CN105948753B - The method that segmented prepares pressureless sintering silicon carbide ceramic liner - Google Patents

The method that segmented prepares pressureless sintering silicon carbide ceramic liner Download PDF

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CN105948753B
CN105948753B CN201610284938.XA CN201610284938A CN105948753B CN 105948753 B CN105948753 B CN 105948753B CN 201610284938 A CN201610284938 A CN 201610284938A CN 105948753 B CN105948753 B CN 105948753B
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silicon carbide
liner
biscuit
prepares
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CN105948753A (en
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郑浦
杨新领
李志强
任付生
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Zhejiang Dongxin New Material Technology Co ltd
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Zhejiang Xinxin Mstar Technology Ltd
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Abstract

The invention discloses a kind of methods that segmented prepares pressureless sintering silicon carbide ceramic liner, comprising the following steps: 1~4 part of carbon source and 1~4 part of B are added in 95~98 parts of silicon carbide micro-powders4C is as sintering aid, as major ingredient, then sequentially adds 40~60 parts of deionized waters, the water soluble polymer binder solution that 5~10 parts of mass concentrations are 8~12%, 2~6 parts of lubricants, uniform stirring is at aqueous slurries；Aqueous slurries progress mist projection granulating, sealing is aging；Resulting aging rear powder successively carries out forming of green body, pre-burning de-waxing, biscuit vehicle system, sintering；Gains are sintered through grinding, are obtained ceramic-lined.

Description

The method that segmented prepares pressureless sintering silicon carbide ceramic liner
Technical field
The present invention relates to a kind of preparation methods of segmented pressureless sintering silicon carbide ceramic liner.
Background technique
With the development of ultra-fine grinding techniques and nanotechnology, after sand mill is as tumbling ball mill, vertical ball mill Third generation extra-fine grinding equipment obtains more and more in fields such as medicine, electronics, mineral, metallurgy, papermaking, ink, cosmetics Using.
Sand mill master wear-resistant liner to be applied is polyurethane, nylon, aluminium oxide, stainless steel, zirconium oxide currently on the market Etc. materials, the thermal coefficient of these types of material it is low be respectively 0.59,0.35,30,33-55,3.0W/mk, stainless steel, aluminium oxide Low with the hardness of zirconium oxide, wear-resisting and corrosion resistance is poor, and sand mill speed of agitator is high, and accumulation of heat is tight in high-speed agitating process Weight, serious wear.Silicon carbide ceramics liner mainly has in reaction sintering silicon carbide ceramic liner and pressureless sintering silicon carbide ceramic Lining, reaction sintering silicon carbide ceramic contain 8~12% free silica, there is the carbon residue not reacted completely on a small quantity, and microstructure is equal Even consistency is poor, limits it in the application of harsh grinding operating condition；And pressureless sintering silicon carbide ceramic even density, resistance to acid and alkali It is good, and the high 140W/mk of thermal conductivity, hardness are greater than 92 (Rockwell hardness) and are only second to diamond and cubic boron nitride, are being sanded Wearability is good when applying in machine, thermal diffusivity is good, greatly reduces the introducing of impurity, excellent properties make it in sand mill field application is got over Carry out wider, the performance of each material liner such as table 1 on existing market.
Table 1
At present prepare silicon carbide ceramics liner biscuit feasible method have injection forming, gel casting forming, isostatic pressing, It is dry-pressing formed.Injection forming is suitable for thin-wall product, but complex technical process, and it is more to influence forming factors, is also easy to produce stomata, opens The defects of splitting, deforming, pressureless sintering silicon carbide original powder granularity < more for producing reaction sintering silicon carbide ceramic liner 1 μm, particle is easy to reunite, and the big part pressureless sintering silicon carbide ceramic technology of injection forming is immature, almost without report；Gel Injection molding can efficiently control particle agglomeration, prepare uniform, high-intensitive green body, but due to the starting of China's gel casting process compared with In evening, certain key technologies are also unresolved, and it is also immature such as to produce pressureless sintering silicon carbide ceramic technology with the technical industry metaplasia；Deng The blank density of hydrostatic profile is evenly distributed, but since the sintering shrinkage of pressureless sintering silicon carbide is very big, molding green body size It being difficult to be precisely controlled, stock size surplus is larger, and it is serious to the waste of powder, furthermore, large-scale equal pressing equipment is complicated, auxiliary Equipment is more, and cost is higher.
Dry-pressing formed advantage is that production process is simple, and consistency is high, and product size is accurate, and surface quality is high, equipment machine Tool high degree of automation, may be implemented continuous production；The disadvantage is that being difficult to form for the product of article shape complexity, mold Abrasion is big, and pressure is unevenly distributed, density unevenness.
In contrast, sand mill liner is mostly the cylindrical shape of simple shape.Therefore, injection forming and gel casting forming by It is immature in complex technical process, technology, the reasons such as forming factors are more, and production efficiency is low are influenced, are not had compared to dry-pressing formed Advantage, but green body of the dry-pressing formed biscuit height higher than 400mm is difficult to suppress, while yield rate since frictional resistance is big It is low.
Saint-Gobain of external France, Germany match thinkling sound Tyke can directly accomplish grinding for 1200mm high using large-scale cold isostatic press Grinding barrel, high production cost, price are extremely expensive.
Summary of the invention
The technical problem to be solved in the present invention is to provide the sides that a kind of segmented prepares pressureless sintering silicon carbide ceramic liner Method, the present invention is high using dry-pressing formed combination isostatic pressing preparation consistency, structure is uniform, has some strength, Ke Yijin The mach green body of row, sintered density is up to 3.10g/cm after sintering3, due to using segmented, can control very well The precision of product mill processing, processing efficiency and yield rate.
In order to solve the above technical problem, the present invention provides a kind of segmenteds to prepare pressureless sintering silicon carbide ceramic liner Method, it is characterized in that the following steps are included:
1), mixing:
1~4 part of (preferably 3 parts) carbon source and 1~4 part of (preferably 2 parts) B are added in 95~98 parts of silicon carbide micro-powders4C (D50=1.0~3.0 μm) be used as sintering aid, as major ingredient, then sequentially add 40~60 parts (preferably 50 parts) go from Sub- water, 5~10 parts of mass concentrations are the water soluble polymer binder solution (aqueous solution) of 8~12% (preferably 10%), 2~ 6 parts of (preferably 3 parts) lubricants, uniform stirring is at (can carry out in the ball mill) aqueous slurries；
Above part refers both to parts by weight；
2), mist projection granulating:
Aqueous slurries obtained by step 1) are subjected to mist projection granulating, control inlet temperature is 200~350 DEG C (preferably 250 DEG C), outlet temperature be 100~180 DEG C (preferably 120 DEG C), prepare resulting mist projection granulating powder sealed under room temperature environment it is old Rotten 3~10 days (preferably 5 days) obtain aging rear powder；
Remarks explanation: atomization disk rotating speed is 8000~12000r/min, prepares resulting mist projection granulating powder moisture control and exists 0.8~2% (quality %)；
3), forming of green body:
By step 2) it is resulting it is aging after powder is fitted into mold, first carry out it is dry-pressing formed, then carry out again grade static pressure at Reason, to obtain biscuit (for fine and close, uniform biscuit)；
4), pre-burning de-waxing:
The resulting biscuit of step 3) is put into vacuum wax expelling furnace, 600~900 DEG C at a temperature of keep the temperature 2~5h of pre-burning Hour (preferably 800 DEG C, 4h)；
5), biscuit vehicle system:
Required shape is made in biscuit vehicle after the resulting pre-burning of step 4)；
6) it, is sintered:
The resulting biscuit of step 5) is put into vacuum sintering furnace, under the protection of inert gas, in 2080~2200 DEG C 0.5~1.5h of temperature；
Gains are sintered through grinding (belonging to routine techniques), are obtained ceramic-lined.
Remarks explanation:
Grinding specifically refers to that gains (sintered body) will be sintered according to drawing in large-scale flat stone mill, inner circle mill, outer circle Mill processing is carried out on mill；This belongs to routine techniques.
The following performance detection of resulting ceramic-lined progress:
The product processed (that is, ceramic-lined) drainage is detected into bulk density, bulk density requirement >=3.10g/ cm3, visual examination grinding drum internal circular surfaces, which are not allow for stomata (stomatas that 200 μm of >), to be existed, and detection hardness HRA requirement >= 91。
The improvement of the method for pressureless sintering silicon carbide ceramic liner is prepared as segmented of the invention:
The silicon carbide micro-powder D50(meso-position radius)=0.4~0.8 μm；
The carbon source is carbon black (nanometer carbon black, D50=30nm), aquadag (D50=0.3 μm)；
The water soluble polymer binder is polyvinyl alcohol, methylcellulose；
The lubricant is glycerol, water-soluble paraffin wax emulsions (solid content 30%).
The further improvements in methods of pressureless sintering silicon carbide ceramic liner are prepared as segmented of the invention:
It is the liner of 1200mm grinding drum when manufacturing height, and requiring the outer diameter (overall diameter) of the liner is 300mm, internal diameter When (interior diameter) is 282mm,
The liner is divided into 4 sections to process, controls the size of every section of liner biscuit are as follows: outer diameter 365mm, internal diameter 335mm, High 363mm (control that above-mentioned size can be realized by mold)；
It is dry-pressing formed under 1000 tons of four-column hydraulic press, pressure 20MPa, dwell time 100s；So use polybag (flexible plastic pouch) wraps, be put into cold isostatic press carry out isostatic pressing, pressure 200Mpa, dwell time 15min, from And obtain biscuit (for fine and close, the uniform biscuit of structure).
The further improvements in methods of pressureless sintering silicon carbide ceramic liner are prepared as segmented of the invention:
As grinding make obtained by every section of liner internal circular surfaces based on verticality≤20 μm of end face, end face it is bright and clean Spend≤0.2 μm (when can guarantee that 4 sections of liners are used cooperatively in this way, and being able to achieve gapless fit closely).
The present invention has following technical advantage:
1. the present invention has expanded pressureless sintering silicon carbide ceramic in the application in sand mill field, existing sand is fundamentally solved Grinding machine high-volume uses polyurethane liner, not wear-resisting, the serious problem of accumulation of heat；
2. the present invention uses dry-pressing combination isostatic pressing, than traditional injection forming, preparation process is more simple, product matter Amount is more preferable；
3. since regular industrial is generally higher than 1.2m using the height of the liner of sand mill, pressureless sintering silicon carbide ceramic Need biscuit height to be prepared to be greater than 1.5m, dry-pressing formed fashionable dress powder height needs up to 3m or more, cannot carry out it is dry-pressing formed, The present invention provides the thinking that a kind of segmented prepares sand mill liner, and the liner prepared is fitted into sand mill, can be improved Efficiency is produced and processed, production cost is reduced, while in client's use process, which section goes wrong, and can replace which section, is greatly dropped Low-maintenance use cost；
4, the present invention is that a cylinder is divided into four sections, and dry-pressing formed combination isostatic pressing is ground after sintering Processing, carries out unified installation after the assay was approved, and the equipment routinely produced and used at present can satisfy processing request completely, greatly mention High finished product rate reduces production cost, and if directly doing the grinding drum of 1200mm high, all devices require to purchase again, pole It is big to increase machining difficulty and production cost.
Specific embodiment
Embodiment 1, preparation specification are 300mm (outer diameter) * 282mm (internal diameter) * 1200 (height) mm pressureless sintering preparation carbonization The liner is divided into 4 sections and processed by the ceramic-lined method of silicon；Successively follow the steps below:
1), mixing:
In 95 parts of silicon carbide (D50=0.5 μm) in nanometer carbon black (D as sintering aid is added50=30nm) 3 parts and B4C Then 2 parts of (D50=1.0 μm) sequentially adds 50 parts of deionized waters as solvent as major ingredient, and 5 parts of polyvinyl alcohol water solution (mass concentration of polyvinyl alcohol is 10%) is used as binder, and 3 parts of water-soluble paraffin wax emulsions (solid content 30%) are used as lubricant, It is stirred into aqueous slurries in the ball mill；
2), mist projection granulating:
Aqueous slurries obtained by step 1) are subjected to mist projection granulating, at 250 DEG C, outlet temperature control exists for inlet temperature control 120 DEG C, atomization disk rotating speed is 10000r/min, prepares resulting mist projection granulating powder moisture control in 1.0% (quality %), then Seal at room temperature aging 5 days it is spare；
3), forming of green body:
Highly it is 1200mm grinding drum by this according to product drawing size, is equally divided into 4 sections, every section of height is 300mm, That is, every section of grinding drum dimensions is 300mm (outer diameter) * 282mm (internal diameter) * 300 (height) mm, according to the shrinkage ratio of product with stay There is machining allowance, the size of control compacting biscuit is 365mm (outer diameter) * 335mm (internal diameter) * 363 (height) mm, selects matched steel The resulting aging rear powder of step 2) is fitted into mold by mold, and dry-pressing formed under 1000 tons of four-column hydraulic press, pressure is 20MPa, dwell time 100s wrap the biscuit suppressed with flexible plastic pouch, be put into cold isostatic press carry out etc. it is quiet Pressure processing, pressure 200Mpa, dwell time 15min, to obtain fine and close, the uniform biscuit of structure.
4), pre-burning (de-waxing):
The resulting biscuit of step 3) is put into pre-burning in vacuum wax expelling furnace, calcined temperature is 800 DEG C, keeps the temperature 4h.
5), biscuit vehicle system:
Vehicle system is carried out to the biscuit after pre-burning in strict accordance with drawing, the margin of tolerance grinds machining allowance within 0.2mm 0.6mm。
6) it, is sintered:
The biscuit processed is fitted into vacuum sintering furnace, argon gas protection is filled with, is sintered in 2100 DEG C, kept the temperature 1h.By the sample sintered drainage detection density, density 3.12g/cm3, density meets the requirements, then carry out grinding plus Work；
7), grinding:
The product that will be sintered first carries out end face mill processing on large-sized numerical control flat stone mill, controls every section of grinding drum height For 300 ± 0.1mm, both ends of the surface polishing is then carried out on numerical control double-sided, guarantees finish≤0.2 μm of end face；Then big Workpiece one end is caught with three-jaw on type inner circle mill, the gauge outfit of dial gauge is pressed in grinding drum inner circle, grinding drum is then rotated, is seen The variation of pointer on table is examined, adjusts the bounce of grinding drum control table within ± 0.05mm, then starts mill processing inner circle, Midway is tested correction with amesdial, and inner circle mill is machined to 282 ± 0.1mm, guarantee verticality of the inner circle based on end face≤20 μ m；Then plug is made, plug is covered in inner circle, peripheral milling processing is then carried out on large-scale peripheral milling, is carried out with amesdial The inspection of concentricity, the bounce of control table is within ± 0.05mm, and then excircle dimension is machined to 300 ± 0.1mm, will add Then the pure and fresh clean drying of the good grinding drum ultrasonic wave of work carries out inside and outside circle size on three coordinate detectors, concentricity, puts down The detection of row degree, flatness, meeting drawing requirement is qualified product.
8), performance detection
By pressureless sintering silicon carbide ceramic grinding drum obtained by above-mentioned steps, visual examination internal circular surfaces do not have stomata, drain Method detects bulk density 3.14g/cm3, detect Rockwell hardness (HRA) 92.5.
Embodiment 2, by the " nanometer carbon black (D in 1 step 1) of embodiment50=30nm) " it is changed to " aquadag (D50=0.3 μm) ", remaining is equal to embodiment 1；Its performance test results are as follows: it is 3.08g/cm that drainage, which detects bulk density,3, Rockwell is hard Spend (HRA) 90.
Embodiment 3, by the " B in 1 step 1) of embodiment4C(D50=1.0 μm) 2 parts " it is changed to " B4C(D50=3.0 μm) 2 parts " Remaining is equal to embodiment 1；Its performance test results are as follows: it is 3.12g/cm that drainage, which detects bulk density,3, Rockwell hardness (HRA)91。
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (2)

1. the method that segmented prepares pressureless sintering silicon carbide ceramic liner, it is characterized in that the following steps are included:
1), mixing:
3 parts of carbon sources and 2 parts of B are added in 95~98 parts of silicon carbide micro-powders4C is as sintering aid, as major ingredient, then successively It is added 50 parts of deionized waters, the water soluble polymer binder solution that 5~10 parts of mass concentrations are 10%, 3 parts of lubricants, uniformly Stir into aqueous slurries；
Above part refers both to parts by weight；
The silicon carbide micro-powder D50=0.4~0.8 μm；
The carbon source is carbon black, aquadag；
The water soluble polymer binder is polyvinyl alcohol, methylcellulose；
The lubricant is glycerol, water-soluble paraffin wax emulsions；
2), mist projection granulating:
Aqueous slurries obtained by step 1) are subjected to mist projection granulating, control inlet temperature is 200~350 DEG C, outlet temperature is 100~ It 180 DEG C, prepares resulting mist projection granulating powder and is sealed under room temperature environment aging 3~10 days, obtain aging rear powder；
3), forming of green body:
By step 2) it is resulting it is aging after powder be fitted into mold, first carry out dry-pressing formed, then carry out isostatic pressing again, from And obtain biscuit；
When the liner that manufacture height is 1200mm grinding drum, and when to require the outer diameter of the liner be 300mm, internal diameter is 282mm,
The liner is divided into 4 sections to process, controls the size of every section of liner biscuit are as follows: outer diameter 365mm, internal diameter 335mm are high 363mm；
It is dry-pressing formed under 1000 tons of four-column hydraulic press, pressure 20MPa, dwell time 100s；So wrapped up with polybag It is good, it is put into cold isostatic press and carries out isostatic pressing, pressure 200Mpa, dwell time 15min, to obtain biscuit；
4), pre-burning de-waxing:
The resulting biscuit of step 3) is put into vacuum wax expelling furnace, 600~900 DEG C at a temperature of keep the temperature 2~5h of pre-burning hours；
5), biscuit vehicle system:
Required shape is made in biscuit vehicle after the resulting pre-burning of step 4)；
6) it, is sintered:
The resulting biscuit of step 5) is put into vacuum sintering furnace, under the protection of inert gas, in 2080~2200 DEG C of temperature 0.5~1.5h of degree heat preservation；
Gains are sintered through grinding, are obtained ceramic-lined.
2. the method that segmented according to claim 1 prepares pressureless sintering silicon carbide ceramic liner, it is characterized in that:
As grinding make obtained by every section of liner internal circular surfaces based on verticality≤20 μm of end face, the finish of end face≤ 0.2μm。
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CN106747459A (en) * 2017-01-21 2017-05-31 安徽东迅密封科技有限公司 Anti-corrosion abrasion-resistant sintered silicon carbon seal and its processing technology
CN109776094A (en) * 2017-11-10 2019-05-21 中国建筑材料科学研究总院有限公司 Ultraprecise ceramic guide rail and preparation method thereof
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