CN106966718A - It is a kind of that 3D printing barium-strontium titanate powder material is prepared for adhesive with sugar - Google Patents
It is a kind of that 3D printing barium-strontium titanate powder material is prepared for adhesive with sugar Download PDFInfo
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- CN106966718A CN106966718A CN201710128234.8A CN201710128234A CN106966718A CN 106966718 A CN106966718 A CN 106966718A CN 201710128234 A CN201710128234 A CN 201710128234A CN 106966718 A CN106966718 A CN 106966718A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/665—Local sintering, e.g. laser sintering
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Abstract
The invention discloses a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar, it is characterised in that first granulates nano barium phthalate ceramic powder, makes its particle diameter in 80 ~ 120 μ ms;Then in grinder, added by mass percentage concentration, granulate strontium-barium titanate ceramic powder:85% ~ 92%, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:0.5% ~ 2%, 30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar:5% ~ 10%, melamine:0.5% ~ 1.5%, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters:1% ~ 3%, grinding obtains 3D printing barium-strontium titanate powder material, resulting 3D printing barium-strontium titanate powder material.The 3D printing barium-strontium titanate powder material with it is laser sintered can straight forming, sphericity is high, and good fluidity, formed precision is high, and simple with technique, and production cost is low, it is easy to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of laser sintered 3D printing rapid shaping powder body material, belong to rapid shaping
Material Field, more particularly to a kind of method and laser sintered 3D for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar
Printing shaping.
Background technology
Sugar is the refined sugar that the molasses squeezed out by sugarcane and beet are made, and is by each molecular dehydration contracting of glucose and fructose
The disaccharide for the irreducibility closed, is heated to 160 DEG C, is just melted into thick transparent liquid, is crystallized again during cooling.
Extending heating time, sucrose is to be decomposed into glucose and anhydrofructose.Under 190 ~ 220 DEG C of higher temperature, sucrose is just dehydrated
Condensation turns into caramel.Caramel has very strong cementation, can make powder adhesion together, play a part of binding agent.Adopt
Chemical adhesive is replaced as adhesive with sugar, problem of environmental pollution is reduced.
Barium strontium titanate (Bax Sr1-x TiO3 , abbreviation BST) and it is the solid solution that BaTiO3 and Sr TiO3 are formed.It
It is a kind of excellent thermo-sensitive material, capacitor material and ferroelectric piezoelectric material, with high-k, low-dielectric loss, Curie
Temperature (TC) with composition change and dielectric constant with electric field nonlinear change the features such as, ultra-large dynamic memory,
The fields such as microwave-tuned device have broad application prospects, as one of integrated device field most widely studied material.BST
The electric property of material and the microstructure of the material such as porosity and crystallite dimension are closely related, ultra-fine grain and high compaction
BST has preferable dielectric property, and material physical and chemical performance is excellent, and industrially have a wide range of applications value, with microelectronics
Industry development it is increasingly mature, BST ceramic materials will more and more be paid attention to.
Laser sintered 3D printing belongs to a kind of method of increasing material manufacturing.This technique is also, using laser as energy source, to lead to
Crossing laser beam makes the powder of plastics, wax, ceramics, metal or its compound equably be sintered in processing plane.On the table
Uniform layer overlay very thin powder as raw material, laser beam under control of the computer, by scanner with certain speed
Scanned with energy density by the 2-D data in layering face.After laser beam flying, the powder of relevant position is just sintered into necessarily
The entity lamella of thickness, the place do not scanned remains in that loose powdered.After this layer scanned, then need under
One layer is scanned.It is to be layered thickness and reduce workbench first to cut thickness degree according to object, and powdering roller again spreads powder
It is flat, new one layer of scanning can be started.So repeatedly, until scanning through structure at all levels.Remove excessive powder, and through locating later
Reason, you can obtain product.
In existing moulding material field, the structure for having raw material sources various with part due to SLS rapid shaping techniques
Build the time it is shorter the advantages of, therefore have wide application in rapid shaping field.But most of is organic material and composite wood
A kind of nylon powder material for laser sintering and moulding product is disclosed in material, Chinese invention patent CN1379061A, is passed through
Chemical synthesis and the improvement of technique, are handled the surface of nylon powder material, and it is excellent to have obtained sintering character, moulded products
Intensity is high, and the product of good toughness simplifies the preparation technology of laser sintered nylon material, reduces cost;Chinese invention patent
A kind of laser sintered 3D manufacturing technologies stone plastic composite powder end and preparation method thereof is disclosed in CN103881371.
The application will obtain 3D printing barium-strontium titanate powder with carbohydrate gum stick hot coating to barium strontium titanate surface after granulation
Material directly can be molded using laser sintered 3D printing.Adhesive need not be sprayed in forming process.Advantage is that adhesive is used
Amount greatly reduces, and adhesive used is, using sugar, to reduce environmental pollution, and the quality of product is high.Prepared by the technique of the application
3D printing barium-strontium titanate powder adhesive coating uniform, surface is smooth, good fluidity, be adapted to laser sintered 3D printing into
Type.In addition, the preparation method that the application is provided is simple, cost is low.
The content of the invention
The mesh of the present invention is to provide a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar, quickly
Shaping barium-strontium titanate powder material need not spray binding agent can Direct Laser scanning shaping;
The purpose of the present invention is achieved through the following technical solutions.
A kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar, it is characterised in that this method has
There is following processing step:
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, add by mass percentage, water:52% ~ 58%, it is water-soluble
Starch:0.2% ~ 1.0%, aqueous polyurethane:0.5% ~ 2.0%, polyethylene glycol:0.2% ~ 1.0%, stirring and dissolving adds nano-titanium
Sour titanate ceramicses powder:40% ~ 45%, each component sum is absolutely, then strong stirring, 6 ~ 7h of reaction is spray-dried, obtained
Strontium-barium titanate ceramic powder is granulated, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, added by mass percentage concentration, granulate strontium titanates
Titanate ceramicses powder:85% ~ 92%, grinder rotating speed is opened at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, add stearic
Acid amides:0.5% ~ 2%, 30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar:5% ~ 10%, melamine:0.5% ~ 1.5%,
Isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters:1% ~ 3%, each component sum is a hundred per cent, constant temperature, at 500 revs/min
Rotating speed under grind 40 ~ 50 min, be cooled to room temperature, obtain 3D printing barium-strontium titanate powder material, resulting 3D printing strontium titanates
Barium powder body material, its particle diameter is in the range of 100 ~ 150 μm.
In step(1)Described in spray drying, intake air temperature control is at 110 DEG C, and air outlet temperature is controlled at 90 DEG C,
Air intake flow 250m3/h。
In step(1)Described in polyethylene glycol be polyethylene glycol 200 or polyethylene glycol 400.
In step(2)Described in white sugar be edible soft white sugar or white granulated sugar.
Particle size test method of the present invention is the granularity equivalent diameter size measured using laser particle analyzer.
The present invention compared with the prior art, has the following advantages that and beneficial effect:
(1)The 3D printing barium-strontium titanate powder material that the present invention is obtained, using sugar as adhesive coating in granulation barium strontium titanate
Surface, environmental protection, it is not necessary to which spraying binding agent can straight forming under the conditions of laser sintered.
(2)The 3D printing barium-strontium titanate powder material that the present invention is obtained, the uniform particle sizes of particle, sphericity is high, mobility
Good the characteristics of, property is stable;Thin-walled model or small parts can be manufactured by this rapid shaping powder material, manufacture is produced
Product have surface gloss high, and intensity is good, the features such as precision is high.
(3)The 3D printing barium-strontium titanate powder material that the present invention is obtained, simple with preparation technology, condition is easily controllable,
Production cost is low, it is easy to industrialized production, it is easy to store, the advantages of pollution-free.
Embodiment
Embodiment 1
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, it is separately added into water:540mL, water soluble starch:5g, water
Property polyurethane:10g, polyethylene glycol:5g, stirring and dissolving adds nano barium phthalate ceramic powder:400g, strong stirring, reaction
6.5h, is then spray-dried, and obtains granulating strontium-barium titanate ceramic powder, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, it is separately added into, granulates strontium-barium titanate ceramic powder:
88g, opens grinder rotating speed at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:1g, grinding
30min, temperature continues to rise to 190 ± 2 DEG C, white sugar:8g, melamine:1g, isopropyl three (dioctyl phosphoric acid acyloxy) titanium
Acid esters:2g, constant temperature grinds 45 min under 500 revs/min of rotating speed, it is cooled to room temperature, obtains 3D printing barium-strontium titanate powder
Material, resulting 3D printing barium-strontium titanate powder material, its particle diameter is in the range of 100 ~ 150 μm.
Embodiment 2
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, it is separately added into water:1040mL, water soluble starch:4g, water
Property polyurethane:36g, polyethylene glycol:20g, stirring and dissolving adds nano barium phthalate ceramic powder:900g is strong stirring, anti-
6h is answered, is then spray-dried, obtains granulating strontium-barium titanate ceramic powder, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, it is separately added into, granulates strontium-barium titanate ceramic powder:
920g, opens grinder rotating speed at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:5g, grinding
30min, temperature continues to rise to 190 ± 2 DEG C, white sugar:50g, melamine:15g, isopropyl three (dioctyl phosphoric acid acyloxy)
Titanate esters:10g, constant temperature grinds 40 min under 500 revs/min of rotating speed, it is cooled to room temperature, obtains 3D printing barium strontium titanate powder
Body material, resulting 3D printing barium-strontium titanate powder material, its particle diameter is in the range of 100 ~ 150 μm.
Embodiment 3
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, it is separately added into water:1160mL, water soluble starch:20g,
Aqueous polyurethane:16g, polyethylene glycol:4g, stirring and dissolving adds nano barium phthalate ceramic powder:800g is strong stirring, anti-
7h is answered, is then spray-dried, obtains granulating strontium-barium titanate ceramic powder, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, it is separately added into, granulates strontium-barium titanate ceramic powder:
850g, opens grinder rotating speed at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:20g, grinding
30min, temperature continues to rise to 190 ± 2 DEG C, white sugar:100g, melamine:12g, (the dioctyl phosphoric acid acyl-oxygen of isopropyl three
Base) titanate esters:18g, constant temperature grinds 50min under 500 revs/min of rotating speed, it is cooled to room temperature, obtains 3D printing barium strontium titanate
Powder body material, resulting 3D printing barium-strontium titanate powder material, its particle diameter is in the range of 100 ~ 150 μm.
Embodiment 4
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, it is separately added into water:1100mL, water soluble starch:14g,
Aqueous polyurethane:20g, polyethylene glycol:16g, stirring and dissolving adds nano barium phthalate ceramic powder:840g, strong stirring,
6.5h is reacted, is then spray-dried, obtains granulating strontium-barium titanate ceramic powder, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, it is separately added into, granulates strontium-barium titanate ceramic powder:
880g, opens grinder rotating speed at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:15g, grinding
30min, temperature continues to rise to 190 ± 2 DEG C, white sugar:70g, melamine:5g, isopropyl three (dioctyl phosphoric acid acyloxy)
Titanate esters:30g, constant temperature grinds 45 min under 500 revs/min of rotating speed, it is cooled to room temperature, obtains 3D printing barium strontium titanate powder
Body material, resulting 3D printing barium-strontium titanate powder material, its particle diameter is in the range of 100 ~ 150 μm.
Embodiment 5
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, it is separately added into water:1120mL, water soluble starch:20g,
Aqueous polyurethane:10g, polyethylene glycol:10g, stirring and dissolving adds nano barium phthalate ceramic powder:860g, strong stirring,
6.5h is reacted, is then spray-dried, obtains granulating strontium-barium titanate ceramic powder, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, it is separately added into, granulates strontium-barium titanate ceramic powder:
900g, opens grinder rotating speed at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, adds stearmide:10g, grinding
30min, temperature continues to rise to 190 ± 2 DEG C, white sugar:60g, melamine:10g, isopropyl three (dioctyl phosphoric acid acyloxy)
Titanate esters:20g, constant temperature grinds 45 min under 500 revs/min of rotating speed, it is cooled to room temperature, obtains 3D printing barium strontium titanate powder
Body material, resulting 3D printing barium-strontium titanate powder material, its particle diameter is in the range of 100 ~ 150 μm.
Application method:3D printing barium-strontium titanate powder material is added to the confession powder cylinder of selective laser sintering and moulding machine
In, dusty material is equably layered in processing plane and is heated to processing temperature by powdering roller, and laser sends laser, meter
The switch of calculation machine control laser and the angle of scanner so that laser beam is in processing plane according to corresponding two-dimensional slice shape
Shape is scanned, after laser beam is inswept, and workbench moves down a thickness, then powdering, laser beam flying, so repeatedly, obtains
Laser sintered part;The mode that wherein laser beam is scanned in processing plane scans for subregion, and laser power is 80 ~ 100W, is swept
Speed is retouched for 1500mm/s, sweep span is 0.1 ~ 0.15mm, lift height is 0.10 ~ 0.2mm, preheating temperature:100 DEG C, plus
Work temperature is 200 ~ 210 DEG C.
Claims (5)
1. a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar, it is characterised in that this method has
Following processing step:
(1)Strontium-barium titanate ceramic powder is granulated to prepare:In the reactor, add by mass percentage, water:52% ~ 58%, it is water-soluble
Starch:0.2% ~ 1.0%, aqueous polyurethane:0.5% ~ 2.0%, polyethylene glycol:0.2% ~ 1.0%, stirring and dissolving adds nano-titanium
Sour titanate ceramicses powder:40% ~ 45%, each component sum is absolutely, then strong stirring, 6 ~ 7h of reaction is spray-dried, obtained
Strontium-barium titanate ceramic powder is granulated, its particle diameter is in 80 ~ 120 μ ms;
(2)The preparation of 3D printing barium-strontium titanate powder material:In grinder, added by mass percentage concentration, granulate strontium titanates
Titanate ceramicses powder:85% ~ 92%, grinder rotating speed is opened at 500 revs/min, grinding, temperature rises to 120 ± 2 DEG C, add stearic
Acid amides:0.5% ~ 2%, 30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar:5% ~ 10%, melamine:0.5% ~ 1.5%,
Isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters:1% ~ 3%, each component sum is a hundred per cent, constant temperature, at 500 revs/min
Rotating speed under grind 40 ~ 50 min, be cooled to room temperature, obtain 3D printing barium-strontium titanate powder material, resulting 3D printing strontium titanates
Barium powder body material, its particle diameter is in the range of 100 ~ 150 μm.
2. a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar according to claim 1, its
It is characterised by, step(1)Described in spray drying, intake air temperature control is at 110 DEG C, and air outlet temperature is controlled at 90 DEG C,
Air intake flow 250m3/h。
3. a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar according to claim 1, its
It is characterised by, step(1)Described in polyethylene glycol be polyethylene glycol 200 or polyethylene glycol 400.
4. a kind of method for preparing 3D printing barium-strontium titanate powder material for adhesive with sugar according to claim 1, its
It is characterised by, step(2)Described in white sugar be edible soft white sugar or white granulated sugar.
5. it is according to claim 1 a kind of made for the method that adhesive prepares 3D printing barium-strontium titanate powder material with sugar
Standby 3D printing barium-strontium titanate powder material.
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CN109095918A (en) * | 2018-08-29 | 2018-12-28 | 济南大学 | A kind of preparation method of 3DP moulding process strontium bismuth titanate dielectric ceramic powder |
CN111793466A (en) * | 2020-07-24 | 2020-10-20 | 石家庄盛华企业集团有限公司 | Environment-friendly wax part binder and preparation method thereof |
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Cited By (5)
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