CN106630960A - 3d printing tantalum nitride ceramic material and preparation method thereof - Google Patents
3d printing tantalum nitride ceramic material and preparation method thereof Download PDFInfo
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses a 3D printing tantalum nitride ceramic material and a preparation method thereof. The preparation method comprises steps as follows: 1), kaolin, hargil, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum, glass fibers and water are mixed and then are calcined, and a calcined product is prepared; 2), polyvinylidene fluoride, methylcellulose, a silane coupling agent and a calcined product are mixed, and a basic material is prepared; 3), the basic material is ground, and the 3D printing tantalum nitride ceramic material is prepared. The liquid phase surface tension of the 3D printing tantalum nitride ceramic material is small, so that few cracks are formed on the surface of ceramic products; the preparation method has the advantages that raw materials are available and the process is simple.
Description
Technical field
The present invention relates to 3D printing material, in particular it relates to 3D printing tantalum nitride ceramic material and preparation method thereof.
Background technology
3D printing material is the important substance basis of 3D printing technique development, and to a certain extent, the development of material is to determine
Can 3D printing be determined the deciding factor being more widely used.At present, 3D printing material mainly include engineering plastics,
Photosensitive resin, rubber type of material, metal material and ceramic material.
3D printing ceramic material is the mixture of ceramic powders and adhesive powder composition.Due to the fusing point of adhesive powder
It is relatively low, adhesive powder will be melted when laser sintered and then ceramic powders are bonded together.After laser sintered, need
Ceramic is placed in temperature controlling stove carries out High Temperature Curing.Existing ceramic material in laser direct sintering, liquid phase surface
Tension force is big, larger thermal stress can be produced in rapid solidification, so as to form more crackle.
The content of the invention
It is an object of the invention to provide a kind of 3D printing tantalum nitride ceramic material and preparation method thereof, the 3D printing tantalum nitride
The liquid phase surface tension of ceramic material is little and then causes the crackle on the surface of ceramic few；Simultaneously the preparation method raw material is easy
, operation it is simple.
To achieve these goals, the invention provides a kind of preparation method of 3D printing tantalum nitride ceramic material, including：
1) kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum, glass fibre and water are mixed
Close, then calcined that calcined product is obtained；
2) Kynoar, methylcellulose, silane coupler are mixed base-material is obtained with calcined product；
3) base-material is ground that 3D printing tantalum nitride ceramic material is obtained.
Present invention also offers a kind of 3D printing tantalum nitride ceramic material, the 3D printing tantalum nitride ceramic material is by above-mentioned
Preparation method be prepared.
In above-mentioned technical proposal, the present invention causes obtained 3D by the synergy of above-mentioned each raw material and each step
Print tantalum nitride ceramic material liquid phase surface tension it is little so that cause ceramic surface crackle it is few；While the preparation side
Method raw material is easy to get, operation is simple.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of 3D printing tantalum nitride ceramic material, including：
1) kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum, glass fibre and water are mixed
Close, then calcined that calcined product is obtained；
2) Kynoar, methylcellulose, silane coupler are mixed base-material is obtained with calcined product；
3) base-material is ground that 3D printing tantalum nitride ceramic material is obtained.
In the step 1 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to further drop
The liquid phase surface tension of low obtained 3D printing tantalum nitride ceramic material, and then the crackle on the surface of ceramic is reduced,
Preferably, in step 1) in, relative to the kaolin of 100 weight portions, the consumption of carclazyte is 17-26 weight portions, the use of tantalum nitride
Measure as 21-29 weight portions, the consumption of boric acid is 14-18 weight portions, and the consumption of glucose is 33-45 weight portions, molybdenum trioxide
Consumption is 5-9 weight portions, and the consumption of nano aluminum is 11-14 weight portions, and the consumption of glass fibre is 17-24 weight portions, the use of water
Measure as 140-180 weight portions.
In the step 1 of the present invention) in, the actual conditions of mixing can be selected in wide scope, but in order to further
The liquid phase surface tension of obtained 3D printing tantalum nitride ceramic material is reduced, and then the crackle on the surface of ceramic is subtracted
It is few, it is preferable that in step 1) in, mixing at least meets following condition：Mixing temperature is 15-35 DEG C, and incorporation time is 40-
60min。
In the step 1 of the present invention) in, the actual conditions of calcining can be selected in wide scope, but in order to further
The liquid phase surface tension of obtained 3D printing tantalum nitride ceramic material is reduced, and then the crackle on the surface of ceramic is subtracted
It is few, it is preferable that in step 1) in, calcining at least meets following condition：Calcining heat is 470-520 DEG C, and calcination time is 7-
10h。
Meanwhile, in the present invention, in order to further reduce the liquid phase surface of obtained 3D printing tantalum nitride ceramic material
Power, so cause ceramic surface crackle reduce, it is preferable that in step 1) calcining before, preparation method also includes
Heating process, specially：First by mixture is from the 15-35 DEG C of ramp with 0.5-0.8 DEG C/min to 150-200 DEG C and protects
Warm 20-40min, then so that the ramp of 1.5-2.5 DEG C/min is to 300-380 DEG C and is incubated 30-40min, finally with 0.8-1
DEG C/min ramp is to 470-520 DEG C and is incubated.
In the step 1 of the present invention) in, the particle diameter of nano aluminum can be selected in wide scope, but in order to further drop
The liquid phase surface tension of low obtained 3D printing tantalum nitride ceramic material, and then the crackle on the surface of ceramic is reduced,
Preferably, in step 1) in, the particle diameter of nano aluminum is 30-40nm.
In the step 2 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to further drop
The liquid phase surface tension of low obtained 3D printing tantalum nitride ceramic material, and then the crackle on the surface of ceramic is reduced,
Preferably, in step 2) in, relative to the calcined product of 100 weight portions, the consumption of Kynoar is 75-90 weight portions, first
The consumption of base cellulose is 25-33 weight portions, and the consumption of silane coupler is 9-16 weight portions.
In the step 2 of the present invention) in, the actual conditions of mixing can be selected in wide scope, but in order to further
The liquid phase surface tension of obtained 3D printing tantalum nitride ceramic material is reduced, and then the crackle on the surface of ceramic is subtracted
It is few, it is preferable that in step 2) in, mixing at least meets following condition：Mixing temperature is 15-35 DEG C, and incorporation time is 20-
40min。
In the step 2 of the present invention) in, the actual conditions of grinding can be selected in wide scope, but in order to further
The liquid phase surface tension of obtained 3D printing tantalum nitride ceramic material is reduced, and then the crackle on the surface of ceramic is subtracted
It is few, it is preferable that in step 3) in, grinding is carried out by the way of ball milling, and ball milling at least meets following condition：Big ball and bead
Mass ratio be 2：1.3-1.5, abrading-ball is 10 with the mass ratio of material：0.8-1.2, rotating speed is 600-1200rpm, Ball-milling Time
For 25-35min.
Present invention also offers a kind of 3D printing tantalum nitride ceramic material, the 3D printing tantalum nitride ceramic material is by above-mentioned
Preparation method be prepared.
Hereinafter will be described the present invention by embodiment.
Embodiment 1
1) by kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum (particle diameter is 35nm), glass fibers
Peacekeeping water is according to 100：20：25：16：39：7：13：19：160 weight ratio mixes 50min at 25 DEG C, then from 25 DEG C with
The ramp of 0.7 DEG C/min is to 180 DEG C and is incubated 30min, then so that the ramp of 2 DEG C/min is to 360 DEG C and is incubated
35min, finally so that the ramp of 0.9 DEG C/min is to 490 DEG C and is incubated 8h so that calcined product is obtained；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH550) according to 100：80：28：14
Weight ratio mix 30min at 25 DEG C be obtained base-material；
3) (big ball is 2 with the mass ratio of bead base-material to be carried out into ball milling：1.4, abrading-ball is 10 with the mass ratio of material：
1.0, rotating speed is 900rpm, and Ball-milling Time is 30min) with prepared 3D printing tantalum nitride ceramic material A1.
Embodiment 2
1) by kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum (particle diameter is 30nm), glass fibers
Peacekeeping water is according to 100：17：21：14：33：5：11：17：140 weight ratio mixes 40min at 15 DEG C, then from 15 DEG C with
The ramp of 0.5 DEG C/min is to 150 DEG C and is incubated 20min, then so that the ramp of 1.5 DEG C/min is to 300 DEG C and is incubated
30min, finally so that the ramp of 0.8 DEG C/min is to 470 DEG C and is incubated 7h so that calcined product is obtained；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH560) according to 100：75：25：9
Weight ratio mixes 20min base-material is obtained at 15 DEG C；
3) (big ball is 2 with the mass ratio of bead base-material to be carried out into ball milling：1.3, abrading-ball is 10 with the mass ratio of material：
0.8, rotating speed is 600rpm, and Ball-milling Time is 25min) with prepared 3D printing tantalum nitride ceramic material A2.
Embodiment 3
1) by kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum (particle diameter is 40nm), glass fibers
Peacekeeping water is according to 100：26：29：18：45：9：14：24：180 weight ratio mixes 60min at 35 DEG C, then from 35 DEG C with
The ramp of 0.8 DEG C/min is to 200 DEG C and is incubated 40min, then so that the ramp of 2.5 DEG C/min is to 380 DEG C and is incubated
40min, finally so that the ramp of 1 DEG C/min is to 520 DEG C and is incubated 10h so that calcined product is obtained；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH570) according to 100：90：33：16
Weight ratio mix 40min at 35 DEG C be obtained base-material；
3) (big ball is 2 with the mass ratio of bead base-material to be carried out into ball milling：1.5, abrading-ball is 10 with the mass ratio of material：
1.2, rotating speed is 1200rpm, and Ball-milling Time is 35min) with prepared 3D printing tantalum nitride ceramic material A3.
Comparative example 1
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B1 is obtained, except that, step 1) in
Unused boric acid.
Comparative example 2
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B2 is obtained, except that, step 1) in
Unused glucose.
Comparative example 3
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B3 is obtained, except that, step 1) in
Unused molybdenum trioxide.
Comparative example 4
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B4 is obtained, except that, step 1) in
Unused nano aluminum.
Comparative example 5
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B5 is obtained, except that, step 1) in
Unused glass fibre.
Comparative example 6
Method according to embodiment 1 is carried out so that 3D printing tantalum nitride ceramic material B6 is obtained, except that, step 2) in
Unused silane coupler.
Detection example 1
Above-mentioned 3D printing tantalum nitride ceramic material is carried out into 3D printing and prints product to be obtained, then detection prints product
The crackle on surface, counts the crackle number (bar/dm of every square of cubic meter2) and average crack length (μm/bar), concrete outcome is shown in Table
1。
Table 1
| Crackle number (bar/dm2) | Average crack length (μm/bar) | |
| A1 | 3 | 0.1 |
| A2 | 1 | 0.2 |
| A3 | 3 | 0.2 |
| B1 | 9 | 0.4 |
| B2 | 7 | 0.6 |
| B3 | 8 | 0.4 |
| B4 | 9 | 0.6 |
| B5 | 9 | 0.7 |
| B6 | 10 | 0.3 |
By above-described embodiment, comparative example and detection example, the obtained 3D printing tantalum nitride ceramics that the present invention is provided
Material has relatively low liquid phase surface tension, and then reduces the crackle on the surface of ceramic.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as it is without prejudice to this
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of 3D printing tantalum nitride ceramic material, it is characterised in that include：
1) kaolin, carclazyte, tantalum nitride, boric acid, glucose, molybdenum trioxide, nano aluminum, glass fibre and water are mixed,
Then calcined that calcined product is obtained；
2) Kynoar, methylcellulose, silane coupler are mixed base-material is obtained with the calcined product；
3) base-material is ground that the 3D printing tantalum nitride ceramic material is obtained.
2. preparation method according to claim 1, wherein, in step 1) in, relative to the kaolinite of 100 weight portions
Soil, the consumption of the carclazyte is 17-26 weight portions, and the consumption of the tantalum nitride is 21-29 weight portions, and the consumption of the boric acid is
14-18 weight portions, the consumption of the glucose is 33-45 weight portions, and the consumption of the molybdenum trioxide is 5-9 weight portions, described
The consumption of nano aluminum is 11-14 weight portions, and the consumption of the glass fibre is 17-24 weight portions, and the consumption of the water is 140-
180 weight portions.
3. preparation method according to claim 2, wherein, in step 1) in, the mixing at least meets following condition：It is mixed
It is 15-35 DEG C to close temperature, and incorporation time is 40-60min.
4. preparation method according to claim 2, wherein, in step 1) in, the calcining at least meets following condition：Forge
It is 470-520 DEG C to burn temperature, and calcination time is 7-10h.
5. preparation method according to claim 4, wherein, in step 1) the calcining before, the preparation method is also
Including heating process, specially：First by mixture from the 15-35 DEG C of ramp with 0.5-0.8 DEG C/min to 150-200 DEG C
And be incubated 20-40min, then so that the ramp of 1.5-2.5 DEG C/min is to 300-380 DEG C and is incubated 30-40min, finally with
The ramp of 0.8-1 DEG C/min is to 470-520 DEG C and is incubated.
6. preparation method according to claim 2, wherein, in step 1) in, the particle diameter of the nano aluminum is 30-40nm.
7. the preparation method according to any one in claim 1-6, wherein, in step 2) in, relative to 100 weight portions
The calcined product, the consumption of the Kynoar is 75-90 weight portions, and the consumption of the methylcellulose is 25-33
Weight portion, the consumption of the silane coupler is 9-16 weight portions.
8. preparation method according to claim 7, wherein, in step 2) in, the mixing at least meets following condition：It is mixed
It is 15-35 DEG C to close temperature, and incorporation time is 20-40min.
9. the preparation method stated according to any one in claim 1-6,8, wherein, in step 3) in, the grinding adopts ball
The mode of mill is carried out, and the ball milling at least meets following condition：Big ball is 2 with the mass ratio of bead：1.3-1.5, abrading-ball with
The mass ratio of material is 10：0.8-1.2, rotating speed is 600-1200rpm, and Ball-milling Time is 25-35min.
10. a kind of 3D printing tantalum nitride ceramic material, it is characterised in that the 3D printing tantalum nitride ceramic material will by right
The preparation method in 1-9 described in any one is asked to be prepared.
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| CN105665697A (en) * | 2016-03-11 | 2016-06-15 | 中山大学惠州研究院 | Metal or ceramic consumable item for FDM 3D printing, preparation method for metal or ceramic consumable item and finished product printing method |
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Application publication date: 20170510 |