CN108975908A - A kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder - Google Patents
A kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder Download PDFInfo
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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
- C04B35/01—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
- C04B35/47—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 based on strontium 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
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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
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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Abstract
The invention discloses a kind of preparation methods for molded through three-dimensional printing technique strontium titanate ceramic powder, which is characterized in that carries out surface preparation to strontium titanates pottery powder and sintering aid using titanate coupling agent TC-F, obtains pretreatment strontium titanates pottery powder；Using Methacrylamide, N, N- methylene-bisacrylamide, polycarboxylate dispersant's configuration aqueous premix；Then in reactor, it is added by mass percentage, pretreatment strontium titanates pottery powder: 30% ~ 35%, aqueous premix: 65% ~ 70%, the sum of each component is absolutely 80 ~ 100min of strong stirring, spray drying, it obtains for molded through three-dimensional printing technique strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.The material on three dimensional printing 3D printer can straight forming, sphericity is high, good fluidity, and formed precision is high, and has preparation process simple, and condition is easily controllable, and production cost is low, easy to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods for being used for three dimensional printing (3DP) technique rapid shaping powder body material, belong to fast
The molding Material Field of speed, in particular to a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder and answer
With.
Background technique
Strontium titanates (SrTiO3) be a kind of cubic perovskite type composite oxides at room temperature, meet stoichiometric ratio
Strontium titanate crystals are insulators, but semiconducting may be implemented in the case where forcing reduction or mixing up donor metal ion.Metatitanic acid
Strontium is important, emerging electron ceramic material, has high dielectric constant and high refraction constant.There is significant piezoelectricity
Can, it is important ferroelectric (the advantages that ferroelectric material is non-volatile with its, switching speed is fast, the high of storage density is anti-radiation, iron
Conductive film can manufacture ferroelectric memory and ferroelectric field effect pipe, and the computer memory made of them leads to present
Traditional magnetic material memory is compared, have storage density is big, access speed is fast, the low Radiation hardness of working voltage is strong,
The features such as operating temperature range is wide, chemical stability is good and non-volatile can also prepare highly sensitive, high stability of new generation
Piezoelectric transducer), have stable electric hysteresis property.In high-temperature superconductor, catalysis, high temperature solid oxide fuel cell, electrode material
Material, electrochemical sensor, sull village bottom material special optical window and sputtering target material of high quality etc. are applied wide
It is general, can be used as dielectric material and photoelectric material, for manufacture high voltage ceramic capacitor, PTC thermistor, grain-boundary layer capacitor,
Electronic component, photochemical catalyst electrode material, manufacturing existing capacitor function again has the piezoresistor 3 etc. for absorbing surge, they are all
With high-performance, high reliability, it is small in size the advantages that.And compared with barium-titanate material, also have that dielectric loss is low, temperature is steady
It is qualitative good, the advantages that high dieletric strength.
Three dimensional printing (3DP) technique, is exactly the 3D printing of today, is Massachusetts Institute Technology Emanual Sachs etc.
What people developed.E.M.Sachs applied for 3DP(Three-Dimensional Printing in 1989) patent, which is
One of the core patent of non-shaped material droplet injection forming scope.3DP technique is similar with SLS technique, using dusty material at
Shape, such as ceramic powders, metal powder.Except that material powder was not connected by sintering, pass through spray head
With bonding agent (such as silica gel) by the section " printing " of part on material powder.The part strength being bonded with bonding agent is lower,
It must also post-process.Specific embodiment is as follows: after upper one layer of bonding, one distance of moulding cylinder decline (it is equal to thickness:
0.013~0.1mm), powder supply cylinder rises a height, if releasing dry powder, and shifts moulding cylinder by powder-laying roller, pave and is pressed
It is real.Under the control of the computer, by the formed data of next construction section, selectively jet binder builds level to spray head.Powdering
Extra powder is collected by powder collection device when roller powdering.Such powder feeding again and again, powdering and jet binder, are finally completed
The bonding of one three-dimensional powder.It is not dry powder by the place of jet binder, plays a supportive role in forming process, and shapes knot
Shu Hou is easier to remove.But this moulding process also has certain limitation, and the dosage of adhesive is big, bad control, gluing
Agent is easy blocking spray head.
The application can improve solid content and drop using the modified strontium titanate ceramic powder of titanate coupling agent TC-F
The viscosity of low slurry improves surface cleanliness.Using Methacrylamide as monomer, N, N- methylene-bisacrylamide is crosslinking
Agent, preparation are used for 3DP moulding process strontium titanate ceramic powder, sprinkling adhesive are not needed in forming process, it is only necessary to which sprinkling is few
The initiator and catalyst of amount avoid the nozzle of adhesive blocking printer, and advantage is that adhesive dosage greatly reduces,
It reduces environmental pollution during subsequent calcination, the quality of product is high.The powder body material uniform particle sizes of the technique preparation of the application, ball
Shape degree is high, good fluidity, is suitble to 3DP technique 3D printing molding.In addition, the method that this patent provides is simple, it is at low cost.
Summary of the invention
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder, which is characterized in that this method tool
There is following processing step:
(1) strontium titanates pottery powder pretreatment: in the ball mill, being added by mass percentage, strontium titanates pottery powder: 93% ~ 96%, it burns
Knot auxiliary agent: 3% ~ 6%, titanate coupling agent TC-F:0.5% ~ 2.5%, the sum of each component is that absolutely, temperature rises to 60 ± 2 DEG C,
Grinding machine is opened, 2-3h is ground, it is dry, obtain pretreatment strontium titanates pottery powder；
(2) aqueous premix is prepared: in the reactor, it is added by mass percentage concentration, deionized water: 88% ~ 92%, and metering system
Amide: 6% ~ 10%, N, N- methylene-bisacrylamide: 0.2% ~ 1.5%, polycarboxylate dispersant: 0.5% ~ 2.0%, the sum of each component
For absolutely, stirring and dissolving adjusts pH 8 or so with ammonium hydroxide, obtains aqueous premix；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being added by mass percentage,
Pretreatment strontium titanates pottery powder: 30% ~ 35%, aqueous premix: 65% ~ 70%, the sum of each component is absolutely strong stirring 80
~ 100min, spray drying are obtained for molded through three-dimensional printing technique strontium titanate ceramic powder, and partial size is in 120 ~ 150 μ ms
It is interior.
The partial size of strontium titanates strontium pottery powder, sintering aid powder described in step (1) is nanometer grade powder.
In step (1) the sintering aid be it is a kind of in lanthanum sesquioxide, neodymium oxide or yttria or
Two kinds of mixing.
At 100 DEG C, air outlet temperature is controlled at 90 DEG C for spray drying intake air temperature control in step (3),
Enter the wind flow 280m3/h。
The molded through three-dimensional printing technique strontium titanate ceramic powder that is used for is in 3D printer printing shaping, printer head
Spraying mass percentage concentration is 6% ammonium persulfate solution and 2% ascorbic acid mixed solution.
It is a further object of the present invention to provide one kind for molded through three-dimensional printing technique strontium titanate ceramic powder in 3D printing
Molding application, feature on machine are as follows: molded through three-dimensional printing technique strontium titanate ceramic powder will be used for and be added in powder supply cylinder, printed
It is 6% ammonium persulfate solution and 2% ascorbic acid mixed solution that spray head, which sprays printer head sprinkling mass percentage concentration,.Tool
Body technology process is as follows: after upper one layer of bonding, moulding cylinder declines a distance (being equal to thickness: 0.013~0.1mm), supplies
Powder cylinder rises a height, if releasing dry powder, and shifts moulding cylinder by powder-laying roller, pave and is compacted.Spray head is in computer control
Under system, the ammonium persulfate solution and 2% that mass percentage concentration is 6% is selectively sprayed by the formed data of next construction section
Ascorbic acid mixed solution, when powder-laying roller powdering, extra powder was collected by powder collection device.Such powder feeding again and again, powdering
It is 6% ammonium persulfate solution and 2% ascorbic acid mixed solution with sprinkling mass percentage concentration, is finally completed a three-dimensional powder
The bonding of body.It is not dry powder by the place of spray solution, plays a supportive role in forming process, and after forming, is easier
Removal.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) what the present invention obtained is used for molded through three-dimensional printing technique strontium titanate ceramic powder, does not need sprinkling binder, spray head spray
Spill extremely low viscosity 6% ammonium persulfate solution and 2% ascorbic acid mixed solution can straight forming, avoid printing head stifled
Plug, substantially reduces adhesive dosage, reduces environmental pollution in calcining, and the quality for improving product is high.
(2) what the present invention that the present invention obtains obtained is used for molded through three-dimensional printing technique strontium titanate ceramic powder, particle
Uniform particle sizes, sphericity is high, good fluidity, is suitble to 3DP technique 3D printing molding；It can be made by this rapid shaping powder material
Thin-walled model or small parts are made, the features such as product is high with surface gloss, and precision is high is produced.
(3) what the present invention that the present invention obtains obtained is used for molded through three-dimensional printing technique strontium titanate ceramic powder, has system
Standby simple process, condition is easily controllable, and production cost is low, easy to industrialized production, and has low-carbon environment-friendly and energy saving etc.
Advantage.
(4) present invention is to improve powder surface property by the modified strontium titanate ceramic powder of titanate coupling agent TC-F and mention
High powder and can reduce the viscosity of slurry in the dispersibility of liquid phase, improve surface cleanliness.
Specific embodiment
Embodiment 1
(1) strontium titanates pottery powder pretreatment: in the ball mill, being separately added into, strontium titanates pottery powder: 940g, sintering aid: 40g,
Titanate coupling agent TC-F:20g, temperature rise to 60 ± 2 DEG C, open grinding machine, grind 2.5h, dry, obtain pretreatment strontium titanates
Tao Fenti；
(2) aqueous premix is prepared: it in the reactor, is separately added into, deionized water: 900 mL, and Methacrylamide: 80g, N,
N- methylene-bisacrylamide: 10g, polycarboxylate dispersant: 10g, stirring and dissolving adjust pH 8 or so with ammonium hydroxide, are premixed
Close solution；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being separately added into, pre-processing titanium
Sour strontium pottery powder: 320g, aqueous premix: 680g, strong stirring 90min, spray drying are obtained for molded through three-dimensional printing work
Skill strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.
Embodiment 2
(1) strontium titanates pottery powder pretreatment: in the ball mill, being separately added into, strontium titanates pottery powder: 960g, sintering aid: 30g,
Titanate coupling agent TC-F:10g, temperature rise to 60 ± 2 DEG C, open grinding machine, grind 2h, dry, obtain pretreatment strontium titanates pottery
Powder；
(2) aqueous premix is prepared: it in the reactor, is separately added into, deionized water: 920 mL, and Methacrylamide: 70g, N,
N- methylene-bisacrylamide: 2g, polycarboxylate dispersant: 5g, stirring and dissolving adjust pH 8 or so with ammonium hydroxide, are pre-mixed
Solution；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being separately added into, pre-processing titanium
Sour strontium pottery powder: 350g, aqueous premix: 650g, strong stirring 80min, spray drying are obtained for molded through three-dimensional printing work
Skill strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.
Embodiment 3
(1) strontium titanates pottery powder pretreatment: in the ball mill, being separately added into, strontium titanates pottery powder: 930g, sintering aid: 55g,
Titanate coupling agent TC-F:15g, temperature rise to 60 ± 2 DEG C, open grinding machine, grind 3h, dry, obtain pretreatment strontium titanates pottery
Powder；
(2) aqueous premix is prepared: it in the reactor, is separately added into, deionized water: 880mL, and Methacrylamide: 100g, N,
N- methylene-bisacrylamide: 5g, polycarboxylate dispersant: 15g, stirring and dissolving adjust pH 8 or so with ammonium hydroxide, are premixed
Close solution；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being separately added into, pre-processing titanium
Sour strontium pottery powder: 300g, aqueous premix: 700g, strong stirring 100min, spray drying are obtained for molded through three-dimensional printing
Technique strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.
Embodiment 4
(1) strontium titanates pottery powder pretreatment: in the ball mill, being separately added into, strontium titanates pottery powder: 935g, sintering aid: 60g,
Titanate coupling agent TC-F:5g, temperature rise to 60 ± 2 DEG C, open grinding machine, grind 2.8h, dry, obtain pretreatment strontium titanates pottery
Powder；
(2) aqueous premix is prepared: it in the reactor, is separately added into, deionized water: 910 mL, and Methacrylamide: 60g, N,
N- methylene-bisacrylamide: 15g, polycarboxylate dispersant: 20g, stirring and dissolving adjust pH 8 or so with ammonium hydroxide, are premixed
Close solution；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being separately added into, pre-processing titanium
Sour strontium pottery powder: 340g, aqueous premix: 660g, strong stirring 95min, spray drying are obtained for molded through three-dimensional printing work
Skill strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.
Embodiment 5
(1) strontium titanates pottery powder pretreatment: in the ball mill, being separately added into, strontium titanates pottery powder: 940g, sintering aid: 50g,
Titanate coupling agent TC-F:10g, temperature rise to 60 ± 2 DEG C, open grinding machine, grind 2.5h, dry, obtain pretreatment strontium titanates
Tao Fenti；
(2) aqueous premix is prepared: it in the reactor, is separately added into, deionized water: 900 mL, and Methacrylamide: 70g, N,
N- methylene-bisacrylamide: 15g, polycarboxylate dispersant: 15g, stirring and dissolving adjust pH 8 or so with ammonium hydroxide, are premixed
Close solution；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being separately added into, pre-processing titanium
Sour strontium pottery powder: 330g, aqueous premix: 670g, strong stirring 90min, spray drying are obtained for molded through three-dimensional printing work
Skill strontium titanate ceramic powder, partial size is in 120 ~ 150 μ ms.
Application method: one kind is answered for molded through three-dimensional printing technique strontium titanate ceramic powder to be molding on 3D printer
With feature are as follows: 3DP moulding process strontium titanate ceramic powder will be used for and be added in powder supply cylinder, printing head sprays printer spray
Head sprinkling mass percentage concentration is 6% ammonium persulfate solution and 2% ascorbic acid mixed solution.Specific embodiment is as follows:
After upper one layer of bonding, moulding cylinder declines a distance (being equal to thickness: 0.013~0.1mm), and powder supply cylinder rises a height,
If releasing dry powder, and moulding cylinder is shifted by powder-laying roller, pave and is compacted.Spray head under the control of the computer, by next construction
The formed data in section selectively spray mass percentage concentration be 6% ammonium persulfate solution mixed with 2% ascorbic acid it is molten
Liquid, when powder-laying roller powdering, extra powder was collected by powder collection device.Such powder feeding again and again, powdering and sprinkling quality percentage
Concentration is 6% ammonium persulfate solution and 2% ascorbic acid mixed solution, is finally completed the bonding of a three-dimensional powder.Not by
The place for spraying solution is dry powder, is played a supportive role in forming process, and after forming, is easier to remove.
Claims (5)
1. a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder, which is characterized in that this method has
Following processing step:
(1) strontium titanates pottery powder pretreatment: in the ball mill, being added by mass percentage, strontium titanates pottery powder: 93% ~ 96%, it burns
Knot auxiliary agent: 3% ~ 6%, titanate coupling agent TC-F:0.5% ~ 2.5%, the sum of each component is that absolutely, temperature rises to 60 ± 2 DEG C,
Grinding machine is opened, 2-3h is ground, it is dry, obtain pretreatment strontium titanates pottery powder；
(2) aqueous premix is prepared: in the reactor, it is added by mass percentage concentration, deionized water: 88% ~ 92%, and metering system
Amide: 6% ~ 10%, N, N- methylene-bisacrylamide: 0.2% ~ 1.5%, polycarboxylate dispersant: 0.5% ~ 2.0%, the sum of each component
For absolutely, stirring and dissolving adjusts pH 8 or so with ammonium hydroxide, obtains aqueous premix；
(3) it is used for the preparation of molded through three-dimensional printing technique strontium titanate ceramic powder: in the reactor, being added by mass percentage,
Pretreatment strontium titanates pottery powder: 30% ~ 35%, aqueous premix: 65% ~ 70%, the sum of each component is absolutely strong stirring 80
~ 100min, spray drying are obtained for molded through three-dimensional printing technique strontium titanate ceramic powder, and partial size is in 120 ~ 150 μ ms
It is interior.
2. a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder according to claim 1,
Be characterized in that, in step (1) strontium titanates strontium pottery powder, sintering aid powder partial size be nanometer grade powder.
3. a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder according to claim 1,
Be characterized in that, in step (1) the sintering aid be it is a kind of in lanthanum sesquioxide, neodymium oxide or yttria or
Two kinds of mixing.
4. a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder according to claim 1,
It is characterized in that, at 100 DEG C, air outlet temperature is controlled at 90 DEG C for spray drying intake air temperature control in step (3),
Enter the wind flow 280m3/h。
5. a kind of preparation method for molded through three-dimensional printing technique strontium titanate ceramic powder according to claim 1 is made
Standby is used for molded through three-dimensional printing technique strontium titanate ceramic powder, which is characterized in that described to be used for molded through three-dimensional printing technique titanium
For sour strontium ceramic powder in 3D printer printing shaping, printer head sprays the ammonium persulfate solution that mass percentage concentration is 6%
With 2% ascorbic acid mixed solution.
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