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CN106699111A - 3d printing titanium oxide ceramic material and preparation method thereof - Google Patents

3d printing titanium oxide ceramic material and preparation method thereof Download PDF

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Publication number
CN106699111A
CN106699111A CN201611060263.7A CN201611060263A CN106699111A CN 106699111 A CN106699111 A CN 106699111A CN 201611060263 A CN201611060263 A CN 201611060263A CN 106699111 A CN106699111 A CN 106699111A
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preparation
titanium oxide
parts
weight
mixing
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黄仲佳
王心生
杨军
姚春
李思文
郑兰斌
吴志华
吕晨
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Anhui Chungu 3D Printing Technology Research Institute of Intelligent Equipment Industry
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Anhui Chungu 3D Printing Technology Research Institute of Intelligent Equipment Industry
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Publication of CN106699111A publication Critical patent/CN106699111A/en
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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

本发明公开了一种3D打印氧化钛陶瓷材料及其制备方法，该制备方法包括：1)将高岭土、硅藻土、氧化钛、硼酸、蔗糖、三氧化钼、纳米铝、玻璃纤维和水进行混合，接着进行煅烧以制得煅烧产物；2)将聚偏氟乙烯、甲基纤维素、硅烷偶联剂与煅烧产物进行混合以制得基料；3)将基料进行研磨以制得3D打印氧化钛陶瓷材料。该3D打印氧化钛陶瓷材料的液相表面张力小进而使得陶瓷制品的表面的裂纹少；同时该制备方法原料易得、工序简单。The invention discloses a 3D printing titanium oxide ceramic material and a preparation method thereof. The preparation method comprises: 1) making kaolin, diatomaceous earth, titanium oxide, boric acid, sucrose, molybdenum trioxide, nano-aluminum, glass fiber and water Mixing, followed by calcination to obtain a calcined product; 2) mixing polyvinylidene fluoride, methyl cellulose, silane coupling agent with the calcined product to obtain a base material; 3) grinding the base material to obtain a 3D Print titanium oxide ceramic material. The liquid-phase surface tension of the 3D printed titanium oxide ceramic material is small so that the cracks on the surface of the ceramic product are reduced; meanwhile, the preparation method has easy-to-obtain raw materials and simple procedures.

Description

3D printing titanium oxide ceramics material and preparation method thereof
Technical field
The present invention relates to 3D printing material, in particular it relates to 3D printing titanium oxide ceramics 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 titanium oxide ceramics material and preparation method thereof, the 3D printing titanium oxide 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 titanium oxide ceramics material, including：
1) kaolin, diatomite, titanium oxide, boric acid, sucrose, 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 titanium oxide ceramics material is obtained.
Present invention also offers a kind of 3D printing titanium oxide ceramics material, the 3D printing titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics material, including：
1) kaolin, diatomite, titanium oxide, boric acid, sucrose, 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 titanium oxide ceramics 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 titanium oxide ceramics 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, diatomaceous consumption is 27-33 weight portions, titanium oxide Consumption is 14-23 weight portions, and the consumption of boric acid is 14-18 weight portions, and the consumption of sucrose is 22-34 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 It is 140-180 weight portions to measure.
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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics material, the 3D printing titanium oxide ceramics 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, diatomite, titanium oxide, boric acid, sucrose, molybdenum trioxide, nano aluminum (particle diameter is 35nm), glass fibers Peacekeeping water is according to 100：30：18：16：28：7：13：19：160 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 titanium oxide ceramics materials A 1.
Embodiment 2
1) by kaolin, diatomite, titanium oxide, boric acid, sucrose, molybdenum trioxide, nano aluminum (particle diameter is 30nm), glass fibers Peacekeeping water is according to 100：27：14：14：22：5：11：17：140 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 titanium oxide ceramics materials A 2.
Embodiment 3
1) by kaolin, diatomite, titanium oxide, boric acid, sucrose, molybdenum trioxide, nano aluminum (particle diameter is 40nm), glass fibers Peacekeeping water is according to 100：33：23：18：34：9：14：24：180 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 titanium oxide ceramics materials A 3.
Comparative example 1
Method according to embodiment 1 is carried out so that 3D printing titanium oxide ceramics 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 titanium oxide ceramics material B2 is obtained, except that, step 1) in Sucrose is not used.
Comparative example 3
Method according to embodiment 1 is carried out so that 3D printing titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics 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 titanium oxide ceramics material B6 is obtained, except that, step 2) in Silane coupler is not used.
Detection example 1
Above-mentioned 3D printing titanium oxide ceramics 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), concrete outcome is shown in Table 1。
Table 1
Crackle number (bar/dm2) Average crack length (μm/bar)
A1 3 0.2
A2 1 0.3
A3 2 0.2
B1 5 0.6
B2 7 0.4
B3 10 0.3
B4 9 0.5
B5 8 0.5
B6 8 0.6
By above-described embodiment, comparative example and detection example, the obtained 3D printing titanium oxide 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)

1.一种3D打印氧化钛陶瓷材料的制备方法，其特征在于，包括：1. A preparation method for 3D printing titanium oxide ceramic material, is characterized in that, comprises: 1)将高岭土、硅藻土、氧化钛、硼酸、蔗糖、三氧化钼、纳米铝、玻璃纤维和水进行混合，接着进行煅烧以制得煅烧产物；1) mixing kaolin, diatomaceous earth, titanium oxide, boric acid, sucrose, molybdenum trioxide, nano-aluminum, glass fiber and water, and then calcining to obtain a calcined product; 2)将聚偏氟乙烯、甲基纤维素、硅烷偶联剂与所述煅烧产物进行混合以制得基料；2) mixing polyvinylidene fluoride, methyl cellulose, and a silane coupling agent with the calcined product to prepare a base material; 3)将所述基料进行研磨以制得所述3D打印氧化钛陶瓷材料。3) Grinding the base material to obtain the 3D printed titanium oxide ceramic material. 2.根据权利要求1所述的制备方法，其中，在步骤1)中，相对于100重量份的所述高岭土，所述硅藻土的用量为27-33重量份，所述氧化钛的用量为14-23重量份，所述硼酸的用量为14-18重量份，所述蔗糖的用量为22-34重量份，所述三氧化钼的用量为5-9重量份，所述纳米铝的用量为11-14重量份，所述玻璃纤维的用量为17-24重量份，所述水的用量为140-180重量份。2. The preparation method according to claim 1, wherein, in step 1), relative to the kaolin of 100 parts by weight, the amount of diatomite is 27-33 parts by weight, and the amount of titanium oxide 14-23 parts by weight, the amount of boric acid is 14-18 parts by weight, the amount of sucrose is 22-34 parts by weight, the amount of molybdenum trioxide is 5-9 parts by weight, the nano-aluminum The dosage is 11-14 parts by weight, the dosage of the glass fiber is 17-24 parts by weight, and the dosage of the water is 140-180 parts by weight. 3.根据权利要求2所述的制备方法，其中，在步骤1)中，所述混合至少满足以下条件：混合温度为15-35℃，混合时间为40-60min。3. The preparation method according to claim 2, wherein, in step 1), the mixing at least meets the following conditions: the mixing temperature is 15-35° C., and the mixing time is 40-60 min. 4.根据权利要求2所述的制备方法，其中，在步骤1)中，所述煅烧至少满足以下条件：煅烧温度为470-520℃，煅烧时间为7-10h。4. The preparation method according to claim 2, wherein, in step 1), the calcination at least satisfies the following conditions: the calcination temperature is 470-520° C., and the calcination time is 7-10 h. 5.根据权利要求4所述的制备方法，其中，在步骤1)的所述煅烧之前，所述制备方法还包括升温工序，具体为：首先将混合物自15-35℃以0.5-0.8℃/min的速率升温至150-200℃并保温20-40min，接着以1.5-2.5℃/min的速率升温至300-380℃并保温30-40min，最后以0.8-1℃/min的速率升温至470-520℃并保温。5. The preparation method according to claim 4, wherein, before the calcination in step 1), the preparation method also includes a heating process, specifically: firstly, the mixture is heated from 15-35°C at 0.5-0.8°C/ Raise the temperature to 150-200°C at a rate of 1 min and keep it warm for 20-40min, then raise the temperature to 300-380°C at a rate of 1.5-2.5°C/min and keep it at a temperature of 30-40min, and finally raise the temperature to 470 at a rate of 0.8-1°C/min -520°C and keep warm. 6.根据权利要求2所述的制备方法，其中，在步骤1)中，所述纳米铝的粒径为30-40nm。6. The preparation method according to claim 2, wherein, in step 1), the particle diameter of the nano-aluminum is 30-40nm. 7.根据权利要求1-6中任意一项所述的制备方法，其中，在步骤2)中，相对于100重量份的所述煅烧产物，所述聚偏氟乙烯的用量为75-90重量份，所述甲基纤维素的用量为25-33重量份，所述硅烷偶联剂的用量为9-16重量份。7. The preparation method according to any one of claims 1-6, wherein, in step 2), relative to 100 parts by weight of the calcined product, the amount of polyvinylidene fluoride is 75-90 parts by weight parts, the amount of the methyl cellulose is 25-33 parts by weight, and the amount of the silane coupling agent is 9-16 parts by weight. 8.根据权利要求7所述的制备方法，其中，在步骤2)中，所述混合至少满足以下条件：混合温度为15-35℃，混合时间为20-40min。8. The preparation method according to claim 7, wherein, in step 2), the mixing at least meets the following conditions: the mixing temperature is 15-35°C, and the mixing time is 20-40min. 9.根据权利要求1-6、8中任意一项述的制备方法，其中，在步骤3)中，所述研磨采用球磨的方式进行，并所述球磨至少满足以下条件：大球与小球的质量比为2：1.3-1.5，磨球与物料的质量比为10：0.8-1.2，转速为600-1200rpm，球磨时间为25-35min。9. The preparation method according to any one of claims 1-6,8, wherein, in step 3), the grinding is carried out by ball milling, and the ball milling at least satisfies the following conditions: large balls and small balls The mass ratio of the ball is 2:1.3-1.5, the mass ratio of the ball to the material is 10:0.8-1.2, the speed is 600-1200rpm, and the ball milling time is 25-35min. 10.一种3D打印氧化钛陶瓷材料，其特征在于，所述3D打印氧化钛陶瓷材料通过权利要求1-9中任意一项所述的制备方法制备而得。10. A 3D printed titanium oxide ceramic material, characterized in that the 3D printed titanium oxide ceramic material is prepared by the preparation method according to any one of claims 1-9.
CN201611060263.7A 2016-11-28 2016-11-28 3d printing titanium oxide ceramic material and preparation method thereof Pending CN106699111A (en)

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