CN106966718B - One kind is that adhesive prepares 3D printing barium-strontium titanate powder material with sugar - Google Patents
One kind is that adhesive prepares 3D printing barium-strontium titanate powder material with sugar Download PDFInfo
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- CN106966718B CN106966718B CN201710128234.8A CN201710128234A CN106966718B CN 106966718 B CN106966718 B CN 106966718B CN 201710128234 A CN201710128234 A CN 201710128234A CN 106966718 B CN106966718 B CN 106966718B
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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 methods for preparing 3D printing barium-strontium titanate powder material with sugar for adhesive, which is characterized in that is first granulated nano barium phthalate ceramic powder, makes its partial size in 80 ~ 120 μ ms;Then it in grinder, is added by mass percentage concentration, granulation strontium-barium titanate ceramic powder: 85% ~ 92%, grinding, temperature rise to 120 ± 2 DEG C, addition stearmide: 0.5% ~ 2%, grind 30min, 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, acquired 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, good fluidity, and formed precision is high, and has simple process, and production cost is low, easy to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods of laser sintered 3D printing rapid shaping powder body material, belong to rapid shaping
Material Field, in particular to a kind of method with sugar for adhesive preparation 3D printing barium-strontium titanate powder material and laser sintered 3D
Printing shaping.
Background technique
Sugar is refined sugar made of the molasses squeezed out sugarcane and beet, is by each molecular dehydration contracting of glucose and fructose
The disaccharide of irreducibility made of conjunction, is heated to 160 DEG C, is just melted into thick transparent liquid, crystallizes again when cooling.
Extending heating time, sucrose are decomposed into glucose and anhydrofructose.Under 190 ~ 220 DEG C of higher temperature, sucrose is just dehydrated
Condensation becomes caramel.Caramel has very strong cementation, can make powder adhesion together, play the role of binder.It adopts
Sugar is used to replace chemical adhesive as adhesive, reduce environmental pollution problem.
Barium strontium titanate (Bax Sr1-x TiO3 , abbreviation BST) and it is the solid solution that BaTiO3 and Sr TiO3 is formed.It
It is a kind of excellent thermo-sensitive material, capacitor material and ferroelectric piezoelectric material, there is high dielectric constant, 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, and become one of the material that integrated device field is most studied extensively.BST
The electric property of material and the microstructure such as porosity and crystallite dimension of material are closely related, ultra-fine grain and high compaction
BST has ideal 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 material will will receive more and more attention.
Laser sintered 3D printing belongs to a kind of method of increasing material manufacturing.This technique is also to lead to using laser as energy source
Crossing laser beam is sintered the powder of plastics, wax, ceramics, metal or its compound equably in processing plane.On the table
The uniform very thin powder of layer overlay as raw material, laser beam under control of the computer, by scanner with certain speed
It is scanned with energy density by the 2-D data in layering face.After laser beam flying, the powder of corresponding position is just sintered into centainly
The entity lamella of thickness, the place that do not scan still maintain loose powdered.After this layer scanned, then need under
One layer is scanned.Thickness degree i.e. layering thickness is first cut according to object and reduces workbench, powdering roller again spreads powder
It is flat, new one layer of scanning can be started.Repeatedly, until scanning through structure at all levels.Remove excessive powder, and passes through and locate later
Reason, can be obtained product.
In existing moulding material field, since SLS rapid shaping technique has the structure of raw material sources multiplicity and part
Build the time it is shorter the advantages that, therefore have wide application in rapid shaping field.But most of is organic material and composite wood
Expect, discloses a kind of nylon powder material for laser sintering and moulding product in Chinese invention patent CN1379061A, pass through
The improvement of chemical synthesis and technique handles 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 process of laser sintered nylon material, reduces costs;Chinese invention patent
A kind of laser sintered 3D manufacturing technology 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
Laser sintered 3D printing molding can be directly used in material.Sprinkling adhesive is not needed in forming process.Advantage is that adhesive is used
Amount greatly reduces, and adhesive used is reduced environmental pollution using sugar, and the quality of product is high.The technique preparation of the application
3D printing barium-strontium titanate powder adhesive coating uniform, surface is smooth, good fluidity, be suitble to laser sintered 3D printing at
Type.In addition, preparation method provided by the present application is simple, it is at low cost.
Summary of the invention
Mesh of the invention is to provide a kind of method for preparing 3D printing barium-strontium titanate powder material with sugar for adhesive, quickly
Molding barium-strontium titanate powder material does not need sprinkling binder can Direct Laser scanning molding;
The purpose of the present invention is achieved through the following technical solutions.
A method of 3D printing barium-strontium titanate powder material being prepared for adhesive with sugar, which is characterized in that this method tool
There is following processing step:
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being added by mass percentage, water: 52% ~ 58%, water
Soluble starch: 0.2% ~ 1.0%, aqueous polyurethane: 0.5% ~ 2.0%, polyethylene glycol: 0.2% ~ 1.0%, stirring and dissolving is added and is received
Rice barium titanate ceramics powder: 40% ~ 45%, the sum of each component is that absolutely, then strong stirring, 6 ~ 7h of reaction are spray-dried,
It obtains being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) it the preparation of 3D printing barium-strontium titanate powder material: in grinder, is added by mass percentage concentration, is granulated titanium
Sour strontium titanate ceramics powder: 85% ~ 92%, grinder rotating speed is opened at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, is added
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%, the sum of each component is absolutely constant temperature, 500
Rev/min revolving speed under grind 40 ~ 50 min, be cooled to room temperature, obtain 3D printing barium-strontium titanate powder material, acquired 3D printing
Barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
The spray drying in step (1), at 110 DEG C, air outlet temperature is controlled at 90 DEG C for intake air temperature control,
Enter the wind flow 250m3/h。
The polyethylene glycol is polyethylene glycol 200 or polyethylene glycol 400 in step (1).
The white sugar described in step (2) is 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.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) the 3D printing barium-strontium titanate powder material that the present invention obtains is being granulated metatitanic acid as adhesive coating using sugar
Strontium barium surface, environmentally protective, not needing sprinkling binder can straight forming under the conditions of laser sintered.
(2) the 3D printing barium-strontium titanate powder material that the present invention obtains, the uniform particle sizes of particle, sphericity is high, mobility
Good feature, property are stablized;Thin-walled model or small parts can be manufactured by this rapid shaping powder material, manufacture is produced
Product have the features such as surface gloss is high, and intensity is good, and precision is high.
(3) the 3D printing barium-strontium titanate powder material that the present invention obtains has preparation process simple, and condition is easily controllable,
The advantages that production cost is low, easy to industrialized production, easily stored, pollution-free.
Specific embodiment
Embodiment 1
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being separately added into water: 540mL, water soluble starch:
5g, aqueous polyurethane: 10g, polyethylene glycol: 5g, stirring and dissolving, add nano barium phthalate ceramic powder: 400g is strongly stirred
It mixes, react 6.5h, be then spray-dried, obtain being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) preparation of 3D printing barium-strontium titanate powder material: in grinder, being separately added into, and is granulated barium-strontium titanate ceramic
Powder: 88g opens grinder rotating speed at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, and stearmide is added: 1g is ground
30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar: 8g, melamine: 1g, isopropyl three (dioctyl phosphoric acid acyloxy)
Titanate esters: 2g, constant temperature grind 45 min under 500 revs/min of revolving speed, it is cooled to room temperature, obtains 3D printing barium strontium titanate powder
Body material, acquired 3D printing barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
Embodiment 2
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being separately added into water: 1040mL, water soluble starch:
4g, aqueous polyurethane: 36g, polyethylene glycol: 20g, stirring and dissolving, add nano barium phthalate ceramic powder: 900g is strongly stirred
It mixes, react 6h, be then spray-dried, obtain being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) preparation of 3D printing barium-strontium titanate powder material: in grinder, being separately added into, and is granulated barium-strontium titanate ceramic
Powder: 920g opens grinder rotating speed at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, and stearmide is added: 5g is ground
30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar: 50g, melamine: 15g, (the dioctyl phosphoric acid acyl-oxygen of isopropyl three
Base) titanate esters: 10g, constant temperature grind 40 min under 500 revs/min of revolving speed, it is cooled to room temperature, obtains 3D printing strontium titanates
Barium powder body material, acquired 3D printing barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
Embodiment 3
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being separately added into water: 1160mL, water soluble starch:
20g, aqueous polyurethane: 16g, polyethylene glycol: 4g, stirring and dissolving, add nano barium phthalate ceramic powder: 800g is strongly stirred
It mixes, react 7h, be then spray-dried, obtain being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) preparation of 3D printing barium-strontium titanate powder material: in grinder, being separately added into, and is granulated barium-strontium titanate ceramic
Powder: 850g opens grinder rotating speed at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, and stearmide: 20g is added,
30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar: 100g, melamine: 12g, (the dioctyl phosphoric acid acyl of isopropyl three
Oxygroup) titanate esters: 18g, constant temperature grind 50min under 500 revs/min of revolving speed, it is cooled to room temperature, obtains 3D printing strontium titanates
Barium powder body material, acquired 3D printing barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
Embodiment 4
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being separately added into water: 1100mL, water soluble starch:
14g, aqueous polyurethane: 20g, polyethylene glycol: 16g, stirring and dissolving, add nano barium phthalate ceramic powder: 840g is strongly stirred
It mixes, react 6.5h, be then spray-dried, obtain being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) preparation of 3D printing barium-strontium titanate powder material: in grinder, being separately added into, and is granulated barium-strontium titanate ceramic
Powder: 880g opens grinder rotating speed at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, and stearmide: 15g is added,
30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar: 70g, melamine: 5g, (the dioctyl phosphoric acid acyl-oxygen of isopropyl three
Base) titanate esters: 30g, constant temperature grind 45 min under 500 revs/min of revolving speed, it is cooled to room temperature, obtains 3D printing strontium titanates
Barium powder body material, acquired 3D printing barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
Embodiment 5
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being separately added into water: 1120mL, water soluble starch:
20g, aqueous polyurethane: 10g, polyethylene glycol: 10g, stirring and dissolving, add nano barium phthalate ceramic powder: 860g is strongly stirred
It mixes, react 6.5h, be then spray-dried, obtain being granulated strontium-barium titanate ceramic powder, partial size is in 80 ~ 120 μ ms;
(2) preparation of 3D printing barium-strontium titanate powder material: in grinder, being separately added into, and is granulated barium-strontium titanate ceramic
Powder: 900g opens grinder rotating speed at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, and stearmide: 10g is added,
30min is ground, temperature continues to rise to 190 ± 2 DEG C, white sugar: 60g, melamine: 10g, (the dioctyl phosphoric acid acyl of isopropyl three
Oxygroup) titanate esters: 20g, constant temperature grind 45 min under 500 revs/min of revolving speed, it is cooled to room temperature, obtains 3D printing metatitanic acid
Strontium barium powder body material, acquired 3D printing barium-strontium titanate powder material, in the range of partial size is 100 ~ 150 μm.
Application method: 3D printing barium-strontium titanate powder material is added to the powder supply 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 idler wheel, and laser issues laser, meter
Calculation machine controls the switch of laser and the angle of scanner, so that laser beam is in processing plane according to corresponding two-dimensional slice shape
Shape is scanned, and after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying obtains repeatedly
Laser sintered part;The mode that wherein laser beam scans in processing plane is subregion scanning, and laser power is 80 ~ 100W, is swept
Retouching speed is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheating temperature: 100 DEG C, is added
Work temperature is 200 ~ 210 DEG C.
Claims (4)
1. a kind of method for preparing 3D printing barium-strontium titanate powder material with sugar for adhesive, which is characterized in that this method has
Following processing step:
(1) it is granulated strontium-barium titanate ceramic powder preparation: in the reactor, being added by mass percentage, water: 52%~58%, water
Soluble starch: 0.2%~1.0%, aqueous polyurethane: 0.5%~2.0%, polyethylene glycol: 0.2%~1.0%, stirring and dissolving,
Add nano barium phthalate ceramic powder: 40%~45%, the sum of each component is absolutely strong stirring, 6~7h of reaction,
Then it is spray-dried, obtains being granulated strontium-barium titanate ceramic powder, partial size is in 80~120 μ ms;
(2) it the preparation of 3D printing barium-strontium titanate powder material: in grinder, is added by mass percentage concentration, is granulated strontium titanates
Titanate ceramics powder: 85%~92%, grinder rotating speed is opened at 500 revs/min, and grinding, temperature rises to 120 ± 2 DEG C, is added hard
Acyl amine: 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%, the sum of each component is a hundred percent,
Constant temperature grinds 40~50min under 500 revs/min of revolving speed, is cooled to room temperature, obtains 3D printing barium-strontium titanate powder material, institute
3D printing barium-strontium titanate powder material is obtained, in the range of partial size is 100~150 μm.
2. a kind of method that 3D printing barium-strontium titanate powder material is prepared for adhesive with sugar according to claim 1,
It being characterized in that, spray drying described in step (1), at 110 DEG C, air outlet temperature is controlled at 90 DEG C for intake air temperature control,
Enter the wind flow 250m3/h。
3. a kind of method that 3D printing barium-strontium titanate powder material is prepared for adhesive with sugar according to claim 1,
It is characterized in that, polyethylene glycol described in step (1) is polyethylene glycol 200 or polyethylene glycol 400.
4. a kind of method for preparing 3D printing barium-strontium titanate powder material with sugar for adhesive according to claim 1 is made
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 |
CN109095917B (en) * | 2018-09-10 | 2021-07-16 | 北京工业大学 | Preparation method of bioactive porous hydroxyapatite/barium titanate composite ceramic based on 3D printing |
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CN106380173B (en) * | 2016-09-07 | 2019-02-22 | 济南大学 | A kind of preparation for laser sintered 3D printing rapid shaping black pottery powder |
CN106348746B (en) * | 2016-09-07 | 2019-06-04 | 济南大学 | A kind of preparation of laser sintered 3D printing molding YAG transparent ceramic powder |
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