CN104744049A - Preparation method of laser sintering 3D printing rapid prototyping silicon nitride powder material - Google Patents
Preparation method of laser sintering 3D printing rapid prototyping silicon nitride powder material Download PDFInfo
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- CN104744049A CN104744049A CN201510125381.0A CN201510125381A CN104744049A CN 104744049 A CN104744049 A CN 104744049A CN 201510125381 A CN201510125381 A CN 201510125381A CN 104744049 A CN104744049 A CN 104744049A
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Abstract
The invention discloses a preparation method of a laser sintering 3D printing rapid prototyping silicon nitride powder material. The preparation method is characterized by comprising the following steps: firstly, pretreating silicon nitride ceramic powder with gamma-methacryloxypropyltrimethoxysilane in an ethyl alcohol solvent to obtain pretreated silicon nitride ceramic powder; then, in percentage by mass, adding 75-88% of the pretreated silicon nitride ceramic powder, 5-15% of phenolic resin, 0.5-1.5% of melamine and 0.2-1.5% of glyceryl tristearate into a grinding miller, starting the grinding miller, grinding for 10min at 200r/min, and adding acetone, wherein the sum of all the components is 100%; starting the grinding miller, grinding for 30min at 200r/min, and drying, thus obtaining the laser sintering 3D printing rapid prototyping silicon nitride powder material. The material can be directly prototyped under the condition of laser sintering; the preparation process is simple, the preparation conditions are easy to control, and the production cost is low; therefore the preparation method of the laser sintering 3D printing rapid prototyping silicon nitride powder material can be easily put into industrial production.
Description
Technical field
The present invention relates to a kind of preparation method printing manufacturing technology powdered molding material for laser sintered 3D, belong to the Material Field of rapid shaping, particularly a kind of laser sintered 3D prints the preparations and applicatio of rapid shaping silicon nitride powder powder material.
Background technology
3D prints (3D printing), is a kind of based on digital model file, use flow-like, Powdered, silk (rod) shape etc. curable, bond, alloying material, carried out the technology of constructed object by the mode of successively solidifying, bonding, fusing.The field such as Making mold, industrial design of being everlasting is used to modeling, after gradually for the direct manufacture of some products, had the component using this technology to print.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), automobile, and aerospace, dentistry and medical industries, education, geographical information system(GIS), civil engineering work, gun and other field are applied all to some extent.3D printing technique appears at the mid-90 in 20th century, is actually the up-to-date rapid molding device of technology such as utilizing photocuring and ply of paper to fold.It is substantially identical with common print principle of work, and printer, built with liquid or powder etc. " printed material ", after being connected, is stacked up " printed material " by conputer controlled from level to level with computer, finally the blueprint on computer is become in kind.This printing technique is called 3D three-dimensional printing technology.Traditional manufacture generally needs to cut starting material or hole, and namely subtracts material manufacture, can be mass-produced; It is by material stacking bonding, fusion from level to level that 3D prints, and namely increases material manufacture; Quick individual character manufacturing can be realized, the shape that traditional manufacture cannot complete can be produced.
In existing formed material field, because SLS (selective laser sintering) rapid shaping technique has the advantages such as raw material sources various and structure time that is part is shorter, therefore have in rapid shaping field and apply more widely.A kind of nylon powder material for laser sintering and moulding goods is disclosed in Chinese invention patent CN1379061A, by the improvement of chemosynthesis and technique, the surface of nylon powder material is processed, obtain sintering character excellent, moulded products intensity is high, the product of good toughness, simplifies the preparation technology of laser sintered nylon material, reduces cost.
The laser sintered a kind of method belonging to increasing material and manufacture.This technique is also take laser apparatus as energy source, by laser beam, the powder of plastics, wax, pottery, metal or its mixture is sintered equably on processing plane.The powder of uniform spreading last layer very thin (submillimeter level) is as raw material on the table, and laser beam under control of the computer, is scanned by the 2-D data of point aspect with certain speed and energy density by scanning device.After laser beam flying, the powder of corresponding position just sinters certain thickness entity lamella into, and the place do not scanned still keeps loose Powdered.After this one deck is scanned, need subsequently to scan lower one deck.First cut layer thickness and layering thickness according to object and reduce worktable, powder is paved by paving powder cylinder again, can start the scanning of new one deck.So repeatedly, until scanned structure at all levels.Remove excessive powder, and through aftertreatment, can product be obtained.
Although the domestic research for new pattern laser sintering for quick formation material is at present a lot, but be mostly confined to the moulding process to existing material, part performance studies, and the precision of institute's steps of manufacturing blanks, intensity and weather resistance etc. also far away can not the requirements of content with funtion part, also do not produce special rapid prototyping material manufacturers.This situation not only affects the quality of rapid laser sintering molding material or molded article, but also is unfavorable for the Industry Promotion of laser sintering rapid prototyping technology.Exploitation easily shaping, that intensity is high, pollution-free, cost is low type material has become the problem that laser sintering rapid prototyping technology primarily solves.
The chemical resistance of silicon nitride ceramics is good, intensity is high, hardness is high, and wear resisting property is good, frictional coefficient is little, high temperature resistant, and the advantages such as density is low, all have application prospect as structured material or functional materials, receive increasing concern in recent years.Silicon nitride ceramics obtains a wide range of applications at industrial circles such as oil, chemical industry, microelectronics, space flight, aviation, papermaking, laser, automobile, mining industry and nuclear power.The preparation method of current silicon nitride ceramics mainly contains: powder compression sintering process, sol-gel method and reaction sintering etc., when adopting aforesaid method to prepare silicon nitride member, need the mould first according to the shape preparation of component with respective shapes, if the shape of component slightly changes, just need again to prepare mould or need to carry out mechanical workout to sample, thus increase preparation cost.Because the restriction aforesaid method being subject to mould is commonly used to the component preparing simple shape.
The present invention is by carrying out top coat modification to silicon nitride powder powder material, and by high molecular adhesive coating to superfine silicon nitride ceramic powder material surface, after the coating obtained, silicon nitride ceramic powder material directly can adopt laser sintering rapid forming.This powder can reach micron order even submicron order, and the powdered material of uniform particle diameter.This material can be shaped precision, abnormal shape, complicated parts quickly and easily, does not need to spray caking agent, greatly simplifies and just do program.The realization be molded on 3D rapidform machine of thin-walled micro parts is made to become possibility; In addition, the method that this patent provides is simple, and cost is low.
Summary of the invention
Order of the present invention is to provide the preparation method that a kind of laser sintered 3D prints rapid shaping silicon nitride powder powder material, and rapid shaping powder does not need to spray binding agent can Direct Laser scanning moulding;
Object of the present invention is achieved through the following technical solutions.
Laser sintered 3D prints a preparation method for rapid shaping silicon nitride powder powder material, is characterised in that the method has following processing step:
(1) silicon nitride ceramic powder pre-treatment: in the reactor, adds by mass percentage, ethanol: 50% ~ 60%, γ-methacryloxypropyl trimethoxy silane: 16% ~ 26%, stir, then add silicon nitride ceramic powder: 22% ~ 32%, each component sum is absolutely, be placed in 45 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 4 ~ 6 h, filter, by washing with alcohol, dry, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add by mass percentage, pre-treatment silicon nitride ceramic powder: 75% ~ 88%, resol: 5% ~ 15%, trimeric cyanamide: 0.5% ~ 1.5%, Tristearoylglycerol: 0.2% ~ 1.5%, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 5% ~ 15%, each component sum is absolutely, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
The particle diameter of silicon nitride ceramic powder described is in step (1) within the scope of 0.5 ~ 1.0 μm;
Resol described in step (2) is novolac resin.
Particle size test method of the present invention is the granularity equivalent diameter size adopting laser particle analyzer to record.
Another object of the present invention is to provide laser sintered 3D and prints the application shaping on 3D printer of rapid shaping silicon nitride powder powder material, feature is: laser sintered 3D is printed rapid shaping silicon nitride powder powder material and join in the confession powder cylinder of selective laser sintering and moulding machine, powdered material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser apparatus sends laser, the switch of computer controlled laser and the angle of scanning device, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, worktable moves down a thickness, repave powder, laser beam flying, so repeatedly, obtain laser sintered, the mode that wherein laser beam scans on processing plane is subregion scanning, and laser power is 40 ~ 50W, and sweep velocity is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheating temperature: 50 DEG C, and processing temperature is 170 ~ 185 DEG C.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention obtains laser sintered 3D and prints rapid shaping silicon nitride powder powder material, and not needing to spray binding agent can straight forming under laser sintered condition.
(2) the present invention obtains 3 laser sintered 3D and prints rapid shaping silicon nitride powder powder material, and particle can reach submicron order even nano level, has meso-position radius grain little, the feature that particle size distribution is narrow, stable in properties; Can manufacture thin-walled model or small component by this rapid shaping powdered material, producing product, to have surface gloss high, and intensity is good, precision high.
(3) the present invention obtains laser sintered 3D and prints rapid shaping silicon nitride powder powder material, and have preparation technology simple, condition is easy to control, and production cost is low, is easy to suitability for industrialized production, has again the advantage such as low-carbon environment-friendly and save energy.
(4) the present invention obtains laser sintered 3D and prints rapid shaping silicon nitride powder powder material, can effective rapid shaping on laser sintered 3D printer, and shaping precision is high.
Embodiment
Embodiment 1
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 70 mL, γ-methacryloxypropyl trimethoxy silane: 19 mL, stir, add silicon nitride ceramic powder again: 25g, be placed in 45 DEG C of constant temperature, strong stirring, back flow reaction 5 h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 80g, resol: 10g, trimeric cyanamide: 1.0g, Tristearoylglycerol: 1.0g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 10 mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Embodiment 2
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 76 mL, γ-methacryloxypropyl trimethoxy silane: 17 mL, stir, add silicon nitride ceramic powder again: 22g, be placed in 50 DEG C of constant temperature, strong stirring, back flow reaction 4 h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 75g, resol: 8g, trimeric cyanamide: 1.5g, Tristearoylglycerol: 1.5g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 18 mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Embodiment 3
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 63 mL, γ-methacryloxypropyl trimethoxy silane: 23 mL, stir, add silicon nitride ceramic powder again: 26g, be placed in 40 DEG C of constant temperature, strong stirring, back flow reaction 6 h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 88g, resol: 5g, trimeric cyanamide: 0.5g, Tristearoylglycerol: 0.5g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 8 mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Embodiment 4
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 66 mL, γ-methacryloxypropyl trimethoxy silane: 15 mL, stir, add silicon nitride ceramic powder again: 32g, be placed in 42 DEG C of constant temperature, strong stirring, back flow reaction 5.5 h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 82g, resol: 12g, trimeric cyanamide: 0.5g, Tristearoylglycerol: 0.5g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 6mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Embodiment 5
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 73 mL, γ-methacryloxypropyl trimethoxy silane: 17 mL, stir, add silicon nitride ceramic powder again: 24g, be placed in 48 DEG C of constant temperature, strong stirring, back flow reaction 4.5h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 76g, resol: 15g, trimeric cyanamide: 1.0g, Tristearoylglycerol: 1.2g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 9 mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Embodiment 6
(1) silicon nitride ceramic powder pre-treatment: in the reactor, add respectively, ethanol: 67 mL, γ-methacryloxypropyl trimethoxy silane: 26 mL, stir, add silicon nitride ceramic powder again: 30g, be placed in 45 DEG C of constant temperature, strong stirring, back flow reaction 5 h, filter, by washing with alcohol, drying, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add respectively, pre-treatment silicon nitride ceramic powder: 86g, resol: 6g, trimeric cyanamide: 1.0g, Tristearoylglycerol: 0.5g, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 12mL, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that the laser sintered 3D obtained prints rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
Using method: laser sintered 3D is printed rapid shaping silicon nitride powder powder material and join in the confession powder cylinder of selective laser sintering and moulding machine, powdered material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser apparatus sends laser, the switch of computer controlled laser and the angle of scanning device, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, worktable moves down a thickness, repave powder, laser beam flying, so repeatedly, laser sintered is obtained; The mode that wherein laser beam scans on processing plane is subregion scanning, and laser power is 40 ~ 50W, and sweep velocity is 1500mm/s, sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheating temperature: 50 DEG C, processing temperature is 170 ~ 185 DEG C, and shaping precision is high.
Claims (4)
1. laser sintered 3D prints a preparation method for rapid shaping silicon nitride powder powder material, and it is characterized in that, the method has following processing step:
(1) silicon nitride ceramic powder pre-treatment: in the reactor, adds by mass percentage, ethanol: 50% ~ 60%, γ-methacryloxypropyl trimethoxy silane: 16% ~ 26%, stir, then add silicon nitride ceramic powder: 22% ~ 32%, each component sum is absolutely, be placed in 45 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 4 ~ 6 h, filter, by washing with alcohol, dry, grinding, obtains pre-treatment silicon nitride ceramic powder;
(2) laser sintered 3D prints the preparation of rapid shaping silicon nitride powder powder material: in shredder, add by mass percentage, pre-treatment silicon nitride ceramic powder: 75% ~ 88%, resol: 5% ~ 15%, trimeric cyanamide: 0.5% ~ 1.5%, Tristearoylglycerol: 0.2% ~ 1.5%, open shredder rotating speed at 200 revs/min, grinding 10min, add acetone again: 5% ~ 15%, each component sum is absolutely, open shredder rotating speed at 200 revs/min, grinding 30min, dry, obtain laser sintered 3D and print rapid shaping silicon nitride powder powder material, the particle diameter that obtained 3 laser sintered 3D print rapid shaping silicon nitride powder powder material is in the scope of 0.5 ~ 1.5 μm.
2. a kind of laser sintered 3D according to claim 1 prints the preparation method of rapid shaping silicon nitride powder powder material, and it is characterized in that, the particle diameter of the silicon nitride ceramic powder described in step (1) is within the scope of 0.5 ~ 1.0 μm.
3. a kind of laser sintered 3D according to claim 1 prints the preparation method of rapid shaping silicon nitride powder powder material, and it is characterized in that, the resol described in step (2) is novolac resin.
4. a kind of laser sintered 3D according to claim 1 prints the laser sintered 3D printing rapid shaping silicon nitride powder powder material prepared by the preparation method of rapid shaping silicon nitride powder powder material, it is characterized in that, laser sintered 3D prints rapid shaping alpha-silicon nitride powders forming materials condition: laser power is 40 ~ 50W, sweep velocity is 1500mm/s, sweep span is 0.1 ~ 0.15mm, lift height is 0.10 ~ 0.2mm, preheating temperature: 50 DEG C, and processing temperature is 170 ~ 185 DEG C.
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| CN106316388A (en) * | 2016-09-07 | 2017-01-11 | 济南大学 | Preparation for laser sintering 3D (three-dimension) printing and molding barium titanate ceramics powder |
| CN106380173A (en) * | 2016-09-07 | 2017-02-08 | 济南大学 | Preparation method of quick-forming black pottery powder for laser sintering 3D (three-dimensional) printing |
| CN107216155A (en) * | 2017-05-31 | 2017-09-29 | 武汉理工大学 | Double film coated ceramic powders of a kind of PF/PVA for laser 3D printing/isostatic cool pressing composite molding and preparation method thereof |
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| CN107825706A (en) * | 2017-12-15 | 2018-03-23 | 佛山三维二次方科技有限公司 | The 3D printing technique of thermoplastic macromolecule material |
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| CN105669208A (en) * | 2016-03-07 | 2016-06-15 | 武汉理工大学 | Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof |
| CN106316388A (en) * | 2016-09-07 | 2017-01-11 | 济南大学 | Preparation for laser sintering 3D (three-dimension) printing and molding barium titanate ceramics powder |
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| CN106316388B (en) * | 2016-09-07 | 2018-10-09 | 济南大学 | A kind of preparation for laser sintered 3D printing molding barium titanate ceramics powder |
| CN107216155B (en) * | 2017-05-31 | 2020-01-14 | 武汉理工大学 | PF/PVA double-coated ceramic powder for laser 3D printing/cold isostatic pressing composite molding and preparation method thereof |
| CN107216155A (en) * | 2017-05-31 | 2017-09-29 | 武汉理工大学 | Double film coated ceramic powders of a kind of PF/PVA for laser 3D printing/isostatic cool pressing composite molding and preparation method thereof |
| CN107352999A (en) * | 2017-07-21 | 2017-11-17 | 成都职业技术学院 | A kind of analog detection method of the laser sintered performance of 3D printing inorganic material powders |
| CN107825706A (en) * | 2017-12-15 | 2018-03-23 | 佛山三维二次方科技有限公司 | The 3D printing technique of thermoplastic macromolecule material |
| CN109987945A (en) * | 2019-05-09 | 2019-07-09 | 西安航空学院 | A kind of preparation method of porous silicon nitride ceramic |
| CN111892408A (en) * | 2020-07-24 | 2020-11-06 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride ceramic powder suitable for 3DP forming process and treatment method |
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