al2O3Additional amount be 3~10%, wherein Y2O3And Al2O3With the mixing of any mass ratio；Through ball mill or vibration mill mixing Uniformly, powder is obtained, is 8~24 hours according to ball mill incorporation time, is 30 minutes~2 according to vibration mill incorporation time Hour.
(3) into powder be added phenolic resin 5~15%, tung oil 3~10%, through batch mixer mixing 2~6 hours, through mud press, Vacuum deairing machine filter mud-pugging 1~3 time, the sealing ageing of gained pug, Aging Temperature is 20~25 DEG C, and digestion time is 1~3 It；
(4) hydraulic piston type or spiral vacuum-extruder extrusion molding are used through step (3) treated pug, obtains section Having a size of 40~300mm*40~300mm, thickness of honeycomb wall is 0.1~1.5mm, and pore size is 0.4~2mm*0.4~2mm bee Nest ceramic body, extruder vacuum degree are 200-500Pa；
(5) by step (4) obtain green body divulging information, be protected from light, at constant temperature air-dry 2~3 days, then be placed in thermostatic drying chamber 60~ It is 1~3 day dry under the conditions of 180 DEG C, obtain green compact；
(6) green compact that step (5) obtain are placed in air furnace and are buried under carbocyclic ring border, or be placed in argon atmosphere in high-temperature atmosphere furnace It protects under environment, keeps the temperature 3~10 hours in 400~800 DEG C, then heating rate is that 3~10 DEG C/min is warming up to 1300-1600 DEG C, room temperature is cooled to the furnace after keeping the temperature 3-12 hour to get ceramic honey comb finished product.
2. the method according to claim 1, wherein utilizing mass concentration in the step (1) is 10-20%'s Dilute hydrochloric acid carries out pickling to Si crystal-cut tailing and removes metal impurities, cleans 3 times through pure water, then to the tailing after pickling It is heated under the conditions of 400 DEG C, removes the high molecular material impurity in tailing, obtain micro mist tailing after cooling.
3. the method according to claim 1, wherein the step (2) be added into micro mist tailing graphite powder, Y2O3+Al2O3Mixture；Y2O3+Al2O3Additional amount be 5%, wherein Y2O3And Al2O3Mass ratio 2:3；Through ball mill or Vibration mill is uniformly mixed, and obtains powder, is 15 hours according to ball mill incorporation time, is 1 according to vibration mill incorporation time Hour.
4. the method according to claim 1, wherein phenolic resin 10% is added into powder for the step (3), Tung oil 7%, through batch mixer mixing 4 hours, through mud press, vacuum deairing machine filter mud-pugging 2 times, the sealing ageing of gained pug was old Changing temperature is 25 DEG C, and digestion time is 2 days.
5. the method according to claim 1, wherein through step (3), treated, and pug is adopted in the step (4) With hydraulic piston type or spiral vacuum-extruder extrusion molding, acquisition sectional dimension is 120mm*120mm, and thickness of honeycomb wall is 1mm, pore size are the ceramic honey comb green body of 1.2mm*1.2mm, and extruder vacuum degree is 300Pa.
6. the method according to claim 1, wherein the green body for obtaining step (4) in the step (5) is logical Wind is protected from light, air-dries 3 days at constant temperature, then dries 2 days under the conditions of being placed in 100 DEG C of thermostatic drying chamber, obtains green compact.
7. the method according to claim 1, wherein the green compact that step (5) obtain are placed in the step (6) It is buried in air furnace under carbocyclic ring border or argon atmosphere is protected in high-temperature atmosphere furnace, keep the temperature 5 hours in 600 DEG C, then heating rate is 6 DEG C/min is warming up to 1500 DEG C, room temperature is cooled to after keeping the temperature 8 hours with the furnace to get ceramic honey comb finished product.
8. the high-performance honeycomb ceramic obtained such as any one of claim 1-7 the method.
CN201811000952.8A 2018-08-30 2018-08-30 A method of high-performance honeycomb ceramic is prepared using Si crystal-cut tailing Pending CN109265176A (en)

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