CN104308072A - Carbon fiber-based precoated sand material for selective laser sintering and preparation method thereof - Google Patents

Carbon fiber-based precoated sand material for selective laser sintering and preparation method thereof Download PDF

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CN104308072A
CN104308072A CN201410467968.5A CN201410467968A CN104308072A CN 104308072 A CN104308072 A CN 104308072A CN 201410467968 A CN201410467968 A CN 201410467968A CN 104308072 A CN104308072 A CN 104308072A
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sand
carbon fiber
precoated sand
laser sintering
selective laser
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CN104308072B (en
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芦刚
毛蒲
严青松
卢百平
余欢
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Nanchang Hangkong University
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Nanchang Hangkong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C1/00Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C1/00Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
    • B22C1/02Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C1/00Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
    • B22C1/16Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
    • B22C1/20Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents
    • B22C1/22Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins
    • B22C1/2233Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

Abstract

The invention discloses a carbon fiber-based precoated sand material for selective laser sintering and a preparation method thereof. The carbon fiber-based precoated sand material comprises chopped carbon fibers, crude sand, an organic binder, a curing agent, a lubricant, a coupling agent and a dispersant. The preparation method comprises the following steps of carrying out surface modification treatment on the chopped carbon fibers, heating the crude sand, adding resin, adding a part of calcium stearate and a prepared coupling agent aqueous solution, adding a chopped fiber-containing urotropine curing agent, adding the rest of the calcium stearate, carrying out cooling and carrying out screening and sand discharge to obtain the product. The carbon fiber-based precoated sand material has the advantages that 1, the carbon fibers have thermal conduction effects, limit integral shrinkage of a sintered part to a certain degree and reduce warp phenomenon in molding, and 2, through laser sintering, the precoated sand substantially improves resin precoated sand thermostability, promotes curing reaction of phenolic resin at locals in the sintered layer and between the sintered layers and obviously improves laser sintering forming part blank strength.

Description

For the carbon fiber-based precoated sand material and preparation method thereof of selective laser sintering
Technical field
The invention belongs to field of novel, be specifically related to a kind of carbon fiber-based precoated sand material for selective laser sintering and preparation method thereof.
Background technology
Selective Laser Sintering (SLS), a kind of using laser as controlled thermal source, by solid freeform technology (the Solid Freeform Fabrication of dusty material selective sintering, SFF), it adopts discrete, accumulation forming principle, computer Computer Aided Design and manufacture, by the three-dimensional CAD model of part is carried out hierarchy slicing process, obtain the cross section profile information of every one deck, again solid powder material is sintered, make bonding mutually between layers, progressively superpose, thus obtain 3D solid fast.Not by the restriction of part shape complex structure degree, without any need for moulds of industrial equipment, and manufacturing cycle short production cost is low.Precoated sand is one of the common used material for selective laser sintering RP technique, its surface is coated with by various adding materials such as phenolic resins, when laser sintering rapid forming technology, make cooling curing after its melted by heat by LASER HEATING phenolic resins, thus precoated sand is bondd form core.
What require along with, complex-shapedization thin-wall light-weighted to foundry goods, dimensional accuracy and surface quality etc. improves constantly, and the complicated sand mold (core) utilizing SLS technology to prepare also has certain gap in institutional framework, mechanical property, dimensional accuracy and surface quality etc.Due to the poor thermal conductivity of precoated sand, laser beam irradiation time is short, precoated sand sintered part ubiquity the defects such as sintering initial strength on the low side and surface quality difference, and the content of binding agent is higher, cause the gas forming amount of sand mold (core) large, gas permeability and collapsibility poor, be difficult to the production requirement meeting high-quality dominance energy intricate casting.
Carbon fiber has low-density, high strength, high-modulus, high temperature resistant, resist chemical, low resistance, high heat conduction, low-thermal-expansion, the characteristic such as chemically-resistant radiation and good biocompatibility.In addition, also have the distinctive flexibility of fiber and programmable, its specific strength and specific modulus are all better than other inorfils.Adopt carbon fiber-reinforced precoated sand material, in laser sintered process, carbon fiber does not participate in the interaction between laser and dusty material in principle, just plays heat conducting effect mutually as one in composition, improves thermal conductivity and the electric conductivity of precoated sand material.In addition, due to the existence of carbon fiber, certain impact must be served on the densified of precoated sand, limit the contraction of sintered part entirety to a certain extent, ensure that the dimensional accuracy of sintered part.
Summary of the invention
The object of the present invention is to provide a kind of carbon fiber-based precoated sand material for selective laser sintering and preparation method thereof; The method is using carbon fiber as the important reinforcement of precoated sand material, carbon fiber is by a kind of polycrystalline fibre of incomplete graphite crystallization along fiber axially-aligned, have the advantage of the compactness strengthening laser sintered of precoated sand, the SLS precoated sand sintered part simultaneously obtained has higher mechanical property and dimensional accuracy.
The major experimental material that the present invention is used:
For the carbon fiber-based precoated sand material of selective laser sintering, its constituent is: roughing sand 90 ~ 95%, chopped carbon fiber are 2.5 ~ 5.0%, organic binder bond 2.5 ~ 3%, curing agent 0.375 ~ 0.51%, lubricant are 0.0015 ~ 0.0018%, coupling agent be 0.0025 ~ 0.003% and dispersant be 0.1125 ~ 0.153%.
Chopped carbon fiber: phosphorus content>=95%, average diameter is 7 ~ 10 μm, and length is 1 ~ 2.5mm, and tensile strength is 3.6 ~ 3.8 GPa, and growth rate is 1.5%, and modulus is 220-240 GPa, and bulk density is 1.76 g/cm 3.
Roughing sand: spherical or extremely spheroidal nice foundry sand, dihedral coefficient≤1.1, composition is Al 2o 3>=75%, Fe 2o 3≤ 5%, TiO 2≤ 5%, refractoriness is 1800 ~ 2000 DEG C, and coefficient of thermal expansion is 0.13%(1000 DEG C of heating 10 minutes), average grain diameter is less than 0.212mm, granularmetric composition 40 ~ 80 order.
Organic binder bond: solid thermoplastics phenolic resins, softening point is 80 ~ 90 DEG C, free phenol content≤1.8%, polymerization speed is (150 DEG C) 58 ~ 70s, in yellow, transparent cake, through pulverizing, being milled into powder, cross packed for standby use after 100 mesh sieves, model is PF-1904.
Curing agent: methenamine (hexa), white crystalline powder, fusing point is 119 ~ 122 DEG C,
About 263 DEG C of distillations.
Lubricant: calcium stearate, evenly trickle white powder, fusing point is greater than 140 DEG C, and fineness is 200 mesh sieve percent of pass >=99.0%.
Coupling agent: silane coupling agent KH-550, colourless transparent liquid, boiling point is 217 DEG C.
Dispersant: hydroxypropyl methylcellulose (HPMC) dispersant.
First the present invention carries out surface modification treatment to chopped carbon fiber, prepare carbon fiber-based precoated sand material by following coating technique flow process again: roughing sand heat-add resin-add part of stearic acid calcium and the coupling agent aqueous solution-add for preparing containing chopped strand urotropine firming agent-adding residue calcium stearate-cooling-screening shakes out, and obtains selective laser sintering carbon fiber-based precoated sand material.
The preparation method of the carbon fiber-based precoated sand material for selective laser sintering of the present invention, is characterized in that step is as follows:
Step one: adopt gamma-ray irradiation facture or electrochemical polymerization method to carry out surface modification treatment to chopped carbon fiber.
Step 2: adopt hot method coating technique, roughing sand is carried out sieve the sand grains obtaining required particle diameter, be heated 180 DEG C ~ 200 DEG C again, be discharged in puddle mixer after roughing sand being cooled to 140 DEG C ~ 160 DEG C, when roughing sand temperature is down to 110 DEG C ~ 130 DEG C, resin is added wherein, roughing sand and resin are fully mixed and even overlay film.
Step 3: the chopped carbon fiber after step one being processed joins in urotropine firming agent according to a certain percentage, then add HPMC dispersant, stirred by ultrasonic vibration, chopped carbon fiber is dispersed in curing agent solution uniformly.
Step 4: the coupling agent aqueous solution adding part calcium stearate He prepare in step 2 gained precoated sand, stir a period of time, when precoated sand temperature is down to about 100 DEG C, the urotropine firming agent that again step 3 be with the addition of chopped carbon fiber adds in precoated sand, resin is made to be cured reaction under heat effect, form a kind of molten not insoluble material, sand grains is bonded together securely, chopped carbon fiber is also evenly distributed in overlay film sand grains simultaneously, obtained carbon fiber-based sand in coating phenolic resin.
Step 5: added in the precoated sand configured by residue calcium stearate, fully mix, put sand, water-cooled is to room temperature, broken, and screening can obtain the carbon fiber-based precoated sand of selective laser sintering.
The invention provides a kind of carbon fiber-based precoated sand material for selective laser sintering, have the following advantages compared with the precoated sand material prepared with traditional approach:
(1) in laser sintered process, carbon fiber does not participate in the interaction between laser and dusty material in principle, just plays heat conducting effect mutually as one in composition.In addition, due to the existence of carbon fiber, certain impact must be served on the densified of coated sand, limit the contraction of sintered part entirety to a certain extent;
(2) adding due to chopped carbon fiber, improve the rate of heat transfer of coated sand material granule inside to a certain extent, this is for the homogenising accelerating precoated sand temperature around carbon fiber, and then reducing the thermograde in sintering region, the warping phenomenon reduced in forming process is very favourable;
(3) precoated sand is after laser sintered melting, and its viscosity significantly reduces, in viscous state.And temperature is higher, its viscosity is lower, is more conducive to the densified of powder particle.But the too high meeting of temperature makes precoated sand produce thermal decomposition, thus reduces the mechanical property of sintered part.Chopped carbon fiber add the heat endurance significantly improving coated sand, facilitate the phenolic resin curing reaction of local and interlayer junction in sinter layer.Secondly, chopped carbon fiber add the effect serving bearing stress, thus reach the effect strengthening the first base intensity of precoated sand sintering forming element.
In a word, the present invention adopts chopped carbon fiber to strengthen selective laser sintering precoated sand material, because coated sand and chopped carbon fiber surface create the bonding of chemistry, the heat endurance of precoated sand is improved, the enhancing effect of chopped strand to precoated sand is fairly obvious, it is high that selective laser sintering carbon fiber-based precoated sand sintered part has first intensity, collapsibility is good, the advantage that gas forming amount is little, can be used for selective laser sintering complex structure, the foundry goods that performance requirement is high, especially for precinct laser sintering technology monolithic molding complexity overlay film sand mold (core) and in high-performance large-scale complex thin wall castings fast precise is shaping, there is superiority in conjunction with model casting, for lifting Aero-Space, the rapid response manufacturing ability of auto industry and other scientific domain has huge using value and bright prospects.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of selective laser sintering carbon fiber-based precoated sand material of the present invention.
Detailed description of the invention
Embodiment 1
A kind of carbon fiber-based precoated sand material for selective laser sintering carries out according to the following steps:
Step one: adopt gamma-ray irradiation facture to carry out surface modification treatment to chopped carbon fiber, first be 7 μm by diameter, length is that the chopped carbon fiber of 2.5mm puts into acetone soln, dry after cleaning 48h, immersed again be equipped with active functional group group concentration be in the irradiation bottle of the tetraethylene-glycol acetone soln of 2 mol/L, by one end maintaining nitrogen purge 2 min of irradiation bottle 2 passages, until sealing after oxygen in eliminating bottle, be placed in Co gamma-ray irradiation source, carry out co-irradiation grafting modification by the irradiation dose of 200kGy.After chopped carbon fiber radiation treatment, more for subsequent use in 50 DEG C of drying 12 h with being placed in vacuum drying oven after acetone cleaning.
Step 2: adopt hot method coating technique, is undertaken the spherical of dihedral coefficient≤1.1 or extremely spheroidal nice foundry sand sieving to obtain 70/270 object five sieve series sand 1000g, Solid thermoplastic's phenolic resins is ground into the even Phenolic resin powder that particle diameter is 60 μm.Again nice foundry sand is heated to 180 DEG C, crossing after nice foundry sand is cooled to 150 DEG C by 50s is discharged in sand muller, when nice foundry sand temperature is down to 120 DEG C, 25g phenolic resins (account for nice foundry sand heavy 2.5%) is added wherein, in puddle mixer, stir 80s, nice foundry sand and phenolic resins are fully mixed and even overlay film.
Step 3: the chopped carbon fiber that step one was processed take 35g(account for nice foundry sand heavy 3.5%) add in the aqueous solution that 3.75g hexa (mass fraction accounting for Phenolic resin powder is 15%) prepares, add 0.12gHPMC dispersant (mass fraction accounting for hexa is 3.0%) again, stirred by ultrasonic vibration, chopped carbon fiber is dispersed in hexa solution uniformly.
Step 4: (mass fraction accounting for Phenolic resin powder is 1% to add 1.5g part calcium stearate (mass fraction accounting for phenolic resins is 6.0%) and 0.25g coupling agent aqueous solution in step 2 gained precoated sand, be made into the aqueous solution that mass fraction is 10%), puddle mixer stirs 35s.When precoated sand temperature is down to 110 DEG C, then the hexa solution that step 3 be with the addition of chopped carbon fiber adds in precoated sand, and puddle mixer stirs 80s, obtained carbon fiber-based sand in coating phenolic resin.
Step 5: again 1.5g is remained calcium stearate (mass fraction accounting for phenolic resins is 6.0%) and add in the precoated sand prepared, puddle mixer stirs 60s and fully mixes, and put sand, water-cooled is to room temperature, broken, screening, can obtain the carbon fiber-based precoated sand of selective laser sintering.
Embodiment 2
A kind of carbon fiber-based precoated sand material for selective laser sintering carries out according to the following steps:
Step one: adopt electrochemical polymerization facture to carry out surface modification treatment to chopped carbon fiber, first it is 7 μm by diameter, length is that the chopped carbon fiber of 1.5mm is put into after acetone soln cleans 48h, be electrolyte again with sulfuric acid, deionized water is solvent, add mass fraction be 1% monomer be made into electrolyte, then be anode with carbon fiber, graphite is negative electrode, at ambient temperature, after carrying out electrolysis polymerization 60s by 90 mA polymerization electric currents, by deionized water, chopped carbon fiber surface is cleaned again, thus the electrolyte ion of removing remained on surface and unconverted monomer, finally put it in vacuum drying oven for subsequent use in 50 DEG C of drying 12 h.
Step 2: adopt hot method coating technique, carries out screening and obtains 70/200 object four sieve series sand 1000g, Solid thermoplastic's phenolic resins is ground into the even Phenolic resin powder that particle diameter is 60 μm by the spherical of dihedral coefficient≤1.1 or extremely spheroidal nice foundry sand.Nice foundry sand is heated to 200 DEG C, crossing after nice foundry sand is cooled to 160 DEG C by 50s is discharged in sand muller, when nice foundry sand temperature is down to 130 DEG C, 30g phenolic resins (account for nice foundry sand heavy 3.0%) is added wherein, in puddle mixer, stir 100s, nice foundry sand and phenolic resins are fully mixed and even overlay film.
Step 3: the chopped carbon fiber that step one was processed take 50g(account for nice foundry sand heavy 5.0%) add in the aqueous solution that 5.1g hexa (mass fraction accounting for Phenolic resin powder is 17%) prepares, add 0.12gHPMC dispersant (mass fraction accounting for hexa is 3.0%) again, stirred by ultrasonic vibration, chopped carbon fiber is dispersed in hexa solution uniformly.
Step 4: (mass fraction accounting for Phenolic resin powder is 1% to add 1.5g part calcium stearate (mass fraction accounting for phenolic resins is 6.0%) and 0.3g coupling agent aqueous solution in step 2 gained precoated sand, be made into the aqueous solution that mass fraction is 10%), puddle mixer stirs 35s.When precoated sand temperature is down to 110 DEG C, then the hexa solution that step 3 be with the addition of chopped carbon fiber adds in precoated sand, and puddle mixer stirs 100s, obtained carbon fiber-based sand in coating phenolic resin.
Step 5: again 1.5g is remained calcium stearate (mass fraction accounting for phenolic resins is 6.0%) and add in the precoated sand prepared, puddle mixer stirs 60s and fully mixes, and put sand, water-cooled is to room temperature, broken, screening, can obtain the carbon fiber-based precoated sand of selective laser sintering.

Claims (9)

1., for the carbon fiber-based precoated sand material of selective laser sintering, its constituent is: roughing sand 90 ~ 95%, chopped carbon fiber are 2.5 ~ 5.0%, organic binder bond 2.5 ~ 3%, curing agent 0.375 ~ 0.51%, lubricant are 0.0015 ~ 0.0018%, coupling agent be 0.0025 ~ 0.003% and dispersant be 0.1125 ~ 0.153%.
2. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described chopped carbon fiber, its phosphorus content >=95%.
3. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described roughing sand is spherical or extremely spheroidal nice foundry sand, and dihedral coefficient≤1.1, composition is Al 2o 3>=75%, Fe 2o 3≤ 5%, TiO 2≤ 5%, refractoriness is 1800 ~ 2000 DEG C, and coefficient of thermal expansion is 0.13%(1000 DEG C of heating 10 minutes), average grain diameter is less than 0.212mm, granularmetric composition 40 ~ 80 order.
4. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, it is characterized in that: described organic binder bond is solid thermoplastics phenolic resins, softening point is 80 ~ 90 DEG C, free phenol content≤1.8%, polymerization speed is (150 DEG C) 58 ~ 70s, in yellow, transparent cake.
5. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described curing agent is methenamine (hexa), white crystalline powder.
6. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described lubricant is calcium stearate, evenly trickle white powder.
7. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described coupling agent is silane coupling agent KH-550, colourless transparent liquid.
8. the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that: described dispersant is hydroxypropyl methylcellulose HPMC dispersant.
9. a preparation method for the carbon fiber-based precoated sand material for selective laser sintering according to claim 1, is characterized in that step is as follows:
Step one: adopt gamma-ray irradiation facture or electrochemical polymerization method to carry out surface modification treatment to chopped carbon fiber;
Step 2: adopt hot method coating technique, roughing sand is carried out sieve the sand grains obtaining required particle diameter, be heated 180 DEG C ~ 200 DEG C again, be discharged in puddle mixer after roughing sand being cooled to 140 DEG C ~ 160 DEG C, when roughing sand temperature is down to 110 DEG C ~ 130 DEG C, resin is added wherein, roughing sand and resin are fully mixed and even overlay film;
Step 3: the chopped carbon fiber after step one being processed joins in urotropine firming agent according to a certain percentage, stirs with ultrasonic vibration, chopped carbon fiber is dispersed in curing agent solution uniformly;
Step 4: the coupling agent aqueous solution adding part calcium stearate He prepare in step 2 gained precoated sand, stir a period of time, when precoated sand temperature is down to about 100 DEG C, the urotropine firming agent that again step 3 be with the addition of chopped carbon fiber adds in precoated sand, resin is made to be cured reaction under heat effect, form a kind of molten not insoluble material, sand grains is bonded together securely, obtained carbon fiber-based sand in coating phenolic resin;
Step 5: added in the precoated sand prepared by residue calcium stearate, fully mix, put sand, water-cooled is to room temperature, and broken, screening, can obtain the carbon fiber-based precoated sand of selective laser sintering.
CN201410467968.5A 2014-09-16 2014-09-16 Carbon fiber-based precoated sand material for selective laser sintering and preparation method thereof Expired - Fee Related CN104308072B (en)

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CN104858356A (en) * 2015-05-07 2015-08-26 马鞍山市恒毅机械制造有限公司 Precoated sand for high-strength crack-resistant hot method and preparation method thereof
CN104889313A (en) * 2015-04-24 2015-09-09 北京仁创科技集团有限公司 Coated sand preparation method
CN105215260A (en) * 2015-09-21 2016-01-06 济南大学 A kind of for the low precoated sand preparation method that gets angry of laser sintered 3D printing
CN105236826A (en) * 2015-10-30 2016-01-13 西南科技大学 Preparation method of thermo-conductive insulation composite material
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CN104858356A (en) * 2015-05-07 2015-08-26 马鞍山市恒毅机械制造有限公司 Precoated sand for high-strength crack-resistant hot method and preparation method thereof
CN105215260A (en) * 2015-09-21 2016-01-06 济南大学 A kind of for the low precoated sand preparation method that gets angry of laser sintered 3D printing
CN105236826A (en) * 2015-10-30 2016-01-13 西南科技大学 Preparation method of thermo-conductive insulation composite material
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CN108296410A (en) * 2017-09-27 2018-07-20 柳州市柳晶科技股份有限公司 A kind of 3D printing high intensity precoated sand and preparation method thereof
CN108296410B (en) * 2017-09-27 2020-04-10 柳州市柳晶科技股份有限公司 3D prints and uses high strength tectorial membrane sand
CN108296420A (en) * 2017-10-27 2018-07-20 柳州市柳晶科技股份有限公司 A kind of 3D printing precoated sand and preparation method thereof
CN107931530A (en) * 2017-11-27 2018-04-20 四川共享铸造有限公司 A kind of sand mold riser runner and preparation method
CN108994257A (en) * 2018-08-28 2018-12-14 宝鸡高新智能制造技术有限公司 A kind of 3D printing forms the casting method of large-scale elaborate inner cavity component
CN110125321A (en) * 2019-04-28 2019-08-16 广西慧思通科技有限公司 A kind of 3D printing precoated sand and preparation method thereof
CN110523913A (en) * 2019-08-31 2019-12-03 新疆泰格迪木国际贸易有限公司 A kind of preparation method of high intensity 3D printing precoated sand
CN111644574A (en) * 2020-06-30 2020-09-11 潍柴动力股份有限公司 Preparation method of reinforced thin-wall sand core
CN111889615A (en) * 2020-07-30 2020-11-06 柳晶(溧阳)环保科技有限公司 High-temperature-resistant precoated sand

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