CN107434412A - The preparation method of improved ceramic powder slurry and direct write shaped three dimensional structure - Google Patents
The preparation method of improved ceramic powder slurry and direct write shaped three dimensional structure Download PDFInfo
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- CN107434412A CN107434412A CN201610358491.6A CN201610358491A CN107434412A CN 107434412 A CN107434412 A CN 107434412A CN 201610358491 A CN201610358491 A CN 201610358491A CN 107434412 A CN107434412 A CN 107434412A
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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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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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
- B33Y10/00—Processes of additive manufacturing
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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
- C04B35/01—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
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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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
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
Abstract
The invention belongs to 3D printing forming technique scope, and in particular to the preparation method of improved ceramic powder slurry and direct write shaped three dimensional structure.The present invention proposes the method that direct write shaping ceramic powder slurry is prepared using two or more dispersants of opposite types, ceramic powder slurry is prepared using certain type of dispersant first, then the related dispersant of one or more types is added in the slurry again, finally obtain not only with certain fluidity but also with certain viscoelastic ceramic powder slurry, and 3-D solid structure is prepared using the slurry.3-D solid structure postmenstruation sintering prepared by the present invention（Heat treatment）Can obtain densification ceramic component and range scale it is wide, can simple realization micron order to decimeter grade control.
Description
Technical field
The present invention relates to 3D printing field shaping technique, and in particular to improved ceramic powder slurry and direct write shaped three dimensional
The preparation method of structure.
Background technology
Direct write forming technique（Direct Ink Writing）It is a kind of new ceramic material 3D printing forming technique【J
A Lewis. Colloidal processing of ceramics. Journal of the American Ceramic
Society, 2000, 83(10): 2341-2359.】.The technology is first by area of computer aided（CAD）The three of design
The pattern of structure is tieed up, the ceramic powder somaplasm being made up of syringe and pin mouth on Z axis is then arranged on by computer controlled automatic
Material conveying device, the slurry in syringe is extruded to the line style fluid of accurate dimension out of pin mouth, while X-Y axles are according to program setting
Track movement, obtain the first Rotating fields by line style fluid deposition on the moving platform.After completing the first formable layer, Z axis horse
Up to the height for driving slurry conveying device to be moved to organization plan determination exactly up, the second formable layer will be in the first Rotating fields
Upper progress.Then, by way of being successively superimposed, the three-dimensional knot of the complex three-dimensional that can not be prepared with traditional moulding process is obtained
Structure.
Direct write forming technique has very high rheological property requirement to ceramic powder slurry.In direct write forming process, it is
Pin mouth is smoothly through, ceramic powder slurry requires good mobility；And after it flows through pin mouth and forms linear fluid,
Slurry requires to lose flowability again, has good mouldability, so as to ensure that the shape of molding structure does not change.To meet
This requirement, numerous researchers adjust slurry by changing the pH of slurry, or the various modes such as ionic strength of increase slurry
The rheological property of material, it is desired to be able to meet the requirement of direct write shaping.Cesarano is used with the thinning rheological property of high shear
Alumina powder slurry carries out direct write shaping【J III Cesarano, T A Baer, P Calvert. Recent
developments in freeform fabrication of dense ceramics from slurry
deposition. Albuquerque, NM: Sandia National Labs., 1997.】；Smay is devised by changing
The pH for becoming slurry obtains a kind of colloidal gel slurry that disclosure satisfy that direct write forming requirements【J E Smay, J Cesarano,
J A Lewis. Colloidal inks for directed assembly of 3-D periodic structures.
Langmuir, 2002, 18(14): 5429-5437】；Li etc. adjusts suspension by changing the ion concentration in suspension
Rheological property【Q Li, J A Lewis. Nanoparticle Inks for Directed Assembly of Three-
dimensional periodic structures. Advanced Materials, 2003, 15(19): 1639-
1643】.Although disclosure satisfy that forming requirements to a certain extent by various modes, still usually there is printhead blocking
Pin etc. makes the phenomenon that direct write shaping can not continue.
The content of the invention
In order to solve the above technical problems, we have proposed improved ceramic powder slurry and the system of direct write shaped three dimensional structure
Preparation Method, its can obtain densification ceramic component and prepared 3-D solid structure range scale it is wide, can simple realization it is micro-
Meter level to decimeter grade control.
To reach above-mentioned purpose, the invention provides a kind of preparation method of improved ceramic powder slurry, its specific step
It is rapid as follows：
1）A certain proportion of water, ceramic powder, sintering aid and a certain dispersant of type are subjected to ball milling, suitable viscosity is made
With the slurry of solid content, wherein, the solid content of powder is 0.01% ~ 99%, the addition of dispersant for powder quality 0.001% ~
10%；
2）The dispersant that one or more opposite types are added in the slurry continues ball milling；
Wherein, the solid content of powder is 0.01% ~ 99%, and the addition of dispersant is the 0.001% ~ 10% of powder quality, two kinds of phases
The mass ratio of anti-dispersant of type is 0.001% ~ 1000%, and the speed of ball milling is the rad/min of 10 rad/min ~ 50.
Preferably, the ceramic powder is in alumina powder, beta-silicon nitride powder, Zirconium powder, aluminium nitride powder
It is a kind of.
Preferably, the sintering aid is one or more in yittrium oxide, lanthana, magnesia.
Preferably, the dispersant is one kind in anionic dispersing agent, cationic dispersing agent.
Preferably, the anionic dispersing agent is polyacrylic, poly class, polystyrene sulphuric acid class, polyphenyl
It is one or more in sulphonic acids, polyvinyl sulfonic acid class, polyvinyl class.
Preferably, in the cationic dispersing agent polyethyleneimine amine hydrochlorate class, polyvinyl pyridine class, polyethylene amine
It is one or more.
Preferably, the abrading-ball that the ball milling uses is a kind of in zirconia ball, alumina balls.
Present invention also offers a kind of preparation method using ceramic powder slurry direct write shaped three dimensional structure, this method bag
Include following steps：
1）Ceramic powder slurry is carried out to be stirred under vacuum 5 min of degasification ~ 30min；
2）Direct write shaping is carried out again, obtains the base substrate of 3-D solid structure；Wherein, temperature control is 20 DEG C ~ 40 DEG C, humid control
For 40% ~ 72%.Direct write briquetting pressure is the PSI of 10PSI ~ 2000；Printhead translational speed is 0.01mm/sec ~ 600mm/sec；
3）It is 60% ~ 82% that the base substrate of shaping is placed in into humidity, and temperature is dried 1 ~ 2 hour under conditions of being 60 DEG C ~ 80 DEG C；
4) base substrate is placed in dumping sintering furnace again, 600 DEG C ~ 800 DEG C is risen to 1 DEG C/min ~ 2.5 DEG C/min heating rate
Insulation carries out dumping in 2 ~ 3 hours;
5) then proceed to 8 DEG C/min ~ 14 DEG C/min heating rate rise to 1400 DEG C ~ 1850 DEG C sinter 2 ~ 3 hours,
Wherein, argon gas is injected after being vacuumized in sintering furnace.
Preferably, the ceramic powder slurry is prepared by the preparation method of above-mentioned improved ceramic powder slurry.
Pass through above-mentioned technical proposal, the beneficial effects of the invention are as follows using the addition opposite types point in ceramic powder slurry
The rheological property that the method for powder carrys out slurry is allowed to the requirement for meeting direct write forming technique, the advantage is that：
First, the rheological property of ceramic powder slurry need to only control the order of addition of various dispersants and addition simply to adjust
Control, obtain the slurry for meeting direct write forming requirements；
When the 2nd, carrying out direct write shaping using ceramic powder slurry proposed by the present invention, it is not easy to phenomena such as gaging somebody, beneficial to straight
The control of write forming technique；
3rd, the present invention is a kind of mould-free forming, and the 3-D solid structure of preparation is that traditional moulding process can not obtain；
4th, the present invention is not limited by material system, applied widely, a variety of ceramics being molded available for shaping by powder,
And prepare the sintered rear part for obtaining densification of 3-D solid structure；
5th, the range scale of 3-D solid structure that prepared by the present invention is wide, can simple realization micron order to decimeter grade control.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
The embodiment of the present invention is described in further detail below.
Embodiment 1. prepares ZrO using dispersant Sodium Polyacrylate and polyethyleneimine hydrochloric acid sodium2Slurry is simultaneously molded micron
Level 3-D solid structure, it is specific as follows：
By 4g anionic dispersing agents Sodium Polyacrylate and Y2O3Stable 200g ZrO2Powder（D50 is 0.8 μm）It is added to
Ball milling is carried out in 12mL deionized waters, then adds 2g cationic dispersing agent polyethyleneimine hydrochloric acid sodium, it is small to continue ball milling 5
When, obtain ZrO2Slurry.Wherein, abrading-ball is 300g zirconia ball, and ball milling speed is 20 rad/min；
By the ZrO of acquisition2Slurry is carried out after being stirred under vacuum degasification 15min, then carries out direct write shaping, obtains crisscross three-dimensional
Stereochemical structure, temperature control are 35 DEG C or so, and humid control 40%, direct write briquetting pressure is 50PSI, printhead translational speed
For 10mm/sec；
It is 60% that the base substrate of shaping is placed in into humidity, and temperature is dried 2 hours under conditions of being 70 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 800 DEG C of insulations are risen to 1.5 DEG C/min heating rate and carry out dumping within 3 hours, are then proceeded to 10 DEG C/min liter
Warm speed rises to 1400 DEG C and sintered 2 hours.
Example 2, Si3N4 powdery pulps are prepared simultaneously using polyethylene of dispersing agent imines, Sodium Polyacrylate and polyvinyl
Grade 3-D solid structure is molded, it is specific as follows：
First by cationic dispersing agent polyethyleneimine 10g and Si3N4 powder 800g（D50 is 12 μm）, 4g sintering aids Y2O3
With 1g La2O3It is added in 50mL deionized waters and carries out ball milling 12 hours, then adds anionic dispersing agent 4g polypropylene
Sour sodium and 3g polyvinyl, continues ball milling 4 hours, obtains Si3N4Slurry, wherein, abrading-ball be 800g zirconia ball, ball milling
Speed is 50 rad/min；
By the Si of acquisition3N4Slurry is carried out after being stirred under vacuum degasification 12min, then carries out direct write shaping, obtains crisscross three
Tie up stereochemical structure.Temperature control is 25 DEG C or so, humid control 60%, and direct write briquetting pressure is 30PSI, and printhead movement is fast
Spend for 20mm/sec；
It is 80% that the base substrate of shaping is placed in into humidity, and temperature is dried 1 hour under conditions of being 80 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 700 DEG C of insulations are risen to 1 DEG C/min heating rate and carry out dumping within 2 hours, are then proceeded to 8 DEG C/min heating
Speed rises to 1820 DEG C and sintered 3 hours, is sintered in Ar2Carried out in atmosphere.
Example 3, Al prepared using dispersant polyacrylic acid and polyethyleneimine hydrochloric acid sodium2O3Slurry is simultaneously molded micron order three
Stereochemical structure is tieed up, it is specific as follows：
It is 5g and Al by anionic dispersing agent polyacrylic acid2O3Powder is 300g（D50 is 1.3 μm）, sintering aid MgO be 3g
It is added in 50mL deionized waters and carries out ball milling 22 hours, then adds cationic dispersing agent 1g polyethyleneimine hydrochloric acid
Sodium, continues ball milling 3 hours, obtains Al2O3Slurry, wherein, abrading-ball is 320g alumina balls, and ball milling speed is 10 rad/min；
The alumina slurry of acquisition is carried out after being stirred under vacuum degasification 6min, then carries out direct write shaping, obtains crisscross three
Stereochemical structure is tieed up, temperature control is 30 DEG C or so, humid control 42%, and direct write briquetting pressure is 40PSI, and printhead movement is fast
Spend for 20mm/sec；
It is 63% that the base substrate of shaping is placed in into humidity, and temperature is dried 1 hour under conditions of being 72 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 600 DEG C of insulations are risen to 2.5 DEG C/min heating rate and carry out dumping within 3 hours, are then proceeded to 8 DEG C/min liter
Warm speed rises to 1500 DEG C and sintered 3 hours.
Example 4, AlN slurries are prepared using dispersants ammonium polyacrylate and polyethyleneimine hydrochloric acid sodium and are molded micron order three
Stereochemical structure is tieed up, it is specific as follows：
By 12g the moon dispersants ammonium polyacrylate and 320g AlN powders（D50 is 3 μm）, 2.2g sintering aids Y2O3's and 3g
La2O3, which is added in 36mL deionized waters, carries out ball milling 20 hours, then adds 2g cationic dispersing agent polyethyleneimines
Hydrochloric acid sodium, continues ball milling 2 hours, obtains AlN slurries, wherein, abrading-ball is 400g zirconia ball, and ball milling speed is 12 rad/
min；
The AlN slurries of acquisition are carried out after being stirred under vacuum degasification 6min, then carry out direct write shaping, crisscross three-dimensional is obtained and stands
Body structure, temperature control are 34 DEG C or so, and humid control 72%, direct write briquetting pressure is 100PSI, and printhead translational speed is
120mm/sec；
It is 62% that the base substrate of shaping is placed in into humidity, and temperature is dried 1.2 hours under conditions of being 75 DEG C；Base substrate is placed in vacuum again
In dumping sintering furnace, with 1.2 DEG C/min heating rate rise to 620 DEG C insulation 2 hours carry out dumping, then proceed to 14 DEG C/
Min heating rate rises to 1520 DEG C of vacuum-sintering 2 hours.
Example 5, ZrO prepared using dispersant Sodium Polyacrylate and polyethyleneimine2Slurry and to be molded micron order three-dimensional vertical
Body structure, it is specific as follows：
By 5g anionic dispersing agents Sodium Polyacrylate and Y2O3Stable 280g ZrO2Powder（D50 is 0.8 μm）, it is added to
Ball milling is carried out in 12mL deionized waters, then adds 1g cationic dispersing agent polyethyleneimines, continues ball milling 15 hours, is obtained
Obtain ZrO2Slurry, wherein, abrading-ball is 350g zirconia ball, and ball milling speed is 22 rad/min；
By the ZrO of acquisition2Slurry is carried out after being stirred under vacuum degasification 12min, then carries out direct write shaping, obtains crisscross three-dimensional
Stereochemical structure.Temperature control is 32 DEG C or so, and humid control 50%, direct write briquetting pressure is 60PSI, printhead translational speed
For 30mm/sec；
It is 60% that the base substrate of shaping is placed in into humidity, and temperature is dried 2 hours under conditions of being 70 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 800 DEG C of insulations are risen to 1.5 DEG C/min heating rate and carry out dumping within 3 hours, are then proceeded to 10 DEG C/min liter
Warm speed rises to 1400 DEG C and sintered 2 hours.
Example 6, Si3N4 powdery pulps are prepared using polyethylene of dispersing agent pyridine and poly and are molded grade three-dimensional
Stereochemical structure, it is specific as follows：
First by 6g cationic dispersing agents polyvinyl pyridine and 600g Si3N4 powders（D50 is 15 μm）, 3g sintering aids
Y2O3With 2g La2O3It is added in 60mL deionized waters and carries out ball milling 15 hours, then adds 10g anionic dispersing agents
Poly, continues ball milling 4 hours, obtains Si3N4Slurry, wherein, abrading-ball be 800g zirconia ball, ball milling speed 50
rad/min；
By the Si of acquisition3N4Slurry is carried out after being stirred under vacuum degasification 12min, then carries out direct write shaping, obtains crisscross three
Stereochemical structure is tieed up, temperature control is 25 DEG C or so, humid control 60%, and direct write briquetting pressure is 30PSI, and printhead movement is fast
Spend for 20mm/sec；
It is 81% that the base substrate of shaping is placed in into humidity, and temperature is dried 2 hours under conditions of being 60 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 650 DEG C of insulations are risen to 1 DEG C/min heating rate and carry out dumping within 2 hours, are then proceeded to 8 DEG C/min heating
Speed rises to 1850 DEG C and sintered 3 hours.It is sintered in Ar2Carried out in atmosphere.
Example 7, Al prepared using polyethylene of dispersing agent sodium sulfonate and polyethyleneimine hydrochloric acid sodium2O3Slurry is simultaneously molded micron
Level 3-D solid structure, it is specific as follows：
By 3g anionic dispersing agents sodium apolate and 200g Al2O3Powder（D50 is 1 μm）, 2g sintering aids MgO
It is added in 40mL deionized waters and carries out ball milling 12 hours, then adds 1g cationic dispersing agent polyethyleneimine hydrochloric acid
Sodium, continues ball milling 3 hours, obtains Al2O3Slurry.Wherein, abrading-ball is 320g zirconia ball, and ball milling speed is 10 rad/min.
By the Al of acquisition2O3Slurry is carried out after being stirred under vacuum degasification 6min, then carries out direct write shaping, is obtained crisscross
3-D solid structure, temperature control are 28 DEG C or so, and humid control 62%, direct write briquetting pressure is 80PSI, and printhead moves
Speed is 120mm/sec；
It is 80% that the base substrate of shaping is placed in into humidity, and temperature is dried 1 hour under conditions of being 72 DEG C；Base substrate is placed in into dumping again to burn
In freezing of a furnace, 600 DEG C of insulations are risen to 1.5 DEG C/min heating rate and carry out dumping within 3 hours, are then proceeded to 8 DEG C/min liter
Warm speed rises to 1550 DEG C and sintered 3 hours.
Example 8, AlN slurries are prepared using dispersant polyphenyl sulfonic acid and polyethyleneimine hydrochloric acid sodium and are molded grade three-dimensional
Stereochemical structure, it is specific as follows：
By 10g the moon dispersant polyphenyl sulfonic acid and 300g AlN powders（D50 is 2 μm）, 3.2g sintering aids Y2O3With 2g's
La2O3It is added in 40mL deionized waters and carries out ball milling 10 hours, then adds 2g cationic dispersing agent polyethyleneimine amine salt
Sour sodium, continues ball milling 2 hours, obtains AlN slurries, wherein, abrading-ball is 400g zirconia ball, and ball milling speed is 12 rad/
min；
The AlN slurries of acquisition are carried out after being stirred under vacuum degasification 6min, then carry out direct write shaping, crisscross three-dimensional is obtained and stands
Body structure.Temperature control is 34 DEG C or so, and humid control 72%, direct write briquetting pressure is 100PSI, and printhead translational speed is
120mm/sec；
It is 82% that the base substrate of shaping is placed in into humidity, and temperature is dried 1.2 hours under conditions of being 64 DEG C；Base substrate is placed in vacuum again
In dumping sintering furnace, with 1.1 DEG C/min heating rate rise to 730 DEG C insulation 2 hours carry out dumping, then proceed to 14 DEG C/
Min heating rate rises to 1600 DEG C of vacuum-sintering 2 hours.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (9)
1. a kind of preparation method of improved ceramic powder slurry, it is characterised in that it is comprised the following steps that：
1）A certain proportion of water, ceramic powder, sintering aid and a certain dispersant of type are subjected to ball milling, suitable viscosity is made
With the slurry of solid content, wherein, the solid content of powder is 0.01% ~ 99%, the addition of dispersant for powder quality 0.001% ~
10%；
2）The dispersant that one or more opposite types are added in the slurry continues ball milling；
Wherein, the solid content of powder is 0.01% ~ 99%, and the addition of dispersant is the 0.001% ~ 10% of powder quality, two kinds of phases
The mass ratio of anti-dispersant of type is 0.001% ~ 1000%, and the speed of ball milling is the rad/min of 10 rad/min ~ 50.
A kind of 2. preparation method of improved ceramic powder slurry according to claim 1, it is characterised in that the ceramics
Powder is one kind in alumina powder, beta-silicon nitride powder, Zirconium powder, aluminium nitride powder.
A kind of 3. preparation method of improved ceramic powder slurry according to claim 1, it is characterised in that the sintering
Auxiliary agent is one or more in yittrium oxide, lanthana, magnesia.
4. the preparation method of a kind of improved ceramic powder slurry according to claim 1, it is characterised in that described scattered
Agent is one kind in anionic dispersing agent, cationic dispersing agent.
A kind of 5. preparation method of improved ceramic powder slurry according to claim 4, it is characterised in that it is described it is cloudy from
Subtype dispersant is polyacrylic, poly class, polystyrene sulphuric acid class, polyphenyl sulphonic acids, polyvinyl sulfonic acid class, poly- second
It is one or more in alkenyl phosphoric acid class.
A kind of 6. preparation method of improved ceramic powder slurry according to claim 4, it is characterised in that it is described sun from
It is one or more in subtype polyethylene of dispersing agent imide hydrochloride salt, polyvinyl pyridine class, polyethylene amine.
A kind of 7. preparation method of improved ceramic powder slurry according to claim 1, it is characterised in that the ball milling
The abrading-ball used is a kind of in zirconia ball, alumina balls.
8. a kind of preparation method using ceramic powder slurry direct write shaped three dimensional structure, it is characterised in that this method is included such as
Lower step：
1）Ceramic powder slurry is carried out to be stirred under vacuum 5 min of degasification ~ 30min；
2）Direct write shaping is carried out again, obtains the base substrate of 3-D solid structure；Wherein, temperature control is 20 DEG C ~ 40 DEG C, humid control
For 40% ~ 72%, direct write briquetting pressure is the PSI of 10PSI ~ 2000；Printhead translational speed is 0.01mm/sec ~ 600mm/sec；
3）It is 60% ~ 82% that the base substrate of shaping is placed in into humidity, and temperature is dried 1 ~ 2 hour under conditions of being 60 DEG C ~ 80 DEG C；
4) base substrate is placed in dumping sintering furnace again, 600 DEG C ~ 800 DEG C is risen to 1 DEG C/min ~ 2.5 DEG C/min heating rate
Insulation carries out dumping in 2 ~ 3 hours;
5) then proceed to 8 DEG C/min ~ 14 DEG C/min heating rate rise to 1400 DEG C ~ 1850 DEG C sinter 2 ~ 3 hours,
Wherein, argon gas is injected after being vacuumized in sintering furnace.
9. a kind of preparation method using ceramic powder slurry direct write shaped three dimensional structure according to claim 8, it is special
Sign is, preparation side of the ceramic powder slurry as the improved ceramic powder slurry any one of claim 1 ~ 7
Method is prepared.
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| CN108298965A (en) * | 2018-01-10 | 2018-07-20 | 苏州拜博机电科技有限公司 | A method of multilevel hole material is prepared using direct write forming technique |
| CN108455972A (en) * | 2018-01-10 | 2018-08-28 | 苏州拜博机电科技有限公司 | A method of regulation and control direct write molding sizing material forming performance |
| CN109111223A (en) * | 2018-09-18 | 2019-01-01 | 中国科学院宁波材料技术与工程研究所 | 3D direct write printing titanium dioxide ceramic composition, slurry, preparation method and application |
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