CN106674828A - 3d printing silicon nitride ceramic material and preparation method thereof - Google Patents
3d printing silicon nitride ceramic material and preparation method thereof Download PDFInfo
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- CN106674828A CN106674828A CN201611060140.3A CN201611060140A CN106674828A CN 106674828 A CN106674828 A CN 106674828A CN 201611060140 A CN201611060140 A CN 201611060140A CN 106674828 A CN106674828 A CN 106674828A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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Abstract
The invention discloses a 3D printing silicon nitride ceramic material and a preparation method of the 3D printing silicon nitride ceramic material. The preparation method comprises the following steps: 1) mixing kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum, glass fiber and water, and then calcining to obtain a calcined product; 2) mixing polyvinylidene fluoride, methylcellulose, a silane coupling agent and the calcined product to prepare a base stock; 3) grinding the base stock to prepare the 3D printing silicon nitride ceramic material. The surface tension of a liquid phase of the 3D printing silicon nitride ceramic material is small, so that cracks on the surface of a ceramic product are less, meanwhile, the raw materials of the preparation method are easy to get, and the process is simple.
Description
Technical field
The present invention relates to 3D printing material, in particular it relates to 3D printing silicon 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 cause that ceramic powders are bonded together.After laser sintered, need
Ceramic is placed in carries out High Temperature Curing in temperature controlling stove.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 silicon nitride ceramic material and preparation method thereof, the 3D printing silicon nitride
The liquid phase surface tension of ceramic material is small and then causes that the crackle on the surface of ceramic is few；The preparation method raw material is easy simultaneously
, operation it is simple.
To achieve these goals, the invention provides a kind of preparation method of 3D printing silicon nitride ceramic material, including：
1) kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum, glass fibre and water are carried out
Mixing, is 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 silicon nitride ceramic material is obtained.
Present invention also offers a kind of 3D printing silicon nitride ceramic material, the 3D printing silicon nitride ceramic material is by above-mentioned
Preparation method be prepared.
In the above-mentioned technical solutions, the present invention causes obtained 3D by the synergy of above-mentioned each raw material and each step
The liquid phase surface tension of printing silicon nitride ceramic material is small and then causes that the crackle on the surface of ceramic 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
Specific embodiment of the invention is described in detail below.It should be appreciated that described herein specific
Implementation method is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The invention provides a kind of preparation method of 3D printing silicon nitride ceramic material, including：
1) kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum, glass fibre and water are carried out
Mixing, is 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 silicon nitride ceramic material is obtained.
In step 1 of the invention) in, the consumption of each material can be selected in scope wide, but in order to further drop
The liquid phase surface tension of low obtained 3D printing silicon nitride ceramic material, and then cause that the crackle on the surface of ceramic is reduced,
Preferably, in step 1) in, relative to the kaolin of 100 weight portions, bentonitic consumption is 57-65 weight portions, silicon nitride
Consumption is 22-31 weight portions, and the consumption of boric acid is 14-18 weight portions, and the consumption of plant ash is 15-20 weight portions, molybdenum trioxide
Consumption be 5-9 weight portions, the consumption of nano aluminum is 11-14 weight portions, and the consumption of glass fibre is 17-24 weight portions, water
Consumption is 140-180 weight portions.
In step 1 of the invention) in, the actual conditions of mixing can be selected in scope wide, but in order to further
The liquid phase surface tension of obtained 3D printing silicon nitride ceramic material is reduced, and then causes that the crackle on the surface of ceramic subtracts
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 step 1 of the invention) in, the actual conditions of calcining can be selected in scope wide, but in order to further
The liquid phase surface tension of obtained 3D printing silicon nitride ceramic material is reduced, and then causes that the crackle on the surface of ceramic subtracts
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 silicon 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：From the 15-35 DEG C of speed with 0.5-0.8 DEG C/min 150-200 DEG C is warming up to first by mixture and protect
Warm 20-40min, is then warming up to 300-380 DEG C and is incubated 30-40min, finally with 0.8-1 with the speed of 1.5-2.5 DEG C/min
DEG C/speed of min is warming up to 470-520 DEG C and is incubated.
In step 1 of the invention) in, the particle diameter of nano aluminum can be selected in scope wide, but in order to further drop
The liquid phase surface tension of low obtained 3D printing silicon nitride ceramic material, and then cause that the crackle on the surface of ceramic is reduced,
Preferably, in step 1) in, the particle diameter of nano aluminum is 30-40nm.
In step 2 of the invention) in, the consumption of each material can be selected in scope wide, but in order to further drop
The liquid phase surface tension of low obtained 3D printing silicon nitride ceramic material, and then cause that 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 step 2 of the invention) in, the actual conditions of mixing can be selected in scope wide, but in order to further
The liquid phase surface tension of obtained 3D printing silicon nitride ceramic material is reduced, and then causes that the crackle on the surface of ceramic subtracts
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 step 2 of the invention) in, the actual conditions of grinding can be selected in scope wide, but in order to further
The liquid phase surface tension of obtained 3D printing silicon nitride ceramic material is reduced, and then causes that the crackle on the surface of ceramic subtracts
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
It is 25-35min.
Present invention also offers a kind of 3D printing silicon nitride ceramic material, the 3D printing silicon nitride ceramic material is by above-mentioned
Preparation method be prepared.
Below will the present invention will be described in detail by embodiment.
Embodiment 1
1) by kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum (particle diameter is 35nm), glass
Fiber and water are according to 100：60：28：16：18：7：13：20：160 weight ratio in 50min is mixed at 25 DEG C, then from 25 DEG C with
The speed of 0.7 DEG C/min is warming up to 180 DEG C and is incubated 30min, is then warming up to 360 DEG C with the speed of 2 DEG C/min and is incubated
35min, is finally warming up to 490 DEG C and is incubated 8h so that calcined product is obtained with the speed of 0.9 DEG C/min；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH550) according to 100：80：28：14
Weight ratio at 25 DEG C mix 30min be obtained base-material；
3) base-material is carried out into ball milling (mass ratio of big ball and bead is 2：1.4, 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 silicon nitride ceramic material A1.
Embodiment 2
1) by kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum (particle diameter is 30nm), glass
Fiber and water are according to 100：57：22：14：15：5：11：17：140 weight ratio in 40min is mixed at 15 DEG C, then from 15 DEG C with
The speed of 0.5 DEG C/min is warming up to 150 DEG C and is incubated 20min, is then warming up to 300 DEG C with the speed of 1.5 DEG C/min and is incubated
30min, is finally warming up to 470 DEG C and is incubated 7h so that calcined product is obtained with the speed of 0.8 DEG C/min；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH560) according to 100：75：25：9
Weight ratio is in mixing 20min at 15 DEG C with prepared base-material；
3) base-material is carried out into ball milling (mass ratio of big ball and bead is 2：1.3, 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 silicon nitride ceramic material A2.
Embodiment 3
1) by kaolin, bentonite, silicon nitride, boric acid, plant ash, molybdenum trioxide, nano aluminum (particle diameter is 40nm), glass
Fiber and water are according to 100：65：31：18：20：9：14：24：180 weight ratio in 60min is mixed at 35 DEG C, then from 35 DEG C with
The speed of 0.8 DEG C/min is warming up to 200 DEG C and is incubated 40min, is then warming up to 380 DEG C with the speed of 2.5 DEG C/min and is incubated
40min, is finally warming up to 520 DEG C and is incubated 10h so that calcined product is obtained with the speed of 1 DEG C/min；
2) by calcined product, Kynoar, methylcellulose, silane coupler (KH570) according to 100：90：33：16
Weight ratio at 35 DEG C mix 40min be obtained base-material；
3) base-material is carried out into ball milling (mass ratio of big ball and bead is 2：1.5, 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 silicon nitride ceramic material A3.
Comparative example 1
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B1 is obtained, except that, step 1) in
Boric acid is not used.
Comparative example 2
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B2 is obtained, except that, step 1) in
Plant ash is not used.
Comparative example 3
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B3 is obtained, except that, step 1) in
Molybdenum trioxide is not used.
Comparative example 4
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B4 is obtained, except that, step 1) in
Nano aluminum is not used.
Comparative example 5
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B5 is obtained, except that, step 1) in
Glass fibre is not used.
Comparative example 6
Method according to embodiment 1 is carried out so that 3D printing silicon nitride ceramic material B6 is obtained, except that, step 2) in
Silane coupler is not used.
Detection example 1
Above-mentioned 3D printing silicon nitride ceramic material is carried out into 3D printing so that printing product is obtained, then detection prints product
The crackle on surface, counts every square of crackle number (bar/dm of cubic meter2) and average crack length (μm/bar).
Table 1
| Crackle number (bar/dm2) | Average crack length (μm/bar) | |
| A1 | 1 | 0.2 |
| A2 | 2 | 0.1 |
| A3 | 1 | 0.3 |
| B1 | 8 | 0.4 |
| B2 | 10 | 0.5 |
| B3 | 9 | 0.5 |
| B4 | 8 | 0.4 |
| B5 | 11 | 0.6 |
| B6 | 7 | 0.5 |
By above-described embodiment, comparative example and detection example, the obtained 3D printing silicon 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 implementation method
Detail, in range of the technology design of the invention, 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 implementation methods of the invention, as long as it is without prejudice to originally
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 silicon nitride ceramic material, it is characterised in that including：
1) kaolin, bentonite, silicon nitride, boric acid, plant ash, 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 the calcined product；
3) base-material is ground that the 3D printing silicon 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 bentonitic consumption is 57-65 weight portions, and the consumption of the silicon nitride is 22-31 weight portions, the consumption of the boric acid
It is 14-18 weight portions, the consumption of the plant ash is 15-20 weight portions, and the consumption of the molybdenum trioxide is 5-9 weight portions, institute
The consumption of nano aluminum is stated for 11-14 weight portions, 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：Mixture is warming up to 150-200 DEG C from the 15-35 DEG C of speed with 0.5-0.8 DEG C/min first
And be incubated 20-40min, be then warming up to 300-380 DEG C with the speed of 1.5-2.5 DEG C/min and be incubated 30-40min, finally with
The speed of 0.8-1 DEG C/min is warming up 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 uses 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 silicon nitride ceramic material, it is characterised in that the 3D printing silicon 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330344A (en) * | 2019-06-19 | 2019-10-15 | 华中科技大学 | A method of high porosity silicon nitride ceramics is prepared based on selective laser sintering |
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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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| US20140264752A1 (en) * | 2013-03-14 | 2014-09-18 | International Business Machines Corporation | Dual three-dimensional (3d) resistor and methods of forming |
| CN104149337A (en) * | 2014-07-02 | 2014-11-19 | 中国电子科技集团公司第五十五研究所 | Photocuring material for three-dimensional printing and application method thereof |
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Application publication date: 20170517 |