CN107324801A - A kind of ceramic injection forming material and preparation method thereof - Google Patents
A kind of ceramic injection forming material and preparation method thereof Download PDFInfo
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- CN107324801A CN107324801A CN201710475789.XA CN201710475789A CN107324801A CN 107324801 A CN107324801 A CN 107324801A CN 201710475789 A CN201710475789 A CN 201710475789A CN 107324801 A CN107324801 A CN 107324801A
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Abstract
The invention discloses a kind of ceramic injection forming material and preparation method thereof, the mass ratio of binding agent and nano ceramic powder is 2 2.5 in the ceramic injection forming material：7.5 8, nano ceramic powder includes the zirconium oxide of mass percent 82.0% 91.0%, 3.0% 6.0% yittrium oxide, 1.0% 2.0% aluminum oxide, 2.0% 4.0% magnesia；Binding agent includes epoxidized soybean oil 2 3%；Optothermal stabilizer 1 2%, high density polyethylene (HDPE) 3 5%, EVA3 5%, polypropylene wax 5 8%, paraffin 10 12%, polyformaldehyde 65 75%.The ceramic injection forming material is used in CIM techniques, can go out to meet 3C electronics and the complicated structural member of the various outward appearances of wearable class product, and the properties of product with high-quality with processing and fabricating.
Description
Technical field
The present invention relates to a kind of ceramic injection forming material and preparation method thereof.
Background technology
The features such as traditional ceramics material has high temperature resistant, corrosion-resistant, intensity is high, hardness is big and be widely used in industrial life
The every field of production, but the brittle sex chromosome mosaicism that traditional ceramics has turns into the master for hindering ceramic material widely to apply at present
One of factor is wanted, and new function ceramics are can to overcome the brittle sex chromosome mosaicism of traditional ceramics, expand the application of ceramics
One large bodies system, progressively applied to 3C electronics and wearing industrial structure part.And nano ceramics not only possesses traditional ceramics material
Advantage, but also there is high tenacity, low temperature superplasticity, but also there is high tenacity, low temperature superplasticity, then
Plus its luxurious outward appearance and the beautiful feel of matter, mobile phone, wearing surface structure part are applied to, with good application prospect.
The preparation method of current nano ceramics has the side such as laminated entity autofrettage, Fused Deposition Modeling method, laser sintered
Method, the complex structural member such as nano ceramics products application to outer frame of mobile phone, Watchcase, process above is difficult to obtain even density,
The complex structural member product that structure is completed.
Ceramic injection forming (CIM) is a kind of novel manufacturing process technology for being combined powder with plastic forming technology,
It is that ceramic powders and binding agent first are carried out into high-temperature fusion, stirring, are well mixed, again crush compound progress after cooling,
Granulation, finally projects into required shape through injection machine.The nanometer metal ceramic that CIM techniques make, it is possible to resolve make complicated
The problems such as structural member nano ceramics.
The content of the invention
It is a primary object of the present invention to overcome the deficiencies in the prior art, there is provided a kind of ceramic injection forming material and its system
Preparation Method.
To achieve the above object, the present invention uses following technical scheme：
A kind of ceramic injection forming material, including nano ceramic powder and binding agent, the binding agent and nanometer pottery
The mass ratio of porcelain powder is 2-2.5：7.5-8；
The nano ceramic powder includes the component of following mass percent：
Zirconium oxide：82.0%-91.0%
Yittrium oxide：3.0%-6.0%
Aluminum oxide：1.0%-2.0%
Magnesia：2.0%-4.0%；
The binding agent includes the component of following mass percent：
Epoxidized soybean oil：2-3%
Optothermal stabilizer：1-2%
High density polyethylene (HDPE)：3-5%
EVA：3-5%
Polypropylene wax：5-8%
Paraffin：10-12%
Polyformaldehyde：65-75%.
Further：
The particle diameter of the nano ceramic powder is 50nm-80nm.
The tap density of the nano ceramic powder is 1.22-1.24g/cm3。
A kind of preparation method of described ceramic injection forming material, comprises the following steps：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added to kneading machine
Middle mixing is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：By through step S2 handle after material send into extruder, extruding pelletization, be made powder injection into
Type feeding.
Further：
The material temperature that the binding agent is controlled in step S1 is 160 ± 10 DEG C, and kneading machine rotating speed is 5-15r/min, kneading machine
Temperature is 180 DEG C -200 DEG C.
Nano-ceramic powder is heated to temperature for 140 ± 10 DEG C in step S1.
It is 20-30r/min that kneading machine rotating speed is controlled in step S2, and kneading machine temperature is 180 DEG C -200 DEG C, and mixing time is
20-30min。
A kind of method that product is made using described ceramic injection forming material, is comprised the following steps：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added to kneading machine
Middle mixing is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：By through step S2 handle after material send into extruder, extruding pelletization, be made powder injection into
Type feeding；
S4. the product is obtained using the feeding progress injection moulding, degreasing, sintering processes of granulation.
Further：
In step S4, carry out injection moulding at a temperature of 160-180 DEG C using the feeding of granulation and obtain green compact；By green compact
Degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed 3.5g/min are carried out in nitric acid debinding furnace；After degreasing
Tender be put into air sintering furnace and be sintered, maximum temperature is between 1400-1500 DEG C during sintering, sintering time 24h.
The product is 3C Electronic Equipment Structural Members.
Beneficial effects of the present invention：
The specific formula of ceramic injection forming material use that the present invention is provided, wherein binding agent and nano ceramic powder
Mass ratio is 2-2.5：7.5-8, nano ceramic powder includes mass percent 82.0%-91.0% zirconium oxide, 3.0%-
6.0% yittrium oxide, 1.0%-2.0% aluminum oxide, 2.0%-4.0% magnesia；Binding agent includes epoxidized soybean oil 2-
3%；Optothermal stabilizer 1-2%, high density polyethylene (HDPE) 3-5%, EVA3-5%, polypropylene wax 5-8%, paraffin 10-12%, poly- first
Aldehyde 65-75%, is used in CIM techniques by the ceramic injection forming material, can go out to meet 3C electronics and wearable class with processing and fabricating
The complicated structural member of the various outward appearances of product, and the properties of product with high-quality.Compared to traditional CIM ceramic materials, the present invention is carried
The ceramic injection forming material of confession has the advantages that more high tenacity, low temperature superplasticity, is particularly advantageous in realizing 3C electronics and wearing
The processing of product complex precise structural member.Experiments verify that, properties of product are with the obvious advantage, performance indications：
Melt index：800~1200g/10min；
The constriction coefficient of feeding is in 1.30~1.40 scopes, representative value 1.35；
Density after sintering：5.8-6.2g/cm3；
Hardness：1200-1400HV；
Fracture toughness ＞ 14Mpa/m1/2。
In addition, compared to dry process, the bulk life of injection moulding is carried out using the ceramic injection forming material as feeding
Production, process costs are lower, and production efficiency is high, good product performance.
Embodiment
Embodiments of the present invention are elaborated below.It is emphasized that what the description below was merely exemplary,
The scope being not intended to be limiting of the invention and its application.
In one embodiment, a kind of ceramic injection forming material, including nano ceramic powder and binding agent, the bonding
The mass ratio of agent and the nano ceramic powder is 2-2.5：7.5-8；
The nano ceramic powder includes the component of following mass percent：
Zirconium oxide：82.0%-91.0%
Yittrium oxide：3.0%-6.0%
Aluminum oxide：1.0%-2.0%
Magnesia：2.0%-4.0%；
The binding agent includes the component of following mass percent：
Epoxidized soybean oil：2-3%
Optothermal stabilizer：1-2%
High density polyethylene (HDPE)：3-5%
EVA：3-5%
Polypropylene wax：5-8%
Paraffin：10-12%
Polyformaldehyde：65-75%.
In a preferred embodiment, the particle diameter of the nano ceramic powder is 50nm-80nm.
In a preferred embodiment, the tap density of the nano ceramic powder is 1.22-1.24g/cm3。
In another embodiment, a kind of preparation method of described ceramic injection forming material comprises the following steps：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added to kneading machine
Middle mixing is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：By through step S2 handle after material send into extruder, extruding pelletization, be made powder injection into
Type feeding.
In a preferred embodiment, the material temperature that the binding agent is controlled in step S1 is 160 ± 10 DEG C, and kneading machine rotating speed is 5-
15r/min, kneading machine temperature is 180 DEG C -200 DEG C.
In a preferred embodiment, nano-ceramic powder is heated to temperature for 140 ± 10 DEG C in step S1.
In a preferred embodiment, controlled in step S2 kneading machine rotating speed be 20-30r/min, kneading machine temperature be 180 DEG C-
200 DEG C, mixing time is 20-30min.
In another embodiment, a kind of method that product is made using described ceramic injection forming material, including with
Lower step：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added to kneading machine
Middle mixing is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：By through step S2 handle after material send into extruder, extruding pelletization, be made powder injection into
Type feeding；
S4. the product is obtained using the feeding progress injection moulding, degreasing, sintering processes of granulation.
In a preferred embodiment, in step S4, injection moulding is carried out at a temperature of 160-180 DEG C using the feeding of granulation
Obtain green compact；Green compact are subjected to degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed in nitric acid debinding furnace
3.5g/min；Tender after degreasing is put into air sintering furnace and is sintered, during sintering maximum temperature 1400-1500 DEG C it
Between, sintering time 24h.
In an exemplary embodiment, the product is 3C Electronic Equipment Structural Members.
In a particular embodiment, a kind of preparation method of ceramic injection forming material, comprises the following steps：
1st, binding agent mixing, ceramics preheating：
The binding agent matched is added in kneading machine and kneaded to being melted into pureed, 160 ± 10 DEG C of material temperature.Kneading machine turns
Speed：5-15r/min, sets kneading machine temperature：180℃-200℃；
Nano-ceramic powder is heated to 140 ± 10 DEG C of temperature on the heating.
2nd, batch mixing：Nano-ceramic powder after preheating is added in the binding agent that the predetermined state has been reached in kneading machine and mixed
Close, nano ceramic powder is uniformly mixed with binding agent and form milky walk shape, kneading machine rotating speed：20-30r/min, if
Determine kneading machine temperature：180 DEG C -200 DEG C, time 20-30min.
3rd, extrusion granulator：Material feeding extruder after being handled through step 2, plasticizing, extrusion, and granulated, it is made
Feedstock of Powder Injection Molding.
Example one：
Feeding is formulated：
Using nano ceramics feeding through injection moulding-degreasing-sintering processes, product is made.
The feeding of granulation carries out injection moulding at a temperature of 160-180 DEG C and obtains green compact；By green compact in nitric acid debinding furnace
Middle carry out degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed 3.5g/min；Tender after degreasing is put into greatly
It is sintered in gas sintering furnace, maximum temperature is between 1400-1500 DEG C during sintering, sintering time 24h.
Example two：
Feeding is formulated：
Using nano ceramics feeding through injection moulding-degreasing-sintering processes, product is made.
The feeding of granulation carries out injection moulding at a temperature of 160-180 DEG C and obtains green compact；By green compact in nitric acid debinding furnace
Middle carry out degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed 3.5g/min；Tender after degreasing is put into greatly
It is sintered in gas sintering furnace, maximum temperature is between 1400-1500 DEG C during sintering, sintering time 24h.
Example three：
Feeding is formulated：
Using nano ceramics feeding through injection moulding-degreasing-sintering processes, product is made.
The feeding of granulation carries out injection moulding at a temperature of 160-180 DEG C and obtains green compact；By green compact in nitric acid debinding furnace
Middle carry out degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed 3.5g/min；Tender after degreasing is put into greatly
It is sintered in gas sintering furnace, maximum temperature is between 1400-1500 DEG C during sintering, sintering time 24h.
Example four：
Feeding is formulated：
Using nano ceramics feeding through injection moulding-degreasing-sintering processes, product is made.
The feeding of granulation carries out injection moulding at a temperature of 160-180 DEG C and obtains green compact；By green compact in nitric acid debinding furnace
Middle carry out degreasing, 130 DEG C of skimming temp, acid filling time 600min, acid filling speed 3.5g/min；Tender after degreasing is put into greatly
It is sintered in gas sintering furnace, maximum temperature is between 1400-1500 DEG C during sintering, sintering time 24h.
Comparative example：
Raw material uses conventional ceramic feeding
Above case study on implementation and contrast case are handled according to following manufacturing process and performance test and (contrast case to feed
Material is without feeding making step)：
1st, the binding agent matched is added in kneading machine and kneaded to being melted into pureed, 160 DEG C of material temperature.Kneading machine turns
Speed：7r/min, sets kneading machine temperature：190℃；
The 2nd, nano-ceramic powder is heated to 140 DEG C of temperature on the heating.
3rd, the nano-ceramic powder after preheating is added in the binding agent that the predetermined state has been reached in kneading machine and mixed, made
Nano ceramic powder uniformly mixes with binding agent and forms milky walk shape, kneading machine rotating speed：30r/min, sets kneading machine
190 DEG C of temperature, time 30min.
4th, the material feeding extruder after being handled through step 2, plasticizing, extrusion, and granulated.
Injection molding process uses identical processing mode：
Raw material is subjected to injection moulding at a temperature of 160-180 DEG C and obtains green compact.
Raw embryo is subjected to degreasing in nitric acid debinding furnace.130 DEG C of skimming temp, acid filling time 600min, acid filling speed
3.5g/min。
Tender after degreasing is put into air sintering furnace and is sintered, during sintering maximum temperature 1400-1500 DEG C it
Between, sintering time 24h.
The test of particular product performance parameters is carried out by the way that feeding is fabricated into standard component.
The processing mode that each example is used is identical, and the melt index of test each group nano ceramics, constriction coefficient, sintering are close respectively
Degree, fracture toughness, hardness.By fracture toughness test national standard GBT 23806-2009《Fine ceramics fracture toughness test proved recipe method》
To be tested, required tender size is：40mm*4mm*3mm.
Test result is as shown in table 1 below：
Table 1
From table result, nano ceramics material flow of the invention is good, the more conventional pottery especially in fracture toughness performance
Porcelain has great advantage.
Above content is to combine specific/preferred embodiment made for the present invention be further described, it is impossible to recognized
The specific implementation of the fixed present invention is confined to these explanations.For general technical staff of the technical field of the invention,
Without departing from the inventive concept of the premise, it can also make some replacements or modification to the embodiment that these have been described,
And these are substituted or variant should all be considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of ceramic injection forming material, it is characterised in that including nano ceramic powder and binding agent, the binding agent and institute
The mass ratio for stating nano ceramic powder is 2-2.5：7.5-8；
The nano ceramic powder includes the component of following mass percent：
Zirconium oxide：82.0%-91.0%
Yittrium oxide：3.0%-6.0%
Aluminum oxide：1.0%-2.0%
Magnesia：2.0%-4.0%；
The binding agent includes the component of following mass percent：
Epoxidized soybean oil：2-3%
Optothermal stabilizer：1-2%
High density polyethylene (HDPE)：3-5%
EVA：3-5%
Polypropylene wax：5-8%
Paraffin：10-12%
Polyformaldehyde：65-75%.
2. ceramic injection forming material as claimed in claim 1, it is characterised in that the particle diameter of the nano ceramic powder is
50nm-80nm。
3. ceramic injection forming material as claimed in claim 1 or 2, it is characterised in that the jolt ramming of the nano ceramic powder
Density is 1.22-1.24g/cm3。
4. a kind of preparation method of ceramic injection forming material as described in any one of claims 1 to 3, it is characterised in that bag
Include following steps：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added in kneading machine and mixed
Refining is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：Material after being handled through step S2 is sent into extruder, extruding pelletization is made powder injection-molded and fed
Material.
5. preparation method as claimed in claim 4, it is characterised in that the material temperature that the binding agent is controlled in step S1 is 160
± 10 DEG C, kneading machine rotating speed is 5-15r/min, and kneading machine temperature is 180 DEG C -200 DEG C.
6. the preparation method as described in claim 4 or 5, it is characterised in that nano-ceramic powder is heated to temperature in step S1
For 140 ± 10 DEG C.
7. the preparation method as described in any one of claim 4 to 6, it is characterised in that control the kneading machine rotating speed to be in step S2
20-30r/min, kneading machine temperature is 180 DEG C -200 DEG C, and mixing time is 20-30min.
8. a kind of ceramic injection forming material using as described in any one of claims 1 to 3 makes the method for product, its feature
It is, comprises the following steps：
S1, the nano ceramic powder is heated to predetermined temperature；The binding agent matched is added in kneading machine and mixed
Refining is to being melted into pureed；
S2, batch mixing：Nano-ceramic powder after preheating is added and mixed in kneading machine with the binding agent, is kneaded；
S3, extrusion granulator：Material after being handled through step S2 is sent into extruder, extruding pelletization is made powder injection-molded and fed
Material；
S4. the product is obtained using the feeding progress injection moulding, degreasing, sintering processes of granulation.
9. method as claimed in claim 8, it is characterised in that in step S4, the temperature using the feeding of granulation at 160-180 DEG C
The lower progress injection moulding of degree obtains green compact；Green compact are subjected to degreasing, 130 DEG C of skimming temp, acid filling time in nitric acid debinding furnace
600min, acid filling speed 3.5g/min；Tender after degreasing is put into air sintering furnace and is sintered, maximum temperature during sintering
Between 1400-1500 DEG C, sintering time 24h.
10. method as claimed in claim 8 or 9, it is characterised in that the product is 3C Electronic Equipment Structural Members.
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