CN107140991B - A kind of ceramic spherical material and the preparation method and application thereof for 3D printing - Google Patents

A kind of ceramic spherical material and the preparation method and application thereof for 3D printing Download PDF

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CN107140991B
CN107140991B CN201710390660.9A CN201710390660A CN107140991B CN 107140991 B CN107140991 B CN 107140991B CN 201710390660 A CN201710390660 A CN 201710390660A CN 107140991 B CN107140991 B CN 107140991B
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spherical material
ceramic
printing
ceramic spherical
nodularization
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CN107140991A (en
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李伶
王营营
李勇
王再义
陈学江
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Abstract

The ceramic spherical material and the preparation method and application thereof that the invention discloses a kind of for 3D printing, comprising the following steps: ingredient, ball milling, drying, sieving, radio frequency plasma nodularization.In addition, the ceramic spherical material being prepared the invention discloses the above method and the application of the ceramic spherical material in 3D printing.The present invention prepares 3D printing ceramic spherical material using radio frequency plasma technology for the first time, and the spherical material that the present invention is prepared forms grain composition, and the 3D printing suitable for ceramics forms, and is also beneficial to the sintering of its green body.

Description

A kind of ceramic spherical material and the preparation method and application thereof for 3D printing
Technical field
The present invention relates to the preparations of the spherical material used in 3D printing, and in particular to a kind of ceramic spherical material for 3D printing And the preparation method and application thereof.
Background technique
With ceramic 3D printing technique especially precinct laser sintering technology (SLS) and UV-curing technology (SLA) Development, also proposed new requirement, the i.e. spheroidization of ceramic powder to ceramic powder raw material.It is contacted when spherical powder particle packing Face is small, and inter-particle voids are few, and apparent density, tap density and the mobility of powder are significantly improved, and spherical powder has Higher specific surface area, reactivity are also high.In UV-curing technology forming process, since the surface mobility of ball is good, It being stirred evenly with light-cured resin, resin content is small, and mobility is best, and the loading of powder can reach 90% or more, Be conducive to the densification of ceramics.
The method for preparing ceramic spherical powder at present includes high-temperature fusion gunite, gas flame method, plasma method etc. The chemical methodes such as physical method and vapor phase method, liquid phase method (sol-gal process, the precipitation method, microemulsion method).There are techniques for chemical method The problems such as complicated, process is difficult to control, the spherical powder volume density of preparation is low, cost is generally higher.Physical method can obtain The high spherical powder of volume density, but the temperature range, clean for requiring heating device to have stable temperature field, can easily be accommodated Thermal source environment (ensures ceramic powder not by secondary pollution).Flame method is not easy to obtain high Oxygen potential and without fixed due to temperature limitations Form quotient；High-temperature fusion gunite Shortcomings in terms of purity and granularity control.Radio frequency plasma nodularization powder-making technique and its Its method is compared, and remarkable advantage is: region of discharge volume is larger, and energy is high.Related radio frequency plasma spheronization techniques preparation 3D is beaten The ceramic spherical material of print yet there are no report.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of ceramic spherical material for 3D printing.
To achieve the goals above, the invention is realized by the following technical scheme:
A kind of preparation method of the ceramic spherical material for 3D printing, comprising the following steps: ingredient, ball milling, drying, mistake Sieve, radio frequency plasma nodularization.
It is preferred: during the radio frequency plasma nodularization: 20~30L/min of working gas flow, side throughput 85~ 120L/min, 5~35g/min of feed rate, 65~90kPa of system pressure, 75~90kW of plasma power.
It is preferred: during the radio frequency plasma nodularization: 20~30L/min of working gas flow, side throughput 100~ 120L/min, 15~35g/min of feed rate, 65~90kPa of system pressure, 85~90kW of plasma power.
It is preferred: 30~60 meshes of the sieving.
Preferred: the ceramic spherical material is Al2O3(2054 DEG C of fusing point), SiO2(1650 ± 50 DEG C of fusing point), ZrO2It is (molten 2700 DEG C of point), TiC (3067 DEG C of fusing point), ZrB (3040 DEG C of fusing point), hydroxyapatite (1650 DEG C of fusing point) or tricalcium phosphate it is (molten 1670 DEG C of point).
The second object of the present invention is to provide a kind of ceramic spherical material being prepared by any of the above-described method, the Ceramic Balls The particle size range of shape material is 0.5~20 μm, Oxygen potential 95-100%.
The third object of the present invention is to provide a kind of spherical material being prepared by any of the above-described method in 3D printing Using.
The fourth object of the present invention is to provide a kind of production being prepared by the spherical material that any of the above-described method is prepared Product, it is preferred: the product being prepared by way of 3D printing by the spherical material that any of the above-described method is prepared.
Compared with prior art, the invention has the following advantages:
(1) ceramic particle in irregular shape by carrier gas by feeding gun spray into plasma arcs after, radiation, convection current, Under four kinds of heat transfer mechanism effects of conduction and chemistry, it is heated rapidly (maximum temperature is up to 10000K) and melts, the particle of melting The very high drop of sphericity, and the quick solidification under high temperature gradient are formed under the action of surface tension, are formed spherical Particle.
(2) although radio frequency plasma technology is a kind of known technology, but it applies primary limitation in 3D printing field In the spherical material preparation of metal and its alloy, the present invention is prepared using radio frequency plasma technology for the first time to make pottery suitable for 3D printing Porcelain spherical shape material, by the comprehensive adjustment of nodularization parameter, the achievable grain composition of spherical shape material (bulky grain: middle particle=1:7~2: 5 or bulky grain: little particle=1:2~2:3 or middle particle: little particle=5:3~7:2 or bulky grain: middle particle: little particle =1:7:2-2:5:3), wherein 10 μm≤bulky grain≤20 μm, 2 μm≤10 μm of particle < middle, 2 μm of 0.5 μm≤little particle <；
(3) pattern of ceramic particle and size are extremely important to the 3D printing molding effect and sintering character of ceramic body, Granule-morphology is closer to spherical shape, and surface mobility is better, and ceramic 3D printing molding effect is better, and the ceramics of grain composition Powder can realize the tightly packed densification sintering to be conducive to its green body, and the spherical pellet rate of the method for the present invention preparation is high, And grain composition is suitble to 3D printing, is conducive to the sintering of blank Densification.
Detailed description of the invention
Fig. 1 is the SiO that embodiment 1 is prepared2Ceramic spherical material micro-structure diagram；
Fig. 2 is the Al that embodiment 2 is prepared2O3Ceramic spherical material micro-structure diagram；
Fig. 3 is the ZrO that embodiment 3 is prepared2Ceramic spherical material micro-structure diagram；
Fig. 4 is the TiC ceramic spherical material micro-structure diagram that embodiment 4 is prepared；
Fig. 5 is the ZrB ceramic spherical material micro-structure diagram that embodiment 5 is prepared；
Fig. 6 is the hydroxylapatite ceramic spherical shape material micro-structure diagram that embodiment 6 is prepared；
Fig. 7 is the calcium phosphate ceramics spherical shape material micro-structure diagram that embodiment 7 is prepared.
Specific embodiment
In order to be better understood by technical solution of the present invention, with reference to the accompanying drawings of the specification with specific embodiment to the present invention It is described further.
Embodiment 1
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weighing a certain amount of to nodularization SiO2Ceramic powders, according to material: ball: water=1:2:3 mass ratio, ball Grind 12h；
Step 2: will be to nodularization SiO2Ceramic powder goes out to grind, and is placed in baking oven and dries to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 45 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 25L/min, side throughput 110L/min, feed rate 20g/min, system pressure 80kPa, plasma power 80kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in Figure 1, prepared SiO21.6-10 μm of partial size of ceramic spherical material, Oxygen potential 95%.
Embodiment 2
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weighing a certain amount of to nodularization Al2O3Ceramic powders, according to material: ball: water=1:2:3 mass ratio, ball Grind 10h；
Step 2: will be to nodularization Al2O3Ceramic powder goes out to grind, and is placed in baking oven and dries to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 50 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 20L/min, side throughput 100L/min, feed rate 15g/min, system pressure 70kPa, plasma power 85kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in Fig. 2, prepared Al2O30.5-3.5 μm of partial size of ceramic spherical material, Oxygen potential 100%.
Embodiment 3
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weighing a certain amount of to nodularization ZrO2Ceramic powders, according to material: ball: water=1:3:3 mass ratio, ball Grind 14h；
Step 2: will be to nodularization ZrO2Ceramic powder goes out to grind, and is placed in baking oven and dries to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 60 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 30L/min, side throughput 100L/min, feed rate 15g/min, system pressure 85kPa, plasma power 90kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in figure 3, prepared ZrO20.5-2.5 μm of partial size of ceramic spherical material, Oxygen potential 100%.
Embodiment 4
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weigh it is a certain amount of to nodularization TiC ceramic powders, according to material: ball: water=1:2:4 mass ratio, ball Grind 15h；
Step 2: will go out grind to nodularization TiC ceramic powder, and be placed in baking oven and dry to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 35 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 23L/min, side throughput 110L/min, feed rate 20g/min, system pressure 65kPa, plasma power 90kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in figure 4,5.3-11.7 μm of partial size prepared of TiC ceramic spherical material, Oxygen potential 100%.
Embodiment 5
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weigh it is a certain amount of to nodularization ZrB ceramic powders, according to material: ball: water=1:4:3 mass ratio, ball Grind 9h；
Step 2: will go out grind to nodularization ZrB ceramic powder, and be placed in baking oven and dry to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 45 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 28L/min, side throughput 100L/min, feed rate 15g/min, system pressure 90kPa, plasma power 83kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in figure 5,1-8 μm of partial size prepared of ZrB ceramic spherical material, Oxygen potential 100%.
Embodiment 6
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weigh it is a certain amount of to nodularization hydroxylapatite ceramic powder, according to material: ball: water=1:4:5 quality Ratio, ball milling 18h；
Step 2: will go out grind to nodularization Hydroxyapatite Ceramic Powder, and be placed in baking oven and dry to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 60 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 22L/min, side throughput 110L/min, feed rate 15g/min, system pressure 75kPa, plasma power 85kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in fig. 6,1.0-5.7 μm of partial size prepared of hydroxylapatite ceramic spherical shape material, Oxygen potential 100%.
Embodiment 7
A kind of preparation method of the ceramic spherical material for 3D printing, steps are as follows:
Step 1: weigh it is a certain amount of to nodularization calcium phosphate ceramics powder, according to material: ball: water=1:2:3 mass ratio Example, ball milling 12h；
Step 2: will go out grind to nodularization calcium phosphate ceramics powder, and be placed in baking oven and dry to constant weight；
Step 3: the ceramic powder after drying sieving: being crossed into 50 meshes；
Step 4: radio frequency plasma nodularization: ceramic powder after sieving is added in radio frequency plasma nodularization powder manufacturing apparatus, Adjustment equipment parameter: working gas flow 25L/min, side throughput 100L/min, feed rate 20g/min, system pressure 80kPa, plasma power 80kW.
Step 5: the collection of ceramic spherical material and the test of partial size and Oxygen potential.
As shown in fig. 7,1.3-10 μm of partial size prepared of calcium phosphate ceramics spherical shape material, Oxygen potential 95%.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein Can technical characteristic replaced mutually and the technical solution that is formed.

Claims (5)

1. a kind of preparation method of the ceramic spherical material for 3D printing, it is characterized in that: the following steps are included: ingredient, ball milling, dry Dry, sieving, radio frequency plasma nodularization,
During the radio frequency plasma nodularization: 20~30L/min of working gas flow, side 85~120L/min of throughput add Expect 5~35g/min of rate, 65~90kPa of system pressure, 75~90kW of plasma power,
The mass ratio of raw material and water is 1:3-1:5 in the mechanical milling process,
30~60 meshes of the sieving,
The ceramic spherical material is Al2O3、SiO2、ZrO2, TiC, ZrB, hydroxyapatite or tricalcium phosphate.
2. the ceramic spherical material that claim 1 the method is prepared.
3. ceramic spherical material as claimed in claim 2, it is characterized in that: particle size range is 0.5~20 μm, Oxygen potential 95- 100%.
4. application of the ceramic spherical material as claimed in claim 2 in 3D printing.
5. the product being prepared by way of 3D printing by ceramic spherical material as claimed in claim 2.
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